Sample records for etched surface morphology

  1. Modeling the characteristic etch morphologies along specific crystallographic orientations by anisotropic chemical etching

    NASA Astrophysics Data System (ADS)

    Li, Kun-Dar; Miao, Jin-Ru

    2018-02-01

    To improve the advanced manufacturing technology for functional materials, a sophisticated control of chemical etching process is highly demanded, especially in the fields of environment and energy related applications. In this study, a phase-field-based model is utilized to investigate the etch morphologies influenced by the crystallographic characters during anisotropic chemical etching. Three types of etching modes are inspected theoretically, including the isotropic, <100> and <111> preferred oriented etchings. Owing to the specific etching behavior along the crystallographic directions, different characteristic surface structures are presented in the simulations, such as the pimple-like, pyramidal hillock and ridge-like morphologies. In addition, the processing parameters affecting the surface morphological formation and evolution are also examined systematically. According to the numerical results, the growth mechanism of surface morphology in a chemical etching is revealed distinctly. While the etching dynamics plays a dominant role on the surface formation, the characteristic surface morphologies corresponding to the preferred etching direction become more apparent. As the atomic diffusion turned into a determinative factor, a smoothened surface would appear, even under the anisotropic etching conditions. These simulation results provide fundamental information to enhance the development and application of anisotropic chemical etching techniques.

  2. Bi-stage time evolution of nano-morphology on inductively coupled plasma etched fused silica surface caused by surface morphological transformation

    NASA Astrophysics Data System (ADS)

    Jiang, Xiaolong; Zhang, Lijuan; Bai, Yang; Liu, Ying; Liu, Zhengkun; Qiu, Keqiang; Liao, Wei; Zhang, Chuanchao; Yang, Ke; Chen, Jing; Jiang, Yilan; Yuan, Xiaodong

    2017-07-01

    In this work, we experimentally investigate the surface nano-roughness during the inductively coupled plasma etching of fused silica, and discover a novel bi-stage time evolution of surface nano-morphology. At the beginning, the rms roughness, correlation length and nano-mound dimensions increase linearly and rapidly with etching time. At the second stage, the roughening process slows down dramatically. The switch of evolution stage synchronizes with the morphological change from dual-scale roughness comprising long wavelength underlying surface and superimposed nano-mounds to one scale of nano-mounds. A theoretical model based on surface morphological change is proposed. The key idea is that at the beginning, etched surface is dual-scale, and both larger deposition rate of etch inhibitors and better plasma etching resistance at the surface peaks than surface valleys contribute to the roughness development. After surface morphology transforming into one-scale, the difference of plasma resistance between surface peaks and valleys vanishes, thus the roughening process slows down.

  3. Investigation of Nitride Morphology After Self-Aligned Contact Etch

    NASA Technical Reports Server (NTRS)

    Hwang, Helen H.; Keil, J.; Helmer, B. A.; Chien, T.; Gopaladasu, P.; Kim, J.; Shon, J.; Biegel, Bryan (Technical Monitor)

    2001-01-01

    Self-Aligned Contact (SAC) etch has emerged as a key enabling technology for the fabrication of very large-scale memory devices. However, this is also a very challenging technology to implement from an etch viewpoint. The issues that arise range from poor oxide etch selectivity to nitride to problems with post etch nitride surface morphology. Unfortunately, the mechanisms that drive nitride loss and surface behavior remain poorly understood. Using a simple langmuir site balance model, SAC nitride etch simulations have been performed and compared to actual etched results. This approach permits the study of various etch mechanisms that may play a role in determining nitride loss and surface morphology. Particle trajectories and fluxes are computed using Monte-Carlo techniques and initial data obtained from double Langmuir probe measurements. Etched surface advancement is implemented using a shock tracking algorithm. Sticking coefficients and etch yields are adjusted to obtain the best agreement between actual etched results and simulated profiles.

  4. Formation and metrology of dual scale nano-morphology on SF(6) plasma etched silicon surfaces.

    PubMed

    Boulousis, G; Constantoudis, V; Kokkoris, G; Gogolides, E

    2008-06-25

    Surface roughness and nano-morphology in SF(6) plasma etched silicon substrates are investigated in a helicon type plasma reactor as a function of etching time and process parameters. The plasma etched surfaces are analyzed by atomic force microscopy. It is found that dual scale nano-roughness is formatted on the silicon surface comprising an underlying nano-roughness and superimposed nano-mounds. Detailed metrological quantification is proposed for the characterization of dual scale surface morphology. As etching proceeds, the mounds become higher, fewer and wider, and the underlying nano-roughness also increases. Increase in wafer temperature leads to smoother surfaces with lower, fewer and wider nano-mounds. A mechanism based on the deposition of etch inhibiting particles during the etching process is proposed for the explanation of the experimental behavior. In addition, appropriately designed experiments are conducted, and they confirm the presence of this mechanism.

  5. Dry etching of copper phthalocyanine thin films: effects on morphology and surface stoichiometry.

    PubMed

    Van Dijken, Jaron G; Brett, Michael J

    2012-08-24

    We investigate the evolution of copper phthalocyanine thin films as they are etched with argon plasma. Significant morphological changes occur as a result of the ion bombardment; a planar surface quickly becomes an array of nanopillars which are less than 20 nm in diameter. The changes in morphology are independent of plasma power, which controls the etch rate only. Analysis by X-ray photoelectron spectroscopy shows that surface concentrations of copper and oxygen increase with etch time, while carbon and nitrogen are depleted. Despite these changes in surface stoichiometry, we observe no effect on the work function. The absorbance and X-ray diffraction spectra show no changes other than the peaks diminishing with etch time. These findings have important implications for organic photovoltaic devices which seek nanopillar thin films of metal phthalocyanine materials as an optimal structure.

  6. Formation of nanostructured silicon surfaces by stain etching

    PubMed Central

    2014-01-01

    In this work, we report the fabrication of ordered silicon structures by chemical etching of silicon in vanadium oxide (V2O5)/hydrofluoric acid (HF) solution. The effects of the different etching parameters including the solution concentration, temperature, and the presence of metal catalyst film deposition (Pd) on the morphologies and reflective properties of the etched Si surfaces were studied. Scanning electron microscopy (SEM) was carried out to explore the morphologies of the etched surfaces with and without the presence of catalyst. In this case, the attack on the surfaces with a palladium deposit begins by creating uniform circular pores on silicon in which we distinguish the formation of pyramidal structures of silicon. Fourier transform infrared spectroscopy (FTIR) demonstrates that the surfaces are H-terminated. A UV-Vis-NIR spectrophotometer was used to study the reflectance of the structures obtained. A reflectance of 2.21% from the etched Si surfaces in the wavelength range of 400 to 1,000 nm was obtained after 120 min of etching while it is of 4.33% from the Pd/Si surfaces etched for 15 min. PMID:25435830

  7. Modification of the Surface Topography and Composition of Ultrafine and Coarse Grained Titanium by Chemical Etching.

    PubMed

    Nazarov, Denis V; Zemtsova, Elena G; Solokhin, Alexandr Yu; Valiev, Ruslan Z; Smirnov, Vladimir M

    2017-01-13

    In this study, we present the detailed investigation of the influence of the etching medium (acidic or basic Piranha solutions) and the etching time on the morphology and surface relief of ultrafine grained (UFG) and coarse grained (CG) titanium. The surface relief and morphology have been studied by means of scanning electron microscopy (SEM), atomic force microscopy (AFM), and the spectral ellipsometry. The composition of the samples has been determined by X-ray fluorescence analysis (XRF) and X-ray Photoelectron Spectroscopy (XPS). Significant difference in the etching behavior of UFG and CG titanium has been found. UFG titanium exhibits higher etching activity independently of the etching medium. Formed structures possess higher homogeneity. The variation of the etching medium and time leads to micro-, nano-, or hierarchical micro/nanostructures on the surface. Significant difference has been found between surface composition for UFG titanium etched in basic and acidic Piranha solution. Based on the experimental data, the possible reasons and mechanisms are considered for the formation of nano- and microstructures. The prospects of etched UFG titanium as the material for implants are discussed.

  8. Modification of the Surface Topography and Composition of Ultrafine and Coarse Grained Titanium by Chemical Etching

    PubMed Central

    Nazarov, Denis V.; Zemtsova, Elena G.; Solokhin, Alexandr Yu.; Valiev, Ruslan Z.; Smirnov, Vladimir M.

    2017-01-01

    In this study, we present the detailed investigation of the influence of the etching medium (acidic or basic Piranha solutions) and the etching time on the morphology and surface relief of ultrafine grained (UFG) and coarse grained (CG) titanium. The surface relief and morphology have been studied by means of scanning electron microscopy (SEM), atomic force microscopy (AFM), and the spectral ellipsometry. The composition of the samples has been determined by X-ray fluorescence analysis (XRF) and X-ray Photoelectron Spectroscopy (XPS). Significant difference in the etching behavior of UFG and CG titanium has been found. UFG titanium exhibits higher etching activity independently of the etching medium. Formed structures possess higher homogeneity. The variation of the etching medium and time leads to micro-, nano-, or hierarchical micro/nanostructures on the surface. Significant difference has been found between surface composition for UFG titanium etched in basic and acidic Piranha solution. Based on the experimental data, the possible reasons and mechanisms are considered for the formation of nano- and microstructures. The prospects of etched UFG titanium as the material for implants are discussed. PMID:28336849

  9. Lithography-free glass surface modification by self-masking during dry etching

    NASA Astrophysics Data System (ADS)

    Hein, Eric; Fox, Dennis; Fouckhardt, Henning

    2011-01-01

    Glass surface morphologies with defined shapes and roughness are realized by a two-step lithography-free process: deposition of an ~10-nm-thin lithographically unstructured metallic layer onto the surface and reactive ion etching in an Ar/CF4 high-density plasma. Because of nucleation or coalescence, the metallic layer is laterally structured during its deposition. Its morphology exhibits islands with dimensions of several tens of nanometers. These metal spots cause a locally varying etch velocity of the glass substrate, which results in surface structuring. The glass surface gets increasingly rougher with further etching. The mechanism of self-masking results in the formation of surface structures with typical heights and lateral dimensions of several hundred nanometers. Several metals, such as Ag, Al, Au, Cu, In, and Ni, can be employed as the sacrificial layer in this technology. Choice of the process parameters allows for a multitude of different glass roughness morphologies with individual defined and dosed optical scattering.

  10. Collective evolution of submicron hillocks during the early stages of anisotropic alkaline wet chemical etching of Si(1 0 0) surfaces

    NASA Astrophysics Data System (ADS)

    Sana, P.; Vázquez, Luis; Cuerno, Rodolfo; Sarkar, Subhendu

    2017-11-01

    We address experimentally the large-scale dynamics of Si(1 0 0) surfaces during the initial stages of anisotropic wet (KOH) chemical etching, which are characterized through atomic force microscopy. These systems are known to lead to the formation of characteristic pyramids, or hillocks, of typical sizes in the nanometric/micrometer scales, thus with the potential for a large number of applications that can benefit from the nanotexturing of Si surfaces. The present pattern formation process is very strongly disordered in space. We assess the space correlations in such a type of rough surface and elucidate the existence of a complex and rich morphological evolution, featuring at least three different regimes in just 10 min of etching. Such a complex time behavior cannot be consistently explained within a single formalism for dynamic scaling. The pyramidal structure reveals itself as the basic morphological motif of the surface throughout the dynamics. A detailed analysis of the surface slope distribution with etching time reveals that the texturing process induced by the KOH etching is rather gradual and progressive, which accounts for the dynamic complexity. The various stages of the morphological evolution can be accurately reproduced by computer-generated surfaces composed by uncorrelated pyramidal structures. To reach such an agreement, the key parameters are the average pyramid size, which increases with etching time, its distribution and the surface coverage by the pyramidal structures.

  11. Inductively coupled BCl 3/Cl 2 /Ar plasma etching of Al-rich AlGaN

    DOE PAGES

    Douglas, Erica A.; Sanchez, Carlos A.; Kaplar, Robert J.; ...

    2016-12-01

    Varying atomic ratios in compound semiconductors is well known to have large effects on the etching properties of the material. The use of thin device barrier layers, down to 25 nm, adds to the fabrication complexity by requiring precise control over etch rates and surface morphology. The effects of bias power and gas ratio of BCl 3 to Cl 2 for inductively coupled plasma etching of high Al content AlGaN were contrasted with AlN in this study for etch rate, selectivity, and surface morphology. Etch rates were greatly affected by both bias power and gas chemistry. Here we detail themore » effects of small variations in Al composition for AlGaN and show substantial changes in etch rate with regards to bias power as compared to AlN.« less

  12. Comparative analysis of barium titanate thin films dry etching using inductively coupled plasmas by different fluorine-based mixture gas

    PubMed Central

    2014-01-01

    In this work, the inductively coupled plasma etching technique was applied to etch the barium titanate thin film. A comparative study of etch characteristics of the barium titanate thin film has been investigated in fluorine-based (CF4/O2, C4F8/O2 and SF6/O2) plasmas. The etch rates were measured using focused ion beam in order to ensure the accuracy of measurement. The surface morphology of etched barium titanate thin film was characterized by atomic force microscope. The chemical state of the etched surfaces was investigated by X-ray photoelectron spectroscopy. According to the experimental result, we monitored that a higher barium titanate thin film etch rate was achieved with SF6/O2 due to minimum amount of necessary ion energy and its higher volatility of etching byproducts as compared with CF4/O2 and C4F8/O2. Low-volatile C-F compound etching byproducts from C4F8/O2 were observed on the etched surface and resulted in the reduction of etch rate. As a result, the barium titanate films can be effectively etched by the plasma with the composition of SF6/O2, which has an etch rate of over than 46.7 nm/min at RF power/inductively coupled plasma (ICP) power of 150/1,000 W under gas pressure of 7.5 mTorr with a better surface morphology. PMID:25278821

  13. Understanding and controlling the step bunching instability in aqueous silicon etching

    NASA Astrophysics Data System (ADS)

    Bao, Hailing

    Chemical etching of silicon has been widely used for more than half a century in the semiconductor industry. It not only forms the basis for current wafer cleaning processes, it also serves as a powerful tool to create a variety of surface morphologies for different applications. Its potential for controlling surface morphology at the atomic scale over micron-size regions is especially appealing. In spite of its wide usage, the chemistry of silicon etching is poorly understood. Many seemingly simple but fundamental questions have not been answered. As a result, the development of new etchants and new etching protocols are based on expensive and tedious trial-and-error experiments. A better understanding of the etching mechanism would direct the rational formulation of new etchants that produce controlled etch morphologies. Particularly, micron-scale step bunches spontaneously develop on the vicinal Si(111) surface etched in KOH or other anisotropic aqueous etchants. The ability to control the size, orientation, density and regularity of these surface features would greatly improve the performance of microelectromechanical devices. This study is directed towards understanding the chemistry and step bunching instability in aqueous anisotropic etching of silicon through a combination of experimental techniques and theoretical simulations. To reveal the cause of step-bunching instability, kinetic Monte Carlo simulations were constructed based on an atomistic model of the silicon lattice and a modified kinematic wave theory. The simulations showed that inhomogeneity was the origin of step-bunching, which was confirmed through STM studies of etch morphologies created under controlled flow conditions. To quantify the size of the inhomogeneities in different etchants and to clarify their effects, a five-parallel-trench pattern was fabricated. This pattern used a nitride mask to protect most regions of the wafer; five evenly spaced etch windows were opened to the Si(110) substrate. Combining data from these etched patterns and surface IR spectra, a modified mechanism, which explained most experimental observations, was proposed. Control of the step-bunching instability was accomplished with a second micromachined etch barrier pattern which consisted of a circular array of seventy-two long, narrow trenches in an etch mask. Using this pattern, well aligned, regularly shaped, evenly-distributed, near-atomically flat terraces in micron size were produced controllably.

  14. Modified TMAH based etchant for improved etching characteristics on Si{1 0 0} wafer

    NASA Astrophysics Data System (ADS)

    Swarnalatha, V.; Narasimha Rao, A. V.; Ashok, A.; Singh, S. S.; Pal, P.

    2017-08-01

    Wet bulk micromachining is a popular technique for the fabrication of microstructures in research labs as well as in industry. However, increasing the throughput still remains an active area of research, and can be done by increasing the etching rate. Moreover, the release time of a freestanding structure can be reduced if the undercutting rate at convex corners can be improved. In this paper, we investigate a non-conventional etchant in the form of NH2OH added in 5 wt% tetramethylammonium hydroxide (TMAH) to determine its etching characteristics. Our analysis is focused on a Si{1 0 0} wafer as this is the most widely used in the fabrication of planer devices (e.g. complementary metal oxide semiconductors) and microelectromechanical systems (e.g. inertial sensors). We perform a systematic and parametric analysis with concentrations of NH2OH varying from 5% to 20% in step of 5%, all in 5 wt% TMAH, to obtain the optimum concentration for achieving improved etching characteristics including higher etch rate, undercutting at convex corners, and smooth etched surface morphology. Average surface roughness (R a), etch depth, and undercutting length are measured using a 3D scanning laser microscope. Surface morphology of the etched Si{1 0 0} surface is examined using a scanning electron microscope. Our investigation has revealed a two-fold increment in the etch rate of a {1 0 0} surface with the addition of NH2OH in the TMAH solution. Additionally, the incorporation of NH2OH significantly improves the etched surface morphology and the undercutting at convex corners, which is highly desirable for the quick release of microstructures from the substrate. The results presented in this paper are extremely useful for engineering applications and will open a new direction of research for scientists in both academic and industrial laboratories.

  15. Tridimensional morphology and kinetics of etch pit on the {l_brace}0 0 0 1{r_brace} plane of sapphire crystal

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Zhang Lunyong; Sun Jianfei, E-mail: jfsun_hit@263.net; Zuo Hongbo

    2012-08-15

    The tridimensional morphology and etching kinetics of the etch pit on the C-{l_brace}0 0 0 1{r_brace} plane of sapphire crystal ({alpha}-Al{sub 2}O{sub 3}) in molten KOH were studied experimentally. It was shown that the etch pit takes on tridimensional morphologies with triangular symmetry same as the symmetric property of the sapphire crystal. Pits like centric and eccentric triangular pyramid as well as hexagonal pyramid were observed, but the latter is less in density. In-depth analyses show the side walls of the etch pits belong to the {l_brace}1 1{sup Macron} 0 2{sup Macron }{r_brace} family, and the triangular pit contains edgesmore » full composed by Al{sup 3+} ions on the etching surface so it is more stable than the hexagonal pit since its edges on the etching surface contains Al{sup 2+} ions. The etch pits developed in a manner of kinematic wave by the step moving with constant speed, which is controlled by the chemical reaction with activation energy of 96.6 kJ/mol between Al{sub 2}O{sub 3} and KOH. - Graphical abstract: Schematic showing the atomic configuration of the predicted side walls of regular triangular pyramid shaped etch pit on the C-{l_brace}0 0 0 1{r_brace} plane of sapphire crystal. Highlights: Black-Right-Pointing-Pointer Observed the tridimensional morphology of etch pits. Black-Right-Pointing-Pointer Figured out the atomic configuration origin of the etch pits. Black-Right-Pointing-Pointer Quantitatively determined the etch rates of the etch pits.« less

  16. High-quality fiber fabrication in buffered hydrofluoric acid solution with ultrasonic agitation.

    PubMed

    Zhong, Nianbing; Liao, Qiang; Zhu, Xun; Wang, Yongzhong; Chen, Rong

    2013-03-01

    An etching method for preparing high-quality fiber-optic sensors using a buffered etchant with ultrasonic agitation is proposed. The effects of etching conditions on the etch rate and surface morphology of the etched fibers are investigated. The effect of surface roughness is discussed on the fibers' optical properties. Linear etching behavior and a smooth fiber surface can be repeatedly obtained by adjusting the ultrasonic power and etchant pH. The fibers' spectral quality is improved as the ratio of the pit depth to size decreases, and the fibers with smooth surfaces are more sensitive to a bacterial suspension than those with rough surfaces.

  17. Ultradeep electron cyclotron resonance plasma etching of GaN

    DOE PAGES

    Harrison, Sara E.; Voss, Lars F.; Torres, Andrea M.; ...

    2017-07-25

    Here, ultradeep (≥5 μm) electron cyclotron resonance plasma etching of GaN micropillars was investigated. Parametric studies on the influence of the applied radio-frequency power, chlorine content in a Cl 2/Ar etch plasma, and operating pressure on the etch depth, GaN-to-SiO 2 selectivity, and surface morphology were performed. Etch depths of >10 μm were achieved over a wide range of parameters. Etch rates and sidewall roughness were found to be most sensitive to variations in RF power and % Cl 2 in the etch plasma. Selectivities of >20:1 GaN:SiO 2 were achieved under several chemically driven etch conditions where a maximummore » selectivity of ~39:1 was obtained using a 100% Cl 2 plasma. The etch profile and (0001) surface morphology were significantly influenced by operating pressure and the chlorine content in the plasma. Optimized etch conditions yielded >10 μm tall micropillars with nanometer-scale sidewall roughness, high GaN:SiO 2 selectivity, and nearly vertical etch profiles. These results provide a promising route for the fabrication of ultradeep GaN microstructures for use in electronic and optoelectronic device applications. In addition, dry etch induced preferential crystallographic etching in GaN microstructures is also demonstrated, which may be of great interest for applications requiring access to non- or semipolar GaN surfaces.« less

  18. Uniformity studies of inductively coupled plasma etching in fabrication of HgCdTe detector arrays

    NASA Astrophysics Data System (ADS)

    Bommena, R.; Velicu, S.; Boieriu, P.; Lee, T. S.; Grein, C. H.; Tedjojuwono, K. K.

    2007-04-01

    Inductively coupled plasma (ICP) chemistry based on a mixture of CH 4, Ar, and H II was investigated for the purpose of delineating HgCdTe mesa structures and vias typically used in the fabrication of second and third generation infrared photo detector arrays. We report on ICP etching uniformity results and correlate them with plasma controlling parameters (gas flow rates, total chamber pressure, ICP power and RF power). The etching rate and surface morphology of In-doped MWIR and LWIR HgCdTe showed distinct dependences on the plasma chemistry, total pressure and RF power. Contact stylus profilometry and cross-section scanning electron microscopy (SEM) were used to characterize the anisotropy of the etched profiles obtained after various processes and a standard deviation of 0.06 μm was obtained for etch depth on 128 x 128 format array vias. The surface morphology and the uniformity of the etched surfaces were studied by plan view SEM. Atomic force microscopy was used to make precise assessments of surface roughness.

  19. Study of Carbon Nanotubes as Etching Masks and Related Applications in the Surface Modification of GaAs-based Light-Emitting Diodes.

    PubMed

    Jin, Yuanhao; Li, Qunqing; Chen, Mo; Li, Guanhong; Zhao, Yudan; Xiao, Xiaoyang; Wang, Jiaping; Jiang, Kaili; Fan, Shoushan

    2015-09-02

    The surface modification of LEDs based on GaAs is realized by super-aligned multiwalled carbon nanotube (SACNT) networks as etching masks. The surface morphology of SACNT networks is transferred to the GaAs. It is found that the light output power of LEDs based on GaAs with a nanostructured surface morphology is greatly enhanced with the electrical power unchanged. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Optimization of surface morphology and scattering properties of TCO/AIT textured glass front electrode for thin film solar cells

    NASA Astrophysics Data System (ADS)

    Addonizio, M. L.; Fusco, L.; Antonaia, A.; Cominale, F.; Usatii, I.

    2015-12-01

    Aluminium induced texture (AIT) method has been used for obtaining highly textured glass substrate suitable for silicon based thin film solar cell technology. Wet etch step parameters of AIT process have been varied and effect of different etchants and different etching times on morphological and optical properties has been analyzed. The resulting morphology features (shape, size distribution, inclination angle) have been optimized in order to obtain the best scattering properties. ZnO:Ga (GZO) films have been deposited by sputtering technique on AIT-processed glass. Two different ZnO surface morphologies have been obtained, strongly depending on the underlying glass substrate morphology induced by different etching times. Very rough and porous texture (σrms ∼ 150 nm) was obtained on glass etched 2 min showing cauliflower-like structure, whereas a softer texture (σrms ∼ 78 nm) was obtained on glass etched 7 min giving wider and smoother U-shaped craters. The effect of different glass textures on optical confinement has been tested in amorphous silicon based p-i-n devices. Devices fabricated on GZO/high textured glass showed a quantum efficiency enhancement due to both an effective light trapping phenomenon and an effective anti-reflective optical behaviour. Short etching time produce smaller cavities (<1 μm) with deep U-shape characterized by high roughness, high inclination angle and low autocorrelation length. This surface morphology promoted a large light scattering phenomenon, as evidenced by haze value and by angular resolved scattering (ARS) behaviour, into a large range of diffraction angles, giving high probability of effective light trapping inside a PV device.

  1. Surface morphology evolution during plasma etching of silicon: roughening, smoothing and ripple formation

    NASA Astrophysics Data System (ADS)

    Ono, Kouichi; Nakazaki, Nobuya; Tsuda, Hirotaka; Takao, Yoshinori; Eriguchi, Koji

    2017-10-01

    Atomic- or nanometer-scale roughness on feature surfaces has become an important issue to be resolved in the fabrication of nanoscale devices in industry. Moreover, in some cases, smoothing of initially rough surfaces is required for planarization of film surfaces, and controlled surface roughening is required for maskless fabrication of organized nanostructures on surfaces. An understanding, under what conditions plasma etching results in surface roughening and/or smoothing and what are the mechanisms concerned, is of great technological as well as fundamental interest. In this article, we review recent developments in the experimental and numerical study of the formation and evolution of surface roughness (or surface morphology evolution such as roughening, smoothing, and ripple formation) during plasma etching of Si, with emphasis being placed on a deeper understanding of the mechanisms or plasma-surface interactions that are responsible for. Starting with an overview of the experimental and theoretical/numerical aspects concerned, selected relevant mechanisms are illustrated and discussed primarily on the basis of systematic/mechanistic studies of Si etching in Cl-based plasmas, including noise (or stochastic roughening), geometrical shadowing, surface reemission of etchants, micromasking by etch inhibitors, and ion scattering/chanelling. A comparison of experiments (etching and plasma diagnostics) and numerical simulations (Monte Carlo and classical molecular dynamics) indicates a crucial role of the ion scattering or reflection from microscopically roughened feature surfaces on incidence in the evolution of surface roughness (and ripples) during plasma etching; in effect, the smoothing/non-roughening condition is characterized by reduced effects of the ion reflection, and the roughening-smoothing transition results from reduced ion reflections caused by a change in the predominant ion flux due to that in plasma conditions. Smoothing of initially rough surfaces as well as non-roughening of initially planar surfaces during etching (normal ion incidence) and formation of surface ripples by plasma etching (off-normal ion incidence) are also presented and discussed in this context.

  2. Deep inductively coupled plasma etching of ELO-GaN grown with high fill factor

    NASA Astrophysics Data System (ADS)

    Gao, Haiyong; Lee, Jaesoong; Ni, Xianfeng; Leach, Jacob; Özgür, Ümit; Morkoç, Hadis

    2011-02-01

    The epitaxial lateral overgrowth (ELO) gallium nitride (GaN) was grown with high fill factor using metal organic chemical vapor deposition (MOCVD). The inductively coupled plasma (ICP) etching of ELO-GaN based on Cl2/Ar/SiCl4 gas mixture was performed. Surface properties of ELO-GaN subjected to ICP etching have been investigated and optimized etching condition in ELO-GaN with ICP etching is presented. Radiofrequency (RF) power and the flow rate of Cl2 gas were modified during the experiments. The window region, wing region and the edge region of ELO-GaN pattern present different etching characteristics. Different etching conditions were studied to get the minimized plasma-induced damage, relatively high etching rates, and excellent surface profiles. Etch depths of the etched ELO-GaN with smooth surface up to about 19 μm were achieved. The most suitable three-step etching condition is discussed with the assessment based on the morphology observation of the etched surface of ELO-GaN patterns.

  3. SEMICONDUCTOR TECHNOLOGY Texturization of mono-crystalline silicon solar cells in TMAH without the addition of surfactant

    NASA Astrophysics Data System (ADS)

    Weiying, Ou; Yao, Zhang; Hailing, Li; Lei, Zhao; Chunlan, Zhou; Hongwei, Diao; Min, Liu; Weiming, Lu; Jun, Zhang; Wenjing, Wang

    2010-10-01

    Etching was performed on (100) silicon wafers using silicon-dissolved tetramethylammonium hydroxide (TMAH) solutions without the addition of surfactant. Experiments were carried out in different TMAH concentrations at different temperatures for different etching times. The surface phenomena, etching rates, surface morphology and surface reflectance were analyzed. Experimental results show that the resulting surface covered with uniform pyramids can be realized with a small change in etching rates during the etching process. The etching mechanism is explained based on the experimental results and the theoretical considerations. It is suggested that all the components in the TMAH solutions play important roles in the etching process. Moreover, TMA+ ions may increase the wettability of the textured surface. A good textured surface can be obtained in conditions where the absorption of OH-/H2O is in equilibrium with that of TMA+/SiO2 (OH)22-.

  4. Influence of pretreatment on the surface characteristics of PLLA fibers and subsequent hydroxyapatite coating.

    PubMed

    Peng, F; Olson, J R; Shaw, M T; Wei, M

    2009-01-01

    A fibrous precursor for bone repair composites was made by coating poly(L-lactide) (PLLA) fibers with hydroxyapatite (HA) using a biomimetic method. To enhance the bonding between the HA coating and the PLLA fiber, PLLA fibers were etched with either sodium hydroxide or sodium hypochlorite to generate carboxyl groups on fiber surfaces. The experiments were designed to determine the influence of etching on the fiber surface morphology and chemistry as well as the subsequent HA coating on the etched fiber surfaces. It was found that the etching pretreatment increased the roughness as well as the hydrophilicity of fibers, indicating that hydrolysis of PLLA chains had taken place on fiber surfaces. The etching pretreatment also promoted HA coating formation by introducing thicker coating on the surface of fibers with a longer etching time, a higher etching concentration, or with NaOCl as the etching agent. A mechanism of surface hydrolysis and oxidation of PLLA was proposed. (c) 2008 Wiley Periodicals, Inc.

  5. Photocatalytic Active Bismuth Fluoride/Oxyfluoride Surface Crystallized 2Bi2O3-B2O3 Glass-Ceramics

    NASA Astrophysics Data System (ADS)

    Sharma, Sumeet Kumar; Singh, V. P.; Chauhan, Vishal S.; Kushwaha, H. S.; Vaish, Rahul

    2018-03-01

    The present article deals with 2Bi2O3-B2O3 (BBO) glass whose photocatalytic activity has been enhanced by the method of wet etching using an aqueous solution of hydrofluoric acid (HF). X-ray diffraction of the samples reveals that etching with an aqueous solution of HF leads to the formation of BiF3 and BiO0.1F2.8 phases. Surface morphology obtained from scanning electron microscopy show granular and plate-like morphology on the etched glass samples. Rhodamine 6G (Rh 6G) has been used to investigate the photocatalytic activity of the as-quenched and etched glasses. Enhanced visible light-driven photocatalytic activity was observed in HF etched glass-ceramics compared to the as-quenched BBO glass. Contact angle of the as-quenched glass was 90.2°, which decreases up to 20.02° with an increase in concentration of HF in the etching solution. Enhanced photocatalytic activity and increase in the hydrophilic nature suggests the efficient treatment of water pollutants by using the prepared surface crystallized glass-ceramics.

  6. High rate dry etching of (BiSb)2Te3 film by CH4/H2-based plasma

    NASA Astrophysics Data System (ADS)

    Song, Junqiang; Shi, Xun; Chen, Lidong

    2014-10-01

    Etching characteristics of p-type (BiSb)2Te3 films were studied with CH4/H2/Ar gas mixture using an inductively coupled plasma (ICP)-reactive ion etching (RIE) system. The effects of gas mixing ratio, working pressure and gas flow rate on the etch rate and the surface morphology were investigated. The vertical etched profile with the etch rate of 600 nm/min was achieved at the optimized processing parameters. X-ray photoelectron spectroscopy (XPS) analysis revealed the non-uniform etching of (BiSb)2Te3 films due to disparate volatility of the etching products. Micro-masking effects caused by polymer deposition and Bi-rich residues resulted in roughly etched surfaces. Smooth surfaces can be obtained by optimizing the CH4/H2/Ar mixing ratio.

  7. Laser-driven fusion etching process

    DOEpatents

    Ashby, C.I.H.; Brannon, P.J.; Gerardo, J.B.

    1987-08-25

    The surfaces of solids are etched by a radiation-driven chemical reaction. The process involves exposing a substrate coated with a layer of a reactant material on its surface to radiation, e.g., a laser, to induce localized melting of the substrate which results in the occurrence of a fusion reaction between the substrate and coating material. The resultant reaction product and excess reactant salt are then removed from the surface of the substrate with a solvent which is relatively inert towards the substrate. The laser-driven chemical etching process is especially suitable for etching ionic substrates, e.g., LiNbO/sub 3/, such as used in electro-optical/acousto-optic devices. It is also suitable for applications wherein the etching process is required to produce an etched ionic substrate having a smooth surface morphology or when a very rapid etching rate is desired.

  8. Laser-driven fusion etching process

    DOEpatents

    Ashby, Carol I. H.; Brannon, Paul J.; Gerardo, James B.

    1989-01-01

    The surfaces of solid ionic substrates are etched by a radiation-driven chemical reaction. The process involves exposing an ionic substrate coated with a layer of a reactant material on its surface to radiation, e.g. a laser, to induce localized melting of the substrate which results in the occurrance of a fusion reaction between the substrate and coating material. The resultant reaction product and excess reactant salt are then removed from the surface of the substrate with a solvent which is relatively inert towards the substrate. The laser-driven chemical etching process is especially suitable for etching ionic salt substrates, e.g., a solid inorganic salt such as LiNbO.sub.3, such as used in electro-optical/acousto-optic devices. It is also suitable for applications wherein the etching process is required to produce an etched ionic substrate having a smooth surface morphology or when a very rapid etching rate is desired.

  9. Effect of EDTA and phosphoric Acid pretreatment on the bonding effectiveness of self-etch adhesives to ground enamel.

    PubMed

    Ibrahim, Ihab M; Elkassas, Dina W; Yousry, Mai M

    2010-10-01

    This in vitro study determined the effect of enamel pretreatment with phosphoric acid and ethylenediaminetetraacetic acid (EDTA) on the bond strength of strong, intermediary strong, and mild self-etching adhesive systems. Ninety sound human premolars were used. Resin composite cylinders were bonded to flat ground enamel surfaces using three self-etching adhesive systems: strong Adper Prompt L-Pop (pH=0.9-1.0), intermediary strong AdheSE (pH=1.6-1.7), and mild Frog (pH=2). Adhesive systems were applied either according to manufacturer instructions (control) or after pretreatment with either phosphoric acid or EDTA (n=10). After 24 hours, shear bond strength was tested using a universal testing machine at a cross-head speed of 0.5 mm/minute. Ultra-morphological characterization of the surface topography and resin/enamel interfaces as well as representative fractured enamel specimens were examined using scanning electron microscopy (SEM). Neither surface pretreatment statistically increased the mean shear bond strength values of either the strong or the intermediary strong self-etching adhesive systems. However, phosphoric acid pretreatment significantly increased the mean shear bond strength values of the mild self-etching adhesive system. SEM examination of enamel surface topography showed that phosphoric acid pretreatment deepened the same etching pattern of the strong and intermediary strong adhesive systems but converted the irregular etching pattern of the mild self-etching adhesive system to a regular etching pattern. SEM examination of the resin/enamel interface revealed that deepening of the etching pattern was consistent with increase in the length of resin tags. EDTA pretreatment had a negligible effect on ultra-morphological features. Use of phosphoric acid pretreatment can be beneficial with mild self-etching adhesive systems for bonding to enamel.

  10. Effect of EDTA and Phosphoric Acid Pretreatment on the Bonding Effectiveness of Self-Etch Adhesives to Ground Enamel

    PubMed Central

    Ibrahim, Ihab M.; Elkassas, Dina W.; Yousry, Mai M.

    2010-01-01

    Objectives: This in vitro study determined the effect of enamel pretreatment with phosphoric acid and ethylenediaminetetraacetic acid (EDTA) on the bond strength of strong, intermediary strong, and mild self-etching adhesive systems. Methods: Ninety sound human premolars were used. Resin composite cylinders were bonded to flat ground enamel surfaces using three self-etching adhesive systems: strong Adper Prompt L-Pop (pH=0.9–1.0), intermediary strong AdheSE (pH=1.6–1.7), and mild Frog (pH=2). Adhesive systems were applied either according to manufacturer instructions (control) or after pretreatment with either phosphoric acid or EDTA (n=10). After 24 hours, shear bond strength was tested using a universal testing machine at a cross-head speed of 0.5 mm/minute. Ultra-morphological characterization of the surface topography and resin/enamel interfaces as well as representative fractured enamel specimens were examined using scanning electron microscopy (SEM). Results: Neither surface pretreatment statistically increased the mean shear bond strength values of either the strong or the intermediary strong self-etching adhesive systems. However, phosphoric acid pretreatment significantly increased the mean shear bond strength values of the mild self-etching adhesive system. SEM examination of enamel surface topography showed that phosphoric acid pretreatment deepened the same etching pattern of the strong and intermediary strong adhesive systems but converted the irregular etching pattern of the mild self-etching adhesive system to a regular etching pattern. SEM examination of the resin/enamel interface revealed that deepening of the etching pattern was consistent with increase in the length of resin tags. EDTA pretreatment had a negligible effect on ultra-morphological features. Conclusions: Use of phosphoric acid pretreatment can be beneficial with mild self-etching adhesive systems for bonding to enamel. PMID:20922162

  11. Effect of etching and airborne particle abrasion on the microstructure of different dental ceramics.

    PubMed

    Borges, Gilberto Antonio; Sophr, Ana Maria; de Goes, Mario Fernando; Sobrinho, Lourenço Correr; Chan, Daniel C N

    2003-05-01

    The ceramic composition and microstructure surface of all-ceramic restorations are important components of an effective bonding substrate. Both hydrofluoric acid etching and airborne aluminum oxide particle abrasion produce irregular surfaces necessary for micromechanical bonding. Although surface treatments of feldspathic and leucite porcelains have been studied previously, the high alumina-containing and lithium disilicate ceramics have not been fully investigated. The purpose of this study was to assess the surface topography of 6 different ceramics after treatment with either hydrofluoric acid etching or airborne aluminum oxide particle abrasion. Five copings each of IPS Empress, IPS Empress 2 (0.8 mm thick), Cergogold (0.7 mm thick), In-Ceram Alumina, In-Ceram Zirconia, and Procera (0.8 mm thick) were fabricated following the manufacturer's instructions. Each coping was longitudinally sectioned into 4 equal parts by a diamond disk. The resulting sections were then randomly divided into 3 groups depending on subsequent surface treatments: Group 1, specimens without additional surface treatments, as received from the laboratory (control); Group 2, specimens treated by use of airborne particle abrasion with 50-microm aluminum oxide; and Group 3, specimens treated with 10% hydrofluoric acid etching (20 seconds for IPS Empress 2; 60 seconds for IPS Empress and Cergogold; and 2 minutes for In-Ceram Alumina, In-Ceram Zirconia, and Procera). Airborne particle abrasion changed the morphologic surface of IPS Empress, IPS Empress 2, and Cergogold ceramics. The surface topography of these ceramics exhibited shallow irregularities not evident in the control group. For Procera, the 50-microm aluminum oxide airborne particle abrasion produced a flattened surface. Airborne particle abrasion of In-Ceram Alumina and In-Ceram Zirconia did not change the morphologic characteristics and the same shallows pits found in the control group remained. For IPS Empress 2, 10% hydrofluoric acid etching produced elongated crystals scattered with shallow irregularities. For IPS Empress and Cergogold, the morphologic characteristic was honeycomb-like on the ceramic surface. The surface treatment of In-Ceram Alumina, In-Ceram Zirconia, and Procera did not change their superficial structure. Hydrofluoric acid etching and airborne particle abrasion with 50-microm aluminum oxide increased the irregularities on the surface of IPS Empress, IPS Empress 2, and Cergogold ceramics. Similar treatment of In-Ceram Alumina, In-Ceram Zirconia, and Procera did not change their morphologic microstructure.

  12. Stain-etched porous silicon nanostructures for multicrystalline silicon-based solar cells

    NASA Astrophysics Data System (ADS)

    Ben Rabha, M.; Hajji, M.; Belhadj Mohamed, S.; Hajjaji, A.; Gaidi, M.; Ezzaouia, H.; Bessais, B.

    2012-02-01

    In this paper, we study the optical, optoelectronic and photoluminescence properties of stain-etched porous silicon nanostructures obtained with different etching times. Special attention is given to the use of the stain-etched PS as an antireflection coating as well as for surface passivating capabilities. The surface morphology has been analyzed by scanning electron microscopy. The evolution of the Si-O and Si-H absorption bands was analyzed by Fourier transform infrared spectrometry before and after PS treatment. Results show that stain etching of the silicon surface drops the total reflectivity to about 7% in the 400-1100 nm wavelength range and the minority carrier lifetime enhances to about 48 μs.

  13. Surface changes of biopolymers PHB and PLLA induced by Ar+ plasma treatment and wet etching

    NASA Astrophysics Data System (ADS)

    Slepičková Kasálková, N.; Slepička, P.; Sajdl, P.; Švorčík, V.

    2014-08-01

    Polymers, especially group of biopolymers find potential application in a wide range of disciplines due to their biodegradability. In biomedical applications these materials can be used as a scaffold or matrix. In this work, the influence of the Ar+ plasma treatment and subsequent wet etching (acetone/water) on the surface properties of polymers were studied. Two biopolymers - polyhydroxybutyrate with 8% polyhydroxyvalerate (PHB) and poly-L-lactic acid (PLLA) were used in these experiments. Modified surface layers were analyzed by different methods. Surface wettability was characterized by determination of water contact angle. Changes in elemental composition of modified surfaces were performed by X-ray Photoelectron Spectroscopy (XPS). Surface morphology and roughness was examined using Atomic Force Microscopy (AFM). Gravimetry method was used to study the mass loss. It was found that the modification from both with plasma and wet etching leads to dramatic changes of surface properties (surface chemistry, morphology and roughness). Rate of changes of these features strongly depends on the modification parameters.

  14. Advanced light-scattering materials: Double-textured ZnO:B films grown by LP-MOCVD

    NASA Astrophysics Data System (ADS)

    Addonizio, M. L.; Spadoni, A.; Antonaia, A.

    2013-12-01

    Double-textured ZnO:B layers with enhanced optical scattering in both short and long wavelength regions have been successfully fabricated using MOCVD technique through a three step process. Growth of double-textured structures has been induced by wet etching on polycrystalline ZnO surface. Our double-layer structure consists of a first ZnO:B layer wet etched and subsequently used as substrate for a second ZnO:B layer deposition. Polycrystalline ZnO:B layers were etched by utilizing diluted solutions of fluoridic acid (HF), chloridric acid (HCl) and phosphoric acid (H3PO4) and their effect on surface morphology modification was systematically investigated. The morphology of the second deposited ZnO layer strongly depended on the surface properties of the etched ZnO first layer. Growth of cauliflower-like texture was induced by protrusions presence on the HCl etched surface. Optimized double-layer structure shows a cauliflower-like double texture with higher RMS roughness and increased spectral haze values in both short and long wavelength regions, compared to conventional pyramidal-like single texture. Furthermore, this highly scattering structure preserves excellent optical and electrical properties.

  15. Morphology modulating the wettability of a diamond film.

    PubMed

    Tian, Shibing; Sun, Weijie; Hu, Zhaosheng; Quan, Baogang; Xia, Xiaoxiang; Li, Yunlong; Han, Dong; Li, Junjie; Gu, Changzhi

    2014-10-28

    Control of the wetting property of diamond surface has been a challenge because of its maximal hardness and good chemical inertness. In this work, the micro/nanoarray structures etched into diamond film surfaces by a maskless plasma method are shown to fix a surface's wettability characteristics, and this means that the change in morphology is able to modulate the wettability of a diamond film from weakly hydrophilic to either superhydrophilic or superhydrophobic. It can be seen that the etched diamond surface with a mushroom-shaped array is superhydrophobic following the Cassie mode, whereas the etched surface with nanocone arrays is superhydrophilic in accordance with the hemiwicking mechnism. In addition, the difference in cone densities of superhydrophilic nanocone surfaces has a significant effect on water spreading, which is mainly derived from different driving forces. This low-cost and convenient means of altering the wetting properties of diamond surfaces can be further applied to underlying wetting phenomena and expand the applications of diamond in various fields.

  16. Nanoporous Silicon Carbide for Nanoelectromechanical Systems Applications

    NASA Technical Reports Server (NTRS)

    Hossain, T.; Khan, F.; Adesida, I.; Bohn, P.; Rittenhouse, T.; Lienhard, Michael (Technical Monitor)

    2003-01-01

    A major goal of this project is to produce porous silicon carbide (PSiC) via an electroless process for eventual utilization in nanoscale sensing platforms. Results in the literature have shown a variety of porous morphologies in SiC produced in anodic cells. Therefore, predictability and reproducibility of porous structures are initial concerns. This work has concentrated on producing morphologies of known porosity, with particular attention paid toward producing the extremely high surface areas required for a porous flow sensor. We have conducted a parametric study of electroless etching conditions and characteristics of the resulting physical nanostructure and also investigated the relationship between morphology and materials properties. Further, we have investigated bulk etching of SiC using both photo-electrochemical etching and inductively-coupled-plasma reactive ion etching techniques.

  17. Bond efficacy and interface morphology of self-etching adhesives to ground enamel.

    PubMed

    Abdalla, Ali I; El Zohairy, Ahmed A; Abdel Mohsen, Mohamed M; Feilzer, Albert J

    2010-02-01

    This study compared the microshear bond strengths to ground enamel of three one-step self-etching adhesive systems, a self-etching primer system and an etch-and-rinse adhesive system. Three self-etching adhesives, Futurabond DC (Voco), Clearfil S Tri Bond (Kuraray) and Hybrid bond (Sun-Medical), a self-etching primer, Clearfil SE Bond (Kuraray), and an etch-and-rinse system, Admira Bond (Voco), were selected. Thirty human molars were used. The root of each tooth was removed and the crown was sectioned into halves. The convex enamel surfaces were reduced by polishing on silicone paper to prepare a flat surface. The bonding systems were applied on this surface. Prior to adhesive curing, a hollow cylinder (2.0 mm height/0.75 mm internal diameter) was placed on the treated surfaces. A resin composite was then inserted into the tube and cured. After water storage for 24 h, the tube was removed and shear bond strength was determined in a universal testing machine at a crosshead speed of 0.5 mm/min. The results were analyzed with ANOVA and the Tukey.-Kramer test at a 59 degrees confidence level. The enamel of five additional teeth was ground, and the etching component of each adhesive was applied and removed with absolute ethanol instead of being light cured. These teeth and selected fractured surfaces were examined by SEM. Adhesion to ground enamel of the Futurabond DC (25 +/- 3.5 MPa) and Clearfil SE Bond (23 +/- 2.9 MPa) self-etching systems was not significantly different from the etch-and-rinse system Admira Bond (27 +/- 2.3 MPa). The two self-etching adhesives Clearfil S Tri bond and Hybrid Bond demonstrated significantly lower bond strengths (14 +/- 1.4 MPa; 11 +/- 1.9 MPa) with no significant differences between them (p < 0.05). Bond strengths to ground enamel of self-etching adhesive systems are dependent on the type of adhesive system. Some of the new adhesive systems showed bond strength values comparable to that of etch-and-rinse systems. There was no correlation between bond strength and morphological changes in enamel.

  18. Recovery of GaN surface after reactive ion etching

    NASA Astrophysics Data System (ADS)

    Fan, Qian; Chevtchenko, S.; Ni, Xianfeng; Cho, Sang-Jun; Morko, Hadis

    2006-02-01

    Surface properties of GaN subjected to reactive ion etching and the impact on device performance have been investigated by surface potential, optical and electrical measurements. Different etching conditions were studied and essentially high power levels and low chamber pressures resulted in higher etch rates accompanying with the roughening of the surface morphology. Surface potential for the as-grown c-plane GaN was found to be in the range of 0.5~0.7 V using Scanning Kevin Probe Microscopy. However, after reactive ion etching at a power level of 300 W, it decreased to 0.1~0.2 V. A nearly linear reduction was observed on c-plane GaN with increasing power. The nonpolar a-plane GaN samples also showed large surface band bending before and after etching. Additionally, the intensity of the near band-edge photoluminescence decreased and the free carrier density increased after etching. These results suggest that the changes in the surface potential may originate from the formation of possible nitrogen vacancies and other surface oriented defects and adsorbates. To recover the etched surface, N II plasma, rapid thermal annealing, and etching in wet KOH were performed. For each of these methods, the surface potential was found to increase by 0.1~0.3 V, also the reverse leakage current in Schottky diodes fabricated on treated samples was reduced considerably compared with as-etched samples, which implies a partial-to-complete recovery from the plasma-induced damage.

  19. Surface smoothing of indium tin oxide film by laser-induced photochemical etching

    NASA Astrophysics Data System (ADS)

    Kang, JoonHyun; Kim, Young-Hwan; Kwon, Seok Joon; Park, Joon-Suh; Park, Kyoung Wan; Park, Jae-Gwan; Han, Il Ki

    2017-12-01

    Surface smoothing of indium tin oxide (ITO) film by laser irradiation was demonstrated. The ITO surface was etched by choline radicals, which were activated by laser irradiation at a wavelength of 532 nm. The RMS surface roughness was improved from 5.6 to 4.6 nm after 10 min of laser irradiation. We also showed the changes in the surface morphology of the ITO film with various irradiation powers and times.

  20. Surface Morphology Evolution Mechanisms of InGaN/GaN Multiple Quantum Wells with Mixture N2/H2-Grown GaN Barrier.

    PubMed

    Zhou, Xiaorun; Lu, Taiping; Zhu, Yadan; Zhao, Guangzhou; Dong, Hailiang; Jia, Zhigang; Yang, Yongzhen; Chen, Yongkang; Xu, Bingshe

    2017-12-01

    Surface morphology evolution mechanisms of InGaN/GaN multiple quantum wells (MQWs) during GaN barrier growth with different hydrogen (H 2 ) percentages have been systematically studied. Ga surface-diffusion rate, stress relaxation, and H 2 etching effect are found to be the main affecting factors of the surface evolution. As the percentage of H 2 increases from 0 to 6.25%, Ga surface-diffusion rate and the etch effect are gradually enhanced, which is beneficial to obtaining a smooth surface with low pits density. As the H 2 proportion further increases, stress relaxation and H 2 over- etching effect begin to be the dominant factors, which degrade surface quality. Furthermore, the effects of surface evolution on the interface and optical properties of InGaN/GaN MQWs are also profoundly discussed. The comprehensive study on the surface evolution mechanisms herein provides both technical and theoretical support for the fabrication of high-quality InGaN/GaN heterostructures.

  1. The influence of surface properties of plasma-etched polydimethylsiloxane (PDMS) on cell growth and morphology.

    PubMed

    Pennisi, Cristian P; Zachar, Vladimir; Gurevich, Leonid; Patriciu, Andrei; Struijk, Johannes J

    2010-01-01

    Polydimethylsiloxane (PDMS) or silicone rubber is a widely used implant material. Approaches to promote tissue integration to PDMS are desirable to avoid clinical problems associated with sliding and friction between tissue and implant. Plasma-etching is a useful way to control cell behavior on PDMS without additional coatings. In this work, different plasma processing conditions were used to modify the surface properties of PDMS substrates. Surface nanotopography and wettability were measured to study their effect on in vitro growth and morphology of fibroblasts. While fluorinated plasma treatments produced nanorough hydrophobic and superhydrophobic surfaces that had negative or little influences on cellular behavior, water vapor/oxygen plasma produced smooth hydrophillic surfaces that enhanced cell growth.

  2. Morphologies of Solid Surfaces Produced Far from Equilibrium

    DTIC Science & Technology

    1991-03-10

    common to all these applications is that thc surface preparation processes used are far from chemical equilibrium. Many of the processes involve an...energetic ion beam, plasma or gas that is used to modify a surface, either by etching or depositing material. The electrical, optical and mechanical...growth, a number of continuum models have been used in the materials science literature, in particular in the context of electron-beam etching of

  3. Shear bond strength and SEM morphology evaluation of different dental adhesives to enamel prepared with ER:YAG laser

    PubMed Central

    Pires, Patrícia T.; Ferreira, João C.; Oliveira, Sofia A.; Azevedo, Álvaro F.; Dias, Walter R.; Melo, Paulo R.

    2013-01-01

    Context: Early observations of enamel surfaces prepared by erbium lasers motivated clinicians to use laser as an alternative to chemical etching. Aims: Evaluate shear bond strength (SBS) values of different dental adhesives on Erbium:Yttrium Aluminum Garnet (Er:YAG) laser prepared enamel and to evaluate possible etching patterns correlations between dental adhesives and SBS values. Subjects and Methods: One hundred bovine incisors were randomly assigned to SBS tests on enamel (n = 15) and to enamel morphology analysis (n = 5) after Er:YAG laser preparation as follows: Group I – 37% phosphoric acid (PA)+ ExciTE®; Group II – ExciTE®; Group III – AdheSE® self-etching; Group IV – FuturaBond® no-rinse. NR; Group V – Xeno® V. Teeth were treated with the adhesive systems and subjected to thermal cycling. SBS were performed in a universal testing machine at 5 mm/min. Statistical Analysis Used: One-way ANOVA and post-hoc tests (P < 0.05). For the morphology evaluation, specimens were immersed in Ethylenediamine tetraacetic acid (EDTA) and the etching pattern analyzed under Scanning Electron Microscope (SEM). Results: Mean bond strengths were Group I – 47.17 ± 1.61 MPa (type I etching pattern); Group II – 32.56 ± 1.64 MPa, Group III – 29.10 ± 1.34 MPa, Group IV – 23.32 ± 1.53 MPa (type III etching pattern); Group V – 24.43 MPa ± 1.55 (type II etching pattern). Conclusions: Different adhesive systems yielded significantly different SBSs. Acid etching significantly increased the adhesion in laser treated enamel. No differences in SBS values were obtained between AdheSE® and ExciTE® without condition with PA. FuturaBond® NR and Xeno® V showed similar SBS, which was lower in comparison to the others adhesives. No correlation between enamel surface morphology and SBS values was observed, except when PA was used. PMID:23853447

  4. Shear bond strength and SEM morphology evaluation of different dental adhesives to enamel prepared with ER:YAG laser.

    PubMed

    Pires, Patrícia T; Ferreira, João C; Oliveira, Sofia A; Azevedo, Alvaro F; Dias, Walter R; Melo, Paulo R

    2013-01-01

    Early observations of enamel surfaces prepared by erbium lasers motivated clinicians to use laser as an alternative to chemical etching. Evaluate shear bond strength (SBS) values of different dental adhesives on Erbium:Yttrium Aluminum Garnet (Er:YAG) laser prepared enamel and to evaluate possible etching patterns correlations between dental adhesives and SBS values. One hundred bovine incisors were randomly assigned to SBS tests on enamel (n = 15) and to enamel morphology analysis (n = 5) after Er:YAG laser preparation as follows: Group I - 37% phosphoric acid (PA)+ ExciTE(®); Group II - ExciTE(®); Group III - AdheSE(®) self-etching; Group IV - FuturaBond(®) no-rinse. NR; Group V - Xeno(®) V. Teeth were treated with the adhesive systems and subjected to thermal cycling. SBS were performed in a universal testing machine at 5 mm/min. One-way ANOVA and post-hoc tests (P < 0.05). For the morphology evaluation, specimens were immersed in Ethylenediamine tetraacetic acid (EDTA) and the etching pattern analyzed under Scanning Electron Microscope (SEM). Mean bond strengths were Group I - 47.17 ± 1.61 MPa (type I etching pattern); Group II - 32.56 ± 1.64 MPa, Group III - 29.10 ± 1.34 MPa, Group IV - 23.32 ± 1.53 MPa (type III etching pattern); Group V - 24.43 MPa ± 1.55 (type II etching pattern). Different adhesive systems yielded significantly different SBSs. Acid etching significantly increased the adhesion in laser treated enamel. No differences in SBS values were obtained between AdheSE(®) and ExciTE(®) without condition with PA. FuturaBond(®) NR and Xeno(®) V showed similar SBS, which was lower in comparison to the others adhesives. No correlation between enamel surface morphology and SBS values was observed, except when PA was used.

  5. Light emitting diode with high aspect ratio submicron roughness for light extraction and methods of forming

    DOEpatents

    Li, Ting [Ventura, CA

    2011-04-26

    The surface morphology of an LED light emitting surface is changed by applying a reactive ion etch (RIE) process to the light emitting surface. High aspect ratio, submicron roughness is formed on the light emitting surface by transferring a thin film metal hard-mask having submicron patterns to the surface prior to applying a reactive ion etch process. The submicron patterns in the metal hard-mask can be formed using a low cost, commercially available nano-patterned template which is transferred to the surface with the mask. After subsequently binding the mask to the surface, the template is removed and the RIE process is applied for time duration sufficient to change the morphology of the surface. The modified surface contains non-symmetric, submicron structures having high aspect ratio which increase the efficiency of the device.

  6. Metal-assisted chemical etch porous silicon formation method

    DOEpatents

    Li, Xiuling; Bohn, Paul W.; Sweedler, Jonathan V.

    2004-09-14

    A thin discontinuous layer of metal such as Au, Pt, or Au/Pd is deposited on a silicon surface. The surface is then etched in a solution including HF and an oxidant for a brief period, as little as a couple seconds to one hour. A preferred oxidant is H.sub.2 O.sub.2. Morphology and light emitting properties of porous silicon can be selectively controlled as a function of the type of metal deposited, Si doping type, silicon doping level, and/or etch time. Electrical assistance is unnecessary during the chemical etching of the invention, which may be conducted in the presence or absence of illumination.

  7. Change in surface properties of zirconia and initial attachment of osteoblastlike cells with hydrophilic treatment.

    PubMed

    Watanabe, Hiroaki; Saito, Kensuke; Kokubun, Katsutoshi; Sasaki, Hodaka; Yoshinari, Masao

    2012-01-01

    The objectives of this study were to characterize change in surface properties of tetragonal zirconia polycrystals (TZP) after hydrophilic treatment, and to determine the effect of such changes on initial attachment of osteoblast-like cells. Roughened surfaces were produced by alumina-blasting and acid-etching. Hydrophilic treatment comprised application of immediately after blasting and acid-etching (Blast/Etch), oxygen plasma (O2-Plasma), ultraviolet light (UV). Specimens stored in air were used as a control. The water contact angle was determined and surface analysis was performed using an X-ray photoelectron spectroscopy. Blast/Etch, O2-Plasma and UV specimens showed superhydrophilicity, and these hydrophilic treatments to TZP elicited a marked decrease in carbon content and an increase in hydroxyl groups. Hydrophilic treatments enhanced initial attachment of osteoblast-like cells and a change in cell morphologies. These results indicate that Blast/Etch, O2-Plasma, or UV treatment has potential in the creation and maintenance of superhydrophilic surfaces and enhancing initial attachment of osteoblast-like cells.

  8. Oxygen and nitrogen plasma etching of three-dimensional hydroxyapatite/chitosan scaffolds fabricated by additive manufacturing

    NASA Astrophysics Data System (ADS)

    Myung, Sung-Woon; Kim, Byung-Hoon

    2016-01-01

    Three-dimensional (3D) chitosan and hydroxyapatite (HAp)/chitosan (CH) scaffolds were fabricated by additive manufacturing, then their surfaces were etched with oxygen (O2) and nitrogen (N2) plasma. O2 and N2 plasma etching was performed to increase surface properties such as hydrophilicity, roughness, and surface chemistry on the scaffolds. After etching, hydroxyapatite was exposed on the surface of 3D HAp/CH scaffolds. The surface morphology and chemical properties were characterized by contact angle measurement, scanning electron microscopy, X-ray diffraction, and attenuated total reflection Fourier infrared spectroscopy. The cell viability of 3D chitosan scaffolds was examined by 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide assay. The differentiation of preosteoblast cells was evaluated by alkaline phosphatase assay. The cell viability was improved by O2 and N2 plasma etching of 3D chitosan scaffolds. The present fabrication process for 3D scaffolds might be applied to a potential tool for preparing biocompatible scaffolds.

  9. Surface morphology and dislocation characteristics near the surface of 4H-SiC wafer using multi-directional scanning transmission electron microscopy.

    PubMed

    Sato, Takahiro; Orai, Yoshihisa; Suzuki, Yuya; Ito, Hiroyuki; Isshiki, Toshiyuki; Fukui, Munetoshi; Nakamura, Kuniyasu; Schamp, C T

    2017-10-01

    To improve the reliability of silicon carbide (SiC) electronic power devices, the characteristics of various kinds of crystal defects should be precisely understood. Of particular importance is understanding the correlation between the surface morphology and the near surface dislocations. In order to analyze the dislocations near the surface of 4H-SiC wafers, a dislocation analysis protocol has been developed. This protocol consists of the following process: (1) inspection of surface defects using low energy scanning electron microscopy (LESEM), (2) identification of small and shallow etch pits using KOH low temperature etching, (3) classification of etch pits using LESEM, (4) specimen preparation of several hundred nanometer thick sample using the in-situ focused ion beam micro-sampling® technique, (5) crystallographic analysis using the selected diffraction mode of the scanning transmission electron microscope (STEM), and (6) determination of the Burgers vector using multi-directional STEM (MD-STEM). The results show a correlation between the triangular terrace shaped surface defects and an hexagonal etch pit arising from threading dislocations, linear shaped surface defects and elliptical shaped etch pits arising from basal plane dislocations. Through the observation of the sample from two orthogonal directions via the MD-STEM technique, a basal plane dislocation is found to dissociate into an extended dislocation bound by two partial dislocations. A protocol developed and presented in this paper enables one to correlate near surface defects of a 4H-SiC wafer with the root cause dislocations giving rise to those surface defects. © The Author 2017. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

  10. Morphological effects of MMPs inhibitors on the dentin bonding

    PubMed Central

    Li, He; Li, Tianbo; Li, Xiuying; Zhang, Zhimin; Li, Penglian; Li, Zhenling

    2015-01-01

    Matrix metalloproteinases (MMPs) have been studied extensively, and MMP inhibitors have been used as dental pretreatment agents prior to dentin bonding because they reduce collagen fiber degradation and improve bonding strength. However, morphologic characteristics of the collagen network after etching and of the post-adhesive dentin hybrid layers (DHL) after MMP inhibitors pretreatment have not been evaluated. Thus, we investigated demineralized dentin pretreated with chlorhexidine (CHX) and minocycline (MI) in an etch- and -rinse adhesive system with field emission scanning electron microscopy (FESEM) and immuno-gold labeling markers to observe the collagen network and DHL. FESEM revealed after CHX and MI, a demineralized dentin surface and improved collagen network formation, reduced collagen degradation, and distinct gold-labeling signals. Applying adhesive after either MMP inhibitor created a better dentin interface as evidenced by immuno-gold staining, better adhesive penetration, and higher DHL quality. With microtensile bond strength tests (µTBS) we estimated bonding strength using µTBS data. Immediate µTBS was enhanced with MMP inhibitor application to the bonding surface, and the CHX group was significantly different than non-treated etched surfaces, but no significant change was detected in the MI group. Surface micromorphology of the fractured dentin resin restoration showed that the CHX group had a better resin and dentin tube combination. Both MMP inhibitors created uniform resin coverage. Thus, morphologic results and µTBS data suggest that CHX and MI can inhibit MMP activity, improve immediate bonding strength, and enhance dentin bonding stability with an etch- and -rinse adhesive system. PMID:26379873

  11. Study on the formation of dodecagonal pyramid on nitrogen polar GaN surface etched by hot H3PO4

    NASA Astrophysics Data System (ADS)

    Qi, S. L.; Chen, Z. Z.; Fang, H.; Sun, Y. J.; Sang, L. W.; Yang, X. L.; Zhao, L. B.; Tian, P. F.; Deng, J. J.; Tao, Y. B.; Yu, T. J.; Qin, Z. X.; Zhang, G. Y.

    2009-08-01

    Hot phosphor acid (H3PO4) etching is presented to form a roughened surface with dodecagonal pyramids on laser lift-off N face GaN grown by metalorganic chemical vapor deposition. A detailed analysis of time evolution of surface morphology is described as a function of etching temperature. The activation energy of the H3PO4 etching process is 1.25 eV, indicating the process is reaction-limited scheme. And it is found that the oblique angle between the facets and the base plane increases as the temperature increases. Thermodynamics and kinetics related factors of the formation mechanism of the dodecagonal pyramid are also discussed. The light output power of a vertical injection light-emitting-diode (LED) with proper roughened surface shows about 2.5 fold increase compared with that of LED without roughened surface.

  12. Light emitting diode with high aspect ratio submicron roughness for light extraction and methods of forming

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Li, Ting

    The surface morphology of an LED light emitting surface is changed by applying a reactive ion etch (RIE) process to the light emitting surface. High aspect ratio, submicron roughness is formed on the light emitting surface by transferring a thin film metal hard-mask having submicron patterns to the surface prior to applying a reactive ion etch process. The submicron patterns in the metal hard-mask can be formed using a low cost, commercially available nano-patterned template which is transferred to the surface with the mask. After subsequently binding the mask to the surface, the template is removed and the RIE processmore » is applied for time duration sufficient to change the morphology of the surface. The modified surface contains non-symmetric, submicron structures having high aspect ratio which increase the efficiency of the device.« less

  13. Decalin-assisted light emitting porous Si formation and its optical, surface and morphological properties

    NASA Astrophysics Data System (ADS)

    Karatutlu, Ali; Istengir, Sumeyra; Cosgun, Sedat; Seker, Isa; Unal, Bayram

    2017-11-01

    In this research paper, light emitting porous silicon (Lep-Si) samples were fabricated by a surfactant-mediated chemical stain etching solution in order to form homogenous luminescent nanostructures at room temperature. As an industrially important solvent, decalin (decahydronaphtalene) was used as a surfactant in the HF/HNO3 solutions in order to control the etching process. Morphological, surface and optical properties of the Lep-Si samples were examined using atomic force microscopy, X-ray photoelectron spectroscopy, photoluminescence (PL) spectroscopy, and laser scanning confocal microscopy (LSCM) techniques. These characterization techniques were correlated with the various etching times including depth dependent luminescence profiles for the first time. We report the optimum conditions for production of the most efficient Lep-Si using decalin (decahydronaphtalene) and possible structural origins of light emission using the depth dependent luminescence measurements.

  14. In vivo effect of a self-etching primer on dentin.

    PubMed

    Milia, E; Lallai, M R; García-Godoy, F

    1999-08-01

    To determine the ultrastructural aspects of the dentin collagen area in the cavity preparation floor produced in vivo after phosphoric acid acid-etching or after using Clearfil Liner Bond 2 self-etching primer (LB2 Primer). Twenty-four non-carious third molars scheduled for extraction from young adult patients (16-30 years old) were used. Conventional Class I cavities (+/- 2 mm deep) were prepared on the occlusal surfaces of all teeth using a cylindrical diamond bur on a high-speed handpiece with copious water spray. To avoid dehydration of the dentin, the smear layer-covered dentin was briefly air-dried for 2 seconds. Cavities were assigned at random to the following groups: Group A: Dentin etched for 15 seconds with 34% phosphoric acid, rinsed for 20 seconds and then briefly air-dried for 2 seconds with oil-free compressed air leaving the surfaces slightly moist. Group B: LB2 Primer was applied to the cavity surfaces for 30 seconds and then briefly air-dried to remove the solvent. Group C: The untreated dentin smear layer was used as a control. In all three groups, the cavities were filled incrementally with a resin-based composite (APX), light curing every increment for 40 seconds. After 30 minutes, the teeth were extracted atraumatically and the samples immediately prepared for evaluation with the transmission electron microscope. The use of a self-etching primer did not produce significant morphological changes in the moist dentin substrate. Adverse morphological conditions where observed when there was an excess water on the dentin surface. Phosphoric acid altered the collagen more severely than the self-etching primer.

  15. [Brushing abrasion of the enamel surface after erosion].

    PubMed

    Lipei, Chen; Xiangke, Ci; Xiaoyan, Ou

    2017-08-01

    Objective A study was conducted to compare the effect of different enamel remineralization periods after erosion on the depth of brushing abrasion. Methods Ten volunteers were selected for a 4-day experiment. A total of 60 enamels were randomly assigned into six groups (A-F) and placed in intraoral palatal devices. On the first day, the palatal devices were placed in oral cavity (24 h) . On the following three days, brushing experiments were performed extraorally, two times per day. The specific experimental method of brushing follows these next steps. First, the group F specimens were covered with a film of wax, and then acid etched for 2 min. Subsequently, the film of wax was detached. The groups from A to D were brushed after remineralization at the following time intervals: group A, 0 min; group B, 20 min; group C, 40 min; group D, 60 min. Erosion and remineralization were performed on group E, but without brushing. Remineralization was performed on group F, but without acid etching and brushing. The depth of enamel abrasion was determined by a mechanical profilometer. The surface morphology of the enamel blocks was observed using a scanning electron microscope. Results 1) The depth of abrasion was different in varied enamel remineralization time after acid etching. The statistical significant differences between groups were as follows. 2) When the time of enamel remineralization after acid etching was short, the surface depression in the electron microscope was deep, and the surface morphology was rough. Conclusion Brushing immediately after acid etching would cause much serious abrasion to the enamel surface. Brushing after 60 min can effectively reduce the abrasion of acid etching enamel.

  16. Enhancement on the Surface Hydrophobicity and Oleophobicity of an Organosilicon Film by Conformity Deposition and Surface Fluorination Etching.

    PubMed

    Xu, Zheng-Wen; Zhang, Yu-Kai; Chen, Tai-Hong; Chang, Jin-How; Lee, Tsung-Hsin; Li, Pei-Yu; Liu, Day-Shan

    2018-06-26

    In this work, the surface morphology of a hydrophobic organosilicon film was modified as it was deposited onto a silver seed layer with nanoparticles. The surface hydrophobicity evaluated by the water contact angle was significantly increased from 100° to 128° originating from the surface of the organosilicon film becoming roughened, and was deeply relevant to the Ag seed layer conform deposition. In addition, the organosilicon film became surface oleophobic and the surface hydrophobicity was improved due to the formation of the inactive C-F chemical on the surface after the carbon tetrafluoride glow discharge etching. The surface hydrophobicity and oleophobicity of the organosilicon film could be further optimized with water and oleic contact angles of about 138° and 61°, respectively, after an adequate fluorination etching.

  17. Plasma surface modification of polypropylene track-etched membrane to improve its performance properties

    NASA Astrophysics Data System (ADS)

    Kravets, L. I.; Elinson, V. M.; Ibragimov, R. G.; Mitu, B.; Dinescu, G.

    2018-02-01

    The surface and electrochemical properties of polypropylene track-etched membrane treated by plasma of nitrogen, air and oxygen are studied. The effect of the plasma-forming gas composition on the surface morphology is considered. It has been found that the micro-relief of the membrane surface formed under the gas-discharge etching, changes. Moreover, the effect of the non-polymerizing gas plasma leads to formation of oxygen-containing functional groups, mostly carbonyl and carboxyl. It is shown that due to the formation of polar groups on the surface and its higher roughness, the wettability of the plasma-modified membranes improves. In addition, the presence of polar groups on the membrane surface layer modifies its electrochemical properties so that conductivity of plasma-treated membranes increase.

  18. Effect of an aggressive medium on discontinuous deformation of aluminum-magnesium alloy AlMg6

    NASA Astrophysics Data System (ADS)

    Shibkov, A. A.; Denisov, A. A.; Zolotov, A. E.; Kochegarov, S. S.

    2017-01-01

    It is experimentally shown that the molecular (chemical) process of surface etching of deformed aluminum-magnesium alloy AlMg6 causes the development of a macroscopic plastic strain step with an amplitude of a few percent. Using numerical simulation of the polycrystalline solid etching process, it is shown that the corrosion front morphology varies during etching from Euclid (flat) to fractal (rough). The results obtained show the key role of the surface state on the development of macroscopic mechanical instability of a material exhibiting the Portevin-Le Chatelier effect.

  19. Bio-inspired silicon nanospikes fabricated by metal-assisted chemical etching for antibacterial surfaces

    NASA Astrophysics Data System (ADS)

    Hu, Huan; Siu, Vince S.; Gifford, Stacey M.; Kim, Sungcheol; Lu, Minhua; Meyer, Pablo; Stolovitzky, Gustavo A.

    2017-12-01

    The recently discovered bactericidal properties of nanostructures on wings of insects such as cicadas and dragonflies have inspired the development of similar nanostructured surfaces for antibacterial applications. Since most antibacterial applications require nanostructures covering a considerable amount of area, a practical fabrication method needs to be cost-effective and scalable. However, most reported nanofabrication methods require either expensive equipment or a high temperature process, limiting cost efficiency and scalability. Here, we report a simple, fast, low-cost, and scalable antibacterial surface nanofabrication methodology. Our method is based on metal-assisted chemical etching that only requires etching a single crystal silicon substrate in a mixture of silver nitrate and hydrofluoric acid for several minutes. We experimentally studied the effects of etching time on the morphology of the silicon nanospikes and the bactericidal properties of the resulting surface. We discovered that 6 minutes of etching results in a surface containing silicon nanospikes with optimal geometry. The bactericidal properties of the silicon nanospikes were supported by bacterial plating results, fluorescence images, and scanning electron microscopy images.

  20. Morphology and electronic properties of silicon carbide surfaces

    NASA Astrophysics Data System (ADS)

    Nie, Shu

    2007-12-01

    Several issues related to SiC surfaces are studied in the thesis using scanning tunneling microscopy/spectroscopy (STM/S) and atomic force microscopy (AFM). Specific surfaces examined include electropolished SiC, epitaxial graphene on SiC, and vicinal (i.e. slightly miscut from a low-index direction) SiC that have been subjected to high temperature hydrogen-etching. The electropolished surfaces are meant to mimic electrochemically etched SiC, which forms a porous network. The chemical treatment of the surface is similar between electropolishing and electrochemical etching, but the etching conditions are slightly different such that the former produces a flat surface (that is amenable to STM study) whereas the latter produces a complex 3-dimensional porous network. We have used these porous SiC layers as semi-permeable membranes in a biosensor, and we find that the material is quite biocompatible. The purpose of the STM/STS study is to investigate the surface properties of the SiC on the atomic scale in an effort to explain this biocompatibility. The observed tunneling spectra are found to be very asymmetric, with a usual amount of current at positive voltages but no observable current at negative voltages. We propose that this behavior is due to surface charge accumulating on an incompletely passivated surface. Measurements on SiC surfaces prepared by various amounts of hydrogen-etching are used to support this interpretation. Comparison with tunneling computations reveals a density of about 10 13 cm-2 fixed charges on both the electro-polished and the H-etched surfaces. The relatively insulating nature observed on the electro-polished SiC surface may provide an explanation for the biocompatibility of the surface. Graphene, a monolayer of carbon, is a new material for electronic devices. Epitaxial graphene on SiC is fabricated by the Si sublimation method in which a substrate is heated up to about 1350°C in ultra-high vacuum (UHV). The formation of the graphene is monitored using low-energy electron diffraction (LEED) and Auger electron spectroscopy, and the morphology of the graphitized surface is studied using AFM and STM. Use of H-etched SiC substrates enables a relatively flat surface morphology, although residual steps remain due to unintentional miscut of the wafers. Additionally, some surface roughness in the form of small pits is observed, possibly due to the fact that the surface treatments (H-etching and UHV annealing) having been performed in separate vacuum chambers with an intervening transfer through air. Field-effect transistors have been fabricated with our graphene layers; they show a relatively strong held effect at room temperature, with an electron mobility of 535 cm 2/Vs. This value is somewhat lower than that believed to be theoretically possible for this material, and one possible reason may be the nonideal morphology of the surface (i.e. because of the observed steps and pits). Tunneling spectra of the graphene reveal semi-metallic behavior, consistent with that theoretically expected for an isolated layer of graphene. However, additional discrete states are observed in the spectra, possibly arising from bonding at the graphene/SiC interface. The observation of these states provides important input towards an eventual determination of the complete interface structure, and additionally, such states may be relevant in determining the electron mobility of the graphene. Stepped vicinal SIC{0001} substrates are useful templates for epitaxial growth of various types of layers: thick layers of compound semiconductor (in which the steps help preserving the stacking arrangement in the overlayer), monolayers of graphene, or submonolayer semiconductor layers that form quantum wires along the step edges. Step array produced by H-etching of vicinal SiC (0001) and (0001¯) with various miscut angles have been studied by AFM. H-etching is found to produce full unit-cell-high steps on the (0001) Si-face surfaces, but half unit-cell-high steps on the (0001¯) C-face surfaces. These observations are consistent with an asymmetry in the surface energy (i.e. etch rate) of the two types of step terminations occurring on the different surfaces. For high miscut angles, facet formation is observed on the vicinal Si-face, but less so on the C-face. This difference is interpreted in terms of a lower surface energy of the C-face. In terms of applying the stepped surfaces as a template, a much better uniformity in the step-step separation is found for the C-face surfaces.

  1. Effect of surface etching on the oxidation behavior of plasma chromizing-treated AISI440B stainless steel

    NASA Astrophysics Data System (ADS)

    Meng, T. X.; Guo, Q.; Xi, W.; Ding, W. Q.; Liu, X. Z.; Lin, N. M.; Yu, S. W.; Liu, X. P.

    2018-03-01

    Double glow plasma surface alloying was applied to prepare chromizing layer in the surface of AISI440B stainless steel. Prior to chromizing, the stainless steel was etched by microwave plasma chemical vapor deposition to change the surface morphology and composition, and then heated for chromizing at 950 °C for 3 h. The cyclical oxidation of steel after chromizing was carried out at 900 °C for 100 h. Scanning electron microscopy, glow discharge optical emission spectrometer and X-ray diffractometer were used to characterize microstructure, composition and phase structure of alloyed and oxidized samples. The results show that the surface was composed of the Cr-rich top layer and Cr23C6, Cr7C3 and {Cr,Fe}7C3 below layer after chromizing. The bonding between the chromizing layer and the substrate after etching treatment was obviously strengthened. AISI440B steel shows a poor oxidation resistance and the weight gain oxidized for 100 h was up to 31.1 mg/cm2. Weight gains for chromizing and etching + chromizing treated samples were 0.67 mg/cm2 and 8 mg/cm2, respectively. Both oxidized surfaces of chromizing and etching + chromizing were composed of Cr2O3, but the oxide scale of etching + chromizing treated samples was more compact than that of samples without etching.

  2. Mechanical and chemical effects of ion-texturing biomedical polymers

    NASA Technical Reports Server (NTRS)

    Weigand, A. J.; Cenkus, M. A.

    1979-01-01

    To determine whether sputter etching may provide substantial polymer surface texturing with insignificant changes in chemical and mechanical properties, an 8 cm beam diameter, electron bombardment, argon ion source was used to sputter etch (ion-texture process) nine biomedical polymers. The materials included silicone rubber, 32% carbon impregnated polyolefin, polyoxymethylene, polytetrafluoroethylene, ultrahigh molecular weight (UHMW) polyethylene, UHMW polyethylene with carbon fibers (10%), and several polyurethanes (bioelectric, segmented, and cross linked). Ion textured microtensile specimens of each material except UHMW polyethylene and UHMW polyethylene with 10% carbon fibers were used to determine the effect of ion texturing on tensile properties. Scanning electron microscopy was used to determine surface morphology changes, and electron spectroscopy for chemical analysis was used to analyze the near surface chemical changes that result from ion texturing. Ion energies of 500 eV with beam current densities ranging from 0.08 to 0.19 mA/sq cm were used to ion texture the various materials. Standard microtensile specimens of seven polymers were exposed to a saline environment for 24 hours prior to and during the tensile testing. The surface chemical changes resulting from sputter etching are minimal in spite of the often significant changes in the surface morphology.

  3. Correlation between surface properties and wettability of multi-scale structured biocompatible surfaces

    NASA Astrophysics Data System (ADS)

    Gorodzha, S. N.; Surmeneva, M. A.; Prymak, O.; Wittmar, A.; Ulbricht, M.; Epple, M.; Teresov, A.; Koval, N.; Surmenev, R. A.

    2015-11-01

    The influence of surface properties of radio-frequency (RF) magnetron deposited hydroxyapatite (HA) and Si-containing HA coatings on wettability was studied. The composition and morphology of the coatings fabricated on titanium (Ti) were characterized using atomic force microscopy (AFM) and X-ray diffraction (XRD). The surface wettability was studied using contact angle analysis. Different geometric parameters of acid-etched (AE) and pulse electron beam (PEB)-treated Ti substrates and silicate content in the HA films resulted in the different morphology of the coatings at micro- and nano- length scales. Water contact angles for the HA coated Ti samples were evaluated as a combined effect of micro roughness of the substrate and nano-roughness of the HA films resulting in higher water contact angles compared with acid-etched (AE) or pulse electron beam (PEB) treated Ti substrates.

  4. Fabrication of low reflective nanopore-type black Si layer using one-step Ni-assisted chemical etching for Si solar cell application

    NASA Astrophysics Data System (ADS)

    Takaloo, AshkanVakilipour; Kolahdouz, Mohammadreza; Poursafar, Jafar; Es, Firat; Turan, Rasit; Ki-Joo, Seung

    2018-03-01

    Nanotextured Si fabricated through metal-assisted chemical etching (MACE) technique exhibits a promising potential for producing antireflective layer for photovoltaic (PV) application. In this study, a novel single-step nickel (Ni) assisted etching technique was applied to produce an antireflective, nonporous Si (black Si) in an aqueous solution containing hydrofluoric acid (HF), hydrogen peroxide (H2O2) and NiSO4 at 40 °C. Field emission scanning electron microscope was used to characterize different morphologies of the textured Si. Optical reflection measurements of samples were carried out to compare the reflectivity of different morphologies. Results indicated that vertical as well as horizontal pores with nanosized diameters were bored in the Si wafer after 1 h treatment in the etching solution containing different molar ratios of H2O2 to HF. Increasing H2O2 concentration in electrochemical etching solution had a considerable influence on the morphology due to higher injection of positive charges from Ni atoms onto the Si surface. Optimized concentration of H2O2 led to formation of an antireflective layer with 2.1% reflectance of incident light.

  5. Modification of Patterned Nanoporous Gold Thin Film Electrodes via Electro-annealing and Electrochemical Etching

    NASA Astrophysics Data System (ADS)

    Dorofeeva, Tatiana

    Nanostructured materials have had a major impact on various fields, including medicine, catalysis, and energy storage, for the major part due to unique phenomena that arise at nanoscale. For this reason, there is a sustained need for new nanostructured materials, techniques to pattern them, and methods to precisely control their nanostructure. To that end, the primary focus of this dissertation is to demonstrate novel techniques to fabricate and tailor the morphology of a class of nanoporous metals, obtained by a process known as dealloying. In this process, while the less noble constituent of an alloy is chemically dissolved, surface-diffusion of the more noble constituent leads to self-assembly of a bicontinuous ligament network with characteristic porosity of ˜70% and ligament diameter of 10s of nanometers. As a model material produced by dealloying, this work employ nanoporous gold (np-Au), which has attracted significant attention of desirable features, such as high effective surface area, electrical conductivity, well-defined thiol-based surface modification strategies, microfabrication-compatibility, and biocompatibility. The most commonly method used to modify the morphology of np-Au is thermal treatment, where the enhanced diffusivity of the surface atoms leads to ligament (and consequently pore) coarsening. This method, however, is not conducive to modifying the morphology of thin films at specific locations on the film, which is necessary for creating devices that may need to contain different morphologies on a single device. In addition, coarsening attained by thermal treatment also leads to an undesirable reduction in effective surface area. In response to these challenges, this work demonstrates two different techniques that enables in situ modification of np-Au thin film electrodes obtained by sputter-deposition of a precursors silver-rich gold-silver alloy. The first method, referred to as electro-annealing, is achieved by injecting electrical current to np-Au electrodes, which leads coarsening due to a combination of Joule heating and other mechanisms. This method offers the capability to anneal different electrodes to varying degrees of coarsening in one step, by employing electrodes patterns with different cross-sectional areas - easily attained since np-Au can be patterned into arbitrary shapes via photolithography - to control electrode resistivity, thus current density and the amount of electro-annealing of an electrode. A surprising finding was that electro-annealing lead to electrode coarsening at much lower temperatures than conventional thermal treatment, which was attributed to augmented electron-surface atom interactions at high current densities that may in turn enhance surface atom diffusivity. A major advantage of electro-annealing is the ability to monitor the resistance change of the electrode (surrogate for electrode morphology) in real-time and vary the electro-annealing current accordingly to establish a closed-loop electro-annealing configuration. In nanostructured materials, the electrical resistance is often a function of nanostructure, thus changes in resistance can be directly linked to morphological changes of the electrode. Examination of the underlying mechanisms of nanostructure-dependent resistance change revealed that both ligament diameter and grain size play a role in dictating the observed electrode resistance change. The second method relies on electrochemical etching of ligaments to modify electrode morphology in order to maintain both a high effective surface area and large pores for unhindered transport of molecules to/from the ligament surfaces - an important consideration for many physico-chemical processes, such fuel cells, electrochemical sensors, and drug delivery platforms. The advantage of this method over purely chemical approach is that while an entire sample in exposed to the chemical reagent, the etching process does not occur until the necessary electrochemical potential is applied. Similar to the electro-annealing methods, electrical addressability allows for differentially modifying the morphology individual electrodes on a single substrate. The results of this study also revealed that electrochemical etching is a combination of coarsening and etching processes, where the optimization of etching parameters makes it possible precisely control the etching by favoring one process over the other. In summary, the two techniques, taken together in combination with np-Au's compatibility with microfabrication processes, can be extended to create multiple electrode arrays that display different morphologies for studying structure?property relationships and tuning catalysts/sensors for optimal performance.

  6. Fabrication of micro-patterned aluminum surfaces for low ice adhesion strength

    NASA Astrophysics Data System (ADS)

    Jeon, Jaehyeon; Jang, Hanmin; Chang, Jinho; Lee, Kwan-Soo; Kim, Dong Rip

    2018-05-01

    We report a fabrication method to obtain a low-ice-adhesion aluminum surface by surface texturing using solution etching and subsequent thin-film coating. Specifically, the textured surface has microstructures of a low aspect ratio, that is, with a much smaller height than width. Such microstructures can effectively reduce ice-adhesion strengths by sliding the ice during detachment. Because our method is based on solution etching, it can be applied to curved surfaces with complex shapes for uniformly constructing the morphology of a low-ice-adhesion aluminum surface. Finally, the low-ice-adhesion aluminum surface reduces the ice-adhesion strengths by up to 95%.

  7. Etching of germanium-tin using ammonia peroxide mixture

    NASA Astrophysics Data System (ADS)

    Dong, Yuan; Ong, Bin Leong; Wang, Wei; Zhang, Zheng; Pan, Jisheng; Gong, Xiao; Tok, Eng-Soon; Liang, Gengchiau; Yeo, Yee-Chia

    2015-12-01

    The wet etching of germanium-tin (Ge1-xSnx) alloys (4.2% < x < 16.0%) in ammonia peroxide mixture (APM) is investigated. Empirical fitting of the data points indicates that the etch depth of Ge1-xSnx is proportional to the square root of the etch time t and decreases exponentially with increasing x for a given t. In addition, X-ray photoelectron spectroscopy results show that increasing t increases the intensity of the Sn oxide peak, whereas no obvious change is observed for the Ge oxide peak. This indicates that an accumulation of Sn oxide on the Ge1-xSnx surface decreases the amount of Ge atoms exposed to the etchant, which accounts for the decrease in etch rate with increasing etch time. Atomic force microscopy was used to examine the surface morphologies of the Ge0.918Sn0.082 samples. Both root-mean-square roughness and undulation periods of the Ge1-xSnx surface were observed to increase with increasing t. This work provides further understanding of the wet etching of Ge1-xSnx using APM and may be used for the fabrication of Ge1-xSnx-based electronic and photonic devices.

  8. A study of GaN-based LED structure etching using inductively coupled plasma

    NASA Astrophysics Data System (ADS)

    Wang, Pei; Cao, Bin; Gan, Zhiyin; Liu, Sheng

    2011-02-01

    GaN as a wide band gap semiconductor has been employed to fabricate optoelectronic devices such as light-emitting diodes (LEDs) and laser diodes (LDs). Recently several different dry etching techniques for GaN-based materials have been developed. ICP etching is attractive because of its superior plasma uniformity and strong controllability. Most previous reports emphasized on the ICP etching characteristics of single GaN film. In this study dry etching of GaN-based LED structure was performed by inductively coupled plasmas (ICP) etching with Cl2 as the base gas and BCl3 as the additive gas. The effects of the key process parameters such as etching gases flow rate, ICP power, RF power and chamber pressure on the etching properties of GaN-based LED structure including etching rate, selectivity, etched surface morphology and sidewall was investigated. Etch depths were measured using a depth profilometer and used to calculate the etch rates. The etch profiles were observed with a scanning electron microscope (SEM).

  9. Preparation of composite micro/nano structure on the silicon surface by reactive ion etching: Enhanced anti-reflective and hydrophobic properties

    NASA Astrophysics Data System (ADS)

    Zeng, Yu; Fan, Xiaoli; Chen, Jiajia; He, Siyu; Yi, Zao; Ye, Xin; Yi, Yougen

    2018-05-01

    A silicon substrate with micro-pyramid structure (black silicon) is prepared by wet chemical etching and then subjected to reactive ion etching (RIE) in the mixed gas condition of SF6, CHF3 and He. We systematically study the impacts of flow rates of SF6, CHF3 and He, the etching pressure and the etching time on the surface morphology and reflectivity through various characterizations. Meanwhile, we explore and obtain the optimal combination of parameters for the preparation of composite structure that match the RIE process based on the basis of micro-pyramid silicon substrate. The composite sample prepared under the optimum parameters exhibits excellent anti-reflective performance, hydrophobic, self-cleaning and anti-corrosive properties. Based on the above characteristics, the composite micro/nano structure can be applied to solar cells, photodetectors, LEDs, outdoor devices and other important fields.

  10. Reduction of structural defects in thick 4H-SiC epitaxial layers grown on 4° off-axis substrates

    NASA Astrophysics Data System (ADS)

    Yazdanfar, M.; Ivanov, I. G.; Pedersen, H.; Kordina, O.; Janzén, E.

    2013-06-01

    By carefully controlling the surface chemistry of the chemical vapor deposition process for silicon carbide (SiC), 100 μm thick epitaxial layers with excellent morphology were grown on 4° off-axis SiC substrates at growth rates exceeding 100 μm/h. In order to reduce the formation of step bunching and structural defects, mainly triangular defects, the effect of varying parameters such as growth temperature, C/Si ratio, Cl/Si ratio, Si/H2 ratio, and in situ pre-growth surface etching time are studied. It was found that an in-situ pre growth etch at growth temperature and pressure using 0.6% HCl in hydrogen for 12 min reduced the structural defects by etching preferentially on surface damages of the substrate surface. By then applying a slightly lower growth temperature of 1575 °C, a C/Si ratio of 0.8, and a Cl/Si ratio of 5, 100 μm thick, step-bunch free epitaxial layer with a minimum triangular defect density and excellent morphology could be grown, thus enabling SiC power device structures to be grown on 4° off axis SiC substrates.

  11. Morphological Evaluation of the Adhesive/Enamel interfaces of Two-step Self-etching Adhesives and Multimode One-bottle Self-etching Adhesives.

    PubMed

    Sato, Takaaki; Takagaki, Tomohiro; Matsui, Naoko; Hamba, Hidenori; Sadr, Alireza; Nikaido, Toru; Tagami, Junji

    To evaluate the acid-base resistant zone (ABRZ) at the adhesive/enamel interface of self-etching adhesives with or without prior phosphoric acid etching. Four adhesives were used in 8 groups: Clearfil SE Bond (SEB), Optibond XTR (XTR), Scotchbond Universal Adhesive (SBU), and Clearfil BOND SE ONE (ONE) without prior phosphoric-acid etching, and each adhesive with phosphoric acid etching for 10 s (P-SEB, P-XTR, P-SBU and P-ONE, respectively). After application of self-etching adhesives on ground enamel surfaces of human teeth, a flowable composite was placed. For observation of the acid-base resistant zone (ABRZ), the bonded interface was exposed to demineralizing solution (pH 4.5) for 4.5 h, followed by 5% NaOCl with ultrasonication for 20 min. After the acid-base challenge, morphological attributes of the interface were observed using SEM. ABRZ formation was confirmed in all groups. The funnel-shaped erosion beneath the interface was present in SBU and ONE, where nearly 10 to 15 μm of enamel was dissolved. With phosphoric acid etching, the ABRZs were obviously thicker compared with no phosphoric acid etching. Enamel beneath the bonding interface was more susceptible to acid dissolution in SBU and ONE. In the case of the one-bottle self-etching adhesives and universal adhesives that intrinsically have higher pH values, enamel etching should be recommended to improve the interfacial quality.

  12. The effect of different chemical agents on human enamel: an atomic force and scanning electron microscopy study

    NASA Astrophysics Data System (ADS)

    Rominu, Roxana O.; Rominu, Mihai; Negrutiu, Meda Lavinia; Sinescu, Cosmin; Pop, Daniela; Petrescu, Emanuela

    2010-12-01

    PURPOSE: The goal of our study was to investigate the changes in enamel surface roughess induced by the application of different chemical substances by atomic force microscopy and scanning electron microscopy. METHOD: Five sound human first upper premolar teeth were chosen for the study. The buccal surface of each tooth was treated with a different chemical agent as follows: Sample 1 - 38% phosphoric acid etching (30s) , sample 2 - no surface treatment (control sample), 3 - bleaching with 37.5 % hydrogen peroxide (according to the manufacturer's instructions), 4 - conditioning with a self-etching primer (15 s), 5 - 9.6 % hydrofluoric acid etching (30s). All samples were investigated by atomic force microscopy in a non-contact mode and by scanning electron microscopy. Several images were obtained for each sample, showing evident differences regarding enamel surface morphology. The mean surface roughness and the mean square roughness were calculated and compared. RESULTS: All chemical substances led to an increased surface roughness. Phosphoric acid led to the highest roughness while the control sample showed the lowest. Hydrofluoric acid also led to an increase in surface roughness but its effects have yet to be investigated due to its potential toxicity. CONCLUSIONS: By treating the human enamel with the above mentioned chemical compounds a negative microretentive surface is obtained, with a morphology depending on the applied substance.

  13. Effects of a non-rinse conditioner on the enamel of primary teeth.

    PubMed

    Fava, Marcelo; Myaki, Silvio Issáo; Arana-Chavez, Victor Elias; Fava-de-Moraes, Flavio

    2003-01-01

    The aim of this in vitro study was to evaluate by scanning electron microscopy the morphological aspects of the enamel of primary teeth after etching with 36% phosphoric acid or a non-rinse conditioner. Ten naturally exfoliated anterior primary teeth were selected. The samples were subjected to prophylaxis with pumice paste and water using a low-speed hand piece. Etching was done on the buccal surface. Specimens were divided into 2 groups: G1 (n=10): etching with 36% phosphoric acid gel - Conditioner 36 (Dentsply) for 20 s, followed by water rinse for 15 s; G2 (n=10): etching with NRC - Non Rinse Conditioner (Dentsply) for 20 s, followed by air drying for 15 s. The samples were dehydrated, mounted on metal stubs, coated with gold and observed with Jeol JSM-6100 scanning electron microscope. Electron-micrographic analysis showed that both etching agents were effective for etching the enamel of primary teeth causing the formation of microporosities on the enamel surface, although the etching pattern was more effective with the use of 36% phosphoric acid gel.

  14. Electrodeposited Ni nanowires-track etched P.E.T. composites as selective solar absorbers

    NASA Astrophysics Data System (ADS)

    Lukhwa, R.; Sone, B.; Kotsedi, L.; Madjoe, R.; Maaza, M.

    2018-05-01

    This contribution reports on the structural, optical and morphological properties of nanostructured flexible solar-thermal selective absorber composites for low temperature applications. The candidate material in the system is consisting of electrodeposited nickel nano-cylinders embedded in track-etched polyethylene terephthalate (PET) host membrane of pore sizes ranging between 0.3-0.8µm supported by conductive nickel thin film of about 0.5µm. PET were irradiated with 11MeV/u high charged xenon (Xe) ions at normal incidence. The tubular and metallic structure of the nickel nano-cylinders within the insulator polymeric host forms a typical ceramic-metal nano-composite "Cermet". The produced material was characterized by the following techniques: X-ray diffraction (XRD) for structural characterization to determine preferred crystallographic structure, and grain size of the materials; Scanning electron microscopy (SEM) to determine surface morphology, particle size, and visual imaging of distribution of structures on the surface of the substrate; Atomic force microscopy (AFM) to characterize surface roughness, surface morphology, and film thickness, and UV-Vis-NIR spectrophotometer to measure the reflectance, then to determine solar absorption

  15. Facile method for preparing superoleophobic surfaces with hierarchical microcubic/nanowire structures

    NASA Astrophysics Data System (ADS)

    Kwak, Wonshik; Hwang, Woonbong

    2016-02-01

    To facilitate the fabrication of superoleophobic surfaces having hierarchical microcubic/nanowire structures (HMNS), even for low surface tension liquids including octane (surface tension = 21.1 mN m-1), and to understand the influences of surface structures on the oleophobicity, we developed a convenient method to achieve superoleophobic surfaces on aluminum substrates using chemical acid etching, anodization and fluorination treatment. The liquid repellency of the structured surface was validated through observable experimental results the contact and sliding angle measurements. The etching condition required to ensure high surface roughness was established, and an optimal anodizing condition was determined, as a critical parameter in building the superoleophobicity. The microcubic structures formed by acid etching are essential for achieving the formation of the hierarchical structure, and therefore, the nanowire structures formed by anodization lead to an enhancement of the superoleophobicity for low surface tension liquids. Under optimized morphology by microcubic/nanowire structures with fluorination treatment, the contact angle over 150° and the sliding angle less than 10° are achieved even for octane.

  16. Cl 2-based dry etching of the AlGaInN system in inductively coupled plasmas

    NASA Astrophysics Data System (ADS)

    Cho, Hyun; Vartuli, C. B.; Abernathy, C. R.; Donovan, S. M.; Pearton, S. J.; Shul, R. J.; Han, J.

    1998-12-01

    Cl 2-Based inductively coupled plasmas with low additional d.c. self-biases (-100 V) produce convenient etch rates (500-1500 Å·min -1) for GaN, AlN, InN, InAlN and InGaN. A systematic study of the effects of additive gas (Ar, N 2, H 2), discharge composition and ICP source power and chuck power on etch rate and surface morphology has been performed. The general trends are to go through a maximum in etch rate with percent Cl 2 in the discharge for all three mixtures and to have an increase (decrease) in etch rate with source power (pressure). Since the etching is strongly ion-assisted, anisotropic pattern transfer is readily achieved. Maximum etch selectivities of approximately 6 for InN over the other nitrides were obtained.

  17. Morphological evolution and characterization of GaN pyramid arrays fabricated by photo-assisted chemical etching

    NASA Astrophysics Data System (ADS)

    Zhang, Shiying; Xiu, Xiangqian; Xu, Qingjun; Li, Yuewen; Hua, Xuemei; Chen, Peng; Xie, Zili; Liu, Bin; Zhou, Yugang; Han, Ping; Zhang, Rong; Zheng, Youdou

    2016-12-01

    GaN pyramid arrays have been successfully synthesized by selective photo-assisted chemical etching in a K2S2O8/KOH solution. A detailed analysis of time evolution of surface morphology has been conducted, which describes an etching process of GaN pyramids. Room temperature cathodoluminescence images indicate that these pyramids are composed of crystalline GaN surrounding dislocations, which is caused by the greater recombination rate of electrons and holes at dislocation than that of crystalline GaN. The Raman results show a stress relaxation in GaN pyramids compared with unetched GaN. The optical property of both unetched GaN and GaN pyramids has been studied by photoluminescence. The formation mechanism and feature of GaN pyramids are also rationally explained.

  18. Composition, morphology and surface recombination rate of HCl-isopropanol treated and vacuum annealed InAs(1 1 1)A surfaces

    NASA Astrophysics Data System (ADS)

    Kesler, V. G.; Seleznev, V. A.; Kovchavtsev, A. P.; Guzev, A. A.

    2010-05-01

    X-ray photoelectron spectroscopy and atomic force microscopy were used to examine the chemical composition and surface morphology of InAs(1 1 1)A surface chemically etched in isopropanol-hydrochloric acid solution (HCl-iPA) and subsequently annealed in vacuum in the temperature range 200-500 °C. Etching for 2-30 min resulted in the formation of "pits" and "hillocks" on the sample surface, respectively 1-2 nm deep and high, with lateral dimensions 50-100 nm. The observed local formations, whose density was up to 3 × 10 8 cm -2, entirely vanished from the surface after the samples were vacuum-annealed at temperatures above 300 °C. Using a direct method, electron beam microanalysis, we have determined that the defects of the hillock type includes oxygen and excessive As, while the "pits" proved to be identical in their chemical composition to InAs. Vacuum anneals were found to cause a decrease in As surface concentration relative to In on InAs surface, with a concomitant rise of surface recombination rate.

  19. Damage-Free Smooth-Sidewall InGaAs Nanopillar Array by Metal-Assisted Chemical Etching.

    PubMed

    Kong, Lingyu; Song, Yi; Kim, Jeong Dong; Yu, Lan; Wasserman, Daniel; Chim, Wai Kin; Chiam, Sing Yang; Li, Xiuling

    2017-10-24

    Producing densely packed high aspect ratio In 0.53 Ga 0.47 As nanostructures without surface damage is critical for beyond Si-CMOS nanoelectronic and optoelectronic devices. However, conventional dry etching methods are known to produce irreversible damage to III-V compound semiconductors because of the inherent high-energy ion-driven process. In this work, we demonstrate the realization of ordered, uniform, array-based In 0.53 Ga 0.47 As pillars with diameters as small as 200 nm using the damage-free metal-assisted chemical etching (MacEtch) technology combined with the post-MacEtch digital etching smoothing. The etching mechanism of In x Ga 1-x As is explored through the characterization of pillar morphology and porosity as a function of etching condition and indium composition. The etching behavior of In 0.53 Ga 0.47 As, in contrast to higher bandgap semiconductors (e.g., Si or GaAs), can be interpreted by a Schottky barrier height model that dictates the etching mechanism constantly in the mass transport limited regime because of the low barrier height. A broader impact of this work relates to the complete elimination of surface roughness or porosity related defects, which can be prevalent byproducts of MacEtch, by post-MacEtch digital etching. Side-by-side comparison of the midgap interface state density and flat-band capacitance hysteresis of both the unprocessed planar and MacEtched pillar In 0.53 Ga 0.47 As metal-oxide-semiconductor capacitors further confirms that the surface of the resultant pillars is as smooth and defect-free as before etching. MacEtch combined with digital etching offers a simple, room-temperature, and low-cost method for the formation of high-quality In 0.53 Ga 0.47 As nanostructures that will potentially enable large-volume production of In 0.53 Ga 0.47 As-based devices including three-dimensional transistors and high-efficiency infrared photodetectors.

  20. Highly roughened polycaprolactone surfaces using oxygen plasma-etching and in vitro mineralization for bone tissue regeneration: fabrication, characterization, and cellular activities.

    PubMed

    Kim, YongBok; Kim, GeunHyung

    2015-01-01

    Herein, poly(ɛ-caprolactone) (PCL) surfaces were treated to form various roughness values (R(a)=290-445 nm) and polar functional groups on the surfaces using a plasma-etching process, followed by immersion into simulated body fluid (SBF) for apatite formation. The surface morphology, chemical composition, and mean roughness of the plasma-etched PCL surfaces were measured, and various physical and morphological properties (water contact angles, protein absorption ability, and crystallite size of the apatite layer) of the in vitro mineralized PCL surfaces were evaluated. The roughened PCL surface P-3, which was treated with a sufficient plasma exposure time (4 h), achieved homogeneously distributed apatite formation after soaking in SBF for 7 days, as compared with other surfaces that were untreated or plasma-treated for 30 min or 2 h. Furthermore, to demonstrate their feasibility as a biomimetic surface, pre-osteoblast cells (MC3T3-E1) were cultured on the mineralized PCL surfaces, and cell viability, DAPI-phalloidin fluorescence assay, and alizarin red-staining of the P-3 surface were highly improved compared to the P-1 surface treated with a 30-min plasma exposure time; compared to untreated mineralized PCL surface (N-P), P-3 showed even greater improvements in cell viability and DAPI-phalloidin fluorescence assay. Based on these results, we found that the mineralized PCL surface supplemented with the appropriate plasma treatment can be implicitly helpful to achieve rapid hard tissue regeneration. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. Porosity and thickness effect of porous silicon layer on photoluminescence spectra

    NASA Astrophysics Data System (ADS)

    Husairi, F. S.; Eswar, K. A.; Guliling, Muliyadi; Khusaimi, Z.; Rusop, M.; Abdullah, S.

    2018-05-01

    The porous silicon nanostructures was prepared by electrochemical etching of p-type silicon wafer. Porous silicon prepared by using different current density and fix etching time with assistance of halogen lamp. The physical structure of porous silicon measured by the parameters used which know as experimental factor. In this work, we select one of those factors to correlate which optical properties of porous silicon. We investigated the surface morphology by using Surface Profiler (SP) and photoluminescence using Photoluminescence (PL) spectrometer. Different physical characteristics of porous silicon produced when current density varied. Surface profiler used to measure the thickness of porous and the porosity calculated using mass different of silicon. Photoluminescence characteristics of porous silicon depend on their morphology because the size and distribution of pore its self will effect to their exciton energy level. At J=30 mA/cm2 the shorter wavelength produced and it followed the trend of porosity with current density applied.

  2. Morphologies and optical and electrical properties of InGaN/GaN micro-square array light-emitting diode chips.

    PubMed

    Han, Dan; Ma, Shufang; Jia, Zhigang; Liu, Peizhi; Jia, Wei; Shang, Lin; Zhai, Guangmei; Xu, Bingshe

    2018-04-10

    InGaN/GaN micro-square array light-emitting diode (LED) chips (micro-chips) have been prepared via the focused ion beam (FIB) etching technique, which can not only reduce ohmic contact degradation but also control the aspect ratio precisely in three-dimensional (3D) structure LED (3D-LED) device fabrication. The effects of FIB beam current and micro-square array depth on morphologies and optical and electrical properties of the micro-chips have been studied. Our results show that sidewall surface morphology and optical and electrical properties of the micro-chips degrade with increased beam current. After potassium hydroxide etching with different times, an optimal current-voltage and luminescence performance can be obtained. Combining the results of cathodoluminescence mappings and light output-current characteristics, the light extraction efficiency of the micro-chips is reduced as FIB etch depth increases. The mechanisms of micro-square depth on light extraction have been revealed by 3D finite difference time domain.

  3. Gold surface plasmon crystal structure based-on polystyrene template for biosensor application.

    PubMed

    Cheng, Min-Zhuo; Zhang, Jing; Bao, Dequan; Huang, Xiwei

    2018-05-21

    In this communication, we assembled ordered polystyrene (PS) microsphere array as a template with the drop-coating method, and the oxygen plasma was used to etch the template to adjust the spacing between the PS microspheres. Nano-triangular gold array and silver nano-pyramid array were obtained by ion beam sputtering to deposit precious metal gold and silver. We observed the surface morphology of Au and Au/Ag composite films by scanning electron microscope and characterized the films by X-ray diffraction and ultraviolet/visible light spectrophotometer. The results show that the etching time of oxygen plasma has an obvious effect in adjusting the spacing between PSs and has a significant effect on the morphology of Au structure. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Hybrid silicon honeycomb/organic solar cells with enhanced efficiency using surface etching.

    PubMed

    Liu, Ruiyuan; Sun, Teng; Liu, Jiawei; Wu, Shan; Sun, Baoquan

    2016-06-24

    Silicon (Si) nanostructure-based photovoltaic devices are attractive for their excellent optical and electrical performance, but show lower efficiency than their planar counterparts due to the increased surface recombination associated with the high surface area and roughness. Here, we demonstrate an efficiency enhancement for hybrid nanostructured Si/polymer solar cells based on a novel Si honeycomb (SiHC) structure using a simple etching method. SiHC structures are fabricated using a combination of nanosphere lithography and plasma treatment followed by a wet chemical post-etching. SiHC has shown superior light-trapping ability in comparison with the other Si nanostructures, along with a robust structure. Anisotropic tetramethylammonium hydroxide etching not only tunes the final surface morphologies of the nanostructures, but also reduces the surface roughness leading to a lower recombination rate in the hybrid solar cells. The suppressed recombination loss, benefiting from the reduced surface-to-volume ratio and roughness, has resulted in a high open-circuit voltage of 600 mV, a short-circuit current of 31.46 mA cm(-2) due to the light-trapping ability of the SiHCs, and yields a power conversion efficiency of 12.79% without any other device structure optimization.

  5. Multiscale characterization of partially demineralized superficial and deep dentin surfaces.

    PubMed

    Pelin, Irina M; Trunfio-Sfarghiu, Ana-Maria; Farge, Pierre; Piednoir, Agnes; Pirat, Christophe; Ramos, Stella M M

    2013-08-01

    The objective of this study was to address the following question: 'Which properties are modified in partially demineralized surfaces, compared with non-demineralized dentin surfaces, following orthophosphoric acid-etching as performed in clinical procedures?'. For this purpose, the complementary techniques atomic force microscopy/spectroscopy, scanning electron microscopy, energy-dispersive X-ray spectroscopy, and contact angle measurements were used to provide a multiscale characterization of the dentin substrate undergoing the acidic preconditioning designed to enhance wetting. Special attention was given to the influence of the etching pretreatment on the nanomechanical properties at different levels of dentin surfaces, in both dry and hydrated conditions. The four-sided pyramid model (extended Hertz contact model) proved to be accurate for calculating the apparent Young's modulus, offering new information on the elasticity of dentin. The modulus value notably decreased following etching and surface hydration. This study underlines that after the acid etching pretreatment the contribution of the nanomechanical, morphological, and physicochemical modifications has a strong influence on the dentin adhesion properties and thus plays a significant role in the coupling of the adhesive-resin composite build-up material at the dentin surface. © 2013 Eur J Oral Sci.

  6. Surface roughness in XeF{sub 2} etching of a-Si/c-Si(100)

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Stevens, A.A.E.; Beijerinck, H.C.W.

    2005-01-01

    Single wavelength ellipsometry and atomic force microscopy (AFM) have been applied in a well-calibrated beam-etching experiment to characterize the dynamics of surface roughening induced by chemical etching of a {approx}12 nm amorphous silicon (a-Si) top layer and the underlying crystalline silicon (c-Si) bulk. In both the initial and final phase of etching, where either only a-Si or only c-Si is exposed to the XeF{sub 2} flux, we observe a similar evolution of the surface roughness as a function of the XeF{sub 2} dose proportional to D(XeF{sub 2}){sup {beta}} with {beta}{approx_equal}0.2. In the transition region from the pure amorphous to themore » pure crystalline silicon layer, we observe a strong anomalous increase of the surface roughness proportional to D(XeF{sub 2}){sup {beta}} with {beta}{approx_equal}1.5. Not only the growth rate of the roughness increases sharply in this phase, also the surface morphology temporarily changes to a structure that suggests a cusplike shape. Both features suggest that the remaining a-Si patches on the surface act effectively as a capping layer which causes the growth of deep trenches in the c-Si. The ellipsometry data on the roughness are corroborated by the AFM results, by equating the thickness of the rough layer to 6 {sigma}, with {sigma} the root-mean-square variation of the AFM's distribution function of height differences. In the AFM data, the anomalous behavior is reflected in a too small value of {sigma} which again suggests narrow and deep surface features that cannot be tracked by the AFM tip. The final phase morphology is characterized by an effective increase in surface area by a factor of two, as derived from a simple bilayer model of the reaction layer, using the experimental etch rate as input. We obtain a local reaction layer thickness of 1.5 monolayer consistent with the 1.7 ML value of Lo et al. [Lo et al., Phys. Rev. B 47, 648 (1993)] that is also independent of surface roughness.« less

  7. Etching of germanium-tin using ammonia peroxide mixture

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Dong, Yuan; Ong, Bin Leong; Wang, Wei

    The wet etching of germanium-tin (Ge{sub 1-x}Sn{sub x}) alloys (4.2% < x < 16.0%) in ammonia peroxide mixture (APM) is investigated. Empirical fitting of the data points indicates that the etch depth of Ge{sub 1-x}Sn{sub x} is proportional to the square root of the etch time t and decreases exponentially with increasing x for a given t. In addition, X-ray photoelectron spectroscopy results show that increasing t increases the intensity of the Sn oxide peak, whereas no obvious change is observed for the Ge oxide peak. This indicates that an accumulation of Sn oxide on the Ge{sub 1-x}Sn{sub x} surface decreases the amount ofmore » Ge atoms exposed to the etchant, which accounts for the decrease in etch rate with increasing etch time. Atomic force microscopy was used to examine the surface morphologies of the Ge{sub 0.918}Sn{sub 0.082} samples. Both root-mean-square roughness and undulation periods of the Ge{sub 1-x}Sn{sub x} surface were observed to increase with increasing t. This work provides further understanding of the wet etching of Ge{sub 1-x}Sn{sub x} using APM and may be used for the fabrication of Ge{sub 1-x}Sn{sub x}-based electronic and photonic devices.« less

  8. Improving Resonance Characteristics of Gas Sensors by Chemical Etching of Quartz Plates

    NASA Astrophysics Data System (ADS)

    Raicheva, Z.; Georgieva, V.; Grechnikov, A.; Gadjanova, V.; Angelov, Ts; Vergov, L.; Lazarov, Y.

    2012-12-01

    The paper presents the results of the influence of the etching process of AT-cut quartz plates on the resonance parameters and the QCM sensors. Quartz wafers (100 μm thick, with a diameter of 8 mm), divided into five groups, have been etched in [NH4]2 F2: H2O = 1:1 solution at temperatures in the range from 70°C to 90°C. The influence of etching temperature on the surface morphology of quartz wafers has been estimated by Atomic Force Microscopy (AFM). A correlation between the etching temperature and the dynamic characteristics is obtained. The optimal etching conditions for removing the surface damages caused by the mechanical treatment of the quartz wafers and for obtaining a clean surface were determined. The typical parameters of fabricated resonators on the quartz plates etched in the temperature range from 70°C to 90°C are as follows: Frequency, Fs 16 MHz ± 100 kHz Motional resistance, Rs less 10 Ω Motional inductance, Lq higher than 3 mH Motional capacitance, Cq less 30 fF Static capacitance, Co around 5 pF Quality factor, Q from 46 000 to 70 000 Sorption properties of QCM - MoO3 are evaluated at NH3 concentrations in the interval from 100 ppm to 500 ppm.

  9. Morphological and chemical characteristics of different titanium surfaces treated by bicarbonate and glycine powder air abrasive systems.

    PubMed

    Menini, Maria; Piccardo, Paolo; Baldi, Domenico; Dellepiane, Elena; Pera, Paolo

    2015-02-01

    This in vitro study investigated possible morphological and chemical changes induced by glycine or sodium bicarbonate powder air polishing on machined and acid-etched titanium surfaces. The glycine powder (granulometry <65 μm) and sodium bicarbonate powder (granulometry <150 μm) were applied on 2 machined healing abutments and on 2 acid-etched healing abutments. The samples were characterized by scanning electron microscopy coupled with energy dispersive x-ray spectroscopy. The analyses were performed at different steps: (1) as received, right after opening the abutment packaging; (2) after 20 minutes air exposure; (3) after aging in artificial saliva; (4) after glycine or sodium bicarbonate powder air polishing for 5 seconds; (5) after repetition of steps 3 and 4 with longer time of polishing (20 seconds). Air polishing using glycine and sodium bicarbonate powder seemed to be safe for professional oral hygiene of titanium dental implants, although acid-etched abutments and abutments treated with bicarbonate harbored more salts. This might indicate a greater plaque accumulation in a clinical situation. However, this result has to be investigated in vivo to understand its clinical relevance.

  10. Influence of the doping type and level on the morphology of porous Si formed by galvanic etching

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Pyatilova, O. V., E-mail: 5ilova87@gmail.com; Gavrilov, S. A.; Shilyaeva, Yu. I.

    The formation of porous silicon (por-Si) layers by the galvanic etching of single-crystal Si samples (doped with boron or phosphorus) in an HF/C{sub 2}H{sub 5}OH/H{sub 2}O{sub 2} solution is investigated. The por-Si layers are analyzed by the capillary condensation of nitrogen and scanning electron microscopy (SEM). The dependences of the morphological characteristics of por-Si (pore diameter, specific surface area, pore volume, and thickness of the pore walls), which determine the por-Si combustion kinetics, on the dopant type and initial wafer resistivity are established.

  11. Wet etching technique for fabrication of a high-quality plastic optical fiber sensor.

    PubMed

    Zhao, Mingfu; Dai, Lang; Zhong, Nianbing; Wang, Zhengkun; Chen, Ming; Li, Bingxin; Luo, Binbin; Tang, Bin; Shi, Shenghui; Song, Tao; Zou, Xue

    2017-11-01

    In this study, a simple wet etching technique is developed by employing aqueous solutions of acetic acid and ultrasonic irradiation for the fabrication of a high-quality plastic optical fiber (POF) sensor. The effects of acetic acid concentration and temperature and ultrasonic power on the etching rate and surface morphology of the etched POFs are investigated. The transmission spectrum and sensitivity of the etched POF sensors are evaluated using glucose solutions. We discovered that the POF sensors, which are fabricated using an aqueous solution of acetic acid with a concentration of 80 vol. % under an ultrasonic power of 130 W and temperature of 25°C, exhibit good light transmission and a high sensitivity of 9.10  [(RIU)(g/L)] -1 in the glucose solutions.

  12. Silicon macroporous arrays with high aspect ratio prepared by ICP etching

    NASA Astrophysics Data System (ADS)

    Wang, Guozheng; Yang, Bingchen; Wang, Ji; Yang, Jikai; Duanmu, Qingduo

    2018-02-01

    This paper reports on a macroporous silicon arrays with high aspect ratio, the pores of which are of 162, 205, 252, 276μm depths with 6, 10, 15 and 20 μm diameters respectively, prepared by Multiplex Inductively Coupled Plasma (ICP) etching. It was shown that there are very differences in process of high aspect ratio microstructures between the deep pores, a closed structure, and deep trenches, a open structure. The morphology and the aspect ratio dependent etching were analyzed and discussed. The macroporous silicon etched by ICP process yield an uneven, re-entrant, notched and ripples surface within the pores. The main factors effecting on the RIE lag of HARP etching are the passivation cycle time, the pressure of reactive chamber, and the platen power of ICP system.

  13. Effect of the addition of SF6 and N2 in inductively coupled SiCl4 plasma for GaN etching

    NASA Astrophysics Data System (ADS)

    Oubensaid, E. H.; Duluard, C. Y.; Pichon, L. E.; Pereira, J.; Boufnichel, M.; Lefaucheux, P.; Dussart, R.; Ranson, P.

    2009-07-01

    The GaN etching by SiCl4 plasma is considered in an ICP tool. By respecting some material limitations, it has been possible to etch the gallium nitride in pure SiCl4 plasma, with an etch rate of 19 nm min-1. This result is comparable to other reported results. Thereafter, the combination of SiCl4 with SF6 and N2 was tested in order to increase the etch rate. The addition of SF6 in the plasma has enabled us to reach an etch rate of 53 nm min-1. However, best results were obtained with the addition of N2, with an increase of the etch rate by a factor of 6. Mass spectrometry was also performed in order to determine the effects of the additional gases. The surface morphology of the GaN was also analysed by scanning electron microscope after etching.

  14. Tissue response to peritoneal implants

    NASA Technical Reports Server (NTRS)

    Picha, G. J.

    1980-01-01

    Peritoneal implants were fabricated from poly 2-OH, ethyl methacrylate (HEMA), polyetherurethane (polytetramethylene glycol 1000 MW, 1,4 methylene disocynate, and ethyl diamine), and untreated and sputter treated polytetrafluoroethylene (PTFE). The sputter treated PTFE implants were produced by an 8 cm diameter argon ion source. The treated samples consisted of ion beam sputter polished samples, sputter etched samples (to produce a microscopic surface cone texture) and surface pitted samples (produced by ion beam sputtering to result in 50 microns wide by 100 microns deep square pits). These materials were implanted in rats for periods ranging from 30 minutes to 14 days. The results were evaluated with regard to cell type and attachment kinetics onto the different materials. Scanning electron microscopy and histological sections were also evaluated. In general the smooth hydrophobic surfaces attracted less cells than the ion etched PTFE or the HEMA samples. The ion etching was observed to enhance cell attachment, multinucleated giant cell (MNGC) formation, cell to cell contact, and fibrous capsule formation. The cell responsed in the case of ion etched PTFE to an altered surface morphology. However, equally interesting was the similar attachment kinetics of HEMA verses the ion etched PTFE. However, HEMA resulted in a markedly different response with no MNGC's formation, minimal to no capsule formation, and sample coverage by a uniform cell layer.

  15. Effect of application mode on interfacial morphology and chemistry between dentin and self-etch adhesives

    PubMed Central

    Zhang, Ying; Wang, Yong

    2012-01-01

    Objective To investigate the influence of application mode on the interfacial morphology and chemistry between dentin and self-etch adhesives with different aggressiveness. Methods The occlusal one-third of the crown was removed from un-erupted human third molars, followed by abrading with 600 grit SiC under water. Rectangular dentin slabs were prepared by sectioning the tooth specimens perpendicular to the abraded surfaces. The obtained dentin slabs were treated with one of the two one-step self-etch adhesives: Adper Easy Bond (AEB, PH~2.5) and Adper Prompt L-Pop (APLP, PH~0.8) with (15s, active application) or without (15s, inactive application) agitation. The dentin slabs were fractured and the exposed adhesive/dentin (A/D) interfaces were examined with micro-Raman spectroscopy and scanning electron microscopy (SEM). Results The interfacial morphology, degree of dentin demineralization (DD) and degree of conversion (DC) of the strong self-etch adhesive APLP showed more significant dependence on the application mode than the mild AEB. APLP exhibited inferior bonding at the A/D interface if applied without agitation, evidenced by debonding from the dentin substrate. The DDs and DCs of the APLP with agitation were higher than those of without agitation in the interface, in contrast to the comparable DD and DC values of two AEB specimen groups with different application modes. Raman spectral analysis revealed the important role of chemical interaction between acid monomers of self-etch adhesives and dentin in the above observations. Conclusion The chemical interaction with dentin is especially important for improving the DC of the strong self-etching adhesive at the A/D interface. Agitation could benefit polymerization efficacy of the strong self-etch adhesive through enhancing the chemical interaction with tooth substrate. PMID:23153573

  16. Focused ion beam micromachining of TiNi film on Si( 1 1 1 )

    NASA Astrophysics Data System (ADS)

    Xie, D. Z.; Ngoi, B. K. A.; Ong, A. S.; Fu, Y. Q.; Lim, B. H.

    2003-11-01

    Having an excellent shape memory effect, titanium-nickel (TiNi) thin films are often used for fabrication of microactuators in microelectromechanical systems. In this work, the Ga + focused ion beam (FIB) etching characteristics of TiNi thin films has been investigated. The thin films were deposited on Si(1 1 1) wafers by co-sputtering NiTi and Ti targets using a magnetron-sputtering system. Some patterns have been etched on the surface of the films by FIB. Atomic force microscopy has been used to analyze the surface morphology of the etched areas. It is found that the etched depth depends linearly on the ion dose per area with a slope of 0.259 μm/(nC/μm 2). However, the etching depth decreases with increasing the ion beam current. The root-mean-square (RMS) surface roughness changes nonlinearly with ion dose and reaches a minimum of about 5.00 nm at a dose of about 0.45 nC/μm 2. The RMS decreases with increasing ion beam current and reaches about 4.00 nm as the ion beam current is increased to 2 nA.

  17. Morphology-Driven Control of Metabolite Selectivity Using Nanostructure-Initiator Mass Spectrometry

    DOE PAGES

    Gao, Jian; Louie, Katherine B.; Steinke, Philipp; ...

    2017-05-26

    Nanostructure-initiator mass spectrometry (NIMS) is a laser desorption/ionization analysis technique based on the vaporization of a nanostructure-trapped liquid "initiator" phase. Here we report an intriguing relationship between NIMS surface morphology and analyte selectivity. Scanning electron microscopy and spectroscopic ellipsometry were used to characterize the surface morphologies of a series of NIMS substrates generated by anodic electrochemical etching. Mass spectrometry imaging was applied to compare NIMS sensitivity of these various surfaces toward the analysis of diverse analytes. The porosity of NIMS surfaces was found to increase linearly with etching time where the pore size ranged from 4 to 12 nm withmore » corresponding porosities estimated to be 7-70%. Surface morphology was found to significantly and selectively alter NIMS sensitivity. The small molecule ( < 2k Da) sensitivity was found to increase with increased porosity, whereas low porosity had the highest sensitivity for the largest molecules examined. Estimation of molecular sizes showed that this transition occurs when the pore size is < 3× the maximum of molecular dimensions. While the origins of selectivity are unclear, increased signal from small molecules with increased surface area is consistent with a surface area restructuring-driven desorption/ionization process where signal intensity increases with porosity. In contrast, large molecules show highest signal for the low-porosity and small-pore-size surfaces. We attribute this to strong interactions between the initiator-coated pore structures and large molecules that hinder desorption/ionization by trapping large molecules. This finding may enable us to design NIMS surfaces with increased specificity to molecules of interest.« less

  18. Inductively Coupled Plasma and Electron Cyclotron Resonance Plasma Etching of InGaAlP Compound Semiconductor System

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Abernathy, C.R.; Hobson, W.S.; Hong, J.

    1998-11-04

    Current and future generations of sophisticated compound semiconductor devices require the ability for submicron scale patterning. The situation is being complicated since some of the new devices are based on a wider diversity of materials to be etched. Conventional IUE (Reactive Ion Etching) has been prevalent across the industry so far, but has limitations for materials with high bond strengths or multiple elements. IrI this paper, we suggest high density plasmas such as ECR (Electron Cyclotron Resonance) and ICP (Inductively Coupled Plasma), for the etching of ternary compound semiconductors (InGaP, AIInP, AlGaP) which are employed for electronic devices like heterojunctionmore » bipolar transistors (HBTs) or high electron mobility transistors (HEMTs), and photonic devices such as light-emitting diodes (LEDs) and lasers. High density plasma sources, opeiating at lower pressure, are expected to meet target goals determined in terms of etch rate, surface morphology, surface stoichiometry, selectivity, etc. The etching mechanisms, which are described in this paper, can also be applied to other III-V (GaAs-based, InP-based) as well as III-Nitride since the InGaAIP system shares many of the same properties.« less

  19. Morphological Study on Porous Silicon Carbide Membrane Fabricated by Double-Step Electrochemical Etching

    NASA Astrophysics Data System (ADS)

    Omiya, Takuma; Tanaka, Akira; Shimomura, Masaru

    2012-07-01

    The structure of porous silicon carbide membranes that peeled off spontaneously during electrochemical etching was studied. They were fabricated from n-type 6H SiC(0001) wafers by a double-step electrochemical etching process in a hydrofluoric electrolyte. Nanoporous membranes were obtained after double-step etching with current densities of 10-20 and 60-100 mA/cm2 in the first and second steps, respectively. Microporous membranes were also fabricated after double-step etching with current densities of 100 and 200 mA/cm2. It was found that the pore diameter is influenced by the etching current in step 1, and that a higher current is required in step 2 when the current in step 1 is increased. During the etching processes in steps 1 and 2, vertical nanopore and lateral crack formations proceed, respectively. The influx pathway of hydrofluoric solution, expansion of generated gases, and transfer limitation of positive holes to the pore surface are the key factors in the peeling-off mechanism of the membrane.

  20. Bioactive Surface Modification of Hydroxyapatite

    PubMed Central

    Okazaki, Yohei; Hiasa, Kyou; Yasuda, Keisuke; Nogami, Keisuke; Mizumachi, Wataru; Hirata, Isao

    2013-01-01

    The purpose of this study was to establish an acid-etching procedure for altering the Ca/P ratio of the nanostructured surface of hydroxyapatite (HAP) by using surface chemical and morphological analyses (XPS, XRD, SEM, surface roughness, and wettability) and to evaluate the in vitro response of osteoblast-like cells (MC3T3-E1 cells) to the modified surfaces. This study utilized HAP and HAP treated with 10%, 20%, 30%, 40%, 50%, or 60% phosphoric acid solution for 10 minutes at 25°C, followed by rinsing 3 times with ultrapure water. The 30% phosphoric acid etching process that provided a Ca/P ratio of 1.50, without destruction of the grain boundary of HAP, was selected as a surface-modification procedure. Additionally, HAP treated by the 30% phosphoric acid etching process was stored under dry conditions at 25°C for 12 hours, and the Ca/P ratio approximated to 1.00 accidentally. The initial adhesion, proliferation, and differentiation (alkaline phosphatase (ALP) activity and relative mRNA level for ALP) of MC3T3-E1 cells on the modified surfaces were significantly promoted (P < 0.05 and 0.01). These findings show that the 30% phosphoric acid etching process for the nanostructured HAP surface can alter the Ca/P ratio effectively and may accelerate the initial adhesion, proliferation, and differentiation of MC3T3-E1 cells. PMID:23862150

  1. Morphological and chemical characterization of the dentin/resin cement interface produced with a self-etching primer.

    PubMed

    Walker, Mary P; Wang, Yong; Spencer, Paulette

    2002-01-01

    The purpose of this study was to analyze a resin cement/dentin interface by comparing the diffusion of a resin cement into dentin surfaces pretreated with a self-etching primer with or without pretreatment by conventional acid etching. Dentin surfaces of 8 unerupted human third molars were treated with a self-etch primer (Panavia 21) with or without conventional phosphoric acid pretreatment. Panavia 21 resin cement was applied according to manufacturer's instructions. Dentin/resin cement interface sections from each tooth were examined with scanning electron microscopy and micro-Raman spectroscopy. When the self-etch primer was used following conventional acid pretreatment, the resin cement did not penetrate to the depth of the zone of demineralized dentin, leaving a substantial area of exposed dentin matrix at the dentin/cement interface. In contrast, there was substantial resin cement diffusion throughout the demineralized dentin when the self-etch primer was used without acid etching pretreatment. The in vitro evaluation of resin cement penetration throughout the zone of demineralized dentin is an important step in identifying sites of exposed dentin matrix that may promote postoperative sensitivity and may leave the dentin/resin cement interface vulnerable to premature degradation under clinical conditions. In this study, the self-etch primer used alone produced substantial resin cement penetration and left no exposed dentin matrix at the dentin/resin cement interface.

  2. Catalyst and processing effects on metal-assisted chemical etching for the production of highly porous GaN

    NASA Astrophysics Data System (ADS)

    Geng, Xuewen; Duan, Barrett K.; Grismer, Dane A.; Zhao, Liancheng; Bohn, Paul W.

    2013-06-01

    Metal-assisted chemical etching is a facile method to produce micro-/nanostructures in the near-surface region of gallium nitride (GaN) and other semiconductors. Detailed studies of the production of porous GaN (PGaN) using different metal catalysts and GaN doping conditions have been performed in order to understand the mechanism by which metal-assisted chemical etching is accomplished in GaN. Patterned catalysts show increasing metal-assisted chemical etching activity to n-GaN in the order Ag < Au < Ir < Pt. In addition, the catalytic behavior of continuous films is compared to discontinuous island films. Continuous metal films strongly shield the surface, hindering metal-assisted chemical etching, an effect which can be overcome by using discontinuous films or increasing the irradiance of the light source. With increasing etch time or irradiance, PGaN morphologies change from uniform porous structures to ridge and valley structures. The doping type plays an important role, with metal-assisted chemical etching activity increasing in the order p-GaN < intrinsic GaN < n-GaN. Both the catalyst identity and the doping type effects are explained by the work functions and the related band offsets that affect the metal-assisted chemical etching process through a combination of different barriers to hole injection and the formation of hole accumulation/depletion layers at the metal-semiconductor interface.

  3. Preparation of superhydrophobic titanium surfaces via electrochemical etching and fluorosilane modification

    NASA Astrophysics Data System (ADS)

    Lu, Yao; Xu, Wenji; Song, Jinlong; Liu, Xin; Xing, Yingjie; Sun, Jing

    2012-12-01

    The preparation of superhydrophobic surfaces on hydrophilic metal substrates depends on both surface microstructures and low surface energy modification. In this study, a simple and inexpensive electrochemical method for preparing robust superhydrophobic titanium surfaces is reported. The neutral sodium chloride solution is used as electrolyte. Fluoroalkylsilane (FAS) was used to reduce the surface energy of the electrochemically etched surface. Scanning electron microscopy (SEM) images, energy-dispersive spectroscopy (EDS), Fourier transform infrared spectroscopy (FTIR) spectra, and contact angle measurement are performed to characterize the morphological features, chemical composition, and wettability of the titanium surfaces. Stability and friction tests indicate that the prepared titanium surfaces are robust. The analysis of electrolyte, reaction process, and products demonstrates that the electrochemical processing is very inexpensive and environment-friendly. This method is believed to be easily adaptable for use in large-scale industry productions to promote the application of superhydrophobic titanium surfaces in aviation, aerospace, shipbuilding, and the military industry.

  4. Correlation between optical properties surface morphology of porous silicon electrodeposited by Fe3+ ion

    NASA Astrophysics Data System (ADS)

    Mabrouk, Asma; Lorrain, N.; Haji, M. L.; Oueslati, Meherzi

    2015-01-01

    In this paper, we analyze the photoluminescence spectra (PL) of porous silicon (PS) layer which is elaborated by electrochemical etching and passivated by Fe3+ ions (PSF) via current density, electro-deposition and temperature measurements. We observe unusual surface morphology of PSF surface and anomalous emission behavior. The PSF surface shows regular distribution of cracks, leaving isolated regions or ;platelets; of nearly uniform thickness. These cracks become more pronounced for high current densities. The temperature dependence of the PL peak energy (EPL) presents anomalous behaviors, i.e., the PL peak energy shows a successive red/blue/redshift (S-shaped behavior) with increasing temperature that we attribute to the existence of strong potential fluctuations induced by the electrochemical etching of PS layers. A competition process between localized and delocalized excitons is used to discuss these PL properties. In this case, the potential confinement plays a key role on the enhancement of PL intensity in PSF. To explain the temperature dependence of the PL intensity, we have proposed a recombination model based on the tunneling and dissociation of excitons.

  5. Fabrication of Meso-Porous Sintered Metal Thin Films by Selective Etching of Silica Based Sacrificial Template

    PubMed Central

    Dumée, Ludovic F.; She, Fenghua; Duke, Mikel; Gray, Stephen; Hodgson, Peter; Kong, Lingxue

    2014-01-01

    Meso-porous metal materials have enhanced surface energies offering unique surface properties with potential applications in chemical catalysis, molecular sensing and selective separation. In this paper, commercial 20 nm diameter metal nano-particles, including silver and copper were blended with 7 nm silica nano-particles by shear mixing. The resulted powders were cold-sintered to form dense, hybrid thin films. The sacrificial silica template was then removed by selective etching in 12 wt% hydrofluoric acid solutions for 15 min to reveal a purely metallic meso-porous thin film material. The impact of the initial silica nano-particle diameter (7–20 nm) as well as the sintering pressure (5–20 ton·m−2) and etching conditions on the morphology and properties of the final nano-porous thin films were investigated by porometry, pyknometery, gas and liquid permeation and electron microscopy. Furthermore, the morphology of the pores and particle aggregation during shear mixing were assessed through cross-sectioning by focus ion beam milling. It is demonstrated that meso-pores ranging between 50 and 320 nm in average diameter and porosities up to 47% can be successfully formed for the range of materials tested. PMID:28344241

  6. A comparative study of different bleaching agents on the morphology of human enamel: an in vitro SEM study.

    PubMed

    Uthappa, Roshan; Suprith, M L; Bhandary, Shreetha; Dash, Sumit

    2012-11-01

    The purpose of the study was to compare two different commercial bleaching agents, Opalescence with Colgate Platinum, and 30% phosphoric acid used as aggressive agent on the morphology of human enamel. Ten freshly extracted, noncarious, human maxillary central incisors extracted for periodontal reasons were used in this study. The labial surface of the disinfected teeth were polished using a polishing paste with the help of rubber cup and a slow speed handpiece. Each tooth was sectioned at cement-enamel junction and the crown was separated into four specimens, all taken from labial surface. Group 1 was treated with Colgate Platinum for 7 hours, group 2 with Opalescence for 7 hours, group 3 was treated with 30% phosphoric acid for 30 seconds and group 4 was untreated and used as control. After the treatment period, the specimens were washed with normal saline and stored in sterile bottle and sealed. Photomicrographs obtained from the scanning electron microscopy (SEM) after surface treatments were examined for no alteration, slight alteration, moderate alteration and severe alterations. The specimens treated with commercial bleaching agents revealed no enamel surface morphologic alterations compared to control group. The specimen treated with phosphoric acid showed severe alterations. Ten percent carbamide peroxide evaluated in this study does not etch tooth enamel or alter enamel surface morphology as do conventional etching techniques. Carbamine peroxide is a safe and effective tooth whitening agent even when used for extended period of time. The enamel surface remains smooth which reduces caries due to plaque collection.

  7. Determination of the dissolution slowness surface by study of etched shapes I. Morphology of the dissolution slowness surface and theoretical etched shapes

    NASA Astrophysics Data System (ADS)

    Leblois, T.; Tellier, C. R.

    1992-07-01

    We propose a theoretical model for the anisotropic etching of crystals, in order to be applied in the micromachining. The originality of the model is due to the introduction of dissolution tensors to express the representative surface of the dissolution slowness. The knowledge of the equation of the slowness surface allows us to determine the trajectories of all the elements which compose the starting surface. It is then possible to construct the final etched shape by numerical simulation. Several examples are given in this paper which show that the final etched shapes are correlated to the extrema of the dissolution slowness. Since the slowness surface must be determined from experiments, emphasis is placed on difficulties encountered when we correlate theory to experiments. Nous avons modélisé le processus de dissolution anisotrope des cristaux en vue d'une application à la simulation des formes obtenues par photolithogravure chimique. La principale originalité de ce modèle tient à l'introduction de tenseurs de dissolution pour exprimer la surface représentative de la lenteur de dissolution. La connaissance de l'équation de la lenteur de dissolution permet de calculer les trajectoires des différents éléments constituant la surface de départ puis de reconstituer par simulation la forme dissoute. Les simulations démontrent que les formes limites des cristaux dissous sont corrélées aux extrema de la lenteur de dissolution. La détermination de la surface de la lenteur se faisant à partir de mesures expérimetales, nous nous sommes efforcés de montrer toutes les difficultés attachées à cette analyse.

  8. Performance of a new one-step multi-mode adhesive on etched vs non-etched enamel on bond strength and interfacial morphology.

    PubMed

    de Goes, Mario Fernando; Shinohara, Mirela Sanae; Freitas, Marcela Santiago

    2014-06-01

    To compare microtensile bond strength (μTBS) and interfacial morphology of a new one-step multimode adhesive with a two-step self-etching adhesive and two etch-and-rinse adhesives systems on enamel. Thirty human third molars were sectioned to obtain two enamel fragments. For μTBS, 48 enamel surfaces were ground using 600-grit SiC paper and randomly assigned into 6 groups (n = 8): nonetched Scotchbond Universal [SBU]; etched SBU [SBU-et]; non-etched Clearfil SE Bond [CSE]; etched CSE [CSE-et]; Scotchbond Multi-PURPOSE [SBMP]; Excite [EX]. The etched specimens were conditioned with 37% phosphoric acid for 30 s, each adhesive system was applied according to manufacturers' instructions, and composite resin blocks (Filtek Supreme Plus, 3M ESPE) were incrementally built up. Specimens were sectioned into beams with a cross-sectional area of 0.8-mm2 and tested under tension (1 mm/min). The data were analyzed with oneway ANOVA and Fisher's PLSD (α = 0.05). For interface analysis, two samples from each group were embedded in epoxy resin, polished, and then observed using scanning electron microscopy (SEM). The μTBS values (in MPa) and the standard deviations were: SBU = 27.4 (8.5); SBU-et = 33.6 (9.3); CSE = 28.5 (8.3); CSE-et = 34.2 (9.0); SBMP = 30.4 (11.0); EX = 23.3 (8.2). CSE-et and SBU-et presented the highest bond strength values, followed by SBMP, CSE, and SBU which did not differ significantly from each other. EX showed the statistically significantly lowest bond strength values. SEM images of interfaces from etched samples showed long adhesive-resin tags penetrating into demineralized enamel. Preliminary etching of enamel significantly increased bond strength for the new one-step multimode adhesive SBU and two-step self-etching adhesive CSE.

  9. SEM analysis of enamel surface treated by Er:YAG laser: influence of irradiation distance.

    PubMed

    Souza-Gabriel, A E; Chinelatti, M A; Borsatto, M C; Pécora, J D; Palma-Dibb, R G; Corona, S A M

    2008-07-01

    Depending on the distance of laser tip to dental surface a specific morphological pattern should be expected. However, there have been limited reports that correlate the Er:YAG irradiation distance with dental morphology. To assess the influence of Er:YAG laser irradiation distance on enamel morphology, by means of scanning electron microscopy (SEM). Sixty human third molars were employed to obtain discs (approximately =1 mm thick) that were randomly assigned to six groups (n=10). Five groups received Er:YAG laser irradiation (80 mJ/2 Hz) for 20 s, according to the irradiation distance: 11, 12, 14, 16, or 17 mm and the control group was treated with 37% phosphoric acid for 15 s. The laser-irradiated discs were bisected. One hemi-disc was separated for superficial analysis without subsequent acid etching, and the other one, received the phosphoric acid for 15 s. Samples were prepared for SEM. Laser irradiation at 11 and 12 mm provided an evident ablation of enamel, with evident fissures and some fused areas. At 14, 16 and 17 mm the superficial topography was flatter than in the other distances. The subsequent acid etching on the lased-surface partially removed the disorganized tissue. Er:YAG laser in defocused mode promoted slight morphological alterations and seems more suitable for enamel conditioning than focused irradiation. The application of phosphoric acid on lased-enamel surface, regardless of the irradiation distance, decreased the superficial irregularities.

  10. Synthesis and catalytic performance of SiO2@Ni and hollow Ni microspheres

    NASA Astrophysics Data System (ADS)

    Liu, Xin; Liu, Yanhua; Shi, Xueting; Yu, Zhengyang; Feng, Libang

    2016-11-01

    Nickel (Ni) catalyst has been widely used in catalytic reducing reactions such as catalytic hydrogenation of organic compounds and catalytic reduction of organic dyes. However, the catalytic efficiency of pure Ni is low. In order to improve the catalytic performance, Ni nanoparticle-loaded microspheres can be developed. In this study, we have prepared Ni nanoparticle-loaded microspheres (SiO2@Ni) and hollow Ni microspheres using two-step method. SiO2@Ni microspheres with raspberry-like morphology and core-shell structure are synthesized successfully using SiO2 microsphere as a template and Ni2+ ions are adsorbed onto SiO2 surfaces via electrostatic interaction and then reduced and deposited on surfaces of SiO2 microspheres. Next, the SiO2 cores are removed by NaOH etching and the hollow Ni microspheres are prepared. The NaOH etching time does no have much influence on the crystal structure, shape, and surface morphology of SiO2@Ni; however, it can change the phase composition evidently. The hollow Ni microspheres are obtained when the NaOH etching time reaches 10 h and above. The as-synthesized SiO2@Ni microspheres exhibit much higher catalytic performance than the hollow Ni microspheres and pure Ni nanoparticles in the catalytic reduction of methylene blue. Meanwhile, the SiO2@Ni catalyst has high stability and hence it can be recycled for reuse.

  11. Effect of different electrolytes on porous GaN using photo-electrochemical etching

    NASA Astrophysics Data System (ADS)

    Al-Heuseen, K.; Hashim, M. R.; Ali, N. K.

    2011-05-01

    This article reports the properties and the behavior of GaN during the photoelectrochemical etching process using four different electrolytes. The measurements show that the porosity strongly depends on the electrolyte and highly affects the surface morphology of etched samples, which has been revealed by scanning electron microscopy (SEM) images. Peak intensity of the photoluminescence (PL) spectra of the porous GaN samples was observed to be enhanced and strongly depend on the electrolytes. Among the samples, there is a little difference in the peak position indicating that the change of porosity has little influence on the PL peak shift, while it highly affecting the peak intensity. Raman spectra of porous GaN under four different solution exhibit phonon mode E 2 (high), A 1 (LO), A 1 (TO) and E 2 (low). There was a red shift in E 2 (high) in all samples, indicating a relaxation of stress in the porous GaN surface with respect to the underlying single crystalline epitaxial GaN. Raman and PL intensities were high for samples etched in H 2SO 4:H 2O 2 and KOH followed by the samples etched in HF:HNO 3 and in HF:C 2H 5OH.

  12. Effects of titanium surface topography on morphology and in vitro activity of human gingival fibroblasts.

    PubMed

    Ramaglia, L; Capece, G; Di Spigna, G; Bruno, M P; Buonocore, N; Postiglione, L

    2013-01-01

    The aim of the present study was to evaluate in vitro the biological behavior of human gingival fibroblasts cultured on two different titanium surfaces. Titanium test disks were prepared with a machined, relatively smooth (S) surface or a rough surface (O) obtained by a double acid etching procedure. Primary cultures of human gingival fibroblasts were plated on the experimental titanium disks and cultured up to 14 days. Titanium disk surfaces were analysed by scanning electron microscopy (SEM). Cell proliferation and a quantitative analysis by ELISA in situ of ECM components as CoI, FN and TN were performed. Results have shown different effects of titanium surface microtopography on cell expression and differentiation. At 96 hours of culture on experimental surfaces human gingival fibroblasts displayed a favourable cell attachment and proliferation on both surfaces although showing some differences. Both the relatively smooth and the etched surfaces interacted actively with in vitro cultures of human gingival fibroblasts, promoting cell proliferation and differentiation. Results suggested that the microtopography of a double acid-etched rough surface may induce a greater Co I and FN production, thus conditioning in vivo the biological behaviour of human gingival fibroblasts during the process of peri-implant soft tissue healing.

  13. Shallow V-Shape Nanostructured Pit Arrays in Germanium Using Aqua Regia Electroless Chemical Etching

    PubMed Central

    Chaabane, Ibtihel; Banerjee, Debika; Touayar, Oualid; Cloutier, Sylvain G.

    2017-01-01

    Due to its high refractive index, reflectance is often a problem when using Germanium for optoelectronic devices integration. In this work, we propose an effective and low-cost nano-texturing method for considerably reducing the reflectance of bulk Germanium. To do so, uniform V-shape pit arrays are produced by wet electroless chemical etching in a 3:1 volume ratio of highly-concentrated hydrochloridric and nitric acids or so-called aqua regia bath using immersion times ranging from 5 to 60 min. The resulting pit morphology, the crystalline structure of the surface and the changes in surface chemistry after nano-patterning are all investigated. Finally, broadband near-infrared reflectance measurements confirm a significant reduction using this simple wet etching protocol, while maintaining a crystalline, dioxide-free, and hydrogen-passivated surface. It is important to mention that reflectance could be further reduced using deeper pits. However, most optoelectronic applications such as photodetectors and solar cells require relatively shallow patterning of the Germanium to allow formation of a pn-junction close to the surface. PMID:28773215

  14. Growth and dislocation studies of β-HMX.

    PubMed

    Gallagher, Hugh G; Sherwood, John N; Vrcelj, Ranko M

    2014-01-01

    The defect structure of organic materials is important as it plays a major role in their crystal growth properties. It also can play a subcritical role in "hot-spot" detonation processes of energetics and one such energetic is cyclotetramethylene-tetranitramine, in the commonly used beta form (β-HMX). The as-grown crystals grown by evaporation from acetone show prismatic, tabular and columnar habits, all with {011}, {110}, (010) and (101) faces. Etching on (010) surfaces revealed three different types of etch pits, two of which could be identified with either pure screw or pure edge dislocations, the third is shown to be an artifact of the twinning process that this material undergoes. Examination of the {011} and {110} surfaces show only one type of etch pit on each surface; however their natural asymmetry precludes the easy identification of their Burgers vector or dislocation type. Etching of cleaved {011} surfaces demonstrates that the etch pits can be associated with line dislocations. All dislocations appear randomly on the crystal surfaces and do not form alignments characteristic of mechanical deformation by dislocation slip. Crystals of β-HMX grown from acetone show good morphological agreement with that predicted by modelling, with three distinct crystal habits observed depending upon the supersaturation of the growth solution. Prismatic habit was favoured at low supersaturation, while tabular and columnar crystals were predominant at higher super saturations. The twin plane in β-HMX was identified as a (101) reflection plane. The low plasticity of β-HMX is shown by the lack of etch pit alignments corresponding to mechanically induced dislocation arrays. On untwinned {010} faces, two types of dislocations exist, pure edge dislocations with b = [010] and pure screw dislocations with b = [010]. On twinned (010) faces, a third dislocation type exists and it is proposed that these pits are associated with pure screw dislocations with b = [010]. Graphical abstractEtch pits on the twinned (010) face of β-HMX.

  15. DOE Office of Scientific and Technical Information (OSTI.GOV)

    Yue, Mengyao; Zhou, Baoming; Jiao, Kunyan

    A switchable surface that promotes either hydrophobic or hydrophilic wettability of poly (L-lactide) (PLLA) microfibrous membranes is obtained by CF₄ microwave plasma treatment in this paper. The results indicated that both etching and grafting process occurred during the CF₄ plasma treatment and these two factors synergistically affected the final surface wettability of PLLA membranes. When plasma treatment was taken under a relatively low power, the surface wettability of PLLA membranes turned from hydrophobic to hydrophilic. Especially when CF₄ plasma treatment was taken under 100 W for 10 min and 150 W for 5 min, the water contact angle sharply decreasedmore » from 116 ± 3.0° to ~0°. According to Field-emission scanning electron microscopy (FESEM) results, the PLLA fibers were notably etched by CF₄ plasma treatment. Combined with the X-ray photoelectron spectroscopy (XPS) measurements, only a few fluorine-containing groups were grafted onto the surface, so the etching effect directly affected the surface wettability of PLLA membranes in low plasma power condition. However, with the plasma power increasing to 200 W, the PLLA membrane surface turned to hydrophobic again. In contrast, the morphology changes of PLLA fiber surfaces were not obvious while a large number of fluorine-containing groups grafted onto the surface. So the grafting effect gradually became the major factor for the final surface wettability.« less

  16. Development of Functional Surfaces on High-Density Polyethylene (HDPE) via Gas-Assisted Etching (GAE) Using Focused Ion Beams.

    PubMed

    Sezen, Meltem; Bakan, Feray

    2015-12-01

    Irradiation damage, caused by the use of beams in electron and ion microscopes, leads to undesired physical/chemical material property changes or uncontrollable modification of structures. Particularly, soft matter such as polymers or biological materials is highly susceptible and very much prone to react on electron/ion beam irradiation. Nevertheless, it is possible to turn degradation-dependent physical/chemical changes from negative to positive use when materials are intentionally exposed to beams. Especially, controllable surface modification allows tuning of surface properties for targeted purposes and thus provides the use of ultimate materials and their systems at the micro/nanoscale for creating functional surfaces. In this work, XeF2 and I2 gases were used in the focused ion beam scanning electron microscope instrument in combination with gallium ion etching of high-density polyethylene surfaces with different beam currents and accordingly different gas exposure times resulting at the same ion dose to optimize and develop new polymer surface properties and to create functional polymer surfaces. Alterations in the surface morphologies and surface chemistry due to gas-assisted etching-based nanostructuring with various processing parameters were tracked using high-resolution SEM imaging, complementary energy-dispersive spectroscopic analyses, and atomic force microscopic investigations.

  17. BOND STRENGTH AND MORPHOLOGY OF ENAMEL USING SELF-ETCHING ADHESIVE SYSTEMS WITH DIFFERENT ACIDITIES

    PubMed Central

    Moura, Sandra Kiss; Reis, Alessandra; Pelizzaro, Arlete; Dal-Bianco, Karen; Loguercio, Alessandro Dourado; Arana-Chavez, Victor Elias; Grande, Rosa Helena Miranda

    2009-01-01

    Objectives: To assess the bond strength and the morphology of enamel after application of self-etching adhesive systems with different acidities. The tested hypothesis was that the performance of the self-etching adhesive systems does not vary for the studied parameters. Material and methods: Composite resin (Filtek Z250) buildups were bonded to untreated (prophylaxis) and treated (burcut or SiC-paper) enamel surfaces of third molars after application of four self-etching and two etch-and-rinse adhesive systems (n=6/condition): Clearfil SE Bond (CSE); OptiBond Solo Plus Self-Etch (OP); AdheSe (AD); Tyrian Self Priming Etching (TY), Adper Scotchbond Multi-Purpose Plus (SBMP) and Adper Single Bond (SB). After storage in water (24 h/37°C), the bonded specimens were sectioned into sticks with 0.8 mm2 cross-sectional area and the microtensile bond strength was tested at a crosshead speed of 0.5 mm/min. The mean bond strength values (MPa) were subjected to two-way ANOVA and Tukey's test (α=0.05). The etching patterns of the adhesive systems were also observed with a scanning electron microscope. Results: The main factor adhesive system was statistically significant (p<0.05). The mean bond strength values (MPa) and standard deviations were: CSE (20.5±3.5), OP (11.3±2.3), AD (11.2±2.8), TY (11.1±3.0), SBMP (21.9±4.0) and SB (24.9±3.0). Different etching patterns were observed for the self-etching primers depending on the enamel treatment and the pH of the adhesive system. Conclusion: Although there is a tendency towards using adhesive systems with simplified application procedures, this may compromise the bonding performance of some systems to enamel, even when the prismless enamel is removed. PMID:19668991

  18. Etching characteristics of Si{110} in 20 wt% KOH with addition of hydroxylamine for the fabrication of bulk micromachined MEMS

    NASA Astrophysics Data System (ADS)

    Rao, A. V. Narasimha; Swarnalatha, V.; Pal, P.

    2017-12-01

    Anisotropic wet etching is a most widely employed for the fabrication of MEMS/NEMS structures using silicon bulk micromachining. The use of Si{110} in MEMS is inevitable when a microstructure with vertical sidewall is to be fabricated using wet anisotropic etching. In most commonly employed etchants (i.e. TMAH and KOH), potassium hydroxide (KOH) exhibits higher etch rate and provides improved anisotropy between Si{111} and Si{110} planes. In the manufacturing company, high etch rate is demanded to increase the productivity that eventually reduces the cost of end product. In order to modify the etching characteristics of KOH for the micromachining of Si{110}, we have investigated the effect of hydroxylamine (NH2OH) in 20 wt% KOH solution. The concentration of NH2OH is varied from 0 to 20% and the etching is carried out at 75 °C. The etching characteristics which are studied in this work includes the etch rates of Si{110} and silicon dioxide, etched surface morphology, and undercutting at convex corners. The etch rate of Si{110} in 20 wt% KOH + 15% NH2OH solution is measured to be four times more than that of pure 20 wt% KOH. Moreover, the addition of NH2OH increases the undercutting at convex corners and enhances the etch selectivity between Si and SiO2.

  19. Solvothermal synthesis of selenium nano and microspheres deposited on silicon surface by microwave-assisted method

    NASA Astrophysics Data System (ADS)

    Ahmad, Muthanna

    2016-10-01

    This work describes a new application of the solvothermal method, based on the microwave heating, for the synthesis of nano and microparticles of selenium. The reaction of selenium with hydrofluoric acid on the silicon surface is induced by microwave irradiation under high pressure and temperature of 60 bar and 160 °C, respectively. This method allows the deposition of spherical-like particles on the in situ etched silicon surface. The size of deposited selenium spheres scales from tens of nanometers up to tens of micrometers. The morphology and composition of the deposited selenium were analyzed by various analytical techniques. The formation dynamic of spherical structure is explained on the base of reduction of selenium species by hydrogen inside gas bubbles which are generated on the silicon surface by the etching process.

  20. Surface pre-treatment of aluminium by cleaning, chemical ething and conversion coating

    NASA Astrophysics Data System (ADS)

    Zaki, Mohammad Hafizudden Mohd; Mohd, Yusairie; Isa, Nik Norziehana Che

    2017-12-01

    Surface pre-treatment is one of the critical treatments for surface modification of aluminium (Al). In this study, pre-treatment of Al surface involved three stages; (1) cleaning (polishing and degreasing), (2) chemical etching (alkaline and acid) and (3) conversion coating (ie: zincate treatment). Cleaning process of Al was conducted by polishing and degreasing with acetone while etching process was done by immersion in 1.25 M NaOH solution (i.e: alkaline etching) followed with acid etching using 8 M HNO3 solution. The zincate treatment was conducted via electroless coating method by immersion of Al into a bath solution containing 0.5 M Zn(NO3)2, 0.1 M HNO3 and 0.2 M NaBH4 (reducing agent) for one hour. Different temperatures (ie: 25 °C, 50 °C, 75 °C, 90 °C) of bath solutions at pH 4 were used to investigate the effect of temperature on zincate treatment. Surface morphology and chemical composition of the pre-treated Al were characterized using Field Emission Scanning Electron Microscopy (FESEM) and Energy Dispersion X-ray analysis (EDX), respectively. The results showed that oxide layer on Al surface decreased after chemical etching process. Temperature of zincate solution has significantly affected the conversion coating process of aluminium. It was found that zinc oxide (ZnO) and zinc borate (ZnO.B2O3) were dominantly formed after zincate treatment at high temperature (ie:90 °C) with curved blade-like structure and composition of Zn, B and O with 13.70 wt.%, 3.52 wt.% and 54.39 wt.%, respectively. However, zincate treatment at low temperature (ie:<50 °C) has produced low metallic Zn.

  1. Fabrication of ZnO photonic crystals by nanosphere lithography using inductively coupled-plasma reactive ion etching with CH{sub 4}/H{sub 2}/Ar plasma on the ZnO/GaN heterojunction light emitting diodes

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Chen, Shr-Jia; Chang, Chun-Ming; Kao, Jiann-Shiun

    2010-07-15

    This article reports fabrication of n-ZnO photonic crystal/p-GaN light emitting diode (LED) by nanosphere lithography to further booster the light efficiency. In this article, the fabrication of ZnO photonic crystals is carried out by nanosphere lithography using inductively coupled plasma reactive ion etching with CH{sub 4}/H{sub 2}/Ar plasma on the n-ZnO/p-GaN heterojunction LEDs. The CH{sub 4}/H{sub 2}/Ar mixed gas gives high etching rate of n-ZnO film, which yields a better surface morphology and results less plasma-induced damages of the n-ZnO film. Optimal ZnO lattice parameters of 200 nm and air fill factor from 0.35 to 0.65 were obtained from fittingmore » the spectrum of n-ZnO/p-GaN LED using a MATLAB code. In this article, we will show our recent result that a ZnO photonic crystal cylinder has been fabricated using polystyrene nanosphere mask with lattice parameter of 200 nm and radius of hole around 70 nm. Surface morphology of ZnO photonic crystal was examined by scanning electron microscope.« less

  2. Shear Bond Strength of Self-etching Adhesives to Cavities Prepared by Diamond Bur or Er,Cr:YSGG Laser and Effect of Prior Acid Etching.

    PubMed

    Jhingan, Pulkit; Sachdev, Vinod; Sandhu, Meera; Sharma, Karan

    2015-12-01

    To compare and evaluate shear bond strength of self-etching adhesives bonded to cavities prepared by diamond bur or Er,Cr:YSGG laser and the effect of prior acid etching on shear bond strength. Ninety-six caries-free human premolars were selected and divided into 2 groups depending on mode of cavity preparation (48 teeth each). Cavities were prepared with Er,Cr:YSGG laser in group 1 and diamond burs in an air-turbine handpiece in group 2. Groups 1 and 2 were further subdivided into three subgroups of 8 teeth each, which were bonded with sixth- or seventh-generation adhesives with or without prior acid etching, followed by restoration of all samples with APX Flow. These samples were subjected to shear bond strength testing. In addition, the surface morphology of 24 samples each from groups 1 and 2 was evaluated using SEM. Data were analyzed using the Shapiro-Wilk test, one- and two-way ANOVA, the t-test, and the least significant difference test, which showed that the data were normally distributed (p > 0.05). The shear bond strength of adhesives in cavities prepared by Er,Cr:YSGG laser was significantly higher than in diamond bur-prepared cavities (p < 0.05). SEM analysis showed a smear-layer-free anfractuous surface on laser-ablated teeth, in contrast to conventional bur-prepared teeth. The Er,Cr:YSGG laser-ablated surface proved to be more receptive for adhesion than those prepared by diamond bur irrespective of the bonding agent used. Seventh-generation adhesives yielded higher shear bond strength than did sixth-generation adhesives. Prior acid etching decreased the shear bond strength of self-etching adhesives.

  3. Surface Morphology of Undoped and Doped ZnSe Films

    NASA Technical Reports Server (NTRS)

    George, T.; Hayes, M.; Chen, H.; Chattopadhyay, K.; Thomas E.; Morgan, S.; Burger, A.

    1998-01-01

    Rare-earth doped ions in polar II-VI semiconductors have recently played an important role in the optical properties of materials and devices. In this study, undoped ZnSe and erbium doped ZnSe films were grown by radio frequency (RF) magnetron sputtering method. Atomic Force Microscopy (AFM) was used together with optical microscopy and UV-Vis spectroscopy to characterize the films. Doped samples were found to have higher surface roughness and quite different surface morphology compared to that of undoped samples. The grown films generally show a relatively smooth and uniform surface indicating that they are of overall good quality. The impact of plasma etching on ZnSe:Er film examined under AFM is also discussed.

  4. Photoelectrochemical etching of epitaxial InGaN thin films: Self-limited kinetics and nanostructuring

    DOE PAGES

    Xiao, Xiaoyin; Fischer, Arthur J.; Coltrin, Michael E.; ...

    2014-10-22

    We report here the characteristics of photoelectrochemical (PEC) etching of epitaxial InGaN semiconductor thin films using narrowband lasers with linewidth less than ~1 nm. In the initial stages of PEC etching, when the thin film is flat, characteristic voltammogram shapes are observed. At low photo-excitation rates, voltammograms are S-shaped, indicating the onset of a voltage-independent rate-limiting process associated with electron-hole-pair creation and/or annihilation. At high photo-excitation rates, voltammograms are superlinear in shape, indicating, for the voltage ranges studied here, a voltage-dependent rate-limiting process associated with surface electrochemical oxidation. As PEC etching proceeds, the thin film becomes rough at the nanoscale,more » and ultimately evolves into an ensemble of nanoparticles. As a result, this change in InGaN film volume and morphology leads to a characteristic dependence of PEC etch rate on time: an incubation time, followed by a rise, then a peak, then a slow decay.« less

  5. [Observation of topography and analysis of surface contamination of titanium implant after roughness treatment].

    PubMed

    Cao, Hongdan; Yang, Xiaodong; Wu, Dayi; Zhang, Xingdong

    2007-04-01

    The roughness treatment of dental implant surface could improve the bone bonding and increase the success rate of implant, but the difference of diverse treatments is still unknown. In this study using scanning electron microscopy (SEM), energy disperse spectrometer (EDS) and the test of contact angle, we studied the microstructure, surface contamination and surface energy, and hence conducted a comparative analysis of the following surface roughness treatments: Polished Treatment (PT), Sandblasting with Alumina(SA), Sandblasting with Aluminia and Acid-etched (SAA), Sandblasting with Titanium Acid-etched (STA), Electro-erosion Treatment(ET). The result of SEM showed that the surface displayed irregularities after roughness treatments and that the surface properties of different roughness treatments had some distinctions. SAA and SA had some sharp edges and protrutions; the STA showed a regular pattern like honeycomb, but the ET sample treated by electric erosion exhibited the deeper pores of different sizes and the pores with a perforated secondary structure. The EDS indicated that the surface was contaminated after the treatment with foreign materials; the SA surface had some embedded contaminations even after acid etching. The measurement of water contact angle indicated that the morphology correlated with the surface treatments. These findings suggest that the distinction of surface structure and composition caused by different treatments may result in the disparity in biological behavior of dental implant.

  6. The thickness correction of sol-gel coating using ion-beam etching in the preparation of antireflection coating

    NASA Astrophysics Data System (ADS)

    Dong, Siyu; Xie, Lingyun; He, Tao; Jiao, Hongfei; Bao, Ganghua; Zhang, Jinlong; Wang, Zhanshan; Cheng, Xinbin

    2017-09-01

    For the sol-gel method, it is still challenging to achieve excellent spectral performance when preparing antireflection (AR) coating by this way. The difficulty lies in controlling the film thickness accurately. To correct the thickness error of sol-gel coating, a hybrid approach that combined conventional sol-gel process with ion-beam etching technology was proposed in this work. The etching rate was carefully adjusted and calibrated to a relatively low value for removing the redundant material. Using atomic force microscope (AFM), it has been demonstrated that film surface morphology will not be changed in this process. After correcting the thickness error, an AR coating working at 1064 nm was prepared with transmittance higher than 99.5%.

  7. Advanced Mitigation Process (AMP) for Improving Laser Damage Threshold of Fused Silica Optics

    NASA Astrophysics Data System (ADS)

    Ye, Xin; Huang, Jin; Liu, Hongjie; Geng, Feng; Sun, Laixi; Jiang, Xiaodong; Wu, Weidong; Qiao, Liang; Zu, Xiaotao; Zheng, Wanguo

    2016-08-01

    The laser damage precursors in subsurface of fused silica (e.g. photosensitive impurities, scratches and redeposited silica compounds) were mitigated by mineral acid leaching and HF etching with multi-frequency ultrasonic agitation, respectively. The comparison of scratches morphology after static etching and high-frequency ultrasonic agitation etching was devoted in our case. And comparison of laser induce damage resistance of scratched and non-scratched fused silica surfaces after HF etching with high-frequency ultrasonic agitation were also investigated in this study. The global laser induce damage resistance was increased significantly after the laser damage precursors were mitigated in this case. The redeposition of reaction produce was avoided by involving multi-frequency ultrasonic and chemical leaching process. These methods made the increase of laser damage threshold more stable. In addition, there is no scratch related damage initiations found on the samples which were treated by Advanced Mitigation Process.

  8. Advanced Mitigation Process (AMP) for Improving Laser Damage Threshold of Fused Silica Optics

    PubMed Central

    Ye, Xin; Huang, Jin; Liu, Hongjie; Geng, Feng; Sun, Laixi; Jiang, Xiaodong; Wu, Weidong; Qiao, Liang; Zu, Xiaotao; Zheng, Wanguo

    2016-01-01

    The laser damage precursors in subsurface of fused silica (e.g. photosensitive impurities, scratches and redeposited silica compounds) were mitigated by mineral acid leaching and HF etching with multi-frequency ultrasonic agitation, respectively. The comparison of scratches morphology after static etching and high-frequency ultrasonic agitation etching was devoted in our case. And comparison of laser induce damage resistance of scratched and non-scratched fused silica surfaces after HF etching with high-frequency ultrasonic agitation were also investigated in this study. The global laser induce damage resistance was increased significantly after the laser damage precursors were mitigated in this case. The redeposition of reaction produce was avoided by involving multi-frequency ultrasonic and chemical leaching process. These methods made the increase of laser damage threshold more stable. In addition, there is no scratch related damage initiations found on the samples which were treated by Advanced Mitigation Process. PMID:27484188

  9. Comparison of bond strength and surface morphology of dental enamel for acid and Nd-YAG laser etching

    NASA Astrophysics Data System (ADS)

    Parmeswearan, Diagaradjane; Ganesan, Singaravelu; Ratna, P.; Koteeswaran, D.

    1999-05-01

    Recently, laser pretreatment of dental enamel has emerged as a new technique in the field of orthodontics. However, the changes in the morphology of the enamel surface is very much dependent on the wavelength of laser, emission mode of the laser, energy density, exposure time and the nature of the substance absorbing the energy. Based on these, we made a comparative in vitro study on laser etching with acid etching with reference to their bond strength. Studies were conducted on 90 freshly extracted, non carious, human maxillary or mandibular anteriors and premolars. Out of 90, 60 were randomly selected for laser irradiation. The other 30 were used for conventional acid pretreatment. The group of 60 were subjected to Nd-YAG laser exposure (1060 nm, 10 Hz) at differetn fluences. The remaining 30 were acid pretreated with 30% orthophosphoric acid. Suitable Begg's brackets were selected and bound to the pretreated surface and the bond strength were tested using Instron testing machine. The bond strength achieved through acid pretreatment is found to be appreciably greater than the laser pretreated tooth. Though the bond strength achieved through the acid pretreated tooth is found to be significantly greater than the laser pretreated specimens, the laser pretreatement is found to be successful enough to produce a clinically acceptable bond strength of > 0.60 Kb/mm. Examination of the laser pre-treated tooth under SEM showed globule formation which may produce the mechanical interface required for the retention of the resin material.

  10. Switchable hydrophobic/hydrophilic surface of electrospun poly (l-lactide) membranes obtained by CF₄microwave plasma treatment

    DOE PAGES

    Yue, Mengyao; Zhou, Baoming; Jiao, Kunyan; ...

    2014-11-29

    A switchable surface that promotes either hydrophobic or hydrophilic wettability of poly (L-lactide) (PLLA) microfibrous membranes is obtained by CF₄ microwave plasma treatment in this paper. The results indicated that both etching and grafting process occurred during the CF₄ plasma treatment and these two factors synergistically affected the final surface wettability of PLLA membranes. When plasma treatment was taken under a relatively low power, the surface wettability of PLLA membranes turned from hydrophobic to hydrophilic. Especially when CF₄ plasma treatment was taken under 100 W for 10 min and 150 W for 5 min, the water contact angle sharply decreasedmore » from 116 ± 3.0° to ~0°. According to Field-emission scanning electron microscopy (FESEM) results, the PLLA fibers were notably etched by CF₄ plasma treatment. Combined with the X-ray photoelectron spectroscopy (XPS) measurements, only a few fluorine-containing groups were grafted onto the surface, so the etching effect directly affected the surface wettability of PLLA membranes in low plasma power condition. However, with the plasma power increasing to 200 W, the PLLA membrane surface turned to hydrophobic again. In contrast, the morphology changes of PLLA fiber surfaces were not obvious while a large number of fluorine-containing groups grafted onto the surface. So the grafting effect gradually became the major factor for the final surface wettability.« less

  11. Simultaneous ion sputter polishing and deposition

    NASA Technical Reports Server (NTRS)

    Rutledge, S.; Banks, B.; Brdar, M.

    1981-01-01

    Results of experiments to study ion beam sputter polishing in conjunction with simultaneous deposition as a mean of polishing copper surfaces are presented. Two types of simultaneous ion sputter polishing and deposition were used in these experiments. The first type utilized sputter polishing simultaneous with vapor deposition, and the second type utilized sputter polishing simultaneous with sputter deposition. The etch and deposition rates of both techniques were studied, as well as the surface morphology and surface roughness.

  12. Plasma treatment of polymers for improved adhesion

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Kelber, J.A.

    1988-01-01

    A variety of plasma treatments of polymer surfaces for improved adhesion are reviewed: noble and reactive gas treatment of fluoropolymers; noble and reactive treatment of polyolefins, and plasma-induced amination of polymer fibers. The plasma induced surface chemical and morphological changes are discussed, as are the mechanisms of adhesion to polymeric adhesives, particularly epoxy. Noble gas plasma etching of flouropolymers produces a partially defluorinated, textured surface. The mechanical interlocking of this textured surface is the primary cause of improved adhesion to epoxy. Reactive gas plasmas also induce defluorination, but oxygen containing gases cause continual ablation of the fluoropolymer surface. Noble andmore » reactive gas (exept for hydrogen) etching of polyolefins results in surface oxidation and improved adhesion via hydrogen bonding of these oxygen containing groups across the interface. The introduction of amine groups to a polymer surface by amonia or amine plasma treatment generally results in improved adhesion to epoxy. However, amine-epoxy ring interactions can be severely effected by steric factors due to chemical groups surrounding the amine. 41 refs.« less

  13. Facile design of ultra-thin anodic aluminum oxide membranes for the fabrication of plasmonic nanoarrays.

    PubMed

    Hao, Qi; Huang, Hao; Fan, Xingce; Hou, Xiangyu; Yin, Yin; Li, Wan; Si, Lifang; Nan, Haiyan; Wang, Huaiyu; Mei, Yongfeng; Qiu, Teng; Chu, Paul K

    2017-03-10

    Ultra-thin anodic aluminum oxide (AAO) membranes are efficient templates for the fabrication of patterned nanostructures. Herein, a three-step etching method to control the morphology of AAO is described. The morphological evolution of the AAO during phosphoric acid etching is systematically investigated and a nonlinear growth mechanism during unsteady-state anodization is revealed. The thickness of the AAO can be quantitatively controlled from ∼100 nm to several micrometers while maintaining the tunablity of the pore diameter. The AAO membranes are robust and readily transferable to different types of substrates to prepare patterned plasmonic nanoarrays such as nanoislands, nanoclusters, ultra-small nanodots, and core-satellite superstructures. The localized surface plasmon resonance from these nanostructures can be easily tuned by adjusting the morphology of the AAO template. The custom AAO template provides a platform for the fabrication of low-cost and large-scale functional nanoarrays suitable for fundamental studies as well as applications including biochemical sensing, imaging, photocatalysis, and photovoltaics.

  14. Facile design of ultra-thin anodic aluminum oxide membranes for the fabrication of plasmonic nanoarrays

    NASA Astrophysics Data System (ADS)

    Hao, Qi; Huang, Hao; Fan, Xingce; Hou, Xiangyu; Yin, Yin; Li, Wan; Si, Lifang; Nan, Haiyan; Wang, Huaiyu; Mei, Yongfeng; Qiu, Teng; Chu, Paul K.

    2017-03-01

    Ultra-thin anodic aluminum oxide (AAO) membranes are efficient templates for the fabrication of patterned nanostructures. Herein, a three-step etching method to control the morphology of AAO is described. The morphological evolution of the AAO during phosphoric acid etching is systematically investigated and a nonlinear growth mechanism during unsteady-state anodization is revealed. The thickness of the AAO can be quantitatively controlled from ˜100 nm to several micrometers while maintaining the tunablity of the pore diameter. The AAO membranes are robust and readily transferable to different types of substrates to prepare patterned plasmonic nanoarrays such as nanoislands, nanoclusters, ultra-small nanodots, and core-satellite superstructures. The localized surface plasmon resonance from these nanostructures can be easily tuned by adjusting the morphology of the AAO template. The custom AAO template provides a platform for the fabrication of low-cost and large-scale functional nanoarrays suitable for fundamental studies as well as applications including biochemical sensing, imaging, photocatalysis, and photovoltaics.

  15. Creating micro-scale surface topology to achieve anisotropic wettability on an aluminum surface

    NASA Astrophysics Data System (ADS)

    Sommers, Andrew D.; Jacobi, Anthony M.

    2006-08-01

    A technique for fabricating micropatterned aluminum surfaces with parallel grooves 30 µm wide and tens of microns in depth is described. Standard photolithographic techniques are used to obtain this precise surface-feature patterning. Positive photoresists, S1813 and AZ4620, are selected to mask the surface, and a mixture of BCl3 and Cl2 gases is used to perform the etching. Experimental data show that a droplet placed on the micro-grooved aluminum surface using a micro-syringe exhibits an increased apparent contact angle, and for droplets condensed on these etched surfaces, more than a 50% reduction in the volume needed for the onset of droplet sliding is manifest. No chemical surface treatment is necessary to achieve this water repellency; it is accomplished solely by an anisotropic surface morphology that manipulates droplet geometry and creates and exploits discontinuities in the three-phase contact line. These micro-structured surfaces are proposed for use in a broad range of air-cooling applications, where the management of condensate and defrost liquid on the heat transfer surface is essential to the energy-efficient operation of the machine.

  16. Microleakage of Self-Etch Adhesive System in Class V Cavities Prepared by Using Er:YAG Laser with Different Pulse Modes.

    PubMed

    Phanombualert, Jutipond; Chimtim, Pijitta; Heebthamai, Thitirat; Weera-Archakul, Wilawan

    2015-09-01

    In vitro studies evaluated cementum surface morphology and microleakage of three different energy density parameters of Erbium: Yttrium Aluminum Garnet (Er:YAG) laser compared with diamond bur preparation on class V cavities with self-etch adhesive system and composite resin restoration. Standard class V cavities were prepared at cervical area below the cementoenamel junction (CEJ) in 80 extracted premolars, by using a diamond bur on the buccal surface. All teeth were randomly allocated into four groups: Group 1, diamond bur; Group 2, Er:YAG 50 mJ/15 Hz, 3.77 J/cm(2); Group 3, Er:YAG 75 mJ/15 Hz, 5.65 J/cm(2); and Group 4, Er:YAG 100 mJ/15 Hz, 7.53 J/cm(2). Five cavities from each group were evaluated by scanning electron microscopy (SEM). The 15 remaining cavities from each group were restored with self-etch adhesive and nano-hybrid composite. After thermocycling, all sample teeth were immersed in 0.2% methylene blue dye and sectioned buccolingually. Statistics were analyzed using the one way ANOVA and Mann-Whitney U tests with Bonferroni correction. The morphology showed micro-irregularities in the cementum surface of the laser group with the absence of a smear layer. The microstructure characteristics were increased surface roughness followed by increasing laser energy transmission. The Er:YAG laser groups were statistically significant, with less microleakage than the diamond bur group (p<0.05). There was statistically significant difference between the occlusal and gingival microleakage in all the groups (p<0.05). When the laser groups were compared, the lowest microleakage was achieved with energy density at 3.77 J/cm(2) on the occlusal and gingival cementum margin, which showed less microleakage than at energy densities of 5.65 and 7.53 J/cm(2) with Er:YAG laser. These observations indicate that the micro-irregularities of the cementum surface could facilitate the formation of a hybridization zone with a self-etch adhesive system. Therefore, the microleakage of Er:YAG laser irradiation was significantly decreased compared with diamond bur cavities.

  17. Determination of total fluoride in HF/HNO3/H2SiF6 etch solutions by new potentiometric titration methods.

    PubMed

    Weinreich, Wenke; Acker, Jörg; Gräber, Iris

    2007-03-30

    In the photovoltaic industry the etching of silicon in HF/HNO(3) solutions is a decisive process for cleaning wafer surfaces or to produce certain surface morphologies like polishing or texturization. With regard to cost efficiency, a maximal utilisation of etch baths in combination with highest quality and accuracy is strived. To provide an etch bath control realised by a replenishment with concentrated acids the main constituents of these HF/HNO(3) etch solutions including the reaction product H(2)SiF(6) have to be analysed. Two new methods for the determination of the total fluoride content in an acidic etch solution based on the precipitation titration with La(NO(3))(3) are presented within this paper. The first method bases on the proper choice of the reaction conditions, since free fluoride ions have to be liberated from HF and H(2)SiF(6) at the same time to be detected by a fluoride ion-selective electrode (F-ISE). Therefore, the sample is adjusted to a pH of 8 for total cleavage of the SiF(6)(2-) anion and titrated in absence of buffers. In a second method, the titration with La(NO(3))(3) is followed by a change of the pH-value using a HF resistant glass-electrode. Both methods provide consistent values, whereas the analysis is fast and accurate, and thus, applicable for industrial process control.

  18. Self-Healing Thermal Annealing: Surface Morphological Restructuring Control of GaN Nanorods

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Conroy, Michele; Li, Haoning; Zubialevich, Vitaly Z.

    With advances in nanolithography and dry etching, top-down methods of nanostructuring have become a widely used tool for improving the efficiency of optoelectronics. These nano dimensions can offer various benefits to the device performance in terms of light extraction and efficiency, but often at the expense of emission color quality. Broadening of the target emission peak and unwanted yellow luminescence are characteristic defect-related effects due to the ion beam etching damage, particularly for III–N based materials. In this article we focus on GaN based nanorods, showing that through thermal annealing the surface roughness and deformities of the crystal structure canmore » be “self-healed”. Correlative electron microscopy and atomic force microscopy show the change from spherical nanorods to faceted hexagonal structures, revealing the temperature-dependent surface morphology faceting evolution. The faceted nanorods were shown to be strain- and defect-free by cathodoluminescence hyperspectral imaging, micro-Raman, and transmission electron microscopy (TEM). In-situ TEM thermal annealing experiments allowed for real time observation of dislocation movements and surface restructuring observed in ex-situ annealing TEM sampling. This thermal annealing investigation gives new insight into the redistribution path of GaN material and dislocation movement post growth, allowing for improved understanding and in turn advances in optoelectronic device processing of compound semiconductors.« less

  19. Micro/nano hierarchical structured titanium treated by NH4OH/H2O2 for enhancing cell response

    PubMed Central

    Yuan, Xin; Kang, Yi; Zuo, Jun; Xie, Youneng; Ma, Li; Ren, Xuelei; Bian, Zeyu; Zhou, Kechao; Wang, Xiyang; Yu, Zhiming

    2018-01-01

    In this paper, two kinds of titanium surfaces with novel micro/nano hierarchical structures, namely Etched (E) surface and Sandblast and etched (SE) surface, were successfully fabricated by NH4OH and H2O2 mixture. And their cellular responses of MG63 were investigated compared with Sandblast and acid-etching (SLA) surface. Scanning electron microscope (SEM), Surface profiler, X-ray photoelectron spectroscopy (XPS), and Contact angle instrument were employed to assess the surface morphologies, roughness, chemistry and wettability respectively. Hierarchical structures with micro holes of 10–30 μm in diameter and nano pits of tens of nanometers in diameter formed on both E and SE surfaces. The size of micro holes is very close to osteoblast cell, which makes them wonderful beds for osteoblast. Moreover, these two kinds of surfaces possess similar roughness and superior hydrophilicity to SLA. Reactive oxygen species were detected on E and SE surface, and thus considerable antimicrobial performance and well fixation can be speculated on them. The cell experiments also demonstrated a boost in cell attachment, and that proliferation and osteogenic differentiation were achieved on them, especially on SE surface. The results indicate that the treatment of pure titanium with H2O2/NH4OH is an effective technique to improve the initial stability of implants and enhance the osseointegration, which may be a promising surface treatment to titanium implant. PMID:29723214

  20. Effect of Er:YAG laser pulse duration on the shear bond strength of bleached dentin

    NASA Astrophysics Data System (ADS)

    Yu, Ping; Yu, Dandan; Zhao, Peng; Xu, Zhou; Gao, Shanshan

    2017-11-01

    The influence of different Er:YAG laser pulse durations on the shear bond strength (SBS) of bleached dentin was investigated in this study. In total, 176 crowns of extracted human premolars were cut horizontally, embedded and ground to expose the sound dentin. Of these, 132 specimens were bleached with 12% hydrogen peroxide (HP) and divided into three groups, irradiated by an Er:YAG laser with different pulse lengths of 50 µs super short pulse (SSP), 100 µs moderate short pulse (MSP) and 300 µs short pulse (SP), respectively. The energy density of the three groups was the same at about 15.73 J cm-2 for each. Then, each group was further divided into two subgroups according to whether it had been etched with 37% phosphoric acid or not. The control group (N  =  22) was bleached and etched with acid while the blank group (N  =  22) was just etched with acid. The surface morphology of the dentin was observed using scanning electron microscopy (SEM). The SBS of the composite resin to the conditioned dentin was tested with a universal testing machine. It was found that the SBS of the dentin significantly decreased after bleaching treatment, while it was possible to restore it using Er:YAG laser irradiation. Lasers with various pulse durations led to different surface morphologies but had no effect on the SBS. The SSP laser was more suitable on account of it resulting in less thermal damage, and additional acid etching was not necessary for the irradiated bleached dentin in the clinic because it could not further improve the SBS value.

  1. Chemical method for producing smooth surfaces on silicon wafers

    DOEpatents

    Yu, Conrad

    2003-01-01

    An improved method for producing optically smooth surfaces in silicon wafers during wet chemical etching involves a pre-treatment rinse of the wafers before etching and a post-etching rinse. The pre-treatment with an organic solvent provides a well-wetted surface that ensures uniform mass transfer during etching, which results in optically smooth surfaces. The post-etching treatment with an acetic acid solution stops the etching instantly, preventing any uneven etching that leads to surface roughness. This method can be used to etch silicon surfaces to a depth of 200 .mu.m or more, while the finished surfaces have a surface roughness of only 15-50 .ANG. (RMS).

  2. Effect of fabrication parameters on morphological and optical properties of highly doped p-porous silicon

    NASA Astrophysics Data System (ADS)

    Zare, Maryam; Shokrollahi, Abbas; Seraji, Faramarz E.

    2011-09-01

    Porous silicon (PS) layers were fabricated by anodization of low resistive (highly doped) p-type silicon in HF/ethanol solution, by varying current density, etching time and HF concentration. Atomic force microscopy (AFM) and field emission scanning electron microscope (FESEM) analyses were used to investigate the physical properties and reflection spectrum was used to investigate the optical behavior of PS layers in different fabrication conditions. Vertically aligned mesoporous morphology is observed in fabricated films and with HF concentration higher than 20%. The dependence of porosity, layer thickness and rms roughness of the PS layer on current density, etching time and composition of electrolyte is also observed in obtained results. Correlation between reflectivity and fabrication parameters was also explored. Thermal oxidation was performed on some mesoporous layers that resulted in changes of surface roughness, mean height and reflectivity of the layers.

  3. A study of laser surface treatment in bonded repair of composite aircraft structures.

    PubMed

    Li, Shaolong; Sun, Ting; Liu, Chang; Yang, Wenfeng; Tang, Qingru

    2018-03-01

    Surface pre-treatment is one of the key processes in bonded repair of aircraft carbon fibre reinforced polymer composites. This paper investigates the surface modification of physical and chemical properties by laser ablation and conventional polish treatment techniques. Surface morphology analysed by laser scanning confocal microscopy and scanning electron microscopy showed that a laser-treated surface displayed higher roughness than that of a polish-treated specimen. The laser-treated laminate exhibited more functional groups in the form of O 1 s/C 1 s atomic ratio of 30.89% for laser-treated and 20.14% for polish-treated as evidenced by X-ray photoelectron spectroscopy observation. Contact angle goniometry demonstrated that laser treatment can provide increased surface free energy and wettability. In the light of mechanical interlocking, molecular bonding and thermodynamics theories on adhesion, laser etching process displayed enhanced bonding performance relative to the polishing surface treatment. These properties resulted in an increased single lap shear strength and a cohesive failure mode for laser etching while an adhesive failure mode occurred in polish-treated specimen.

  4. A study of laser surface treatment in bonded repair of composite aircraft structures

    NASA Astrophysics Data System (ADS)

    Li, Shaolong; Sun, Ting; Liu, Chang; Yang, Wenfeng; Tang, Qingru

    2018-03-01

    Surface pre-treatment is one of the key processes in bonded repair of aircraft carbon fibre reinforced polymer composites. This paper investigates the surface modification of physical and chemical properties by laser ablation and conventional polish treatment techniques. Surface morphology analysed by laser scanning confocal microscopy and scanning electron microscopy showed that a laser-treated surface displayed higher roughness than that of a polish-treated specimen. The laser-treated laminate exhibited more functional groups in the form of O 1 s/C 1 s atomic ratio of 30.89% for laser-treated and 20.14% for polish-treated as evidenced by X-ray photoelectron spectroscopy observation. Contact angle goniometry demonstrated that laser treatment can provide increased surface free energy and wettability. In the light of mechanical interlocking, molecular bonding and thermodynamics theories on adhesion, laser etching process displayed enhanced bonding performance relative to the polishing surface treatment. These properties resulted in an increased single lap shear strength and a cohesive failure mode for laser etching while an adhesive failure mode occurred in polish-treated specimen.

  5. A study of laser surface treatment in bonded repair of composite aircraft structures

    PubMed Central

    Sun, Ting; Liu, Chang; Yang, Wenfeng; Tang, Qingru

    2018-01-01

    Surface pre-treatment is one of the key processes in bonded repair of aircraft carbon fibre reinforced polymer composites. This paper investigates the surface modification of physical and chemical properties by laser ablation and conventional polish treatment techniques. Surface morphology analysed by laser scanning confocal microscopy and scanning electron microscopy showed that a laser-treated surface displayed higher roughness than that of a polish-treated specimen. The laser-treated laminate exhibited more functional groups in the form of O 1 s/C 1 s atomic ratio of 30.89% for laser-treated and 20.14% for polish-treated as evidenced by X-ray photoelectron spectroscopy observation. Contact angle goniometry demonstrated that laser treatment can provide increased surface free energy and wettability. In the light of mechanical interlocking, molecular bonding and thermodynamics theories on adhesion, laser etching process displayed enhanced bonding performance relative to the polishing surface treatment. These properties resulted in an increased single lap shear strength and a cohesive failure mode for laser etching while an adhesive failure mode occurred in polish-treated specimen. PMID:29657748

  6. High density plasma etching of magnetic devices

    NASA Astrophysics Data System (ADS)

    Jung, Kee Bum

    Magnetic materials such as NiFe (permalloy) or NiFeCo are widely used in the data storage industry. Techniques for submicron patterning are required to develop next generation magnetic devices. The relative chemical inertness of most magnetic materials means they are hard to etch using conventional RIE (Reactive Ion Etching). Therefore ion milling has generally been used across the industry, but this has limitations for magnetic structures with submicron dimensions. In this dissertation, we suggest high density plasmas such as ECR (Electron Cyclotron Resonance) and ICP (Inductively Coupled Plasma) for the etching of magnetic materials (NiFe, NiFeCo, CoFeB, CoSm, CoZr) and other related materials (TaN, CrSi, FeMn), which are employed for magnetic devices like magnetoresistive random access memories (MRAM), magnetic read/write heads, magnetic sensors and microactuators. This research examined the fundamental etch mechanisms occurring in high density plasma processing of magnetic materials by measuring etch rate, surface morphology and surface stoichiometry. However, one concern with using Cl2-based plasma chemistry is the effect of residual chlorine or chlorinated etch residues remaining on the sidewalls of etched features, leading to a degradation of the magnetic properties. To avoid this problem, we employed two different processing methods. The first one is applying several different cleaning procedures, including de-ionized water rinsing or in-situ exposure to H2, O2 or SF6 plasmas. Very stable magnetic properties were achieved over a period of ˜6 months except O2 plasma treated structures, with no evidence of corrosion, provided chlorinated etch residues were removed by post-etch cleaning. The second method is using non-corrosive gas chemistries such as CO/NH3 or CO2/NH3. There is a small chemical contribution to the etch mechanism (i.e. formation of metal carbonyls) as determined by a comparison with Ar and N2 physical sputtering. The discharge should be NH3-rich to achieve the highest etch rates. Several different mask materials were investigated, including photoresist, thermal oxide and deposited oxide. Photoresist etches very rapidly in CO/NH 3 and use of a hard mask is necessary to achieve pattern transfer. Due to its physically dominated nature, the CO/NH3 chemistry appears suited to shallow etch depth (≤0.5mum) applications, but mask erosion leads to sloped feature sidewalls for deeper features.

  7. Nanotexturing of polystyrene surface in fluorocarbon plasmas: from sticky to slippery superhydrophobicity.

    PubMed

    Mundo, Rosa Di; Palumbo, Fabio; d'Agostino, Riccardo

    2008-05-06

    In this work plasma etching processes have been studied to roughen and fluorinate polystyrene surface as an easy method to achieve a superhydrophobic slippery character. Radiofrequency discharges have been fed with CF(4)/O(2) mixtures and the effect of the O(2):CF(4) ratio, the input power, and the treatment duration have been investigated in terms of wettability, with focus on sliding performances. For this purpose, surface morphological variations, evaluated by means of scanning electron microscopy and atomic force microscopy, together with the chemical assessment by X-ray photoelectron spectroscopy, have been correlated with water contact angle hysteresis and volume resolved sliding angle measurements. Results indicate that by increasing the height and decreasing the density of the structures formed by etching, within a tailored range, a transition from sticky to slippery superhydrophobicity occurs. A short treatment time (5 min) is sufficient to obtain such an effect, provided that a high power input is utilized. Optimized surfaces show a unaltered transparency to visible light according to the low roughness produced.

  8. Effect of Reduced Phosphoric Acid Pre-etching Times 
on Enamel Surface Characteristics and Shear Fatigue Strength Using Universal Adhesives.

    PubMed

    Tsujimoto, Akimasa; Fischer, Nicholas; Barkmeier, Wayne; Baruth, Andrew; Takamizawa, Toshiki; Latta, Mark; Miyazaki, Masashi

    2017-01-01

    To examine the effect of reduced phosphoric acid pre-etching times on enamel fatigue bond strength of universal adhesives and surface characteristics by using atomic force microscopy (AFM). Three universal adhesives were used in this study (Clearfil Universal Bond [C], G-Premio Bond [GP], Scotchbond Universal Adhesive [SU]). Four pre-etching groups were employed: enamel pre-etched with phosphoric acid and immediately rinsed with an air-water spray, and enamel pre-etched with phosphoric acid for 5, 10, or 15 s. Ground enamel was used as the control group. For the initial bond strength test, 15 specimens per etching group for each adhesive were used. For the shear fatigue test, 20 specimens per etching group for each adhesive were loaded using a sine wave at a frequency of 20 Hz for 50,000 cycles or until failure occurred. Initial shear bond strengths and fatigue shear strengths of composite adhesively bonded to ground and pre-etched enamel were determined. AFM observations of ground and pre-etched enamel were also conducted, and surface roughness as well as surface area were evaluated. The initial shear bond strengths and fatigue shear strengths of the universal adhesives in the pre-etched groups were significantly higher than those of the control group, and were not influenced by the pre-etching time. Significantly higher surface roughness and surface area of enamel surfaces in pre-etched groups were observed compared with those in the control group. While the surface area was not significantly influenced by etching time, surface roughness of the enamel surfaces in the pre-etched groups significantly increased with pre-etching time. The results of this in vitro study suggest that reduced phosphoric acid pre-etching times do not impair the fatigue bond strength of universal adhesives. Although fatigue bond strength and surface area were not influenced by phosphoric-acid etching times, surface roughness increased with increasing etching time.

  9. Formation of Nanocones on Highly Oriented Pyrolytic Graphite by Oxygen Plasma

    PubMed Central

    Vesel, Alenka; Eleršič, Kristina; Modic, Martina; Junkar, Ita; Mozetič, Miran

    2014-01-01

    Improvement in hemocompatibility of highly oriented pyrolytic graphite (HOPG) by formation of nanostructured surface by oxygen plasma treatment is reported. We have showed that by appropriate fine tuning of plasma and discharge parameters we are able to create nanostructured surface which is densely covered with nanocones. The size of the nanocones strongly depended on treatment time. The optimal results in terms of material hemocompatibility were obtained after treatment with oxygen plasma for 15 s, when both the nanotopography and wettability were the most favorable, since marked reduction in adhesion and activation of platelets was observed on this surface. At prolonged treatment times, the rich surface topography was lost and thus also its antithrombogenic properties. Chemical composition of the surface was always more or less the same, regardless of its morphology and height of the nanocones. Namely, on all plasma treated samples, only a few atomic percent of oxygen was found, meaning that plasma caused mostly etching, leading to changes in the surface morphology. This indicates that the main preventing mechanism against platelets adhesion was the right surface morphology. PMID:28788553

  10. Copper-assisted, anti-reflection etching of silicon surfaces

    DOEpatents

    Toor, Fatima; Branz, Howard

    2014-08-26

    A method (300) for etching a silicon surface (116) to reduce reflectivity. The method (300) includes electroless deposition of copper nanoparticles about 20 nanometers in size on the silicon surface (116), with a particle-to-particle spacing of 3 to 8 nanometers. The method (300) includes positioning (310) the substrate (112) with a silicon surface (116) into a vessel (122). The vessel (122) is filled (340) with a volume of an etching solution (124) so as to cover the silicon surface (116). The etching solution (124) includes an oxidant-etchant solution (146), e.g., an aqueous solution of hydrofluoric acid and hydrogen peroxide. The silicon surface (116) is etched (350) by agitating the etching solution (124) with, for example, ultrasonic agitation, and the etching may include heating (360) the etching solution (124) and directing light (365) onto the silicon surface (116). During the etching, copper nanoparticles enhance or drive the etching process.

  11. The Effect of Phosphoric Acid Pre-etching Times on Bonding Performance and Surface Free Energy with Single-step Self-etch Adhesives.

    PubMed

    Tsujimoto, A; Barkmeier, W W; Takamizawa, T; Latta, M A; Miyazaki, M

    2016-01-01

    The purpose of this study was to evaluate the effect of phosphoric acid pre-etching times on shear bond strength (SBS) and surface free energy (SFE) with single-step self-etch adhesives. The three single-step self-etch adhesives used were: 1) Scotchbond Universal Adhesive (3M ESPE), 2) Clearfil tri-S Bond (Kuraray Noritake Dental), and 3) G-Bond Plus (GC). Two no pre-etching groups, 1) untreated enamel and 2) enamel surfaces after ultrasonic cleaning with distilled water for 30 seconds to remove the smear layer, were prepared. There were four pre-etching groups: 1) enamel surfaces were pre-etched with phosphoric acid (Etchant, 3M ESPE) for 3 seconds, 2) enamel surfaces were pre-etched for 5 seconds, 3) enamel surfaces were pre-etched for 10 seconds, and 4) enamel surfaces were pre-etched for 15 seconds. Resin composite was bonded to the treated enamel surface to determine SBS. The SFEs of treated enamel surfaces were determined by measuring the contact angles of three test liquids. Scanning electron microscopy was used to examine the enamel surfaces and enamel-adhesive interface. The specimens with phosphoric acid pre-etching showed significantly higher SBS and SFEs than the specimens without phosphoric acid pre-etching regardless of the adhesive system used. SBS and SFEs did not increase for phosphoric acid pre-etching times over 3 seconds. There were no significant differences in SBS and SFEs between the specimens with and without a smear layer. The data suggest that phosphoric acid pre-etching of ground enamel improves the bonding performance of single-step self-etch adhesives, but these bonding properties do not increase for phosphoric acid pre-etching times over 3 seconds.

  12. Dicalcium phosphate (CaHPO4·2H2O) precipitation through ortho- or meta-phosphoric acid-etching: effects on the durability and nanoleakage/ultra-morphology of resin-dentine interfaces.

    PubMed

    Feitosa, Victor Pinheiro; Bazzocchi, Maria Giulia; Putignano, Angelo; Orsini, Giovanna; Luzi, Arlinda Luzi; Sinhoreti, Mário Alexandre Coelho; Watson, Timothy F; Sauro, Salvatore

    2013-11-01

    To compare the effects of two etching procedures using meta-phosphoric (MPA) or ortho-phosphoric acid (OPA) on dentine demineralisation, resin-dentine bonds durability and interface nanoleakage/ultra-morphology. Middle-dentine specimens were etched using 37% OPA (15s) or 40% MPA (60s) and submitted to infrared spectroscopy (FTIR) or ultra-morphology dye-assisted (calcium-staining) confocal microscopy (Ca-CLSM). A three-step etch-and-rinse adhesive was formulated, applied onto dentine and light-cured for 30s before composite build-up. After 24h, the dentine-bonded specimens were cut into 1mm(2) beams; half were immediately submitted to microtensile bond strength (μTBS) and half stored in DW for six months. The μTBS results were analysed with repeated-measures ANOVA and Tukey's test (p<0.05). Further teeth were bonded and prepared for interface nanoleakage/ultra-morphology confocal evaluation. FTIR and Ca-CLSM analyses showed dicalcium phosphate dihydrate (Brushite) precipitation in MPA-etched dentine and on the bottom (front of demineralisation) of the OPA-etched dentine. Statistical analysis showed similar μTBS for both etching procedures after 24h. The μTBS of specimens in OPA-group dropped significantly (p<0.05) after six month; the specimens in the MPA group showed no statistically difference (p>0.05). CLSM depicted no evident sign of nanoleakage within the resin-dentine interface of the MPA-treated specimens, while the specimens in OPA-group presented intense nanoleakage and interface degradation. The use of MPA (60s) as an alternative dentine conditioning agent in etch-and-rinse bonding procedures may be a suitable strategy to create more durable resin-dentine bonds. Copyright © 2013 Elsevier Ltd. All rights reserved.

  13. Surface characteristics and damage distributions of diamond wire sawn wafers for silicon solar cells

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Sopori, Bhushan; Devayajanam, Srinivas; Basnyat, Prakash

    2016-01-01

    This paper describes surface characteristics, in terms of its morphology, roughness and near-surface damage of Si wafers cut by diamond wire sawing (DWS) of Si ingots under different cutting conditions. Diamond wire sawn Si wafers exhibit nearly-periodic surface features of different spatial wavelengths, which correspond to kinematics of various movements during wafering, such as ingot feed, wire reciprocation, and wire snap. The surface damage occurs in the form of frozen-in dislocations, phase changes, and microcracks. The in-depth damage was determined by conventional methods such as TEM, SEM and angle-polishing/defect-etching. However, because these methods only provide local information, we have alsomore » applied a new technique that determines average damage depth over a large area. This technique uses sequential measurement of the minority carrier lifetime after etching thin layers from the surfaces. The lateral spatial damage variations, which seem to be mainly related to wire reciprocation process, were observed by photoluminescence and minority carrier lifetime mapping. Our results show a strong correlation of damage depth on the diamond grit size and wire usage.« less

  14. Surface passivation of nano-textured fluorescent SiC by atomic layer deposited TiO2

    NASA Astrophysics Data System (ADS)

    Lu, Weifang; Ou, Yiyu; Jokubavicius, Valdas; Fadil, Ahmed; Syväjärvi, Mikael; Petersen, Paul Michael; Ou, Haiyan

    2016-07-01

    Nano-textured surfaces have played a key role in optoelectronic materials to enhance the light extraction efficiency. In this work, morphology and optical properties of nano-textured SiC covered with atomic layer deposited (ALD) TiO2 were investigated. In order to obtain a high quality surface for TiO2 deposition, a three-step cleaning procedure was introduced after RIE etching. The morphology of anatase TiO2 indicates that the nano-textured substrate has a much higher surface nucleated grain density than a flat substrate at the beginning of the deposition process. The corresponding reflectance increases with TiO2 thickness due to increased surface diffuse reflection. The passivation effect of ALD TiO2 thin film on the nano-textured fluorescent 6H-SiC sample was also investigated and a PL intensity improvement of 8.05% was obtained due to the surface passivation.

  15. Impact of the De-Alloying Kinetics and Alloy Microstructure on the Final Morphology of De-Alloyed Meso-Porous Metal Films

    PubMed Central

    Lin, Bao; Kong, Lingxue; Hodgson, Peter D.; Dumée, Ludovic F.

    2014-01-01

    Nano-textured porous metal materials present unique surface properties due to their enhanced surface energy with potential applications in sensing, molecular separation and catalysis. In this paper, commercial alloy foils, including brass (Cu85Zn15 and Cu70Zn30) and white gold (Au50Ag50) foils have been chemically de-alloyed to form nano-porous thin films. The impact of the initial alloy micro-structure and number of phases, as well as chemical de-alloying (DA) parameters, including etchant concentration, time and solution temperature on the final nano-porous thin film morphology and properties were investigated by electron microscopy (EM). Furthermore, the penetration depth of the pores across the alloys were evaluated through the preparation of cross sections by focus ion beam (FIB) milling. It is demonstrated that ordered pores ranging between 100 nm and 600 nm in diameter and 2–5 μm in depth can be successfully formed for the range of materials tested. The microstructure of the foils were obtained by electron back-scattered diffraction (EBSD) and linked to development of pits across the material thickness and surface during DA. The role of selective etching of both noble and sacrificial metal phases of the alloy were discussed in light of the competitive surface etching across the range of microstructures and materials tested. PMID:28344253

  16. Mechanical strength and hydrophobicity of cotton fabric after SF6 plasma treatment

    NASA Astrophysics Data System (ADS)

    Kamlangkla, K.; Paosawatyanyong, B.; Pavarajarn, V.; Hodak, Jose H.; Hodak, Satreerat K.

    2010-08-01

    Surface treatments to tailor fabric properties are in high demand by the modern garment industry. We studied the effect of radio-frequency inductively coupled SF plasma on the surface characteristics of cotton fabric. The duration of the treatment and the SF pressure were varied systematically. We measured the hydrophobicity of treated cotton as a function of storage time and washing cycles. We used the weight loss (%) along with the etching rate, the tensile strength, the morphology changes and the hydrophobicity of the fabric as observables after treatments with different plasma conditions. The weight loss remains below 1% but it significantly increases when the treatment time is longer than 5 min. Substantial changes in the surface morphology of the fiber are concomitant with the increased etching rate and increased weight loss with measurable consequences in their mechanical characteristics. The measured water absorption time reaches the maximum of 210 min when the SF pressure is higher than 0.3 Torr. The water contact angle ( 149°) and the absorption time (210 min) of cotton treated with extreme conditions appear to be durable as long as the fabric is not washed. X-ray photoelectron spectroscopy analysis reveals that the water absorption time of the fabric follows the same increasing trend as the fluorine/carbon ratio at the fabric surface and atom density of fluorine measured by Ar actinometer.

  17. Sculpting the internal architecture of fluorescent silica particles via a template-free approach.

    PubMed

    Rosu, Cornelia; Gorman, Andrew J; Cueto, Rafael; Dooley, Kerry M; Russo, Paul S

    2016-04-01

    Particles with an open, porous structure can be used to deliver payloads. It is often of interest to detect such particles in tissue or materials, which is facilitated by addition of dye. A straightforward approach leading to fluorescent, porous silica particles is described. The particles are etched with 3mM aqueous sodium hydroxide, taking advantage of the etching rate difference between normal silica and an interior band of silica that contains covalently attached dye. No additional steps, such as dye labeling or thermal annealing, are required. Etching modeled the internal structure of the fluorescent silica particles by creating meso/macropores and voids, as reflected by nitrogen absorption measurements. In order to investigate whether a polymer shell influences etching, certain composite particles are top-coated with poly(l-lysine) representing neutral or positive charged surfaces under typical pH conditions in living systems. The polypeptide-coated fluorescent silica cores exhibit the same porous morphology as uncoated homologs. The polypeptide topcoat does little to alter the permeation by the etching agent. Preservation of size during etching, confirmed by dynamic light scattering, transmission electron microscopy and small-angle X-ray scattering, simplifies the use of these template-free porous fluorescent particles as platforms for drug encapsulation, drug carriers and in vivo imaging. Copyright © 2016 Elsevier Inc. All rights reserved.

  18. FIB Secondary Etching Method for Fabrication of Fine CNT Forest Metamaterials

    NASA Astrophysics Data System (ADS)

    Pander, Adam; Hatta, Akimitsu; Furuta, Hiroshi

    2017-10-01

    Anisotropic materials, like carbon nanotubes (CNTs), are the perfect substitutes to overcome the limitations of conventional metamaterials; however, the successful fabrication of CNT forest metamaterial structures is still very challenging. In this study, a new method utilizing a focused ion beam (FIB) with additional secondary etching is presented, which can obtain uniform and fine patterning of CNT forest nanostructures for metamaterials and ranging in sizes from hundreds of nanometers to several micrometers. The influence of the FIB processing parameters on the morphology of the catalyst surface and the growth of the CNT forest was investigated, including the removal of redeposited material, decreasing the average surface roughness (from 0.45 to 0.15 nm), and a decrease in the thickness of the Fe catalyst. The results showed that the combination of FIB patterning and secondary etching enabled the growth of highly aligned, high-density CNT forest metamaterials. The improvement in the quality of single-walled CNTs (SWNTs), defined by the very high G/D peak ratio intensity of 10.47, demonstrated successful fine patterning of CNT forest for the first time. With a FIB patterning depth of 10 nm and a secondary etching of 0.5 nm, a minimum size of 150 nm of CNT forest metamaterials was achieved. The development of the FIB secondary etching method enabled for the first time, the fabrication of SWNT forest metamaterials for the optical and infrared regime, for future applications, e.g., in superlenses, antennas, or thermal metamaterials.

  19. Microstructural characterization of Ti-6Al-4V alloy subjected to the duplex SMAT/plasma nitriding.

    PubMed

    Pi, Y; Faure, J; Agoda-Tandjawa, G; Andreazza, C; Potiron, S; Levesque, A; Demangel, C; Retraint, D; Benhayoune, H

    2013-09-01

    In this study, microstructural characterization of Ti-6Al-4V alloy, subjected to the duplex surface mechanical attrition treatment (SMAT)/nitriding treatment, leading to improve its mechanical properties, was carried out through novel and original samples preparation methods. Instead of acid etching which is limited for morphological characterization by scanning electron microscopy (SEM), an original ion polishing method was developed. Moreover, for structural characterization by transmission electron microscopy (TEM), an ion milling method based with the use of two ions guns was also carried out for cross-section preparation. To demonstrate the efficiency of the two developed methods, morphological investigations were done by traditional SEM and field emission gun SEM. This was followed by structural investigations through selected area electron diffraction (SAED) coupled with TEM and X-ray diffraction techniques. The results demonstrated that ionic polishing allowed to reveal a variation of the microstructure according to the surface treatment that could not be observed by acid etching preparation. TEM associated to SAED and X-ray diffraction provided information regarding the nanostructure compositional changes induced by the duplex SMAT/nitriding process. Copyright © 2013 Wiley Periodicals, Inc.

  20. The effect of axial ion parameters on the properties of glow discharge polymer in T2B/H2 plasma

    NASA Astrophysics Data System (ADS)

    Ai, Xing; He, Xiao-Shan; Huang, Jing-Lin; He, Zhi-Bing; Du, Kai; Chen, Guo

    2018-03-01

    Glow discharge polymer (GDP) films were fabricated using plasma-enhanced chemical vapor deposition. The main purpose of this work was to explore the correlations of plasma parameters with the surface morphology and chemical structure of GDP films. The intensities of main positive ions and ion energy as functions of axial distances in T2B/H2 plasma were diagnosed using energy-resolved mass spectrometry. The surface morphology and chemical structure were characterized as functions of axial distances using a scanning electron microscope and Fourier transform infrared spectroscopy, respectively. As the axial distance increases, both the intensities of positive ions and high energy ions decreases, and dissociation weakens while polymerization enhances. This leads to the weakening of the cross-linking structure of GDP films and the formation of dome defects on films. Additionally, high energy ions could introduce a strong etching effect to form etching pits. Therefore, an axial distance of about 20 mm was found to be the optimal plasma parameter to prepare the defect-free GDP films. These results could help one to find the optimal plasma parameters for GDP film deposition.

  1. Influence of Er:YAG and Ti:sapphire laser irradiation on the microtensile bond strength of several adhesives to dentin.

    PubMed

    Portillo, M; Lorenzo, M C; Moreno, P; García, A; Montero, J; Ceballos, L; Fuentes, M V; Albaladejo, A

    2015-02-01

    The aim of the present study was to evaluate the influence of erbium:yttrium-aluminum-garnet (Er:YAG) and Ti:sapphire laser irradiation on the microtensile bond strength (MTBS) of three different adhesive systems to dentin. Flat dentin surfaces from 27 molars were divided into three groups according to laser irradiation: control, Er:YAG (2,940 nm, 100 μs, 2.7 W, 9 Hz) and Ti:sapphire laser (795 nm, 120 fs, 1 W, 1 kHz). Each group was divided into three subgroups according to the adhesive system used: two-step total-etching adhesive (Adper Scotchbond 1 XT, from now on XT), two-step self-etching adhesive (Clearfil SE Bond, from now on CSE), and all-in-one self-etching adhesive (Optibond All-in-One, from now on OAO). After 24 h of water storage, beams of section at 1 mm(2) were longitudinally cut from the samples. Each beam underwent traction test in an Instron machine. Fifteen polished dentin specimens were used for the surface morphology analysis by scanning electron microscopy (SEM). Failure modes of representative debonded microbars were SEM-assessed. Data were analyzed by ANOVA, chi-square test, and multiple linear regression (p < 0.05). In the control group, XT obtained higher MTBS than that of laser groups that performed equally. CSE showed higher MTBS without laser than that with laser groups, where Er:YAG attained higher MTBS than ultrashort laser. When OAO was used, MTBS values were equal in the three treatments. CSE obtained the highest MTBS regardless of the surface treatment applied. The Er:YAG and ultrashort laser irradiation reduce the bonding effectiveness when a two-step total-etching adhesive or a two-step self-etching adhesive are used and do not affect their effectiveness when an all-in-one self-etching adhesive is applied.

  2. Scanning electron microscopy evaluation of the effect of etching agents on human enamel surface.

    PubMed

    Zanet, Caio G; Arana-Chavez, Victor E; Fava, Marcelo

    2006-01-01

    Acid etching promotes microporosities on enamel surface, which provide a better bonding surface to adhesive materials. The purpose of this study was to comparatively analyze the microstructure of enamel surface after etching with 37% phosphoric acid or with two self-etching primers, Non-rinse conditioner (NRC) and Clearfil SE Bond (CSEB) using scanning electron microscopy. Thirty sound premolars were divided into 3 groups with ten teeth each: Group 1: the buccal surface was etched with 37% phosphoric acid for 15 seconds; Group 2: the buccal surface was etched with NRC for 20 seconds; Group 3: the buccal surface was etched with CSEB for 20 seconds. Teeth from Group 1 were rinsed with water; teeth from all groups were air-dried for 15 seconds. After that, all specimens were processed for scanning electron microscopy and analyzed in a Jeol 6100 SEM. The results showed deeper etching when the enamel surface was etched with 37% phosphoric acid, followed by NRC and CSEB. It is concluded that 37% phosphoric acid is still the best agent for a most effective enamel etching.

  3. Plasma nanotexturing of silicon surfaces for photovoltaics applications: influence of initial surface finish on the evolution of topographical and optical properties

    PubMed Central

    FISCHER, GUILLAUME; DRAHI, ETIENNE; FOLDYNA, MARTIN; GERMER, THOMAS A.; JOHNSON, ERIK V.

    2018-01-01

    Using a plasma to generate a surface texture with feature sizes on the order of tens to hundreds of nanometers (“nanotexturing”) is a promising technique being considered to improve efficiency in thin, high-efficiency crystalline silicon solar cells. This study investigates the evolution of the optical properties of silicon samples with various initial surface finishes (from mirror polish to various states of micron-scale roughness) during a plasma nanotexturing process. It is shown that during said process, the appearance and growth of nanocone-like structures are essentially independent of the initial surface finish, as quantified by the auto-correlation function of the surface morphology. During the first stage of the process (2 min to 15 min etching), the reflectance and light-trapping abilities of the nanotextured surfaces are strongly influenced by the initial surface roughness; however, the differences tend to diminish as the nanostructures become larger. For the longest etching times (15 min or more), the effective reflectance is less than 5 % and a strong anisotropic scattering behavior is also observed for all samples, leading to very elevated levels of light-trapping. PMID:29220984

  4. Temperature-Dependent Nanofabrication on Silicon by Friction-Induced Selective Etching.

    PubMed

    Jin, Chenning; Yu, Bingjun; Xiao, Chen; Chen, Lei; Qian, Linmao

    2016-12-01

    Friction-induced selective etching provides a convenient and practical way for fabricating protrusive nanostructures. A further understanding of this method is very important for establishing a controllable nanofabrication process. In this study, the effect of etching temperature on the formation of protrusive hillocks and surface properties of the etched silicon surface was investigated. It is found that the height of the hillock produced by selective etching increases with the etching temperature before the collapse of the hillock. The temperature-dependent selective etching rate can be fitted well by the Arrhenius equation. The etching at higher temperature can cause rougher silicon surface with a little lower elastic modulus and hardness. The contact angle of the etched silicon surface decreases with the etching temperature. It is also noted that no obvious contamination can be detected on silicon surface after etching at different temperatures. As a result, the optimized condition for the selective etching was addressed. The present study provides a new insight into the control and application of friction-induced selective nanofabrication.

  5. Phase Analysis of Laser Direct Etching and Water Assisted Laser Combined Etching of SiC Ceramics

    NASA Astrophysics Data System (ADS)

    Yuan, Genfu; Cong, Qidong; Zhang, Chen; Xie, Bingbing

    2017-12-01

    In this study, to discover the etching mechanism of SiC ceramics under laser direct etching and water-jet assisted laser combined etching, the phenomena of substance change on the etched surface were investigated. Also, the rules of substance transfer in etching are discussed. The elemental content change and the phase change of the etching products on the etched surface were analyzed by energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD), respectively. These studies showed a high amount of carbon black on the etched surface, because of the decomposition of SiC ceramics under the high-power-density laser irradiation. SiC decomposed to Si under the laser irradiation, and the subsequent chemical reaction of Si and O2 easily produced SiO2. The SiO2 on the etched surface melted and vaporized, whereas most of SiO2 was removed through splashing, changing the chemical composition of the etched surface. Following the water jet introduction, an increased amount of O existed on the combined etching surface, because the chemical reaction of SiC and H2O easily produced SiO2 under the high-power-density laser irradiation.

  6. Characterization and properties of micro- and nanowires of controlled size, composition, and geometry fabricated by electrodeposition and ion-track technology

    PubMed Central

    2012-01-01

    Summary The combination of electrodeposition and polymeric templates created by heavy-ion irradiation followed by chemical track etching provides a large variety of poly- and single-crystalline nanowires of controlled size, geometry, composition, and surface morphology. Recent results obtained by our group on the fabrication, characterization and size-dependent properties of nanowires synthesized by this technique are reviewed, including investigations on electrical resistivity, surface plasmon resonances, and thermal instability. PMID:23365800

  7. Correlation between oxidant concentrations, morphological aspects and etching kinetics of silicon nanowires during silver-assist electroless etching

    NASA Astrophysics Data System (ADS)

    Moumni, Besma; Jaballah, Abdelkader Ben

    2017-12-01

    Silicon porosification by silver assisted chemical etching (Ag-ACE) for a short range of H2O2 concentration is reported. We experimentally show that porous silicon (PSi) is obtained for 1% H2O2, whereas silicon nanowires (SiNWs) appeared by simply tuning the concentration of H2O2 to relatively high concentrations up to 8%. The morphological aspects are claimed by scanning electron microscopy proving that the kinetics of SiNWs formation display nonlinear relationships versus H2O2 concentration and etching time. A semi-qualitative electrochemical etching model based on local anodic, Ic, and cathodic, Ia, currents is proposed to explain the different morphological changes, and to unveil the formation pathways of both PS and SiNWs. More importantly, an efficient antireflective character for silicon solar cell (reflectance close to 2%) is realized at 8% H2O2. In addition, the luminescence of the prepared Si-nanostructures is claimed by photoluminescence which exhibit a large enhancement of the intensity and a blue shift for narrow and deep SiNWs.

  8. Surface engineering on CeO2 nanorods by chemical redox etching and their enhanced catalytic activity for CO oxidation

    NASA Astrophysics Data System (ADS)

    Gao, Wei; Zhang, Zhiyun; Li, Jing; Ma, Yuanyuan; Qu, Yongquan

    2015-07-01

    Controllable surface properties of nanocerias are desired for various catalytic processes. There is a lack of efficient approaches to adjust the surface properties of ceria to date. Herein, a redox chemical etching method was developed to controllably engineer the surface properties of ceria nanorods. Ascorbic acid and hydrogen peroxide were used to perform the redox chemical etching process, resulting in a rough surface and/or pores on the surface of ceria nanorods. Increasing the etching cycles induced a steady increase of the specific surface area, oxygen vacancies and surface Ce3+ fractions. As a result, the etched nanorods delivered enhanced catalytic activity for CO oxidation, compared to the non-etched ceria nanorods. Our method provides a novel and facile approach to continuously adjust the surface properties of ceria for practical applications.Controllable surface properties of nanocerias are desired for various catalytic processes. There is a lack of efficient approaches to adjust the surface properties of ceria to date. Herein, a redox chemical etching method was developed to controllably engineer the surface properties of ceria nanorods. Ascorbic acid and hydrogen peroxide were used to perform the redox chemical etching process, resulting in a rough surface and/or pores on the surface of ceria nanorods. Increasing the etching cycles induced a steady increase of the specific surface area, oxygen vacancies and surface Ce3+ fractions. As a result, the etched nanorods delivered enhanced catalytic activity for CO oxidation, compared to the non-etched ceria nanorods. Our method provides a novel and facile approach to continuously adjust the surface properties of ceria for practical applications. Electronic supplementary information (ESI) available: Diameter distributions of as-prepared and etched samples, optical images, specific catalytic data of CO oxidation and comparison of CO oxidation. See DOI: 10.1039/c5nr01846c

  9. Surface topography and chemistry shape cellular behavior on wide band-gap semiconductors.

    PubMed

    Bain, Lauren E; Collazo, Ramon; Hsu, Shu-Han; Latham, Nicole Pfiester; Manfra, Michael J; Ivanisevic, Albena

    2014-06-01

    The chemical stability and electrical properties of gallium nitride make it a promising material for the development of biocompatible electronics, a range of devices including biosensors as well as interfaces for probing and controlling cellular growth and signaling. To improve the interface formed between the probe material and the cell or biosystem, surface topography and chemistry can be applied to modify the ways in which the device interacts with its environment. PC12 cells are cultured on as-grown planar, unidirectionally polished, etched nanoporous and nanowire GaN surfaces with and without a physisorbed peptide sequence that promotes cell adhesion. While cells demonstrate preferential adhesion to roughened surfaces over as-grown flat surfaces, the topography of that roughness also influences the morphology of cellular adhesion and differentiation in neurotypic cells. Addition of the peptide sequence generally contributes further to cellular adhesion and promotes development of stereotypic long, thin neurite outgrowths over alternate morphologies. The dependence of cell behavior on both the topographic morphology and surface chemistry is thus demonstrated, providing further evidence for the importance of surface modification for modulating bio-inorganic interfaces. Copyright © 2014 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

  10. Reactions of Atomic Oxygen (O(3P)) with Polybutadienes and Related Polymers

    NASA Technical Reports Server (NTRS)

    Golub, Morton A.; Lerner, Narcinda R.; Wydeven, Theodore

    1987-01-01

    Thin films of the following polymers were exposed at ambient temperature to ground-state oxygen atoms (O(3P)), generated by a radio-frequency glow discharge in O2: cis- and trans-1,4-polybutadienes (CB and TB), amorphous 1,2-polybutadiene (VB), polybutadienes with different 1,4/1,2 contents, trans polypentenamer (TP), cis and trans polyoctenamers (CO and TO), and ethylene-propylene rubber (EPM). Transmission infrared spectra of CB and TB films revealed extensive surface recession, or etching, unaccompanied by any microstructural changes within the films, demonstrating that the reactions were confined to the surface layers. Contrary to the report by Rabek, Lucki, and Ranby (1979), there was no O(3P)-induced cis-trans isomerization in CB or TB. From weight-loss measurements, etch rates for polybutadienes were found to be markedly dependent on vinyl content, decreasing by two orders of magnitude from CB (2% 1,2) to structures with 30 to 40% 1,2 double bonds, thereafter increasing by half an order of magnitude to VB (97% 1,2). Relative etch rates for EMP and the polyalkenamers were in the order: EMP is greater than CO (or TO) is greater than TP is greater than CB. The sole non-elastomer examined, TB, had an etch rate about six times that of CB, ascribable to a morphology difference. Cis/trans content had a negligible effect on the etch rate of the polyalkenamers. Mechanisms involving crosslinking through units are proposed for the unexpected protection imparted to polybutadienes by the 1,2 double bonds.

  11. Atomic force microscopy studies of homoepitaxial GaN layers grown on GaN template by laser MBE

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Choudhary, B. S.; Rajasthan Technical University, Rawatbhata Road, Kota 324010; Singh, A.

    We have grown homoepitaxial GaN films on metal organic chemical vapor deposition (MOCVD) grown 3.5 µm thick GaN on sapphire (0001) substrate (GaN template) using an ultra-high vacuum (UHV) laser assisted molecular beam epitaxy (LMBE) system. The GaN films were grown by laser ablating a polycrystalline solid GaN target in the presence of active r.f. nitrogen plasma. The influence of laser repetition rates (10-30 Hz) on the surface morphology of homoepitaxial GaN layers have been studied using atomic force microscopy. It was found that GaN layer grown at 10 Hz shows a smooth surface with uniform grain size compared to the rough surfacemore » with irregular shape grains obtained at 30 Hz. The variation of surface roughness of the homoepitaxial GaN layer with and without wet chemical etching has been also studied and it was observed that the roughness of the film decreased after wet etching due to the curved structure/rough surface.« less

  12. Enhancement of Device Performances in GaN-Based Light-Emitting Diodes Using Nano-Sized Surface Pit.

    PubMed

    Yeon, Seunghwan; Son, Taejoon; Shin, Dong Su; Jung, Kyung-Young; Park, Jinsub

    2015-07-01

    We report the improvement in optical and electrical properties of GaN-based green light-emitting diodes (LEDs) with nano-sized etch pits formed by the surface chemical etching. In order to control the density and sizes of etch pits formed on top surface of green LEDs, H3PO4 solution is used as a etchant with different etching time. When the etching time was increased from 0 min to 20 min, both the etch pit size and density were gradually increased. The improvement of extraction efficiency of LEDs using surface etching method can be attributed to the enlarged escape angle of generated photon by roughened p-GaN surface. The finite-difference time-domain (FDTD) simulation results well agreed with experimentally observed results. Moreover, the LED with etched p-GaN surface for 5 min shows the lowest leakage current value and the further increase of etching time resulting in increase of densities of the large-sized etch pit makes the degradation of electrical properties of LEDs.

  13. The impact of hydrofluoric acid etching followed by unfilled resin on the biaxial strength of a glass-ceramic.

    PubMed

    Posritong, Sumana; Borges, Alexandre Luiz Souto; Chu, Tien-Min Gabriel; Eckert, George J; Bottino, Marco A; Bottino, Marco C

    2013-11-01

    To evaluate the null hypotheses that hydrofluoric (HF) acid etching time would neither decrease the biaxial flexural strength of a glass-based veneering ceramic nor enhance it after silane and unfilled resin (UR) applications. Disc-shaped IPS e.max ZirPress specimens were allocated into 12 groups: G1-control (no-etching), G2-30 s, G3-60 s, G4-90 s, G5-120 s, G6-60 s+60 s. Groups (G7-G12) were treated in the same fashion as G1-G6, but followed by silane and UR applications. Surface morphology and roughness (Ra and Rq) of the ceramics were assessed by means of scanning electron microscopy (SEM) and profilometry, respectively. Flexural strength was determined by biaxial testing. Data were analyzed by two-way ANOVA and the Sidak test (α=0.05). Weibull statistics were estimated and finite element analysis (FEA) was carried out to verify the stress concentration end areas of fracture. The interaction (etching time vs. surface treatment) was significant for Ra (p=0.008) and Rq (0.0075). Resin-treated groups presented significantly lower Ra and Rq than non-treated groups, except for the 60s group (p<0.005). SEM revealed that etching affected the ceramic microstructure and that the UR was able to penetrate into the irregularities. A significant effect of etching time (p=0.029) on flexural strength was seen. G7-G12 presented higher strength than G1-G6 (p<0.0001). None of experimental groups failed to show 95% confidence intervals of σ0 and m overlapped. FEA showed lower stress concentration after resin treatment. HF acid etching time did not show a damaging effect on the ceramic flexural strength. Moreover, the flexural strength could be enhanced after UR treatment. Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

  14. Texturization of diamond-wire-sawn multicrystalline silicon wafer using Cu, Ag, or Ag/Cu as a metal catalyst

    NASA Astrophysics Data System (ADS)

    Wang, Shing-Dar; Chen, Ting-Wei

    2018-06-01

    In this work, Cu, Ag, or Ag/Cu was used as a metal catalyst to study the surface texturization of diamond-wire-sawn (DWS) multi-crystalline silicon (mc-Si) wafer by a metal-assisted chemical etching (MACE) method. The DWS wafer was first etched by standard HF-HNO3 acidic etching, and it was labeled as AE-DWS wafer. The effects of ratios of Cu(NO3)2:HF, AgNO3:HF, and AgNO3:Cu(NO3)2 on the morphology of AE-DWS wafer were investigated. After the process of MACE, the wafer was treated with a NaF/H2O2 solution. In this process, H2O2 etched the nanostructure, and NaF removed the oxidation layer. The Si {1 1 1} plane was revealed by etching the wafer in a mixture of 0.03 M Cu(NO3)2 and 1 M HF at 55 °C for 2.5 min. These parallel Si {1 1 1} planes replaced some parallel saw marks on the surface of AE-DWS wafers without forming a positive pyramid or an inverted pyramid structure. The main topography of the wafer is comprised of silicon nanowires grown in <1 0 0> direction when Ag or Ag/Cu was used as a metal catalyst. When silicon is etched in a mixed solution of Cu(NO3)2, AgNO3, HF and H2O2 at 55 °C with a concentration ratio of [Cu2+]/[Ag+] of 50 or at 65 °C with a concentration ratio of [Cu2+]/[Ag+] of 33, a quasi-inverted pyramid structure can be obtained. The reflectivity of the AE-DWS wafers treated with MACE is lower than that of the multiwire-slurry-sawn (MWSS) mc-Si wafers treated with traditional HF + HNO3 etching.

  15. [Comperative study of implant surface characteristics].

    PubMed

    Katona, Bernadett; Daróczi, Lajos; Jenei, Attila; Bakó, József; Hegedus, Csaba

    2013-12-01

    The osseointegration between the implant and its' bone environment is very important. The implants shall meet the following requirements: biocompatibility, rigidity, resistance against corrosion and technical producibility. In our present study surface morphology and material characteristics of different implants (Denti Bone Level, Denti Zirconium C, Bionika CorticaL, Straumann SLA, Straumann SLA Active, Dentsply Ankylos and Biotech Kontact implant) were investigated with scanning electron microscopy and energy-dispersive X-ray spectroscopy. The possible surface alterations caused by the manufacturing technology were also investigated. During grit-blasting the implants' surface is blasted with hard ceramic particles (titanium oxide, alumina, calcium phosphate). Properties of blasting material are critical because the osseointegration of dental implants should not be hampered. The physical and chemical features of blasting particles could importantly affect the produced surfaces of implants. Titanium surfaces with micro pits are created after immersion in mixtures of strong acids. On surfaces after dual acid-etching procedures the crosslinking between fibrin and osteogenetic cells could be enhanced therefore bone formation could be directly facilitated on the surface of the implant. Nowadays there are a number of surface modification techniques available. These can be used as a single method or in combination with each other. The effect of the two most commonly used surface modifications (acid-etching and grit-blasting) on different implants are demonstrated in our investigation.

  16. Plasma variables and tribological properties of coatings in low pressure (0.1 - 10.0 torr) plasma systems

    NASA Technical Reports Server (NTRS)

    Avni, R.; Spalvins, T.

    1984-01-01

    A detailed treatment is presented of the dialog known as plasma surface interactions (PSI) with respect to the coating process and its tribological behavior. Adsorption, morphological changes, defect formation, sputtering, chemical etching, and secondary electron emission are all discussed as promoting and enhancing the surface chemistry, thus influencing the tribological properties of the deposited flux. Phenomenological correlations of rate of deposition, flux composition, microhardness, and wear with the plasma layer variables give an insight to the formation of chemical bonding between the deposited flux and the substrate surface.

  17. In-Situ Atomic Force Microscope Imaging of Calcite Etch Pit Morphology Changes in Undersaturated and 1-Hydroxyethylidene-1,1-diphosphonic Acid Poisoned Solutions

    PubMed Central

    Britt, David W.

    2012-01-01

    Morphology changes in etch pits formed on the (1014) cleavage plane of calcite were induced by varying the ratio of [Ca2+] to [CO32−] in the bulk solution as well as through the addition of the crystal poison 1-hydroxyethylidene-1,1-diphosphonic acid (HEDP). Three distinct morphologies were noted: symmetric rhombic, asymmetric rhombic, and triangular with a rough curved hypotenuse. The latter represents a transient morphology which is only observed during the actual dissolution process, while the former morphologies persist after dissolution is halted. PMID:25125794

  18. Etching Behavior of Aluminum Alloy Extrusions

    NASA Astrophysics Data System (ADS)

    Zhu, Hanliang

    2014-11-01

    The etching treatment is an important process step in influencing the surface quality of anodized aluminum alloy extrusions. The aim of etching is to produce a homogeneously matte surface. However, in the etching process, further surface imperfections can be generated on the extrusion surface due to uneven materials loss from different microstructural components. These surface imperfections formed prior to anodizing can significantly influence the surface quality of the final anodized extrusion products. In this article, various factors that influence the materials loss during alkaline etching of aluminum alloy extrusions are investigated. The influencing variables considered include etching process parameters, Fe-rich particles, Mg-Si precipitates, and extrusion profiles. This study provides a basis for improving the surface quality in industrial extrusion products by optimizing various process parameters.

  19. Study of Thermal Electrical Modified Etching for Glass and Its Application in Structure Etching

    PubMed Central

    Zhan, Zhan; Li, Wei; Yu, Lingke; Wang, Lingyun; Sun, Daoheng

    2017-01-01

    In this work, an accelerating etching method for glass named thermal electrical modified etching (TEM etching) is investigated. Based on the identification of the effect in anodic bonding, a novel method for glass structure micromachining is proposed using TEM etching. To validate the method, TEM-etched glasses are prepared and their morphology is tested, revealing the feasibility of the new method for micro/nano structure micromachining. Furthermore, two kinds of edge effect in the TEM and etching processes are analyzed. Additionally, a parameter study of TEM etching involving transferred charge, applied pressure, and etching roughness is conducted to evaluate this method. The study shows that TEM etching is a promising manufacture method for glass with low process temperature, three-dimensional self-control ability, and low equipment requirement. PMID:28772521

  20. Sputtering. [as deposition technique in mechanical engineering

    NASA Technical Reports Server (NTRS)

    Spalvins, T.

    1976-01-01

    This paper primarily reviews the potential of using the sputtering process as a deposition technique; however, the manufacturing and sputter etching aspects are also discussed. Since sputtering is not regulated by classical thermodynamics, new multicomponent materials can be developed in any possible chemical composition. The basic mechanism for dc and rf sputtering is described. Sputter-deposition is described in terms of the unique advantageous features it offers such as versatility, momentum transfer, stoichiometry, sputter-etching, target geometry (coating complex surfaces), precise controls, flexibility, ecology, and sputtering rates. Sputtered film characteristics, such as strong adherence and coherence and film morphology, are briefly evaluated in terms of varying the sputtering parameters. Also described are some of the specific industrial areas which are turning to sputter-deposition techniques.

  1. Role of strained nano-regions in the formation of subgrains in CaCu3Ti4O12

    NASA Astrophysics Data System (ADS)

    Fang, Tsang-Tse; Wang, Yong-Huei; Kuo, Jui-Chao

    2011-07-01

    Single-phase CaCu3Ti4O12 (CCTO) was synthesized by solid-state reaction. Electron backscatter diffraction, scanning electron microscopy, and atomic force microscopy were adopted to characterize the grain orientation, microstructure, and surface morphology of the CCTO samples with or without thermal etching. Bump strained nano-regions induced by the local compositional disorder at a nano-scale have been discovered, being the origin of the formation of subgrains in CCTO. The proposed mechanism for the formation of subgrains involves the formation of etched pits and subboundaries pertaining to the strained nano-regions rather than dislocation displacement. The dielectric response inside the grains of CCTO relevant to the strained nano-regions is also discussed.

  2. Reactive ion etching of GaN using BCl 3, BCl 3/Ar and BCl 3/ N 2 gas plasmas

    NASA Astrophysics Data System (ADS)

    Basak, D.; Nakanishi, T.; Sakai, S.

    2000-04-01

    Reactive ion etching (RIE) of GaN has been performed using BCl 3 and additives, Ar and N 2, to BCl 3 plasma. The etch rate, surface roughness and the etch profile have been investigated. The etch rate of GaN is found to be 104 nm/min at rf power of 200 W, pressure of 2 Pa, with 9.5 sccm flow rate of BCl 3. The addition of 5 sccm of Ar to 9.5 sccm of BCl 3 reduces the etch rate of GaN while the addition of N 2 does not influence the etch rate significantly. The RIE of GaN layer with BCl 3/Ar and BCl 3/N 2 results in a smoother surface compared to surfaces etched with BCl 3 only. The etched side-wall in BCl 3 plasma makes an angle of 60° with the normal surface, and the angle of inclination is more in cases of BCl 3/Ar and BCl 3/N 2 plasmas. The RIE induced damage to the surface is measured qualitatively by PL measurements. It is observed that the damage to the etched surfaces is similar for all the plasmas.

  3. Effect of Hydrofluoric Acid Etching Time on Titanium Topography, Chemistry, Wettability, and Cell Adhesion

    PubMed Central

    Zahran, R.; Rosales Leal, J. I.; Rodríguez Valverde, M. A.; Cabrerizo Vílchez, M. A.

    2016-01-01

    Titanium implant surface etching has proven an effective method to enhance cell attachment. Despite the frequent use of hydrofluoric (HF) acid, many questions remain unresolved, including the optimal etching time and its effect on surface and biological properties. The objective of this study was to investigate the effect of HF acid etching time on Ti topography, surface chemistry, wettability, and cell adhesion. These data are useful to design improved acid treatment and obtain an improved cell response. The surface topography, chemistry, dynamic wetting, and cell adhesiveness of polished Ti surfaces were evaluated after treatment with HF acid solution for 0, 2; 3, 5, 7, or 10 min, revealing a time-dependent effect of HF acid on their topography, chemistry, and wetting. Roughness and wetting increased with longer etching time except at 10 min, when roughness increased but wetness decreased. Skewness became negative after etching and kurtosis tended to 3 with longer etching time. Highest cell adhesion was achieved after 5–7 min of etching time. Wetting and cell adhesion were reduced on the highly rough surfaces obtained after 10-min etching time. PMID:27824875

  4. Enhancing osseointegration of orthopedic implants with titania nanotube surfaces

    NASA Astrophysics Data System (ADS)

    Baker, Erin A.

    Introduction: As joint arthroplasty surgical procedures increase annually, the development of new strategies, including novel materials and surface modifications, to attain solid bone-implant fixation are needed to increase implant terms of service. In this study, we evaluate two morphologies of titania nanotubes in both in vitro and in vivo experiments to quantify osseointegrative potential and material-level biocompatibility. Materials and Methods: Samples were prepared via an electrochemical etching process. Two different titania nanotube (TiNT) morphologies were produced, Aligned and Trabecular. For the in vitro experiment, Sprague Dawley (SD) rat marrow-derived bone marrow cells (BMC) were seeded on samples. Alkaline phosphatase (ALP) activity, osteocalcin (OC) expression, expression of relevant genes as well as cell attachment and morphology were assessed. In the first in vivo experiment, Kirschner wires were implanted unilaterally into SD rat femora with a TiNT-etched or unmodified (Control) implant. General health assessments and weekly body weights were recorded. At a 12-week endpoint, hematologic, systemic metal ion, and histologic analyses were performed. For the second in vivo experiment, Kirschner wires were implanted bilaterally into SD rat femora, with a TiNT-etched implant in one femora and unmodified (Control) implant as an internal control. At 4- and 12-week endpoints, femora were assessed via biomechanics, undecalcified histology, micro-computed tomography (muCT), and backscattered electron imaging (BEI) to characterize de novo bone formation. Results: In vitro experiments demonstrated BMC attachment and differentiation into osteoblasts as well as greater ALP activity, OC expression, total cell counts, and gene expression (of Col1a1, IGF-1, and osteonectin) on TiNT surfaces versus Controls. Cells on TiNT-etched substrates were smaller in diameter and more eccentric than Controls. In the first in vivo experiment, there were significant differences in body weight between groups at Weeks 9 and 11. There were no significant differences in red or white blood cell function between TiNT groups and Control. Aluminum levels in the lungs were significantly greater in the Trabecular TiNT group compared to Control. Histologic analysis showed significantly fewer granulocytes and neutrophils in the distal region of Trabecular TiNT-implanted femora as well as significantly fewer foreign body giant/multinucleated cells and neutrophils in the midshaft region of Aligned TiNT-implanted femora versus Controls. In the second in vivo experiment, at 12 weeks, microCT analysis showed TiNT implants generated greater bone formation than Controls. Histologic analysis demonstrated 1.5 times greater bone-implant contact in TiNT groups than Controls at 12 weeks. TiNT groups exhibited 1.3 to 3.7 times greater strength of fixation than Controls during pull-out testing. Discussion and Conclusions: In vitro data confirmed BMC attachment and differentiation into osteoblasts as well as osteoblastic phenotypic behavior. A clinically-relevant in vivo model of femoral intramedullary fixation, showed increased bone formation and quality in femora implanted with TiNT-etched implants versus Controls. A second in vivo study showed that TiNT surfaces do not generate systemic effects and may beneficially modulate the periprosthetic inflammatory environment.

  5. In vitro and in vivo evaluation of SLA titanium surfaces with further alkali or hydrogen peroxide and heat treatment.

    PubMed

    Zhang, E W; Wang, Y B; Shuai, K G; Gao, F; Bai, Y J; Cheng, Y; Xiong, X L; Zheng, Y F; Wei, S C

    2011-04-01

    The present study aimed to evaluate the bioactivity of titanium surfaces sandblasted with large-grit corundum and acid etched (SLA) plus further alkali or hydrogen peroxide and heat treatment for dental implant application. Pure titanium disks were mechanically polished as control surface (Ti-control) and then sandblasted with large-grit corundum and acid etched (SLA). Further chemical modifications were conducted using alkali and heat treatment (ASLA) and hydrogen peroxide and heat treatment (HSLA) alternatively. The surface properties were characterized by scanning electron microscopy (SEM), x-ray photoelectron spectroscopy (XPS), and contact angle and roughness measurements. Further evaluation of surface bioactivity was conducted by MC3T3-E1 cell attachment, proliferation, morphology, alkaline phosphatase (ALP) activity and calcium deposition on the sample surfaces. After insertion in the beagle's mandibula for a specific period, cylindrical implant samples underwent micro-CT examination and then histological examination. It was found that ASLA and HSLA surfaces significantly increased the surface wettability and MC3T3-E1 cell attachment percentage, ALP activity and the quality of calcium deposition in comparison with simple SLA and Ti-control surfaces. Animal studies showed good osseointegration of ASLA and HSLA surfaces with host bone. In conclusion, ASLA and HSLA surfaces enhanced the bioactivity of the traditional SLA surface by integrating the advantages of surface topography, composition and wettability.

  6. Effects of the micro-nano surface topography of titanium alloy on the biological responses of osteoblast.

    PubMed

    Yin, Chengcheng; Zhang, Yanjing; Cai, Qing; Li, Baosheng; Yang, Hua; Wang, Heling; Qi, Hua; Zhou, Yanmin; Meng, Weiyan

    2017-03-01

    In clinical applications, osseointegration is essential for the long-term stability of dental implants. Inspired by the hierarchical structure of natural bone, we applied the electrochemical etching (EC) technique to form a micro-nano structure on a titanium alloy (Ti6Al4V) substrate, called EC surface. Sand blasting and acid etching (SLA) and machined (M) methods were employed to generate micro and smooth textures, respectively, as the control groups. The surface topographies of the three substrates were characterized using scanning electron microscopy (SEM). Then, human osteoblast-like cells (MG63) were cultured on substrates, and adhesion, proliferation, morphology, alkaline phosphatase activity (ALP), and gene expression levels of Runt-related transcription factor 2 (RUNX2), osteocalcin (OCN), osteopontin (OPN), and type I collagen (COLIA 1) were analyzed. MG63 cells cultured on the EC Ti alloy substrates displayed better cell adhesion, significant proliferation, and a higher production level of ALP, gene expressions of RUNX2, OCN, OPN and COLIA 1 (p < 0.01 or p < 0.05) compared with those of SLA and M substrates. These results indicate that the micro-nano structure fabricated by electrochemical etching method is beneficial for the biological functions of MG63 cells and may be a promising candidate in dental implants. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 105A: 757-769, 2017. © 2016 Wiley Periodicals, Inc.

  7. Tailored Voltage Waveforms in an SF6 /O2 discharge: slope asymmetry and its effect on surface nanotexturing of silicon

    NASA Astrophysics Data System (ADS)

    Fischer, G.; Drahi, E.; Poulain, G.; Bruneau, B.; Johnson, E. V.

    2016-09-01

    The nanotexturing of the surface of a crystalline silicon (c-Si) wafer for improved photovoltaic performance can be achieved through the use of a SF6 /O2 capacitively coupled reactive ion etching plasma. In this study, we attempt to modify the texturing conditions by taking advantage of slope asymmetries of Tailored Voltage Waveform (TVW) excitation. We show that TVW shapes resembling ``sawtooths'', presenting a large slope asymmetry, induce high ionization asymmetries in the discharge, and that the dominance of this effect strongly depends on both gas mixture and pressure. These asymmetries have been previously observed in other electronegative gas and are due to differing plasma sheath dynamics at powered and grounded electrode in a discharge operating in drift-ambipolar mode. The texturing of c-Si in SF6 /O2 occurs through competing mechanisms, including etching by fluorine radicals and in-situ deposition of micro-masking species. The relative fluxes of etching and passivating species are expected to be strongly varied due to the plasma asymmetry. Morphological and optical characterization of textured c-Si surfaces will give more insight into both the plasma properties and the mechanisms involved in dry nanotexturing. This project has been supported by the French Government in the frame of the program of investment for the future (Programme d'Investissement d'Avenir - ANR-IEED-002-01).

  8. Selective Growth of Metallic and Semiconducting Single Walled Carbon Nanotubes on Textured Silicon.

    PubMed

    Jang, Mira; Lee, Jongtaek; Park, Teahee; Lee, Junyoung; Yang, Jonghee; Yi, Whikun

    2016-03-01

    We fabricated the etched Si substrate having the pyramidal pattern size from 0.5 to 4.2 μm by changing the texturing process parameters, i.e., KOH concentration, etching time, and temperature. Single walled carbon nanotubes (SWNTs) were then synthesized on the etched Si substrates with different pyramidal pattern by chemical vapor deposition. We investigated the optical and electronic properties of SWNT film grown on the etched Si substrates of different morphology by using scanning electron microscopy, Raman spectroscopy and conducting probe atomic force microscopy. We confirmed that the morphology of substrate strongly affected the selective growth of the SWNT film. Semiconducting SWNTs were formed on larger pyramidal sized Si wafer with higher ratio compared with SWNTs on smaller pyramidal sized Si.

  9. Method of sputter etching a surface

    DOEpatents

    Henager, Jr., Charles H.

    1984-01-01

    The surface of a target is textured by co-sputter etching the target surface with a seed material adjacent thereto, while the target surface is maintained at a pre-selected temperature. By pre-selecting the temperature of the surface while sputter etching, it is possible to predetermine the reflectance properties of the etched surface. The surface may be textured to absorb sunlight efficiently and have minimal emittance in the infrared region so as to be well-suited for use as a solar absorber for photothermal energy conversion.

  10. Method of sputter etching a surface

    DOEpatents

    Henager, C.H. Jr.

    1984-02-14

    The surface of a target is textured by co-sputter etching the target surface with a seed material adjacent thereto, while the target surface is maintained at a pre-selected temperature. By pre-selecting the temperature of the surface while sputter etching, it is possible to predetermine the reflectance properties of the etched surface. The surface may be textured to absorb sunlight efficiently and have minimal emittance in the infrared region so as to be well-suited for use as a solar absorber for photothermal energy conversion. 4 figs.

  11. Dissolution of uranophane: An AFM, XPS, SEM and ICP study

    NASA Astrophysics Data System (ADS)

    Schindler, Michael; Freund, Michael; Hawthorne, Frank C.; Burns, Peter C.; Maurice, Patricia A.

    2009-05-01

    Dissolution experiments on single crystals of uranophane and uranophane-β, Ca(H 2O) 5[(UO 2)(SiO 3(OH)] 2, from the Shinkolobwe mine of the Democratic Republic of Congo, were done in an aqueous HCl solution of pH 3.5 for 3 h, in HCl solutions of pH 2 for 5, 10 and 30 min, and in Pb 2+-, Ba-, Sr-, Ca- and Mg-HCl solutions of pH 2 for 30 min. The basal surfaces of the treated uranophane crystals were examined using atomic-force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). Solutions after dissolution experiments on single crystals and synthetic powders were analysed with inductively coupled plasma-optical emission spectroscopy (ICP-OES) and mass spectroscopy (ICP-MS). The morphology of the observed etch pits (measured by AFM) were compared to the morphology, predicted on the basis of the bond-valence deficiency of polyhedron chains along the edges of the basal surface. Etch pits form in HCl solutions of pH 2. Their decrease in depth with the duration of the dissolution experiment is explained with the stepwave dissolution model, which describes the lowering of the surrounding area of an etch pit with continuous waves of steps emanated from the etch pit into the rest of the crystal surface. Hillocks form in an HCl solution of pH 3.5, and the chemical composition of the surface (as indicated by XPS) shows that these hillocks are the result of the precipitation of a uranyl-hydroxy-hydrate phase. Well-orientated hillocks form on the surface of uranophane in a SrCl 2-HCl solution of pH 2. They are part of an aged silica coating of composition Si 2O 2(OH) 4(H 2O) n. An amorphous layer forms on the surface of uranophane in a MgCl 2-HCl solution of pH 2, which has a composition and structure similar to silicic acid. Small crystallites of uranyl-hydroxy-hydrate phases form on the surface of uranophane after treatment in Pb(NO 3) 2-HCl and BaCl 2-HCl solutions of pH 2. Dissolution experiments on synthetic uranophane powders show that in the early stage of the experiments, the dissolution rate of uranophane increase in the sequence Pb(NO 3) 2-HCl < BaCl 2-HCl < CaCl 2-HCl < HCl < SrCl 2-HCl < MgCl 2-HCl, indicating that the dissolution of uranophane is more enhanced in solutions containing divalent cations of small ionic radii and high Lewis acidity (Mg, MgCl +).

  12. Interface and transport properties of metallization contacts to flat and wet-etching roughed N-polar n-type GaN.

    PubMed

    Wang, Liancheng; Liu, Zhiqiang; Guo, Enqing; Yang, Hua; Yi, Xiaoyan; Wang, Guohong

    2013-06-26

    The electrical characteristics of metallization contacts to flat (F-sample, without wet-etching roughed) and wet-etching roughed (R-sample) N-polar (Nitrogen-polar) n-GaN have been investigated. R-sample shows higher contact resistance (Rc) to Al/Ti/Au (~2.5 × 10(-5) Ω·cm(2)) and higher Schottky barriers height (SBH, ~0.386 eV) to Ni/Au, compared with that of F-sample (~1.3 × 10(-6) Ω·cm(2), ~0.154 eV). Reasons accounting for this discrepancy has been detail investigated and discussed: for R-sample, wet-etching process caused surface state and spontaneous polarization variation will degraded its electrical characteristics. Metal on R-sample shows smoother morphology, however, the effect of metal deposition state on electrical characteristics is negligible. Metallization contact area for both samples has also been further considered. Electrical characteristics of metallization contact to both samples show degradation upon annealing. The VLED chip (1 mm × 1 mm), which was fabricated on the basis of a hybrid scheme, coupling the advantage of F- and R-sample, shows the lowest forward voltage (2.75 V@350 mA) and the highest light output power.

  13. Toward Edge-Defined Holey Boron Nitride Nanosheets

    NASA Technical Reports Server (NTRS)

    Lin, Yi; Liao, Yunlong; Chen, Zhongfan; Connell, John W.

    2015-01-01

    "Holey" two-dimensional (2D) nanosheets with well-defined holy morphology and edge chemistry are highly desirable for applications such as energy storage, catalysis, sensing, transistors, and molecular transport/separation. For example, holey grapheme is currently under extensive investigation for energy storage applications because of the improvement in ion transport due to through the thickness pathways provided by the holes. Without the holes, the 2D materials have significant limitations for such applications in which efficient ion transport is important. As part of an effort to apply this approach to other 2D nanomaterials, a method to etch geometrically defined pits or holes on the basal plane surface of hexagonal boron nitride (h-BN) nanosheets has been developed. The etching, conducted via heating in ambient air using metal nanoparticles as catalysts, was facile, controllable, and scalable. Starting h-BN layered crystals were etched and subsequently exfoliated into boron nitride nanosheets (BNNSs). The as-etched and exfoliated h-BN nanosheets possessed defined pit and hole shapes that were comprised of regulated nanostructures at the edges. The current finding are the first step toward the bulk preparation of holey BNNSs with defined holes and edges.

  14. A macro- and nanostructure evaluation of a novel dental implant.

    PubMed

    Tetè, Stefano; Mastrangelo, Filiberto; Traini, Tonino; Vinci, Raffaele; Sammartino, Gilberto; Marenzi, Gaetano; Gherlone, Enrico

    2008-09-01

    Success in implant dentistry also comes from the implant macrodesign and nanostructure of its surface. Titanium implant surface treatments have been shown to enhance osseointegration, maximize bone healing, and bone-to-implant contact for predictable clinical results. The aim of the study, was to evaluate the geometric macrodesign and the surface nanostructure of a novel dental implant full contact covering (FCC) obtained by electrochemical procedures. FCC implants were analyzed by scanning electronic microscope, profilometer, and x-ray photoelectron spectroscopy and compared with commercial sandblasted and sandblasted, large-grit acid-etched dental implants. Sample analysis allowed to distinguish the different implant macrodesigns, the step and the profile of the coils that cover the fixture, and the surface characteristics. FCC implant showed novel macro-characteristic of crestal module, coils, and apical zone compared with sandblasted and sandblasted and acid-etched dental implants. Moreover, the FCC nanostructure surface showed roughness values statistically higher than the 2 other surfaces, with a more homogeneity in a peaks and valleys arrangement. Finally, the x-ray photoelectron spectroscopy analysis detected differences between the examined surfaces, with the presence of several contaminants according to the different treatment procedures. Research on new macrostructures and nano morphology should result in a better qualitative and quantitative osseointegration response, with a predictability of the clinical results and long-term success of the implants.

  15. FY07 LDRD Final Report A Fracture Mechanics and Tribology Approach to Understanding Subsurface Damage on Fused Silica during Grinding and Polishing

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Suratwala, T I; Miller, P E; Menapace, J A

    The objective of this work is to develop a solid scientific understanding of the creation and characteristics of surface fractures formed during the grinding and polishing of brittle materials, specifically glass. In this study, we have experimentally characterized the morphology, number density, and depth distribution of various surface cracks as a function of various grinding and polishing processes (blanchard, fixed abrasive grinding, loose abrasive, pitch polishing and pad polishing). Also, the effects of load, abrasive particle (size, distribution, foreign particles, geometry, velocity), and lap material (pitch, pad) were examined. The resulting data were evaluated in terms of indentation fracture mechanicsmore » and tribological interactions (science of interacting surfaces) leading to several models to explain crack distribution behavior of ground surfaces and to explain the characteristics of scratches formed during polishing. This project has greatly advanced the scientific knowledge of microscopic mechanical damage occurring during grinding and polishing and has been of general interest. This knowledge-base has also enabled the design and optimization of surface finishing processes to create optical surfaces with far superior laser damage resistance. There are five major areas of scientific progress as a result of this LDRD. They are listed in Figure 1 and described briefly in this summary below. The details of this work are summarized through a number of published manuscripts which are included this LDRD Final Report. In the first area of grinding, we developed a technique to quantitatively and statistically measure the depth distribution of surface fractures (i.e., subsurface damage) in fused silica as function of various grinding processes using mixtures of various abrasive particles size distributions. The observed crack distributions were explained using a model that extended known, single brittle indentation models to an ensemble of loaded, sliding particles. The model illustrates the importance of the particle size distribution of the abrasive and its influence on the resulting crack distribution. The results of these studies are summarized in references 1-7. In the second area of polishing, we conducted a series of experiments showing the influence of rogue particles (i.e., particles in the polishing slurry that are larger than base particles) on the creation of scratches on polished surfaces. Scratches can be thought of a as a specific type of sub-surface damage. The characteristics (width, length, type of fractures, concentration) were explained in terms of the rogue particle size, the rogue particle material, and the viscoelastic properties of the lap. The results of these studies are summarized in references 6-7. In the third area of etching, we conducted experiments aimed at understanding the effect of HF:NH{sub 4}F acid etching on surface fractures on fused silica. Etching can be used as a method: (a) to expose sub-surface mechanical damage, (b) to study the morphology of specific mechanical damage occurring by indentation, and (c) to convert a ground surface containing a high concentration of sub-surface mechanical damage into surface roughness. Supporting models have been developed to describe in detail the effect of etching on the morphology and evolution of surface cracks. The results of these studies are summarized in references 8-9. In the fourth area of scratch forensics or scratch fractography, a set of new scratch forensic rule-of-thumbs were developed in order to aid the optical fabricator and process engineer to interpret the cause of scratches and digs on surfaces. The details of how these rules were developed are described in each of the references included in this summary (1-9). Figure 2 provides as a summary of some of the more commonly used rules-of-thumbs that have been developed in this study. In the fifth and final area of laser damage, we demonstrated that the removal of such surface fractures from the surface during optical fabrication can dramatically improve the laser damage.« less

  16. Mesoporous carbon-supported Pd nanoparticles with high specific surface area for cyclohexene hydrogenation: Outstanding catalytic activity of NaOH-treated catalysts

    NASA Astrophysics Data System (ADS)

    Puskás, R.; Varga, T.; Grósz, A.; Sápi, A.; Oszkó, A.; Kukovecz, Á.; Kónya, Z.

    2016-06-01

    Extremely high specific surface area mesoporous carbon-supported Pd nanoparticle catalysts were prepared with both impregnation and polyol-based sol methods. The silica template used for the synthesis of mesoporous carbon was removed by both NaOH and HF etching. Pd/mesoporous carbon catalysts synthesized with the impregnation method has as high specific surface area as 2250 m2/g. In case of NaOH-etched impregnated samples, the turnover frequency of cyclohexene hydrogenation to cyclohexane at 313 K was obtained 14 molecules • site- 1 • s- 1. The specific surface area of HF-etched samples was higher compared to NaOH-etched samples. However, catalytic activity was 3-6 times higher on NaOH-etched samples compared to HF-etched samples, which can be attributed to the presence of sodium and surface hydroxylgroups of the catalysts etched with NaOH solution.

  17. Wrinkles and Folds of Activated Graphene Nanosheets as Fast and Efficient Adsorptive Sites for Hydrophobic Organic Contaminants.

    PubMed

    Wang, Jun; Chen, Baoliang; Xing, Baoshan

    2016-04-05

    To create more wrinkles and folds as available adsorption sites, graphene nanosheets (GNS) were thermally treated with KOH for morphological alteration. The surface structures and properties of the activated graphene nanosheets (AGN) were characterized by BET-N2, SEM, TEM, Raman, XRD, XPS, and FTIR. After KOH etching, the highly crystal structure was altered, self-aggregation of graphene layers were evidently relieved, and more single to few layer graphene nanosheets were created with wrinkles and folds. Also both specific surface area and micropore volume of AGN increased relative to GNS. The adsorption of AGN toward p-nitrotoluene, naphthalene and phenanthrene were greatly enhanced in comparison with GNS, and gradually promoted with increasing degree of KOH etching. Adsorption rate of organic contaminants on AGN was very fast and efficient, whereas small molecules showed higher adsorption rates due to the more porous surface of graphene. In addition to π-π interaction, the high affinities of p-nitrotoluene to AGN are suggested from strong electron charge transfer interactions between nitro groups on p-nitrotoluene and defect sites of AGN. A positively linear correlation between organic molecule uptake and the micropore volume of AGN indicated that pore-filling mechanism may play an important role in adsorption. Morphological wrinkles and folds of graphene nanosheets can be regulated to enhance the adsorption capability and kinetics for efficient pollutant removal and to selectively preconcentrate adsorbates with different sizes for detection.

  18. Flower-like ZnO nanorod arrays grown on HF-etched Si (111): constraining relation between ZnO seed layer and Si (111)

    NASA Astrophysics Data System (ADS)

    Brahma, Sanjaya; Liu, C.-W.; Huang, R.-J.; Chang, S.-J.; Lo, K.-Y.

    2015-11-01

    We demonstrate the formation of self-assembled homogenous flower-like ZnO nanorods over a ZnO seed layer deposited on a HF-etched Si (111) substrate. The typical flower-like morphology of ZnO nanorod arrays is ascribed to the formation of the island-like seed layer which is deposited by the drop method followed by annealing at 300 °C. The island-like ZnO seed layer consists of larger ZnO grains, and is built by constraining of the Si (111) surface due to pattern matching. Pattern matching of Si with ZnO determines the shape and size of the seed layer and this controls the final morphology of ZnO nanorods to be either flower like or vertically aligned. The high quality of the island-like ZnO seed layer enhances the diameter and length of ZnO nanorods. Besides, while the amorphous layer formed during the annealing process would influence the strained ZnO grain, that subsequent amorphous layer will not block the constraining between the ZnO grain and the substrate.

  19. Quenching influence of cell culture medium on photoluminescence and morphological structure of porous silicon

    NASA Astrophysics Data System (ADS)

    Unal, Bayram

    2011-10-01

    In this work, the degradation of visible photoluminescence of porous silicon (PSi) under the influential actions of cell culture medium has been mainly studied in order to comprehend the quenching mechanisms necessitating the cell growth on spongy-like-silicon structures, which could form either micro- and/or nano-dimensional morphologies after stain-etching of the poly- or single-crystalline Si surfaces. Quenching effect of the neuron culture medium on visibly luminescent and non-luminescent porous silicon is found to be quite obvious so that this step of the culture process, especially, over nanostructured silicon is extremely essential for a variety of bionanotechnological applications.

  20. DOE Office of Scientific and Technical Information (OSTI.GOV)

    Yin Yunpeng; Sawin, Herbert H.

    The impact of etching kinetics and etching chemistries on surface roughening was investigated by etching thermal silicon dioxide and low-k dielectric coral materials in C{sub 4}F{sub 8}/Ar plasma beams in an inductive coupled plasma beam reactor. The etching kinetics, especially the angular etching yield curves, were measured by changing the plasma pressure and the feed gas composition which influence the effective neutral-to-ion flux ratio during etching. At low neutral-to-ion flux ratios, the angular etching yield curves are sputteringlike, with a peak around 60 deg. -70 deg. off-normal angles; the surface at grazing ion incidence angles becomes roughened due to ionmore » scattering related ion-channeling effects. At high neutral-to-ion flux ratios, ion enhanced etching dominates and surface roughening at grazing angles is mainly caused by the local fluorocarbon deposition induced micromasking mechanism. Interestingly, the etched surfaces at grazing angles remain smooth for both films at intermediate neutral-to-ion flux ratio regime. Furthermore, the oxygen addition broadens the region over which the etching without roughening can be performed.« less

  1. Tin doped indium oxide anodes with artificially controlled nano-scale roughness using segregated Ag nanoparticles for organic solar cells

    NASA Astrophysics Data System (ADS)

    Kim, Hyo-Joong; Ko, Eun-Hye; Noh, Yong-Jin; Na, Seok-In; Kim, Han-Ki

    2016-09-01

    Nano-scale surface roughness in transparent ITO films was artificially formed by sputtering a mixed Ag and ITO layer and wet etching of segregated Ag nanoparticles from the surface of the ITO film. Effective removal of self-segregated Ag particles from the grain boundaries and surface of the crystalline ITO film led to a change in only the nano-scale surface morphology of ITO film without changes in the sheet resistance and optical transmittance. A nano-scale rough surface of the ITO film led to an increase in contact area between the hole transport layer and the ITO anode, and eventually increased the hole extraction efficiency in the organic solar cells (OSCs). The heterojunction OSCs fabricated on the ITO anode with a nano-scale surface roughness exhibited a higher power conversion efficiency of 3.320%, than that (2.938%) of OSCs made with the reference ITO/glass. The results here introduce a new method to improve the performance of OSCs by simply modifying the surface morphology of the ITO anodes.

  2. Independence of surface morphology and reconstruction during the thermal preparation of perovskite oxide surfaces

    NASA Astrophysics Data System (ADS)

    Jäger, Maren; Teker, Ali; Mannhart, Jochen; Braun, Wolfgang

    2018-03-01

    Using a CO2 laser to directly heat the crystals from the back side, SrTiO3 substrates may be thermally prepared in situ for epitaxy without the need for ex-situ etching and annealing. We find that the formation of large terraces with straight steps at 900-1100 °C is independent of the formation of the ideal surface reconstruction for epitaxy, which requires temperatures in excess of 1200 °C to complete. The process may be universal, at least for perovskite oxide surfaces, as it also works, at different temperatures, for LaAlO3 and NdGaO3, two other widely used oxide substrate materials.

  3. Electroplating chromium on CVD SiC and SiCf-SiC advanced cladding via PyC compatibility coating

    NASA Astrophysics Data System (ADS)

    Ang, Caen; Kemery, Craig; Katoh, Yutai

    2018-05-01

    Electroplating Cr on SiC using a pyrolytic carbon (PyC) bond coat is demonstrated as an innovative concept for coating of advanced fuel cladding. The quantification of coating stress, SEM morphology, XRD phase analysis, and debonding test of the coating on CVD SiC and SiCf-SiC is shown. The residual tensile stress (by ASTM B975) of electroplated Cr is > 1 GPa prior to stress relaxation by microcracking. The stress can remove the PyC/Cr layer from SiC. Surface etching of ∼20 μm and roughening to Ra > 2 μm (by SEM observation) was necessary for successful adhesion. The debonding strength (by ASTM D4541) of the coating on SiC slightly improved from 3.6 ± 1.4 MPa to 5.9 ± 0.8 MPa after surface etching or machining. However, this improvement is limited due to the absence of an interphase, and integrated CVI processing may be required for further advancement.

  4. Transfer-free, lithography-free and fast growth of patterned CVD graphene directly on insulators by using sacrificial metal catalyst.

    PubMed

    Dong, Yibo; Xie, Yiyang; Xu, Chen; Fu, Yafei; Fan, Xing; Li, Xuejian; Wang, Le; Xiong, Fangzhu; Guo, Weiling; Pan, Guanzhong; Wang, Qiuhua; Qian, Fengsong; Sun, Jie

    2018-06-14

    Chemical vapor deposited graphene suffers from two problems: transfer from metal catalysts to insulators, and photoresist induced degradation during patterning. Both result in macroscopic and microscopic damages such as holes, tears, doping, and contamination, translated into property and yield dropping. We attempt to solve the problems simultaneously. A nickel thin film is evaporated on SiO 2 as a sacrificial catalyst, on which surface graphene is grown. A polymer (PMMA) support is spin-coated on the graphene. During the Ni wet etching process, the etchant can permeate the polymer, making the etching efficient. The PMMA/graphene layer is fixed on the substrate by controlling the surface morphology of Ni film during the graphene growth. After etching, the graphene naturally adheres to the insulating substrate. By using this method, transfer-free, lithography-free and fast growth of graphene realized. The whole experiment has good repeatability and controllability. Compared with graphene transfer between substrates, here, no mechanical manipulation is required, leading to minimal damage. Due to the presence of Ni, the graphene quality is intrinsically better than catalyst-free growth. The Ni thickness and growth temperature are controlled to limit the number of layers of graphene. The technology can be extended to grow other two-dimensional materials with other catalysts.

  5. Influence of duration of phosphoric acid pre-etching on bond durability of universal adhesives and surface free-energy characteristics of enamel.

    PubMed

    Tsujimoto, Akimasa; Barkmeier, Wayne W; Takamizawa, Toshiki; Watanabe, Hidehiko; Johnson, William W; Latta, Mark A; Miyazaki, Masashi

    2016-08-01

    The purpose of this study was to evaluate the influence of duration of phosphoric acid pre-etching on the bond durability of universal adhesives and the surface free-energy characteristics of enamel. Three universal adhesives and extracted human molars were used. Two no-pre-etching groups were prepared: ground enamel; and enamel after ultrasonic cleaning with distilled water for 30 s to remove the smear layer. Four pre-etching groups were prepared: enamel pre-etched with phosphoric acid for 3, 5, 10, and 15 s. Shear bond strength (SBS) values of universal adhesive after no thermal cycling and after 30,000 or 60,000 thermal cycles, and surface free-energy values of enamel surfaces, calculated from contact angle measurements, were determined. The specimens that had been pre-etched showed significantly higher SBS and surface free-energy values than the specimens that had not been pre-etched, regardless of the aging condition and adhesive type. The SBS and surface free-energy values did not increase for pre-etching times of longer than 3 s. There were no significant differences in SBS values and surface free-energy characteristics between the specimens with and without a smear layer. The results of this study suggest that phosphoric acid pre-etching of enamel improves the bond durability of universal adhesives and the surface free-energy characteristics of enamel, but these bonding properties do not increase for phosphoric acid pre-etching times of longer than 3 s. © 2016 Eur J Oral Sci.

  6. Correlation between surface chemistry and ion energy dependence of the etch yield in multicomponent oxides etching

    NASA Astrophysics Data System (ADS)

    Bérubé, P.-M.; Poirier, J.-S.; Margot, J.; Stafford, L.; Ndione, P. F.; Chaker, M.; Morandotti, R.

    2009-09-01

    The influence of surface chemistry in plasma etching of multicomponent oxides was investigated through measurements of the ion energy dependence of the etch yield. Using pulsed-laser-deposited CaxBa(1-x)Nb2O6 (CBN) and SrTiO3 thin films as examples, it was found that the etching energy threshold shifts toward values larger or smaller than the sputtering threshold depending on whether or not ion-assisted chemical etching is the dominant etching pathway and whether surface chemistry is enhancing or inhibiting desorption of the film atoms. In the case of CBN films etched in an inductively coupled Cl2 plasma, it is found that the chlorine uptake is inhibiting the etching reaction, with the desorption of nonvolatile NbCl2 and BaCl2 compounds being the rate-limiting step.

  7. Optimization of the buffer surface of CoFeB/MgO/CoFeB-based magnetic tunnel junctions by ion beam milling

    NASA Astrophysics Data System (ADS)

    Martins, L.; Ventura, J.; Ferreira, R.; Freitas, P. P.

    2017-12-01

    Due to their high tunnel magnetoresistance (TMR) ratios at room temperature, magnetic tunnel junctions (MTJs) with a crystalline MgO insulating barrier and CoFeB ferromagnetic (FM) layers are the best candidates for novel magnetic memory applications. To overcome impedance matching problems in electronic circuits, the MgO barrier must have an ultra-low thickness (∼1 nm). Therefore, it is mandatory to optimize the MTJ fabrication process, in order to prevent relevant defects in the MgO barrier that could affect the magnetic and electrical MTJ properties. Here, a smoothing process aiming to decrease the roughness of the buffer surface before the deposition of the full MTJ stack is proposed. An ion beam milling process was used to etch the surface of an MTJ buffer structure with a Ru top layer. The morphologic results prove an effective decrease of the Ru surface roughness with the etching time. The electrical and magnetic results obtained for MTJs with smoothed buffer structures show a direct influence of the buffer roughness and coupling field on the improvement of the TMR ratio.

  8. The Effect of Hydrofluoric Acid Etching Duration on the Surface Micromorphology, Roughness, and Wettability of Dental Ceramics

    PubMed Central

    Ramakrishnaiah, Ravikumar; Alkheraif, Abdulaziz A.; Divakar, Darshan Devang; Matinlinna, Jukka P.; Vallittu, Pekka K.

    2016-01-01

    The current laboratory study is evaluating the effect of hydrofluoric acid etching duration on the surface characteristics of five silica-based glass ceramics. Changes in the pore pattern, crystal structure, roughness, and wettability were compared and evaluated. Seventy-five rectangularly shaped specimens were cut from each material (IPS e-max™, Dentsply Celtra™, Vita Suprinity™, Vita mark II™, and Vita Suprinity FC™); the sectioned samples were finished, polished, and ultrasonically cleaned. Specimens were randomly assigned into study groups: control (no etching) and four experimental groups (20, 40, 80 and 160 s of etching). The etched surfaces’ microstructure including crystal structure, pore pattern, pore depth, and pore width was studied under a scanning electron microscope, and the surface roughness and wettability were analyzed using a non-contact surface profilometer and a contact angle measuring device, respectively. The results were statistically analyzed using one-way analysis of variance (ANOVA) and the post hoc Tukey’s test. The results showed a significant change in the pore number, pore pattern, crystal structure, surface roughness, and wettability with increased etching duration. Etching for a short time resulted in small pores, and etching for longer times resulted in wider, irregular grooves. A significant increase in the surface roughness and wettability was observed with an increase in the etching duration. The findings also suggested a strong association between the surface roughness and wettability. PMID:27240353

  9. Effects of silicon nanowire morphology on optical properties and hybrid solar cell performance

    NASA Astrophysics Data System (ADS)

    Syu, Hong-Jhang; Shiu, Shu-Chia; Hung, Yung-Jr; Lee, San-Liang; Lin, Ching-Fuh

    2012-10-01

    Silicon nanowire (SiNW) arrays are widespread applied on hybrid photovoltaic devices because SiNW arrays can substitute the pyramid texture and anti-reflection coating due to its strong light trapping. Also, SiNWs can be prepared through a cost-efficient process of metal-assisted chemical etching. However, though longer SiNW arrays have lower reflectance, the top of long SiNWs aggregate together to make junction synthesis difficult for SiNW/organic hybrid solar cell. To control and analyze the effect of SiNW array morphology on hybrid solar cells, here we change the metal deposition condition for metal-assisted chemical etching to obtain different SiNW array morphologies. The experiment was separated to two groups, by depositing metal, say, Ag, before etching (BE) or during etching (DE). For group BE, Ag was deposited on n-type Si (n-Si) wafers by thermal evaporation; then etched by H2O2 and HF. For group DE, n-Si was etched by Ag+ and HF directly. Ag was deposited on n-Si during etching process. Afterwards, residual Ag and SiO2 were removed by HNO3 and buffered HF, successively; then Ti and Ag were evaporated on the bottom of Si to be a cathode. Finally, SiNWs were stuck on the poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate) that was spincoated on the ITO coated glass to form SiNW/organic heterojunction. The results show that group BE has reflectance lower than that in group DE in solar spectrum. However, group BE has smaller power conversion efficiency (PCE) of 8.65% and short-circuit current density (Jsc) of 24.94 mA/cm2 than group DE of PCE of 9.47% and Jsc of 26.81 mA/cm2.

  10. Triangle pore arrays fabricated on Si (111) substrate by sphere lithography combined with metal-assisted chemical etching and anisotropic chemical etching

    NASA Astrophysics Data System (ADS)

    Asoh, Hidetaka; Fujihara, Kosuke; Ono, Sachiko

    2012-07-01

    The morphological change of silicon macropore arrays formed by metal-assisted chemical etching using shape-controlled Au thin film arrays was investigated during anisotropic chemical etching in tetramethylammonium hydroxide (TMAH) aqueous solution. After the deposition of Au as the etching catalyst on (111) silicon through a honeycomb mask prepared by sphere lithography, the specimens were etched in a mixed solution of HF and H2O2 at room temperature, resulting in the formation of ordered macropores in silicon along the [111] direction, which is not achievable by conventional chemical etching without a catalyst. In the anisotropic etching in TMAH, the macropores changed from being circular to being hexagonal and finally to being triangular, owing to the difference in etching rate between the crystal planes.

  11. Biotite weathering in a natural forest setting near Derome, Sweden

    NASA Astrophysics Data System (ADS)

    Balogh-Brunstad, Z.; Negrich, K.; Hassenkam, T.; Wallander, H.; Stipp, S. L.

    2011-12-01

    Chemical weathering is a key process in non-nitrogen nutrient acquisition by microbes, fungi and plants. Biotite is commonly the major source of potassium, magnesium and iron. A unique opportunity arose to study natural weathering of biotite by mixed conifer and hardwood forest vegetation and associated microbes and fungi at an abandoned mine site. After the mining stopped over 30 years ago biotite was left behind in piles and the forest vegetation progressively colonized the site. Samples were collected from the top 40 cm of the biotite piles in a vicinity of pine, spruce and birch trees and included some young seedlings. Macroscopic observations documented abundant hyphal growth between the sheets of biotite. We hypothesized that fungal hyphae grow between the sheets to explore the nutrient source and weather the biotite leaving hyphal-sized etched channels on the basal surfaces. Biotite surfaces were examined with atomic force microscopy (AFM) and environmental scanning electron microscopy (ESEM) in their natural state and after removing the biological material from the mineral surfaces. The ESEM images show extensive hyphal colonization and patchy biofilm cover of the entire biotite surface on and within the sheets and at the edges of the particles. Fungal hyphae did not attach strongly to the basal surfaces of the biotite flakes as a result of small particles on the surfaces and the uneven micro-topography. The AFM images illustrate a complex microbial community around the fungal hyphae and detailed fungal morphology. High resolution AFM images show unique globular features of diameter 10-100 nm on all biofilm surfaces. However, removal of the biological material resulted in smooth and un-etched surfaces indicating that either our removal techniques are too invasive and destroy the surface layers of interest, or the etching of the basal surface is not the main mechanism for chemical weathering and base-cation nutrient immobilization in this natural setting. Species-specific interactions at the biofilm-microbe-fungus-mineral interface and spatial distribution in the biotite pile are under further investigation.

  12. Surface morphology and subsurface damaged layer of various glasses machined by 193-nm ArF excimer laser

    NASA Astrophysics Data System (ADS)

    Liao, Yunn-shiuan; Chen, Ying-Tung; Chao, Choung-Lii; Liu, Yih-Ming

    2005-01-01

    Owing to the high bonding energy, most of the glasses are removed by photo-thermal rather than photo-chemical effect when they are ablated by the 193 or 248nm excimer lasers. Typically, the machined surface is covered by re-deposited debris and the sub-surface, sometimes surface as well, is scattered with micro-cracks introduced by thermal stress generated during the process. This study aimed to investigate the nature and extent of the surface morphology and sub-surface damaged (SSD) layer induced by the laser ablation. The effects of laser parameters such as fluence, shot number and repetition rate on the morphology and SSD were discussed. An ArF excimer laser (193 nm) was used in the present study to machine glasses such as soda-lime, Zerodur and BK-7. It is found that the melt ejection and debris deposition tend to pile up higher and become denser in structure under a higher energy density, repetition rate and shot number. There are thermal stress induced lateral cracks when the debris covered top layer is etched away. Higher fluence and repetition rate tend to generate more lateral and median cracks which propagate into the substrate. The changes of mechanical properties of the SSD layer were also investigated.

  13. Atomic force microscopy analysis of different surface treatments of Ti dental implant surfaces

    NASA Astrophysics Data System (ADS)

    Bathomarco, Ti R. V.; Solorzano, G.; Elias, C. N.; Prioli, R.

    2004-06-01

    The surface of commercial unalloyed titanium, used in dental implants, was analyzed by atomic force microscopy. The morphology, roughness, and surface area of the samples, submitted to mechanically-induced erosion, chemical etching and a combination of both, were compared. The results show that surface treatments strongly influence the dental implant physical and chemical properties. An analysis of the length dependence of the implant surface roughness shows that, for scan sizes larger than 50 μm, the average surface roughness is independent of the scanning length and that the surface treatments lead to average surface roughness in the range of 0.37 up to 0.48 μm. It is shown that the implant surface energy is sensitive to the titanium surface area. As the area increases there is a decrease in the surface contact angle.

  14. Microbially mediated barite dissolution in anoxic brines

    USGS Publications Warehouse

    Ouyang, Bingjie; Akob, Denise M.; Dunlap, Darren S.; Renock, Devon

    2017-01-01

    Fluids injected into shale formations during hydraulic fracturing of black shale return with extraordinarily high total-dissolved-solids (TDS) and high concentrations of barium (Ba) and radium (Ra). Barite, BaSO4, has been implicated as a possible source of Ba as well as a problematic mineral scale that forms on internal well surfaces, often in close association with radiobarite, (Ba,Ra)SO4. The dissolution of barite by abiotic processes is well quantified. However, the identification of microbial communities in flowback and produced water necessitates the need to understand barite dissolution in the presence of bacteria. Therefore, we evaluated the rates and mechanisms of abiotic and microbially-mediated barite dissolution under anoxic and hypersaline conditions in the laboratory. Barite dissolution experiments were conducted with bacterial enrichment cultures established from produced water from Marcellus Shale wells located in northcentral Pennsylvania. These cultures were dominated by anaerobic halophilic bacteria from the genus Halanaerobium. Dissolved Ba was determined by ICP-OES and barite surfaces were investigated by SEM and AFM. Our results reveal that: 1) higher amounts of barium (up to ∼5 × ) are released from barite in the presence of Halanaerobium cultures compared to brine controls after 30 days of reaction, 2) etch pits that develop on the barite (001) surface in the presence of Halanaerobium exhibit a morphology that is distinct from those that form during control experiments without bacteria, 3) etch pits that develop in the presence of Halanaerobium exhibit a morphology that is similar to the morphology of etch pits formed in the presence of strong organic chelators, EDTA and DTPA, and 4) experiments using dialysis membranes to separate barite from bacteria suggest that direct contact between the two is not required in order to promote dissolution. These results suggest that Halanaerobium increase the rate of barite dissolution in anoxic and high ionic strength solutions. Additionally, the increase in rate occurs without direct microbe-mineral contact suggesting that metabolites secreted by the bacteria may be responsible for promotion of dissolution. The findings of this study have implications for understanding barium cycling in marine/hypersaline environments, release of barium (and associated radium) from waste solids generated from energy and mining industries, as well as potential for developing new anti-scaling chemicals.

  15. Characterization of perovskite layer on various nanostructured silicon wafer

    NASA Astrophysics Data System (ADS)

    Rostan, Nur Fairuz Mohd; Sepeai, Suhaila; Ramli, Noor Fadhilah; Azhari, Ayu Wazira; Ludin, Norasikin Ahmad; Teridi, Mohd Asri Mat; Ibrahim, Mohd Adib; Zaidi, Saleem H.

    2017-05-01

    Crystalline silicon (c-Si) solar cell dominates 90% of photovoltaic (PV) market. The c-Si is the most mature of all PV technologies and expected to remain leading the PV technology by 2050. The attractive characters of Si solar cell are stability, long lasting and higher lifetime. Presently, the efficiency of c-Si solar cell is still stuck at 25% for one and half decades. Tandem approach is one of the attempts to improve the Si solar cell efficiency with higher bandgap layer is stacked on top of Si bottom cell. Perovskite offers a big potential to be inserted into a tandem solar cell. Perovskite with bandgap of 1.6 to 1.9 eV will be able to absorb high energy photons, meanwhile c-Si with bandgap of 1.124 eV will absorb low energy photons. The high carrier mobility, high carrier lifetime, highly compatible with both solution and evaporation techniques makes perovskite an eligible candidate for perovskite-Si tandem configuration. The solution of methyl ammonium lead iodide (MAPbI3) was prepared by single step precursor process. The perovskite layer was deposited on different c-Si surface structure, namely planar, textured and Si nanowires (SiNWs) by using spin-coating technique at different rotation speeds. The nanostructure of Si surface was textured using alkaline based wet chemical etching process and SiNW was grown using metal assisted etching technique. The detailed surface morphology and absorbance of perovskite were studied in this paper. The results show that the thicknesses of MAPbI3 were reduced with the increasing of rotation speed. In addition, the perovskite layer deposited on the nanostructured Si wafer became rougher as the etching time and rotation speed increased. The average surface roughness increased from ˜24 nm to ˜38 nm for etching time range between 5-60 min at constant low rotation speed (2000 rpm) for SiNWs Si wafer.

  16. Effects of atmospheric air plasma treatment on interfacial properties of PBO fiber reinforced composites

    NASA Astrophysics Data System (ADS)

    Zhang, Chengshuang; Li, Cuiyun; Wang, Baiya; Wang, Bin; Cui, Hong

    2013-07-01

    Poly(p-phenylene benzobisoxazole) (PBO) fiber was modified by atmospheric air plasma treatment. The effects of plasma treatment power and speed on both surface properties of PBO fibers and interfacial properties of PBO/epoxy composites were investigated. Surface chemical composition of PBO fibers were analyzed by X-ray photoelectron spectroscopy (XPS). Surface morphologies of the fibers and interface structures of the composites were examined using scanning electron microscopy (SEM). Interfacial adhesion property of the composites was evaluated by interlaminar shear strength (ILSS). Mechanical properties of PBO multifilament were measured by universal testing machine. The results indicate that atmospheric air plasma treatment introduced some polar or oxygen-containing groups to PBO fiber surfaces, enhanced surface roughness and changed surface morphologies of PBO fibers by plasma etching and oxidative reactions. The plasma treatment also improved interfacial adhesion of PBO/epoxy composites but has little effect on tensile properties of PBO multifilament. The ILSS of PBO/epoxy composites increased to 40.0 MPa after atmospheric air plasma treatment with plasma treatment power of 300 W and treatment speed of 6 m/min.

  17. Characterization of Etch Pit Formation via the Everson-Etching Method on CdZnTe Crystal Surfaces from the Bulk to the Nano-Scale

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Teague, L.; Duff, M.; Cadieux, J.

    2010-09-24

    A combination of atomic force microscopy, optical microscopy, and mass spectrometry was employed to study CdZnTe crystal surface and used etchant solution following exposure of the CdZnTe crystal to the Everson etch solution. We discuss the results of these studies in relationship to the initial surface preparation methods, the performance of the crystals as radiation spectrometers, the observed etch pit densities, and the chemical mechanism of surface etching. Our results show that the surface features that are exposed to etchants result from interactions with the chemical components of the etchants as well as pre-existing mechanical polishing.

  18. DOE Office of Scientific and Technical Information (OSTI.GOV)

    Miao, Yinbin; Mo, Kun; Yao, Tiankai

    Here coordinated experimental efforts to quantitatively correlate crystallographic orientation and surface faceting features in UO2 are reported upon. A sintered polycrystalline UO2 sample was thermally etched to induce the formation of surface faceting features. Synchrotron Laue microdiffraction was used to obtain a precise crystallographic orientation map for the UO2 surface grains. Scanning electron microscopy (SEM) was utilized to collect the detailed information on the surface morphology of the sample. The surface faceting features were found to be highly dependent on the crystallographic orientation. In most cases, Triple-plane structures containing one {100} plane and two {111} planes were found to dominatemore » the surface of UO2. The orientation-faceting relationship established in this study revealed a practical and efficient method of determining crystallographic orientation based on the surface features captured by SEM images.« less

  19. Nanoparticle-based etching of silicon surfaces

    DOEpatents

    Branz, Howard [Boulder, CO; Duda, Anna [Denver, CO; Ginley, David S [Evergreen, CO; Yost, Vernon [Littleton, CO; Meier, Daniel [Atlanta, GA; Ward, James S [Golden, CO

    2011-12-13

    A method (300) of texturing silicon surfaces (116) such to reduce reflectivity of a silicon wafer (110) for use in solar cells. The method (300) includes filling (330, 340) a vessel (122) with a volume of an etching solution (124) so as to cover the silicon surface 116) of a wafer or substrate (112). The etching solution (124) is made up of a catalytic nanomaterial (140) and an oxidant-etchant solution (146). The catalytic nanomaterial (140) may include gold or silver nanoparticles or noble metal nanoparticles, each of which may be a colloidal solution. The oxidant-etchant solution (146) includes an etching agent (142), such as hydrofluoric acid, and an oxidizing agent (144), such as hydrogen peroxide. Etching (350) is performed for a period of time including agitating or stirring the etching solution (124). The etch time may be selected such that the etched silicon surface (116) has a reflectivity of less than about 15 percent such as 1 to 10 percent in a 350 to 1000 nanometer wavelength range.

  20. Controlling the Morphology of Side Chain Liquid Crystalline Block Copolymer Thin Films through Variations in Liquid Crystalline Content

    PubMed Central

    Verploegen, Eric; Zhang, Tejia; Jung, Yeon Sik; Ross, Caroline; Hammond, Paula T.

    2009-01-01

    In this paper we describe methods for manipulating the morphology of side-chain liquid crystalline block copolymers through variations in the liquid crystalline content. By systematically controlling the covalent attachment of side chain liquid crystals to a block copolymer (BCP) backbone, the morphology of both the liquid crystalline (LC) mesophase and the phase segregated BCP microstructures can be precisely manipulated. Increases in LC functionalization lead to stronger preferences for the anchoring of the LC mesophase relative to the substrate and the inter-material dividing surface (IMDS). By manipulating the strength of these interactions the arrangement and ordering of the ultrathin film block copolymer nanostructures can be controlled, yielding a range of morphologies that includes perpendicular and parallel cylinders, as well as both perpendicular and parallel lamellae. Additionally, we demonstrate the utilization of selective etching to create a nanoporous liquid crystalline polymer thin film. The unique control over the orientation and order of the self-assembled morphologies with respect to the substrate will allow for the custom design of thin films for specific nano-patterning applications without manipulation of the surface chemistry or the application of external fields. PMID:18763835

  1. Controlling the morphology of side chain liquid crystalline block copolymer thin films through variations in liquid crystalline content.

    PubMed

    Verploegen, Eric; Zhang, Tejia; Jung, Yeon Sik; Ross, Caroline; Hammond, Paula T

    2008-10-01

    In this paper, we describe methods for manipulating the morphology of side-chain liquid crystalline block copolymers through variations in the liquid crystalline content. By systematically controlling the covalent attachment of side chain liquid crystals to a block copolymer (BCP) backbone, the morphology of both the liquid crystalline (LC) mesophase and the phase-segregated BCP microstructures can be precisely manipulated. Increases in LC functionalization lead to stronger preferences for the anchoring of the LC mesophase relative to the substrate and the intermaterial dividing surface. By manipulating the strength of these interactions, the arrangement and ordering of the ultrathin film block copolymer nanostructures can be controlled, yielding a range of morphologies that includes perpendicular and parallel cylinders, as well as both perpendicular and parallel lamellae. Additionally, we demonstrate the utilization of selective etching to create a nanoporous liquid crystalline polymer thin film. The unique control over the orientation and order of the self-assembled morphologies with respect to the substrate will allow for the custom design of thin films for specific nanopatterning applications without manipulation of the surface chemistry or the application of external fields.

  2. Topical Meeting on Microphysics of Surfaces, Beams, and Adsorbates Held at Santa Fe, New Mexico on 4-6 February 1985.

    DTIC Science & Technology

    1985-12-18

    during excimer laser ablation. Results are %%% Study on the Mechanism of Ion-Assisted Etching, F. H. M. correlated with interferometric measurements of...report on real time interferometric measurements of free electron density and laser induced .,- fluorescence studies of atoms and molecules in the...compared with morphology exam- Ined with Nomarski micrographs and SEM. In addition, the struc- ture and composition of the deposited lines were analysed

  3. Effect of Dentin Wetness on the Bond Strength of Universal Adhesives.

    PubMed

    Choi, An-Na; Lee, Ji-Hye; Son, Sung-Ae; Jung, Kyoung-Hwa; Kwon, Yong Hoon; Park, Jeong-Kil

    2017-10-25

    The effects of dentin wetness on the bond strength and adhesive interface morphology of universal adhesives have been investigated using micro-tensile bond strength (μTBS) testing and confocal laser scanning microscopy (CLSM). Seventy-two human third molars were wet ground to expose flat dentin surfaces. They were divided into three groups according to the air-drying time of the dentin surfaces: 0 (without air drying), 5, and 10 s. The dentin surfaces were then treated with three universal adhesives: G-Premio Bond, Single Bond Universal, and All-Bond Universal in self-etch or etch-and-rinse mode. After composite build up, a μTBS test was performed. One additional tooth was prepared for each group by staining the adhesives with 0.01 wt % of Rhodamine B fluorescent dye for CLSM analysis. The data were analyzed statistically using ANOVA and Tukey's post hoc tests (α = 0.05). Two-way ANOVA showed significant differences among the adhesive systems and dentin moisture conditions. An interaction effect was also observed ( p < 0.05). One-way ANOVA showed that All-Bond Universal was the only material influenced by the wetness of the dentin surfaces. Wetness of the dentin surface is a factor influencing the micro-tensile bond strength of universal adhesives.

  4. Effect of Dentin Wetness on the Bond Strength of Universal Adhesives

    PubMed Central

    Lee, Ji-Hye; Son, Sung-Ae; Jung, Kyoung-Hwa; Kwon, Yong Hoon

    2017-01-01

    The effects of dentin wetness on the bond strength and adhesive interface morphology of universal adhesives have been investigated using micro-tensile bond strength (μTBS) testing and confocal laser scanning microscopy (CLSM). Seventy-two human third molars were wet ground to expose flat dentin surfaces. They were divided into three groups according to the air-drying time of the dentin surfaces: 0 (without air drying), 5, and 10 s. The dentin surfaces were then treated with three universal adhesives: G-Premio Bond, Single Bond Universal, and All-Bond Universal in self-etch or etch-and-rinse mode. After composite build up, a μTBS test was performed. One additional tooth was prepared for each group by staining the adhesives with 0.01 wt % of Rhodamine B fluorescent dye for CLSM analysis. The data were analyzed statistically using ANOVA and Tukey’s post hoc tests (α = 0.05). Two-way ANOVA showed significant differences among the adhesive systems and dentin moisture conditions. An interaction effect was also observed (p < 0.05). One-way ANOVA showed that All-Bond Universal was the only material influenced by the wetness of the dentin surfaces. Wetness of the dentin surface is a factor influencing the micro-tensile bond strength of universal adhesives. PMID:29068404

  5. Simulation of the evolution of fused silica's surface defect during wet chemical etching

    NASA Astrophysics Data System (ADS)

    Liu, Taixiang; Yang, Ke; Li, Heyang; Yan, Lianghong; Yuan, Xiaodong; Yan, Hongwei

    2017-08-01

    Large high-power-laser facility is the basis for achieving inertial confinement fusion, one of whose missions is to make fusion energy usable in the near future. In the facility, fused silica optics plays an irreplaceable role to conduct extremely high-intensity laser to fusion capsule. But the surface defect of fused silica is a major obstacle limiting the output power of the large laser facility and likely resulting in the failure of ignition. To mitigate, or event to remove the surface defect, wet chemical etching has been developed as a practical way. However, how the surface defect evolves during wet chemical etching is still not clearly known so far. To address this problem, in this work, the three-dimensional model of surface defect is built and finite difference time domain (FDTD) method is developed to simulate the evolution of surface defect during etching. From the simulation, it is found that the surface defect will get smooth and result in the improvement of surface quality of fused silica after etching. Comparatively, surface defects (e.g. micro-crack, scratch, series of pinholes, etc.) of a typical fused silica at different etching time are experimentally measured. It can be seen that the simulation result agrees well with the result of experiment, indicating the FDTD method is valid for investigating the evolution of surface defect during etching. With the finding of FDTD simulation, one can optimize the treatment process of fused silica in practical etching or even to make the initial characterization of surface defect traceable.

  6. AFM and SEM study of the effects of etching on IPS-Empress 2 TM dental ceramic

    NASA Astrophysics Data System (ADS)

    Luo, X.-P.; Silikas, N.; Allaf, M.; Wilson, N. H. F.; Watts, D. C.

    2001-10-01

    The aim of this study was to investigate the effects of increasing etching time on the surface of the new dental material, IPS-Empress 2 TM glass ceramic. Twenty one IPS-Empress 2 TM glass ceramic samples were made from IPS-Empress 2 TM ingots through lost-wax, hot-pressed ceramic fabrication technology. All samples were highly polished and cleaned ultrasonically for 5 min in acetone before and after etching with 9.6% hydrofluoric acid gel. The etching times were 0, 10, 20, 30, 60, 90 and 120 s respectively. Microstructure was analysed by scanning electron microscopy (SEM) and atomic force microscopy (AFM) was used to evaluate the surface roughness and topography. Observations with SEM showed that etching with hydrofluoric acid resulted in preferential dissolution of glass matrix, and that partially supported crystals within the glass matrix were lost with increasing etching time. AFM measurements indicated that etching increased the surface roughness of the glass-ceramic. A simple least-squares linear regression was used to establish a relationship between surface roughness parameters ( Ra, RMS), and etching time, for which r2>0.94. This study demonstrates the benefits of combining two microscopic methods for a better understanding of the surface. SEM showed the mode of action of hydrofluoric acid on the ceramic and AFM provided valuable data regarding the extent of surface degradation relative to etching time.

  7. Investigations on diamond nanostructuring of different morphologies by the reactive-ion etching process and their potential applications.

    PubMed

    Kunuku, Srinivasu; Sankaran, Kamatchi Jothiramalingam; Tsai, Cheng-Yen; Chang, Wen-Hao; Tai, Nyan-Hwa; Leou, Keh-Chyang; Lin, I-Nan

    2013-08-14

    We report the systematic studies on the fabrication of aligned, uniform, and highly dense diamond nanostructures from diamond films of various granular structures. Self-assembled Au nanodots are used as a mask in the self-biased reactive-ion etching (RIE) process, using an O2/CF4 process plasma. The morphology of diamond nanostructures is a close function of the initial phase composition of diamond. Cone-shaped and tip-shaped diamond nanostructures result for microcrystalline diamond (MCD) and nanocrystalline diamond (NCD) films, whereas pillarlike and grasslike diamond nanostructures are obtained for Ar-plasma-based and N2-plasma-based ultrananocrystalline diamond (UNCD) films, respectively. While the nitrogen-incorporated UNCD (N-UNCD) nanograss shows the most-superior electron-field-emission properties, the NCD nanotips exhibit the best photoluminescence properties, viz, different applications need different morphology of diamond nanostructures to optimize the respective characteristics. The optimum diamond nanostructure can be achieved by proper choice of granular structure of the initial diamond film. The etching mechanism is explained by in situ observation of optical emission spectrum of RIE plasma. The preferential etching of sp(2)-bonded carbon contained in the diamond films is the prime factor, which forms the unique diamond nanostructures from each type of diamond films. However, the excited oxygen atoms (O*) are the main etching species of diamond film.

  8. Photo-assisted etching of silicon in chlorine- and bromine-containing plasmas

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Zhu, Weiye; Sridhar, Shyam; Liu, Lei

    2014-05-28

    Cl{sub 2}, Br{sub 2}, HBr, Br{sub 2}/Cl{sub 2}, and HBr/Cl{sub 2} feed gases diluted in Ar (50%–50% by volume) were used to study etching of p-type Si(100) in a rf inductively coupled, Faraday-shielded plasma, with a focus on the photo-assisted etching component. Etching rates were measured as a function of ion energy. Etching at ion energies below the threshold for ion-assisted etching was observed in all cases, with Br{sub 2}/Ar and HBr/Cl{sub 2}/Ar plasmas having the lowest and highest sub-threshold etching rates, respectively. Sub-threshold etching rates scaled with the product of surface halogen coverage (measured by X-ray photoelectron spectroscopy) andmore » Ar emission intensity (7504 Å). Etching rates measured under MgF{sub 2}, quartz, and opaque windows showed that sub-threshold etching is due to photon-stimulated processes on the surface, with vacuum ultraviolet photons being much more effective than longer wavelengths. Scanning electron and atomic force microscopy revealed that photo-etched surfaces were very rough, quite likely due to the inability of the photo-assisted process to remove contaminants from the surface. Photo-assisted etching in Cl{sub 2}/Ar plasmas resulted in the formation of 4-sided pyramidal features with bases that formed an angle of 45° with respect to 〈110〉 cleavage planes, suggesting that photo-assisted etching can be sensitive to crystal orientation.« less

  9. Suppression of Lateral Diffusion and Surface Leakage Currents in nBn Photodetectors Using an Inverted Design

    NASA Astrophysics Data System (ADS)

    Du, X.; Savich, G. R.; Marozas, B. T.; Wicks, G. W.

    2018-02-01

    Surface leakage and lateral diffusion currents in InAs-based nBn photodetectors have been investigated. Devices fabricated using a shallow etch processing scheme that etches through the top contact and stops at the barrier exhibited large lateral diffusion current but undetectably low surface leakage. Such large lateral diffusion current significantly increased the dark current, especially in small devices, and causes pixel-to-pixel crosstalk in detector arrays. To eliminate the lateral diffusion current, two different approaches were examined. The conventional solution utilized a deep etch process, which etches through the top contact, barrier, and absorber. This deep etch processing scheme eliminated lateral diffusion, but introduced high surface current along the device mesa sidewalls, increasing the dark current. High device failure rate was also observed in deep-etched nBn structures. An alternative approach to limit lateral diffusion used an inverted nBn structure that has its absorber grown above the barrier. Like the shallow etch process on conventional nBn structures, the inverted nBn devices were fabricated with a processing scheme that only etches the top layer (the absorber, in this case) but avoids etching through the barrier. The results show that inverted nBn devices have the advantage of eliminating the lateral diffusion current without introducing elevated surface current.

  10. High rate dry etching of InGaZnO by BCl3/O2 plasma

    NASA Astrophysics Data System (ADS)

    Park, Wanjae; Whang, Ki-Woong; Gwang Yoon, Young; Hwan Kim, Jeong; Rha, Sang-Ho; Seong Hwang, Cheol

    2011-08-01

    This paper reports the results of the high-rate dry etching of indium gallium zinc oxide (IGZO) at room temperature using BCl3/O2 plasma. We achieved an etch rate of 250 nm/min. We inferred from the x-ray photoelectron spectroscopy analysis that BOx or BOClx radicals generated from BCl3/O2 plasma cause the etching of the IGZO material. O2 initiates the etching of IGZO, and Ar removes nonvolatile byproducts from the surface during the etching process. Consequently, a smooth etched surface results when these gases are added to the etch gas.

  11. Extreme wettability of nanostructured glass fabricated by non-lithographic, anisotropic etching

    PubMed Central

    Yu, Eusun; Kim, Seul-Cham; Lee, Heon Ju; Oh, Kyu Hwan; Moon, Myoung-Woon

    2015-01-01

    Functional glass surfaces with the properties of superhydrophobicity/or superhydrohydrophilicity, anti-condensation or low reflectance require nano- or micro-scale roughness, which is difficult to fabricate directly on glass surfaces. Here, we report a novel non-lithographic method for the fabrication of nanostructures on glass; this method introduces a sacrificial SiO2 layer for anisotropic plasma etching. The first step was to form nanopillars on SiO2 layer-coated glass by using preferential CF4 plasma etching. With continuous plasma etching, the SiO2 pillars become etch-resistant masks on the glass; thus, the glass regions covered by the SiO2 pillars are etched slowly, and the regions with no SiO2 pillars are etched rapidly, resulting in nanopatterned glass. The glass surface that is etched with CF4 plasma becomes superhydrophilic because of its high surface energy, as well as its nano-scale roughness and high aspect ratio. Upon applying a subsequent hydrophobic coating to the nanostructured glass, a superhydrophobic surface was achieved. The light transmission of the glass was relatively unaffected by the nanostructures, whereas the reflectance was significantly reduced by the increase in nanopattern roughness on the glass. PMID:25791414

  12. Maskless micro/nanofabrication on GaAs surface by friction-induced selective etching

    PubMed Central

    2014-01-01

    In the present study, a friction-induced selective etching method was developed to produce nanostructures on GaAs surface. Without any resist mask, the nanofabrication can be achieved by scratching and post-etching in sulfuric acid solution. The effects of the applied normal load and etching period on the formation of the nanostructure were studied. Results showed that the height of the nanostructure increased with the normal load or the etching period. XPS and Raman detection demonstrated that residual compressive stress and lattice densification were probably the main reason for selective etching, which eventually led to the protrusive nanostructures from the scratched area on the GaAs surface. Through a homemade multi-probe instrument, the capability of this fabrication method was demonstrated by producing various nanostructures on the GaAs surface, such as linear array, intersecting parallel, surface mesas, and special letters. In summary, the proposed method provided a straightforward and more maneuverable micro/nanofabrication method on the GaAs surface. PMID:24495647

  13. Method and system for optical figuring by imagewise heating of a solvent

    DOEpatents

    Rushford, Michael C.

    2005-08-30

    A method and system of imagewise etching the surface of a substrate, such as thin glass, in a parallel process. The substrate surface is placed in contact with an etchant solution which increases in etch rate with temperature. A local thermal gradient is then generated in each of a plurality of selected local regions of a boundary layer of the etchant solution to imagewise etch the substrate surface in a parallel process. In one embodiment, the local thermal gradient is a local heating gradient produced at selected addresses chosen from an indexed array of addresses. The activation of each of the selected addresses is independently controlled by a computer processor so as to imagewise etch the substrate surface at region-specific etch rates. Moreover, etching progress is preferably concurrently monitored in real time over the entire surface area by an interferometer so as to deterministically control the computer processor to image-wise figure the substrate surface where needed.

  14. Dynamic secondary ion mass spectroscopy of Au nanoparticles on Si wafer using Bi3+ as primary ion coupled with surface etching by Ar cluster ion beam: The effect of etching conditions on surface structure

    NASA Astrophysics Data System (ADS)

    Park, Eun Ji; Choi, Chang Min; Kim, Il Hee; Kim, Jung-Hwan; Lee, Gaehang; Jin, Jong Sung; Ganteför, Gerd; Kim, Young Dok; Choi, Myoung Choul

    2018-01-01

    Wet-chemically synthesized Au nanoparticles were deposited on Si wafer surfaces, and the secondary ions mass spectra (SIMS) from these samples were collected using Bi3+ with an energy of 30 keV as the primary ions. In the SIMS, Au cluster cations with a well-known, even-odd alteration pattern in the signal intensity were observed. We also performed depth profile SIMS analyses, i.e., etching the surface using an Ar gas cluster ion beam (GCIB), and a subsequent Bi3+ SIMS analysis was repetitively performed. Here, two different etching conditions (Ar1600 clusters of 10 keV energy or Ar1000 of 2.5 keV denoted as "harsh" or "soft" etching conditions, respectively) were used. Etching under harsh conditions induced emission of the Au-Si binary cluster cations in the SIMS spectra of the Bi3+ primary ions. The formation of binary cluster cations can be induced by either fragmentation of Au nanoparticles or alloying of Au and Si, increasing Au-Si coordination on the sample surface during harsh GCIB etching. Alternatively, use of the soft GCIB etching conditions resulted in exclusive emission of pure Au cluster cations with nearly no Au-Si cluster cation formation. Depth profile analyses of the Bi3+ SIMS combined with soft GCIB etching can be useful for studying the chemical environments of atoms at the surface without altering the original interface structure during etching.

  15. Formation of ultra Si/Ti nano thin film for enhancing silicon solar cell efficiency

    NASA Astrophysics Data System (ADS)

    Adam, T.; Dhahi, T. S.; Mohammed, M.; Al-Hajj, A. M.; Hashim, U.

    2017-10-01

    An alternative electrical source has l has become the major quest of every researchers due to it numerous advantages and applications of power supply and as electronic devices are becoming more and more portable. A highly efficient power supply is become inevitable. Thus. in this study, present ultrasonic based assisted fabrication of electrochemical silicon-Titanium nano thin film by in-house simple technique, uniformly silicon Nano film was fabricated and etched with HF (40%): C2H5OH (99%):1:1, < 20 nm pore diameter of silicon was fabricated. The surface and morphology reveal that the method produce uniform nano silicon porous layer with smaller silicon pores with high etching efficiency. The silicon-Titanium integrated nano porous exhibited excellent observation properties with low reflection index ~ 1.1 compared to silicon alone thin film.

  16. Liquid-Assisted Femtosecond Laser Precision-Machining of Silica.

    PubMed

    Cao, Xiao-Wen; Chen, Qi-Dai; Fan, Hua; Zhang, Lei; Juodkazis, Saulius; Sun, Hong-Bo

    2018-04-28

    We report a systematical study on the liquid assisted femtosecond laser machining of quartz plate in water and under different etching solutions. The ablation features in liquid showed a better structuring quality and improved resolution with 1/3~1/2 smaller features as compared with those made in air. It has been demonstrated that laser induced periodic structures are present to a lesser extent when laser processed in water solutions. The redistribution of oxygen revealed a strong surface modification, which is related to the etching selectivity of laser irradiated regions. Laser ablation in KOH and HF solution showed very different morphology, which relates to the evolution of laser induced plasma on the formation of micro/nano-features in liquid. This work extends laser precision fabrication of hard materials. The mechanism of strong absorption in the regions with permittivity (epsilon) near zero is discussed.

  17. Ultrathin Au film on polymer surface for surface plasmon polariton waveguide application

    NASA Astrophysics Data System (ADS)

    Liu, Tong; Ji, Lanting; He, Guobing; Sun, Xiaoqiang; Wang, Fei; Zhang, Daming

    2017-11-01

    Formation of laterally continuous ultrathin gold films on polymer substrates is a technological challenge. In this work, the vacuum thermal evaporation method is adopted to form continuous Au films in the thickness range of 7-17 nm on polymers of Poly(methyl-methacrylate-glycidly-methacrylate) and SU-8 film surface without using the adhesion or metallic seeding layers. Absorption spectrum, scanning electron microscope and atomic force microscope images are used to characterize the Au film thickness, roughness and optical loss. The result shows that molecular-scale structure, surface energy and electronegativity have impacts on the Au film morphology on polymers. Wet chemical etching is used to fabricate 7-nm thick Au stripes embedded in polymer claddings. These long-range surface plasmon polariton waveguides demonstrate the favorable morphological configurations and cross-sectional states. Through the end-fire excitation method, propagation losses of 6-μm wide Au stripes are compared to theoretical values and analyzed from practical film status. The smooth, patternable gold films on polymer provide potential applications to plasmonic waveguides, biosensing, metamaterials and optical antennas.

  18. Fabrication of Monolithic Sapphire Membranes for High Tc Bolometer Array Development

    NASA Technical Reports Server (NTRS)

    Pugel, D. E.; Lakew, B.; Aslam, S.; Wang, L.

    2003-01-01

    This paper examines the effectiveness of Pt/Cr thin film masks for the architecture of monolithic membrane structures in r-plane sapphire. The development of a pinhole-free Pt/Cr composite mask that is resistant to hot H2SO4:H3PO4 etchant, will lead to the fabrication of smooth sapphire membranes whose surfaces are well-suited for the growth of low-noise high Tc films. In particular, the relationship of thermal annealing conditions on the Pt/Cr composite mask system to: (1) changes in the surface morphology and elemental concentration of the Pt/Cr thin film layers and (2) etch pit formation on the sapphire surface will be presented.

  19. A nanoforest structure for practical surface-enhanced Raman scattering substrates

    NASA Astrophysics Data System (ADS)

    Seol, Myeong-Lok; Choi, Sung-Jin; Baek, David J.; Park, Tae Jung; Ahn, Jae-Hyuk; Lee, Sang Yup; Choi, Yang-Kyu

    2012-03-01

    A nanoforest structure for surface-enhanced Raman scattering (SERS) active substrates is fabricated and analyzed. The detailed morphology of the resulting structure can be easily controlled by modifying the process parameters such as initial gold layer thickness and etching time. The applicability of the nanoforest substrate as a label-free SERS immunosensor is demonstrated using influenza A virus subtype H1N1. Selective binding of the H1N1 surface antigen and the anti-H1 antibody is directly detected by the SERS signal differences. Simple fabrication and high throughput with strong in-plane hot-spots imply that the nanoforest structure can be a practical sensing component of a chip-based SERS sensing system.

  20. Influence of application method on surface free-energy and bond strength of universal adhesive systems to enamel.

    PubMed

    Imai, Arisa; Takamizawa, Toshiki; Sai, Keiichi; Tsujimoto, Akimasa; Nojiri, Kie; Endo, Hajime; Barkmeier, Wayne W; Latta, Mark A; Miyazaki, Masashi

    2017-10-01

    The aim of the present study was to determine the influence of different adhesive application methods and etching modes on enamel bond effectiveness of universal adhesives using shear bond strength (SBS) testing and surface free-energy (SFE) measurements. The adhesives Scotchbond Universal, All-Bond Universal, Adhese Universal, and G-Premio Bond were used. Prepared bovine enamel specimens were divided into four groups, based on type of adhesive, and subjected to the following surface treatments: (i) total-etch mode with active application; (ii) total-etch mode with inactive application; (iii) self-etch mode with active application; and (iv) self-etch mode with inactive application. Bonded specimens were subjected to SBS testing. The SFE of the enamel surfaces with adhesive was measured after rinsing with acetone and water. The SBS values in total-etch mode were significantly higher than those in self-etch mode. In total-etch mode, significantly lower SBS values were observed with active application compared with inactive application; in contrast, in self-etch mode there were no significant differences in SBS between active and inactive applications. A reduction in total SFE was observed for active application compared with inactive application. The interaction between etching mode and application method was statistically significant, and the application method significantly affected enamel bond strength in total-etch mode. © 2017 Eur J Oral Sci.

  1. GPU based 3D feature profile simulation of high-aspect ratio contact hole etch process under fluorocarbon plasmas

    NASA Astrophysics Data System (ADS)

    Chun, Poo-Reum; Lee, Se-Ah; Yook, Yeong-Geun; Choi, Kwang-Sung; Cho, Deog-Geun; Yu, Dong-Hun; Chang, Won-Seok; Kwon, Deuk-Chul; Im, Yeon-Ho

    2013-09-01

    Although plasma etch profile simulation has been attracted much interest for developing reliable plasma etching, there still exist big gaps between current research status and predictable modeling due to the inherent complexity of plasma process. As an effort to address this issue, we present 3D feature profile simulation coupled with well-defined plasma-surface kinetic model for silicon dioxide etching process under fluorocarbon plasmas. To capture the realistic plasma surface reaction behaviors, a polymer layer based surface kinetic model was proposed to consider the simultaneous polymer deposition and oxide etching. Finally, the realistic plasma surface model was used for calculation of speed function for 3D topology simulation, which consists of multiple level set based moving algorithm, and ballistic transport module. In addition, the time consumable computations in the ballistic transport calculation were improved drastically by GPU based numerical computation, leading to the real time computation. Finally, we demonstrated that the surface kinetic model could be coupled successfully for 3D etch profile simulations in high-aspect ratio contact hole plasma etching.

  2. Room-Temperature Wet Chemical Synthesis of Au NPs/TiH2/Nanocarved Ti Self-Supported Electrocatalysts for Highly Efficient H2 Generation.

    PubMed

    Amin, Mohammed A; Fadlallah, Sahar A; Alosaimi, Ghaida S; Ahmed, Emad M; Mostafa, Nasser Y; Roussel, Pascal; Szunerits, Sabine; Boukherroub, Rabah

    2017-09-06

    Self-supported electrocatalysts are a new class of materials exhibiting high catalytic performance for various electrochemical processes and can be directly equipped in energy conversion devices. We present here, for the first time, sparse Au NPs self-supported on etched Ti (nanocarved Ti substrate self-supported with TiH 2 ) as promising catalysts for the electrochemical generation of hydrogen (H 2 ) in KOH solutions. Cleaned, as-polished Ti substrates were etched in highly concentrated sulfuric acid solutions without and with 0.1 M NH 4 F at room temperature for 15 min. These two etching processes yielded a thin layer of TiH 2 (the corrosion product of the etching process) self-supported on nanocarved Ti substrates with different morphologies. While F - -free etching process led to formation of parallel channels (average width: 200 nm), where each channel consists of an array of rounded cavities (average width: 150 nm), etching in the presence of F - yielded Ti surface carved with nanogrooves (average width: 100 nm) in parallel orientation. Au NPs were then grown in situ (self-supported) on such etched surfaces via immersion in a standard gold solution at room temperature without using stabilizers or reducing agents, producing Au NPs/TiH 2 /nanostructured Ti catalysts. These materials were characterized by scanning electron microscopy/energy-dispersive spectroscopy (SEM/EDS), grazing incidence X-ray diffraction (GIXRD), and X-ray photoelectron spectroscopy (XPS). GIXRD confirmed the formation of Au 2 Ti phase, thus referring to strong chemical interaction between the supported Au NPs and the substrate surface (also evidenced from XPS) as well as a titanium hydride phase of chemical composition TiH 2 . Electrochemical measurements in 0.1 M KOH solution revealed outstanding hydrogen evolution reaction (HER) electrocatalytic activity for our synthesized catalysts, with Au NPs/TiH 2 /nanogrooved Ti catalyst being the best one among them. It exhibited fast kinetics for the HER with onset potentials as low as -22 mV vs. RHE, high exchange current density of 0.7 mA cm -2 , and a Tafel slope of 113 mV dec -1 . These HER electrochemical kinetic parameters are very close to those measured here for a commercial Pt/C catalyst (onset potential: -20 mV, Tafel slope: 110 mV dec -1 , and exchange current density: 0.75 mA cm -2 ). The high catalytic activity of these materials was attributed to the catalytic impacts of both TiH 2 phase and self-supported Au NPs (active sites for the catalytic reduction of water to H 2 ), in addition to their nanostructured features which provide a large-surface area for the HER.

  3. Assessment of resin-dentin interfacial morphology of two ethanol-based universal adhesives: A scanning electron microscopy study

    PubMed Central

    Awad, Mohamed Moustafa

    2017-01-01

    Objective: The objective of this study was to assess the resin-dentin interfacial morphology created by two universal adhesives using scanning electron microscopy (SEM). Materials and Methods: The occlusal surfaces of ten (n = 5) molars were reduced to expose a flat surface of dentin. Two universal adhesives, Scotchbond Universal Adhesive and Tetric N-Bond Universal, were independently applied to air-dried dentin. Light-cured resin-based composite restorative materials were used to incrementally build a composite “buildup.” The specimen was sectioned mesiodistally to expose the resin-dentin interface. The inner surfaces of the specimens were polished. Samples were immersed in hydrochloric acid and then rinsed using distilled water. This was followed by immersion of the samples in 1% sodium hypochlorite solution. Then, samples were thoroughly rinsing with distilled water. Dehydration of samples was performed using ascending concentration of ethyl alcohol. Prepared samples were observed SEM at magnifications ×1500 and x4000. Results: Both universal adhesives could penetrate dentin-forming well-defined resin tags, lateral branches as well as a uniform hybrid layer. Conclusions: Two tested universal adhesives applied in self-etch mode can infiltrate into dentin-producing high-quality interfacial morphology. Similar interfacial morphology may be due to the similarity in composition and application mode. PMID:28729794

  4. Synthesis and characterization of hybrid micro/nano-structured NiTi surfaces by a combination of etching and anodizing

    NASA Astrophysics Data System (ADS)

    Huan, Z.; Fratila-Apachitei, L. E.; Apachitei, I.; Duszczyk, J.

    2014-02-01

    The purpose of this study was to generate hybrid micro/nano-structures on biomedical nickel-titanium alloy (NiTi). To achieve this, NiTi surfaces were firstly electrochemically etched and then anodized in fluoride-containing electrolyte. With the etching process, the NiTi surface was micro-roughened through the formation of micropits uniformly distributed over the entire surface. Following the subsequent anodizing process, self-organized nanotube structures enriched in TiO2 could be superimposed on the etched surface under specific conditions. Furthermore, the anodizing treatment significantly reduced water contact angles and increased the surface free energy compared to the surfaces prior to anodizing. The results of this study show for the first time that it is possible to create hybrid micro/nano-structures on biomedical NiTi alloys by combining electrochemical etching and anodizing under controlled conditions. These novel structures are expected to significantly enhance the surface biofunctionality of the material when compared to conventional implant devices with either micro- or nano-structured surfaces.

  5. Synthesis and characterization of hybrid micro/nano-structured NiTi surfaces by a combination of etching and anodizing.

    PubMed

    Huan, Z; Fratila-Apachitei, L E; Apachitei, I; Duszczyk, J

    2014-02-07

    The purpose of this study was to generate hybrid micro/nano-structures on biomedical nickel-titanium alloy (NiTi). To achieve this, NiTi surfaces were firstly electrochemically etched and then anodized in fluoride-containing electrolyte. With the etching process, the NiTi surface was micro-roughened through the formation of micropits uniformly distributed over the entire surface. Following the subsequent anodizing process, self-organized nanotube structures enriched in TiO2 could be superimposed on the etched surface under specific conditions. Furthermore, the anodizing treatment significantly reduced water contact angles and increased the surface free energy compared to the surfaces prior to anodizing. The results of this study show for the first time that it is possible to create hybrid micro/nano-structures on biomedical NiTi alloys by combining electrochemical etching and anodizing under controlled conditions. These novel structures are expected to significantly enhance the surface biofunctionality of the material when compared to conventional implant devices with either micro- or nano-structured surfaces.

  6. Creation of superhydrophobic stainless steel surfaces by acid treatments and hydrophobic film deposition.

    PubMed

    Li, Lester; Breedveld, Victor; Hess, Dennis W

    2012-09-26

    In this work, we present a method to render stainless steel surfaces superhydrophobic while maintaining their corrosion resistance. Creation of surface roughness on 304 and 316 grade stainless steels was performed using a hydrofluoric acid bath. New insight into the etch process is developed through a detailed analysis of the chemical and physical changes that occur on the stainless steel surfaces. As a result of intergranular corrosion, along with metallic oxide and fluoride redeposition, surface roughness was generated on the nano- and microscales. Differences in alloy composition between 304 and 316 grades of stainless steel led to variations in etch rate and different levels of surface roughness for similar etch times. After fluorocarbon film deposition to lower the surface energy, etched samples of 304 and 316 stainless steel displayed maximum static water contact angles of 159.9 and 146.6°, respectively. However, etching in HF also caused both grades of stainless steel to be susceptible to corrosion. By passivating the HF-etched samples in a nitric acid bath, the corrosion resistant properties of stainless steels were recovered. When a three step process was used, consisting of etching, passivation and fluorocarbon deposition, 304 and 316 stainless steel samples exhibited maximum contact angles of 157.3 and 134.9°, respectively, while maintaining corrosion resistance.

  7. A Study on Ohmic Contact to Dry-Etched p-GaN

    NASA Astrophysics Data System (ADS)

    Hu, Cheng-Yu; Ao, Jin-Ping; Okada, Masaya; Ohno, Yasuo

    Low-power dry-etching process has been adopted to study the influence of dry-etching on Ohmic contact to p-GaN. When the surface layer of as-grown p-GaN was removed by low-power SiCl4/Cl2-etching, no Ohmic contact can be formed on the low-power dry-etched p-GaN. The same dry-etching process was also applied on n-GaN to understand the influence of the low-power dry-etching process. By capacitance-voltage (C-V) measurement, the Schottky barrier heights (SBHs) of p-GaN and n-GaN were measured. By comparing the change of measured SBHs on p-GaN and n-GaN, it was suggested that etching damage is not the only reason responsible for the degraded Ohmic contacts to dry-etched p-GaN and for Ohmic contact formatin, the original surface layer of as-grown p-GaN have some special properties, which were removed by dry-etching process. To partially recover the original surface of as-grown p-GaN, high temperature annealing (1000°C 30s) was tried on the SiCl4/Cl2-etched p-GaN and Ohmic contact was obtained.

  8. Nickel-Phosphorous Development for Total Solar Irradiance Measurement

    NASA Astrophysics Data System (ADS)

    Carlesso, F.; Berni, L. A.; Vieira, L. E. A.; Savonov, G. S.; Nishimori, M.; Dal Lago, A.; Miranda, E.

    2017-10-01

    The development of an absolute radiometer instrument is currently a effort at INPE for TSI measurements. In this work, we describe the development of black Ni-P coatings for TSI radiometers absorptive cavities. We present a study of the surface blackening process and the relationships between morphological structure, chemical composition and coating absorption. Ni-P deposits with different phosphorous content were obtained by electroless techniques on aluminum substrates with a thin zincate layer. Appropriate phosphorus composition and etching parameters process produce low reflectance black coatings.

  9. Relationship between enamel bond fatigue durability and surface free-energy characteristics with universal adhesives.

    PubMed

    Nagura, Yuko; Tsujimoto, Akimasa; Barkmeier, Wayne W; Watanabe, Hidehiko; Johnson, William W; Takamizawa, Toshiki; Latta, Mark A; Miyazaki, Masashi

    2018-04-01

    The relationship between enamel bond fatigue durability and surface free-energy characteristics with universal adhesives was investigated. The initial shear bond strengths and shear fatigue strengths of five universal adhesives to enamel were determined with and without phosphoric acid pre-etching. The surface free-energy characteristics of adhesive-treated enamel with and without pre-etching were also determined. The initial shear bond strength and shear fatigue strength of universal adhesive to pre-etched enamel were higher than those to ground enamel. The initial shear bond strength and shear fatigue strength of universal adhesive to pre-etched enamel were material dependent, unlike those to ground enamel. The surface free-energy of the solid (γ S ) and the hydrogen-bonding force (γSh) of universal adhesive-treated enamel were different depending on the adhesive, regardless of the presence or absence of pre-etching. The bond fatigue durability of universal adhesives was higher to pre-etched enamel than to ground enamel. In addition, the bond fatigue durability to pre-etched enamel was material dependent, unlike that to ground enamel. The surface free-energy characteristics of universal adhesive-treated enamel were influenced by the adhesive type, regardless of the presence or absence of pre-etching. The surface free-energy characteristics of universal adhesive-treated enamel were related to the results of the bond fatigue durability. © 2018 Eur J Oral Sci.

  10. Facile Synthesis of Robust Free-Standing TiO2 Nanotubular Membranes for Biofiltration Applications

    PubMed Central

    Schweicher, Julien; Desai, Tejal A.

    2014-01-01

    Robust monodisperse nanoporous membranes have a wide range of biotechnological applications, but are often difficult or costly to fabricate. Here, a simple technique is reported to produce free-standing TiO2 nanotubular membranes with through-hole morphology. It consists in a 3-step anodization procedure carried out at room temperature on a Ti foil. The first anodization (1 h at 80 V) is used to pattern the surface of the metallic foil. Then, the second anodization (24 h at 80 V) produces the array of TiO2 nanotubes that will constitute the final membrane. A higher voltage anodization (3-5 minutes at 180 V) is finally applied to detach the TiO2 nanotubular layer from the underlying Ti foil. In order to completely remove the barrier layer that obstructs some pores of the membrane, the latter is etched 2 minutes in a buffered oxide etch solution. The overall process produces 60 μm-thick TiO2 nanotubular membranes with tube openings of 110 nm on one side and 73 nm on the other side. The through-hole morphology of these membranes has been verified by performing diffusion experiments with glucose, insulin and immunoglobulin G where in differences in diffusion rate are observed based on molecular weight. Such biocompatible TiO2 nanotubular membranes, with controlled pore size and morphology, have broad biotechnological and biomedical applications. PMID:24634542

  11. Facile Synthesis of Robust Free-Standing TiO2 Nanotubular Membranes for Biofiltration Applications.

    PubMed

    Schweicher, Julien; Desai, Tejal A

    2014-03-01

    Robust monodisperse nanoporous membranes have a wide range of biotechnological applications, but are often difficult or costly to fabricate. Here, a simple technique is reported to produce free-standing TiO 2 nanotubular membranes with through-hole morphology. It consists in a 3-step anodization procedure carried out at room temperature on a Ti foil. The first anodization (1 h at 80 V) is used to pattern the surface of the metallic foil. Then, the second anodization (24 h at 80 V) produces the array of TiO 2 nanotubes that will constitute the final membrane. A higher voltage anodization (3-5 minutes at 180 V) is finally applied to detach the TiO 2 nanotubular layer from the underlying Ti foil. In order to completely remove the barrier layer that obstructs some pores of the membrane, the latter is etched 2 minutes in a buffered oxide etch solution. The overall process produces 60 μm-thick TiO 2 nanotubular membranes with tube openings of 110 nm on one side and 73 nm on the other side. The through-hole morphology of these membranes has been verified by performing diffusion experiments with glucose, insulin and immunoglobulin G where in differences in diffusion rate are observed based on molecular weight. Such biocompatible TiO 2 nanotubular membranes, with controlled pore size and morphology, have broad biotechnological and biomedical applications.

  12. In vitro bonding effectiveness of three different one-step self-etch adhesives with additional enamel etching.

    PubMed

    Batra, Charu; Nagpal, Rajni; Tyagi, Shashi Prabha; Singh, Udai Pratap; Manuja, Naveen

    2014-08-01

    To evaluate the effect of additional enamel etching on the shear bond strength of three self-etch adhesives. Class II box type cavities were made on extracted human molars. Teeth were randomly divided into one control group of etch and rinse adhesive and three test groups of self-etch adhesives (Clearfil S3 Bond, Futurabond NR, Xeno V). The teeth in the control group (n = 10) were treated with Adper™ Single Bond 2. The three test groups were further divided into two subgroups (n = 10): (i) self-etch adhesive was applied as per the manufacturer's instructions; (ii) additional etching of enamel surfaces was done prior to the application of self-etch adhesives. All cavities were restored with Filtek Z250. After thermocycling, shear bond strength was evaluated using a Universal testing machine. Data were analyzed using anova independent sample's 't' test and Dunnett's test. The failure modes were evaluated with a stereomicroscope at a magnification of 10×. Additional phosphoric acid etching of the enamel surface prior to the application of the adhesive system significantly increased the shear bond strength of all the examined self-etch adhesives. Additional phosphoric acid etching of enamel surface significantly improved the shear bond strength. © 2013 Wiley Publishing Asia Pty Ltd.

  13. The Effects of Acid Etching on the Nanomorphological Surface Characteristics and Activation Energy of Titanium Medical Materials.

    PubMed

    Hung, Kuo-Yung; Lin, Yi-Chih; Feng, Hui-Ping

    2017-10-11

    The purpose of this study was to characterize the etching mechanism, namely, the etching rate and the activation energy, of a titanium dental implant in concentrated acid and to construct the relation between the activation energy and the nanoscale surface topographies. A commercially-pure titanium (CP Ti) and Ti-6Al-4V ELI surface were tested by shot blasting (pressure, grain size, blasting distance, blasting angle, and time) and acid etching to study its topographical, weight loss, surface roughness, and activation energy. An Arrhenius equation was applied to derive the activation energy for the dissolution of CP Ti/Ti-6Al-4V ELI in sulfuric acid (H₂SO₄) and hydrochloric acid (HCl) at different temperatures. In addition, white-light interferometry was applied to measure the surface nanomorphology of the implant to obtain 2D or 3D roughness parameters (Sa, Sq, and St). The nanopore size that formed after etching was approximately 100-500 nm. The surface roughness of CP Ti and Ti-6Al-4V ELI decreased as the activation energy decreased but weight loss increased. Ti-6Al-4V ELI has a higher level of activation energy than Ti in HCl, which results in lower surface roughness after acid etching. This study also indicates that etching using a concentrated hydrochloric acid provided superior surface modification effects in titanium compared with H₂SO₄.

  14. Thermal etching of silver: Influence of rolling defects

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Ollivier, M., E-mail: o.maelig@imperial.ac.uk

    2016-08-15

    Silver is well known to be thermally etched in an oxygen-rich atmosphere and has been extensively studied in the laboratory to understand thermal etching and to limit its effect when this material is used as a catalyst. Yet, in many industrial applications the surface of rolled silver sheets is used without particular surface preparation. Here, it is shown by combining FIB-tomography, FIB-SIMS and analytical SEM that the kinetics of thermal etch pitting are significantly faster on rolled Ag surfaces than on polished surfaces. This occurs due to range of interacting phenomena including (i) the reaction of subsurface carbon-contamination with dissolvedmore » oxygen to form pores that grow to intersect the surface, (ii) surface reconstruction around corrosion pits and surface scratches, and (iii) sublimation at low pressure and high temperature. A method to identify subsurface pores is developed to show that the pores have (111) and (100) internal facets and may be filled with a gas coming from the chemical reaction of oxygen and carbon contamination. - Highlights: Thermal etching of industrial silver sheets vs. polished silver sheets Effect of annealing atmosphere on the thermal etching of silver: surface and subsurface characterization Link between etch pitting and defects induced by rolling. FIB-tomography coupled with EBSD for determining crystal planes of the facets of subsurface pores. FIB-SIMS characterization to probe the gas confined inside subsurface pores.« less

  15. Effect of various surface treatment methods on the bond strength of the heat-pressed ceramic samples.

    PubMed

    Saraçoğlu, A; Cura, C; Cötert, H S

    2004-08-01

    This in vitro study was conducted to evaluate the interaction between the shear bond strength and the surface treatment method for a commercial dental ceramic. Ninety bonded ceramic units were manufactured for this study. Each unit was made by luting two cylinder-shaped ceramic samples to each other with a resin-composite luting agent. The units were then divided into nine groups, containing 10 units in each group. Samples from each group were treated with one of the following: etching with 4.9% hydrofluoric acid for 10, 20 and 40 s, 9.5% hydrofluoric acid for 10, 20 and 40 s, 40% orthophosphoric acid for 40 s, air abrasion with alumina in 50-microm particles, and grinding with a high-speed diamond bur. The treated samples were then silanated and luted with a resin-composite luting agent. The luted units were then loaded to failure. Two samples from each group were neither silanated nor luted after the surface treatment procedure, and morphological changes obtained by various surface treatment regimens were investigated by scanning electron microscopy. A statistically significant difference was observed among the mean shear bond strengths of the groups prepared with different surface treatment techniques (P = 0.00). Hydrofluoric acid appeared to be the most suitable chemical medium to produce a reliable ceramic bond. Etching time and concentration of the acidic medium were also observed as important prognostic variates. Orthophosphoric acid treatment was observed to be the least effective surface treatment method on the heat-pressed ceramic samples. Physical applications such as bur grinding and air blasting maintained stronger bonds than the orthophosphoric acid, while producing weaker bonds than surfaces treated with hydrofluoric acid in all concentrations and etching periods. The effect of the silane priming agent was not considered in this study. Copyright 2004 Blackwell Publishing Ltd.

  16. Semiconductor etching by hyperthermal neutral beams

    NASA Technical Reports Server (NTRS)

    Minton, Timothy K. (Inventor); Giapis, Konstantinos P. (Inventor)

    1999-01-01

    An at-least dual chamber apparatus and method in which high flux beams of fast moving neutral reactive species are created, collimated and used to etch semiconductor or metal materials from the surface of a workpiece. Beams including halogen atoms are preferably used to achieve anisotropic etching with good selectivity at satisfactory etch rates. Surface damage and undercutting are minimized.

  17. Surface chemistry of InP ridge structures etched in Cl{sub 2}-based plasma analyzed with angular XPS

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Bouchoule, Sophie, E-mail: sophie.bouchoule@lpn.cnrs.fr; Cambril, Edmond; Guilet, Stephane

    2015-09-15

    Two x-ray photoelectron spectroscopy configurations are proposed to analyze the surface chemistry of micron-scale InP ridge structures etched in chlorine-based inductively coupled plasma (ICP). Either a classical or a grazing configuration allows to retrieve information about the surface chemistry of the bottom surface and sidewalls of the etched features. The procedure is used to study the stoichiometry of the etched surface as a function of ridge aspect ratio for Cl{sub 2}/Ar and Cl{sub 2}/H{sub 2} plasma chemistries. The results show that the bottom surface and the etched sidewalls are P-rich, and indicate that the P-enrichment mechanism is rather chemically driven.more » Results also evidence that adding H{sub 2} to Cl{sub 2} does not necessarily leads to a more balanced surface stoichiometry. This is in contrast with recent experimental results obtained with the HBr ICP chemistry for which fairly stoichiometric surfaces have been obtained.« less

  18. [Influence of different porcelain surface treatment method on the bonding of metal brackets to porcelain].

    PubMed

    Fan, Cun-Hui; Chen, Jie; Liu, Xin-Qiang; Ma, Xin

    2005-08-01

    To investigate the influence of different porcelain surface treatment methods on the shear bond strength of metal brackets bonded to porcelain. 80 porcelain facets were divided randomly into two groups according to different adhesive material that was used to bond metal brackets. Adhesive material were Jing-Jin enamel adhesive and light-cured composite resin. Each group was further divided into 4 subgroups according to different surface treatment methods, which were acid etching with 37% phosphoric acid (H3PO4), acid etching with 9.6% hydrofluoric acid (HF), deglazing by grinding and silanating the porcelain surface. All specimens were stored in 37 degrees C water for 24 hours and then the shear bond strength and the porcelain fracture after debonding was determined. The porcelain surfaces after HF etching, H3PO4 etching and deglazing by grinding were examined by scanning electron microscopy respectively. The shear bond strengths in the HF etching groups, the deglazing groups and the silanating groups were much greater than that in the phosphoric etching groups (P < 0.01). Adequate orthodontic bonding strength was achieved both when bonded with light-cured composite resin after deglazing by grinding and when bonded with either of these adhesives after HF etching or surface silanating. There were no differences in the rates of porcelain fractures among groups (P > 0.05). HF etching, deglazing by grinding and silanating can all increase the shear bond strength between metal bracket and porcelain. Surface silanating of porcelain is a better surface treatment when metal brackets bonded to porcelain.

  19. Silicon Carbide Etching Using Chlorine Trifluoride Gas

    NASA Astrophysics Data System (ADS)

    Habuka, Hitoshi; Oda, Satoko; Fukai, Yasushi; Fukae, Katsuya; Takeuchi, Takashi; Aihara, Masahiko

    2005-03-01

    The etch rate, chemical reactions and etched surface of β-silicon carbide are studied in detail using chlorine trifluoride gas. The etch rate is greater than 10 μm min-1 at 723 K with a flow rate of 0.1 \\ell min-1 at atmospheric pressure in a horizontal reactor. The maximum etch rate at a substrate temperature of 773 K is 40 μm min-1 with a flow rate of 0.25 \\ell min-1. The step-like pattern that initially exists on the β-silicon carbide surface tends to be smoothed; the root-mean-square surface roughness decreases from its initial value of 5 μm to 1 μm within 15 min; this minimum value is maintained for more than 15 min. Therefore, chlorine trifluoride gas is considered to have a large etch rate for β-silicon carbide associated with making a rough surface smooth.

  20. Unveiling the mechanisms of dressed-photon-phonon etching based on hierarchical surface roughness measure

    NASA Astrophysics Data System (ADS)

    Naruse, Makoto; Yatsui, Takashi; Nomura, Wataru; Kawazoe, Tadashi; Aida, Masaki; Ohtsu, Motoichi

    2013-02-01

    Dressed-photon-phonon (DPP) etching is a disruptive technology in planarizing material surfaces because it completely eliminates mechanical contact processes. However, adequate metrics for evaluating the surface roughness and the underlying physical mechanisms are still not well understood. Here, we propose a two-dimensional hierarchical surface roughness measure, inspired by the Allan variance, that represents the effectiveness of DPP etching while conserving the original two-dimensional surface topology. Also, we build a simple physical model of DPP etching that agrees well with the experimental observations, which clearly shows the involvement of the intrinsic hierarchical properties of dressed photons, or optical near-fields, in the surface processing.

  1. Effect of tetramethylammonium hydroxide/isopropyl alcohol wet etching on geometry and surface roughness of silicon nanowires fabricated by AFM lithography

    PubMed Central

    Yusoh, Siti Noorhaniah

    2016-01-01

    Summary The optimization of etchant parameters in wet etching plays an important role in the fabrication of semiconductor devices. Wet etching of tetramethylammonium hydroxide (TMAH)/isopropyl alcohol (IPA) on silicon nanowires fabricated by AFM lithography is studied herein. TMAH (25 wt %) with different IPA concentrations (0, 10, 20, and 30 vol %) and etching time durations (30, 40, and 50 s) were investigated. The relationships between etching depth and width, and etching rate and surface roughness of silicon nanowires were characterized in detail using atomic force microscopy (AFM). The obtained results indicate that increased IPA concentration in TMAH produced greater width of the silicon nanowires with a smooth surface. It was also observed that the use of a longer etching time causes more unmasked silicon layers to be removed. Importantly, throughout this study, wet etching with optimized parameters can be applied in the design of the devices with excellent performance for many applications. PMID:27826521

  2. Surface Roughness and Morphology Customization of Additive Manufactured Open Porous Ti6Al4V Structures

    PubMed Central

    Pyka, Grzegorz; Kerckhofs, Greet; Papantoniou, Ioannis; Speirs, Mathew; Schrooten, Jan; Wevers, Martine

    2013-01-01

    Additive manufacturing (AM) is a production method that enables the building of porous structures with a controlled geometry. However, there is a limited control over the final surface of the product. Hence, complementary surface engineering strategies are needed. In this work, design of experiments (DoE) was used to customize post AM surface treatment for 3D selective laser melted Ti6Al4V open porous structures for bone tissue engineering. A two-level three-factor full factorial design was employed to assess the individual and interactive effects of the surface treatment duration and the concentration of the chemical etching solution on the final surface roughness and beam thickness of the treated porous structures. It was observed that the concentration of the surface treatment solution was the most important factor influencing roughness reduction. The designed beam thickness decreased the effectiveness of the surface treatment. In this case study, the optimized processing conditions for AM production and the post-AM surface treatment were defined based on the DoE output and were validated experimentally. This allowed the production of customized 3D porous structures with controlled surface roughness and overall morphological properties, which can assist in more controlled evaluation of the effect of surface roughness on various functional properties. PMID:28788357

  3. Surface Roughness and Morphology Customization of Additive Manufactured Open Porous Ti6Al4V Structures.

    PubMed

    Pyka, Grzegorz; Kerckhofs, Greet; Papantoniou, Ioannis; Speirs, Mathew; Schrooten, Jan; Wevers, Martine

    2013-10-22

    Additive manufacturing (AM) is a production method that enables the building of porous structures with a controlled geometry. However, there is a limited control over the final surface of the product. Hence, complementary surface engineering strategies are needed. In this work, design of experiments (DoE) was used to customize post AM surface treatment for 3D selective laser melted Ti6Al4V open porous structures for bone tissue engineering. A two-level three-factor full factorial design was employed to assess the individual and interactive effects of the surface treatment duration and the concentration of the chemical etching solution on the final surface roughness and beam thickness of the treated porous structures. It was observed that the concentration of the surface treatment solution was the most important factor influencing roughness reduction. The designed beam thickness decreased the effectiveness of the surface treatment. In this case study, the optimized processing conditions for AM production and the post-AM surface treatment were defined based on the DoE output and were validated experimentally. This allowed the production of customized 3D porous structures with controlled surface roughness and overall morphological properties, which can assist in more controlled evaluation of the effect of surface roughness on various functional properties.

  4. Caries-preventive effect of fissure sealant containing surface reaction-type pre-reacted glass ionomer filler and bonded by self-etching primer.

    PubMed

    Shimazu, Kisaki; Ogata, Kiyokazu; Karibe, Hiroyuki

    2012-01-01

    We aimed to evaluate the caries-preventive effect of a fissure sealant containing surface reaction-type pre-reacted glass ionomer (S-PRG) filler and bonded by self-etching primer versus those of 2 conventional resin-based sealants bonded by acid etching in terms of its impact on enamel demineralization and remineralization, enamel bond strength, and integrity of debonded enamel surfaces. Demineralization, remineralization, and bond strength on untreated enamel and enamel subsurface lesions of bovine incisors were assessed among the sealants by polarizing microscopy and microradiography; debonded enamel surfaces were examined by scanning electron microscopy. The conventional resin-based sealants bonded by acid etching caused surface defects on the enamel subsurface lesions and significantly increased the lesion depth (p = 0.014), indicative of enamel demineralization. However the S-PRG filler-containing sealant bonded by self-etching primer maintained the enamel surface integrity and inhibited enamel demineralization. No difference in bond strength on both untreated enamel and enamel subsurface lesions was noted among the sealants. An S-PRG filler-containing fissure sealant bonded by self-etching primer can prevent enamel demineralization, microleakage, and gaps without the tags created by acid etching regardless of the enamel condition. Such sealants are suitable for protecting the pits and fissures of immature permanent teeth.

  5. Nanoscale silver-assisted wet etching of crystalline silicon for anti-reflection surface textures.

    PubMed

    Li, Rui; Wang, Shuling; Chuwongin, Santhad; Zhou, Weidong

    2013-01-01

    We report here an electro-less metal-assisted chemical etching (MacEtch) process as light management surface-texturing technique for single crystalline Si photovoltaics. Random Silver nanostructures were formed on top of the Si surface based on the thin film evaporation and annealing process. Significant reflection reduction was obtained from the fabricated Si sample, with approximately 2% reflection over a wide spectra range (300 to 1050 nm). The work demonstrates the potential of MacEtch process for anti-reflection surface texture fabrication of large area, high efficiency, and low cost thin film solar cell.

  6. Fourier Transform Infrared Absorption Spectroscopy of Gas-Phase and Surface Reaction Products during Si Etching in Inductively Coupled Cl2 Plasmas

    NASA Astrophysics Data System (ADS)

    Miyata, Hiroki; Tsuda, Hirotaka; Fukushima, Daisuke; Takao, Yoshinori; Eriguchi, Koji; Ono, Kouichi

    2011-10-01

    A better understanding of plasma-surface interactions is indispensable during etching, including the behavior of reaction or etch products, because the products on surfaces and in the plasma are important in passivation layer formation through their redeposition on surfaces. In practice, the nanometer-scale control of plasma etching would still rely largely on such passivation layer formation as well as ion-enhanced etching on feature surfaces. This paper presents in situ Fourier transform infrared (FTIR) absorption spectroscopy of gas-phase and surface reaction products during inductively coupled plasma (ICP) etching of Si in Cl2. The observation was made in the gas phase by transmission absorption spectroscopy (TAS), and also on the substrate surface by reflection absorption spectroscopy (RAS). The quantum chemical calculation was also made of the vibrational frequency of silicon chloride molecules. The deconvolution of the TAS spectrum revealed absorption features of Si2Cl6 and SiClx (x = 1-3) as well as SiCl4, while that of the RAS spectrum revealed relatively increased absorption features of unsaturated silicon chlorides. A different behavior was also observed in bias power dependence between the TAS and RAS spectra.

  7. Ion beam sputtering of fluoropolymers. [etching polymer films and target surfaces

    NASA Technical Reports Server (NTRS)

    Sovey, J. S.

    1978-01-01

    Ion beam sputter processing rates as well as pertinent characteristics of etched targets and films are described. An argon ion beam source was used to sputter etch and deposit the fluoropolymers PTFE, FEP, and CTFE. Ion beam energy, current density, and target temperature were varied to examine effects on etch and deposition rates. The ion etched fluoropolymers yield cone or spire-like surface structures which vary depending upon the type of polymer, ion beam power density, etch time, and target temperature. Sputter target and film characteristics documented by spectral transmittance measurements, X-ray diffraction, ESCA, and SEM photomicrographs are included.

  8. O2 Plasma Etching and Antistatic Gun Surface Modifications for CNT Yarn Microelectrode Improve Sensitivity and Antifouling Properties.

    PubMed

    Yang, Cheng; Wang, Ying; Jacobs, Christopher B; Ivanov, Ilia N; Venton, B Jill

    2017-05-16

    Carbon nanotube (CNT) based microelectrodes exhibit rapid and selective detection of neurotransmitters. While different fabrication strategies and geometries of CNT microelectrodes have been characterized, relatively little research has investigated ways to selectively enhance their electrochemical properties. In this work, we introduce two simple, reproducible, low-cost, and efficient surface modification methods for carbon nanotube yarn microelectrodes (CNTYMEs): O 2 plasma etching and antistatic gun treatment. O 2 plasma etching was performed by a microwave plasma system with oxygen gas flow and the optimized time for treatment was 1 min. The antistatic gun treatment flows ions by the electrode surface; two triggers of the antistatic gun was the optimized number on the CNTYME surface. Current for dopamine at CNTYMEs increased 3-fold after O 2 plasma etching and 4-fold after antistatic gun treatment. When the two treatments were combined, the current increased 12-fold, showing the two effects are due to independent mechanisms that tune the surface properties. O 2 plasma etching increased the sensitivity due to increased surface oxygen content but did not affect surface roughness while the antistatic gun treatment increased surface roughness but not oxygen content. The effect of tissue fouling on CNT yarns was studied for the first time, and the relatively hydrophilic surface after O 2 plasma etching provided better resistance to fouling than unmodified or antistatic gun treated CNTYMEs. Overall, O 2 plasma etching and antistatic gun treatment improve the sensitivity of CNTYMEs by different mechanisms, providing the possibility to tune the CNTYME surface and enhance sensitivity.

  9. Influence of implant surface topography on bone-regenerative potential and mechanical retention in the human maxilla and mandible.

    PubMed

    Wei, Niu; Bin, Shi; Jing, Zhou; Wei, Sun; Yingqiong, Zhao

    2014-06-01

    To evaluate the short- and mid-term effects of commercial pure (cp) titanium implant surface topography on osseointegration, bone-regenerative potential and mechanical retention in the human maxilla and mandible. 32 micro-implants with the same geometry but with four different surface treatments were implanted in the maxilla and mandible of eight patients. Each patient received four micro-implants, one of each type. Percentage of bone-to-implant contact analysis and histological evaluation was carried 3, 6 and 12 weeks after implantation. Furthermore, reverse removal torque tests were conducted 3 and 6 weeks after implantation to analyze functional bone attachment. Implant surfaces tested were: machined, grit-blasted, acid-etched, and grit-blasted with acid-etch. One-way ANOVA was performed using the multiple comparison Fisher's test to determine significance of observed differences among test groups. The level of significance was established at 5% (P < 0.05). Mean and standard deviations of the test groups were calculated. Surface roughness had a significant correlation with the evolution of bone regeneration. The surfaces with roughness Ra approximately 4 microim (grit-blasted and grit-blasted with acid-etch), showed rapid tissue colonization compared to machine and acid-etched surfaces. The results of reverse removal torque tests confirmed a significant correlation between surface roughness and functional bone attachment. Grit-blasted and grit-blasted with acid etched surfaces showed higher retention values compared to machine and acid-etched implants. This finding was supported by higher bone-to-implant contact observed for rougher surfaces (grit-blasted and grit-blasted with acid etching).

  10. Structure, morphology, and photoluminescence of porous Si nanowires: effect of different chemical treatments

    PubMed Central

    2013-01-01

    The structure and light-emitting properties of Si nanowires (SiNWs) fabricated by a single-step metal-assisted chemical etching (MACE) process on highly boron-doped Si were investigated after different chemical treatments. The Si nanowires that result from the etching of a highly doped p-type Si wafer by MACE are fully porous, and as a result, they show intense photoluminescence (PL) at room temperature, the characteristics of which depend on the surface passivation of the Si nanocrystals composing the nanowires. SiNWs with a hydrogen-terminated nanostructured surface resulting from a chemical treatment with a hydrofluoric acid (HF) solution show red PL, the maximum of which is blueshifted when the samples are further chemically oxidized in a piranha solution. This blueshift of PL is attributed to localized states at the Si/SiO2 interface at the shell of Si nanocrystals composing the porous SiNWs, which induce an important pinning of the electronic bandgap of the Si material and are involved in the recombination mechanism. After a sequence of HF/piranha/HF treatment, the SiNWs are almost fully dissolved in the chemical solution, which is indicative of their fully porous structure, verified also by transmission electron microscopy investigations. It was also found that a continuous porous Si layer is formed underneath the SiNWs during the MACE process, the thickness of which increases with the increase of etching time. This supports the idea that porous Si formation precedes nanowire formation. The origin of this effect is the increased etching rate at sites with high dopant concentration in the highly doped Si material. PMID:24025542

  11. Effect of Holding Time on Surface Films Formed on Molten AZ91D Alloy Protected by Graphite Powder

    NASA Astrophysics Data System (ADS)

    Li, Weihong; Zhou, Jixue; Ma, Baichang; Wang, Jinwei; Wu, Jianhua; Yang, Yuansheng

    2017-10-01

    Graphite powder was adopted to prevent the AZ91D magnesium alloy from oxidizing during the melting and casting process. The microstructure of the resultant surface films formed at 973 K (700 °C) holding for 0, 15, 30, 45, and 60 minutes was investigated by scanning electron microscopy, energy dispersive spectroscopy (EDS), and X-ray diffraction (XRD) after mechanical polishing and chemical etching. The results indicated that the surface films were composed of a protective layer and the underneath particles with different morphology. The protective layer was continuous with a thickness of 200 to 1000 nm mainly consisting of MgO, MgF2, and C, while the underneath particles mainly consisted of MgF2 and MgAl2O4. The surface films were the result of the interaction between the graphite powder, the melt, and the ambient atmosphere. The number and the size of the underneath particles, determining the thickness uniformity of the surface films, and the unevenness of the microsurface morphology increased with holding time. The mechanism of holding time on the resultant surface films was also discussed.

  12. Etching and oxidation of InAs in planar inductively coupled plasma

    NASA Astrophysics Data System (ADS)

    Dultsev, F. N.; Kesler, V. G.

    2009-10-01

    The surface of InAs (1 1 1)A was investigated under plasmachemical etching in the gas mixture CH 4/H 2/Ar. Etching was performed using the RF (13.56 MHz) and ICP plasma with the power 30-150 and 50-300 W, respectively; gas pressure in the reactor was 3-10 mTorr. It was demonstrated that the composition of the subsurface layer less than 5 nm thick changes during plasmachemical etching. A method of deep etching of InAs involving ICP plasma and hydrocarbon based chemistry providing the conservation of the surface relief is proposed. Optimal conditions and the composition of the gas phase for plasmachemical etching ensuring acceptable etch rates were selected.

  13. Restoration of obliterated engraved marks on steel surfaces by chemical etching reagent.

    PubMed

    Song, Qingfang

    2015-05-01

    Chemical etching technique is widely used for restoration of obliterated engraved marks on steel surface in the field of public security. The consumed thickness of steel surface during restoration process is considered as a major criterion for evaluating the efficiency of the chemical etching reagent. The thinner the consumed thickness, the higher the restoration efficiency. According to chemical principles, maintaining the continuous oxidative capabilities of etching reagents and increasing the kinetic rate difference of the reaction between the engraved and non-engraved area with the chemical etching reagent can effectively reduce the consumed steel thickness. The study employed steel surface from the engine case of motorcycle and the car frame of automobile. The chemical etching reagents are composed of nitric acid as the oxidizer, hydrofluoric acid as the coordination agent and mixed with glacial acetic acid or acetone as the solvents. Based on the performance evaluation of three different etching reagents, the one composed of HNO3, HF and acetone gave the best result. Copyright © 2015 Elsevier Ireland Ltd. All rights reserved.

  14. Mud volcanism and morphology of impact craters in Utopia Planitia on Mars: Evidence for the ancient ocean

    NASA Astrophysics Data System (ADS)

    Ivanov, Mikhail A.; Hiesinger, H.; Erkeling, G.; Reiss, D.

    2014-01-01

    Results of our detailed geological mapping and interpretation of the nature and relative and absolute model ages of units and structures in the SW portion of Utopia Planitia (20-45°N, 100-120°E) suggest the following. (1) The size-frequency distribution (SFD) of craters that both are buried by materials of the Vastitas Borealis units (VB) and superpose its surface indicate that the absolute model ages of terrain predating the emplacement of the VB is ˜3.7 Ga. (2) Lack of craters that are partly embayed by materials of the VB in the SW portion of Utopia Planitia implies that the emplacement of the VB was faster than the rate of accumulation of impact craters and is consistent with the geologically short time of emplacement of the VB due to catastrophic release of water from outflow channels (e.g., Carr, M.H. [1996]. Water on Mars. Oxford University Press, New York, p. 229). (3) The SFD of craters that superpose the surface of the VB indicates an absolute model age of ˜3.6-3.5 Ga. The absolute model ages of etched flows, which represent the upper stratigraphic limit of the VB, are estimated to be ˜3.5 Ga. (4) The majority of the larger (i.e., >1 km) impact craters show ejecta morphologies (rampart and pancake-like ejecta) that are indicative of the presence of ice/water in the target materials. The distal portions of the pancake-like ejecta are heavily degraded (not due to embayment). This suggests that these craters formed in targets that contained higher abundances of volatiles. (5) The diameter ranges of the craters with either rampart- or pancake-like ejecta are overlapping (from ˜2 to ˜60 km). Craters with pancake-like ejecta are concentrated within the central portion of the Utopia basin (less than ˜1000 km from the basin center) and rampart craters occur at the periphery of the basin. This pattern of the crater spatial distribution suggests that materials within the center of Utopia Planitia contained more ice/water. (6) Etched flows around the central portion of Utopia Planitia were erupted from beneath of the surface of the VB. Their morphology and pattern of degradation, however, are inconsistent with lava and, instead, indicate formation of the flows due to mud volcanism. (7) Etched flows are spatially associated with giant polygons and there is evidence that these features populated the center portion of Utopia Planitia before it was covered by the Elysium-derived units. The outer (southern) edge of the zone of polygonal troughs and etched flows approximately corresponds to the transition from pancake-like ejecta to rampart ejecta. This suggest that the outer edge of the zone of the polygons and flows may outline the deeper portions of the large body (˜2000 km across) of water/ice that likely existed in the center of Utopia Planitia in late Hesperian.

  15. Formation mechanism of graphite hexagonal pyramids by argon plasma etching of graphite substrates

    NASA Astrophysics Data System (ADS)

    Glad, X.; de Poucques, L.; Bougdira, J.

    2015-12-01

    A new graphite crystal morphology has been recently reported, namely the graphite hexagonal pyramids (GHPs). They are hexagonally-shaped crystals with diameters ranging from 50 to 800 nm and a constant apex angle of 40°. These nanostructures are formed from graphite substrates (flexible graphite and highly ordered pyrolytic graphite) in low pressure helicon coupling radiofrequency argon plasma at 25 eV ion energy and, purportedly, due to a physical etching process. In this paper, the occurrence of peculiar crystals is shown, presenting two hexagonal orientations obtained on both types of samples, which confirms such a formation mechanism. Moreover, by applying a pretreatment step with different time durations of inductive coupling radiofrequency argon plasma, for which the incident ion energy decreases at 12 eV, uniform coverage of the surface can be achieved with an influence on the density and size of the GHPs.

  16. Design of Hybrid Nanostructural Arrays to Manipulate SERS-Active Substrates by Nanosphere Lithography.

    PubMed

    Zhao, Xiaoyu; Wen, Jiahong; Zhang, Mengning; Wang, Dunhui; Wang, Yaxin; Chen, Lei; Zhang, Yongjun; Yang, Jinghai; Du, Youwei

    2017-03-01

    An easy-handling and low-cost method is utilized to controllably fabricate nanopattern arrays as the surface-enhanced Raman scattering (SERS) active substrates with high density of SERS-active areas (hot spots). A hybrid silver array of nanocaps and nanotriangles are prepared by combining magnetron sputtering and plasma etching. By adjusting the etching time of polystyrene (PS) colloid spheres array in silver nanobowls, the morphology of the arrays can be easily manipulated to control the formation and distribution of hot spots. The experimental results show that the hybrid nanostructural arrays have large enhancement factor, which is estimated to be seven times larger than that in the array of nanocaps and three times larger than that in the array of nanorings and nanoparticles. According to the results of finite-difference time-domain simulation, the excellent SERS performance of this array is ascribed to the high density of hot spots and enhanced electromagnetic field.

  17. The Effects of Acid Etching on the Nanomorphological Surface Characteristics and Activation Energy of Titanium Medical Materials

    PubMed Central

    Hung, Kuo-Yung; Lin, Yi-Chih; Feng, Hui-Ping

    2017-01-01

    The purpose of this study was to characterize the etching mechanism, namely, the etching rate and the activation energy, of a titanium dental implant in concentrated acid and to construct the relation between the activation energy and the nanoscale surface topographies. A commercially-pure titanium (CP Ti) and Ti-6Al-4V ELI surface were tested by shot blasting (pressure, grain size, blasting distance, blasting angle, and time) and acid etching to study its topographical, weight loss, surface roughness, and activation energy. An Arrhenius equation was applied to derive the activation energy for the dissolution of CP Ti/Ti-6Al-4V ELI in sulfuric acid (H2SO4) and hydrochloric acid (HCl) at different temperatures. In addition, white-light interferometry was applied to measure the surface nanomorphology of the implant to obtain 2D or 3D roughness parameters (Sa, Sq, and St). The nanopore size that formed after etching was approximately 100–500 nm. The surface roughness of CP Ti and Ti-6Al-4V ELI decreased as the activation energy decreased but weight loss increased. Ti-6Al-4V ELI has a higher level of activation energy than Ti in HCl, which results in lower surface roughness after acid etching. This study also indicates that etching using a concentrated hydrochloric acid provided superior surface modification effects in titanium compared with H2SO4. PMID:29019926

  18. Biomechanical properties of jaw periosteum-derived mineralized culture on different titanium topography.

    PubMed

    Att, Wael; Kubo, Katsutoshi; Yamada, Masahiro; Maeda, Hatsuhiko; Ogawa, Takahiro

    2009-01-01

    This study evaluated the biomechanical properties of periosteum-derived mineralized culture on different surface topographies of titanium. Titanium surfaces modified by machining or by acid etching were analyzed using scanning electron microscopy (SEM). Rat mandibular periosteum-derived cells were cultured on either of the titanium surfaces. Cell proliferation was evaluated by cell counts, and gene expression was analyzed using a reverse-transcriptase polymerase chain reaction. Alkaline phosphatase (ALP) stain assay was employed to evaluate osteoblastic activity. Matrix mineralization was examined via von Kossa stain assay, total calcium deposition, and SEM. The hardness and elastic modulus of mineralized cultures were measured using a nano-indenter. The machined surface demonstrated a flat topographic configuration, while the acid-etched surface revealed a uniform micron-scale roughness. Both cell density and ALP activity were significantly higher on the machined surface than on the acid-etched surface. The expression of bone-related genes was up-regulated or enhanced on the acid-etched surface compared to the machined surface. Von Kossa stain showed significantly greater positive areas for the machined surface compared to the acid-etched surface, while total calcium deposition was statistically similar. Mineralized culture on the acid-etched surface was characterized by denser calcium deposition, more mature collagen deposition on the superficial layer, and larger and denser globular matrices inside the matrix than the culture on the machined surface. The mineralized matrix on the acid-etched surface was two times harder than on the machined surface, whereas the elastic modulus was comparable between the two surfaces. The design of this study can be used as a model to evaluate the effect of implant surface topography on the biomechanical properties of periosteum-derived mineralized culture. The results suggest that mandibular periosteal cells respond to different titanium surface topographies differently enough to produce mineralized matrices with different biomechanical qualities.

  19. Fabrication of precision high quality facets on molecular beam epitaxy material

    DOEpatents

    Petersen, Holly E.; Goward, William D.; Dijaili, Sol P.

    2001-01-01

    Fabricating mirrored vertical surfaces on semiconductor layered material grown by molecular beam epitaxy (MBE). Low energy chemically assisted ion beam etching (CAIBE) is employed to prepare mirrored vertical surfaces on MBE-grown III-V materials under unusually low concentrations of oxygen in evacuated etching atmospheres of chlorine and xenon ion beams. UV-stabilized smooth-surfaced photoresist materials contribute to highly vertical, high quality mirrored surfaces during the etching.

  20. An Ingenious Super Light Trapping Surface Templated from Butterfly Wing Scales

    NASA Astrophysics Data System (ADS)

    Han, Zhiwu; Li, Bo; Mu, Zhengzhi; Yang, Meng; Niu, Shichao; Zhang, Junqiu; Ren, Luquan

    2015-08-01

    Based on the super light trapping property of butterfly Trogonoptera brookiana wings, the SiO2 replica of this bionic functional surface was successfully synthesized using a simple and highly effective synthesis method combining a sol-gel process and subsequent selective etching. Firstly, the reflectivity of butterfly wing scales was carefully examined. It was found that the whole reflectance spectroscopy of the butterfly wings showed a lower level (less than 10 %) in the visible spectrum. Thus, it was confirmed that the butterfly wings possessed a super light trapping effect. Afterwards, the morphologies and detailed architectures of the butterfly wing scales were carefully investigated using the ultra-depth three-dimensional (3D) microscope and field emission scanning electronic microscopy (FESEM). It was composed by the parallel ridges and quasi-honeycomb-like structure between them. Based on the biological properties and function above, an exact SiO2 negative replica was fabricated through a synthesis method combining a sol-gel process and subsequent selective etching. At last, the comparative analysis of morphology feature size and the reflectance spectroscopy between the SiO2 negative replica and the flat plate was conducted. It could be concluded that the SiO2 negative replica inherited not only the original super light trapping architectures, but also the super light trapping characteristics of bio-template. This work may open up an avenue for the design and fabrication of super light trapping materials and encourage people to look for more super light trapping architectures in nature.

  1. Scanning electron microscope investigation of the structural growth in thick sputtered coatings

    NASA Technical Reports Server (NTRS)

    Spalvins, T.

    1975-01-01

    Sputtered S-Monel, silver, and 304 stainless steel coatings and molybdenum disulfide coatings were deposited on mica and metal substrates with various surface finishes to investigate the structural growth of the coating by scanning electron microscopy. The geometry and the surface morphology of the nodules are characterized. Compositional changes within the coating were analyzed by energy dispersive X-ray analysis. Defects in the surface finish act as preferential nucleation sites and form isolated overlapping and complex nodules and various unusual surface overgrowths on the coating. The nodule boundaries are very vulnerable to chemical etching and these nodules do not disappear after full annealing. Further, they have undesirable effects on mechanical properties; cracks are initiated at the nodules when the coating is stressed by mechanical forces.

  2. Sputtered gold mask for deep chemical etching of silicon

    NASA Technical Reports Server (NTRS)

    Pisciotta, B. P.; Gross, C.; Olive, R. S.

    1975-01-01

    Sputtered mask resists chemical attack from acid and has adherence to withstand prolonged submergence in etch solution without lifting from silicon surface. Even under prolonged etch conditions with significant undercutting, gold mask maintained excellent adhesion to silicon surface and imperviousness to acid.

  3. Deep Etching Process Developed for the Fabrication of Silicon Carbide Microsystems

    NASA Technical Reports Server (NTRS)

    Beheim, Glenn M.

    2000-01-01

    Silicon carbide (SiC), because of its superior electrical and mechanical properties at elevated temperatures, is a nearly ideal material for the microminiature sensors and actuators that are used in harsh environments where temperatures may reach 600 C or greater. Deep etching using plasma methods is one of the key processes used to fabricate silicon microsystems for more benign environments, but SiC has proven to be a more difficult material to etch, and etch depths in SiC have been limited to several micrometers. Recently, the Sensors and Electronics Technology Branch at the NASA Glenn Research Center at Lewis Field developed a plasma etching process that was shown to be capable of etching SiC to a depth of 60 mm. Deep etching of SiC is achieved by inductive coupling of radiofrequency electrical energy to a sulfur hexafluoride (SF6) plasma to direct a high flux of energetic ions and reactive fluorine atoms to the SiC surface. The plasma etch is performed at a low pressure, 5 mtorr, which together with a high gas throughput, provides for rapid removal of the gaseous etch products. The lateral topology of the SiC microstructure is defined by a thin film of etch-resistant material, such as indium-tin-oxide, which is patterned using conventional photolithographic processes. Ions from the plasma bombard the exposed SiC surfaces and supply the energy needed to initiate a reaction between SiC and atomic fluorine. In the absence of ion bombardment, no reaction occurs, so surfaces perpendicular to the wafer surface (the etch sidewalls) are etched slowly, yielding the desired vertical sidewalls.

  4. Fabrication of Monolithic Sapphire Membranes for High T(sub c) Bolometer Array Development

    NASA Technical Reports Server (NTRS)

    Pugel, D. E.; Lakew, B.; Aslam, S.; Wang, L.

    2004-01-01

    This paper examines the effectiveness of Pt/Cr thin film masks for the architecture of monolithic membrane structures in r-plane single crystal sapphire. The development of a pinhole-free Pt/Cr composite mask that is resistant to boiling H2SO4:H3PO4 etchant will lead to the fabrication of smooth sapphire membranes whose surfaces are well-suited for the growth of low-noise high Tc films. In particular, the relationship of thermal annealing conditions on the Pt/Cr composite mask system to: (1) changes in the surface morphology (2) elemental concentration of the Pt/Cr thin film layers and (3) etch pit formation on the sapphire surface will be presented.

  5. Real-time observation of morphological transformations in II-VI semiconducting nanobelts via environmental transmission electron microscopy

    DOE PAGES

    Agarwal, Rahul; Zakharov, Dmitri N.; Krook, Nadia M.; ...

    2015-05-01

    It has been observed that wurtzite II–VI semiconducting nanobelts transform into single-crystal, periodically branched nanostructures upon heating. The mechanism of this novel transformation has been elucidated by heating II–VI nanobelts in an environmental transmission electron microscope (ETEM) in oxidizing, reducing and inert atmospheres while observing their structural changes with high spatial resolution. The interplay of surface reconstruction of high-energy surfaces of the wurtzite phase and environment-dependent anisotropic chemical etching of certain crystal surfaces in the branching mechanism of nanobelts has been observed. Understanding of structural and chemical transformations of materials via in situ microscopy techniques and their role in designingmore » new nanostructured materials is discussed.« less

  6. DOE Office of Scientific and Technical Information (OSTI.GOV)

    Chen, Yu; School of Mechanical and Electrical Engineering, Wuhan Institute of Technology, Wuhan 430073; Guo, Zhiguang, E-mail: zguo@licp.cas.cn

    Graphical abstract: A double-metal-assisted chemical etching method is employed to fabricate superhydrophobic surfaces, showing a good superhydrophobicity with the contact angle of about 170°, and the sliding angle of about 0°. Meanwhile, the potential formation mechanism about it is also presented. Highlights: ► A double-metal-assisted chemical etching method is employed to fabricate superhydrophobic surfaces. ► The obtained surfaces show good superhydrophobicity with a high contact angle and low sliding angle. ► The color of the etched substrate dark brown or black and it is so-called black silicon. -- Abstract: Silicon substrates treated by metal-assisted chemical etching have been studied formore » many years since they could be employed in a variety of electronic and optical devices such as integrated circuits, photovoltaics, sensors and detectors. However, to the best of our knowledge, the chemical etching treatment on the same silicon substrate with the assistance of two or more kinds of metals has not been reported. In this paper, we mainly focus on the etching time and finally obtain a series of superhydrophobic silicon surfaces with novel etching structures through two successive etching processes of Cu-assisted and Ag-assisted chemical etching. It is shown that large-scale homogeneous but locally irregular wire-like structures are obtained, and the superhydrophobic surfaces with low hysteresis are prepared after the modifications with low surface energy materials. It is worth noting that the final silicon substrates not only possess high static contact angle and low hysteresis angle, but also show a black color, indicating that the superhydrophobic silicon substrate has an extremely low reflectance in a certain range of wavelengths. In our future work, we will go a step further to discuss the effect of temperature, the size of Cu nanoparticles and solution concentration on the final topography and superhydrophobicity.« less

  7. Optical properties of micromachined polysilicon reflective surfaces with etching holes

    NASA Astrophysics Data System (ADS)

    Zou, Jun; Byrne, Colin; Liu, Chang; Brady, David J.

    1998-08-01

    MUMPS (Multi-User MEMS Process) is receiving increasingly wide use in micro optics. We have investigated the optical properties of the polysilicon reflective surface in a typical MUMPS chip within the visible light spectrum. The effect of etching holes on the reflected laser beam is studied. The reflectivity and diffraction patterns at five different wavelengths have been measured. The optical properties of the polysilicon reflective surface are greatly affected by the surface roughness, the etching holes, as well as the material. The etching holes contribute to diffraction and reduction of reflectivity. This study provides a basis for optimal design of micromachined free-space optical systems.

  8. Inverse metal-assisted chemical etching produces smooth high aspect ratio InP nanostructures.

    PubMed

    Kim, Seung Hyun; Mohseni, Parsian K; Song, Yi; Ishihara, Tatsumi; Li, Xiuling

    2015-01-14

    Creating high aspect ratio (AR) nanostructures by top-down fabrication without surface damage remains challenging for III-V semiconductors. Here, we demonstrate uniform, array-based InP nanostructures with lateral dimensions as small as sub-20 nm and AR > 35 using inverse metal-assisted chemical etching (I-MacEtch) in hydrogen peroxide (H2O2) and sulfuric acid (H2SO4), a purely solution-based yet anisotropic etching method. The mechanism of I-MacEtch, in contrast to regular MacEtch, is explored through surface characterization. Unique to I-MacEtch, the sidewall etching profile is remarkably smooth, independent of metal pattern edge roughness. The capability of this simple method to create various InP nanostructures, including high AR fins, can potentially enable the aggressive scaling of InP based transistors and optoelectronic devices with better performance and at lower cost than conventional etching methods.

  9. Reactive ion etched substrates and methods of making and using

    DOEpatents

    Rucker, Victor C [San Francisco, CA; Shediac, Rene [Oakland, CA; Simmons, Blake A [San Francisco, CA; Havenstrite, Karen L [New York, NY

    2007-08-07

    Disclosed herein are substrates comprising reactive ion etched surfaces and specific binding agents immobilized thereon. The substrates may be used in methods and devices for assaying or isolating analytes in a sample. Also disclosed are methods of making the reactive ion etched surfaces.

  10. Effects of wet etch processing on laser-induced damage of fused silica surfaces

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Battersby, C.L.; Kozlowski, M.R.; Sheehan, L.M.

    1998-12-22

    Laser-induced damage of transparent fused silica optical components by 355 nm illumination occurs primarily at surface defects produced during the grinding and polishing processes. These defects can either be surface defects or sub-surface damage.Wet etch processing in a buffered hydrogen fluoride (HF) solution has been examined as a tool for characterizing such defects. A study was conducted to understand the effects of etch depth on the damage threshold of fused silica substrates. The study used a 355 nm, 7.5 ns, 10 Hz Nd:YAG laser to damage test fused silica optics through various wet etch processing steps. Inspection of the surfacemore » quality was performed with Nomarski microscopy and Total Internal Reflection Microscopy. The damage test data and inspection results were correlated with polishing process specifics. The results show that a wet etch exposes subsurface damage while maintaining or improving the laser damage performance. The benefits of a wet etch must be evaluated for each polishing process.« less

  11. Power ultrasound irradiation during the alkaline etching process of the 2024 aluminum alloy

    NASA Astrophysics Data System (ADS)

    Moutarlier, V.; Viennet, R.; Rolet, J.; Gigandet, M. P.; Hihn, J. Y.

    2015-11-01

    Prior to any surface treatment on an aluminum alloy, a surface preparation is necessary. This commonly consists in performing an alkaline etching followed by acid deoxidizing. In this work, the use of power ultrasound irradiation during the etching step on the 2024 aluminum alloy was studied. The etching rate was estimated by weight loss, and the alkaline film formed during the etching step was characterized by glow discharge optical emission spectrometry (GDOES) and scanning electron microscope (SEM). The benefit of power ultrasound during the etching step was confirmed by pitting potential measurement in NaCl solution after a post-treatment (anodizing).

  12. High-aspect ratio micro- and nanostructures enabled by photo-electrochemical etching for sensing and energy harvesting applications

    NASA Astrophysics Data System (ADS)

    Alhalaili, Badriyah; Dryden, Daniel M.; Vidu, Ruxandra; Ghandiparsi, Soroush; Cansizoglu, Hilal; Gao, Yang; Saif Islam, M.

    2018-03-01

    Photo-electrochemical (PEC) etching can produce high-aspect ratio features, such as pillars and holes, with high anisotropy and selectivity, while avoiding the surface and sidewall damage caused by traditional deep reactive ion etching (DRIE) or inductively coupled plasma (ICP) RIE. Plasma-based techniques lead to the formation of dangling bonds, surface traps, carrier leakage paths, and recombination centers. In pursuit of effective PEC etching, we demonstrate an optical system using long wavelength (λ = 975 nm) infra-red (IR) illumination from a high-power laser (1-10 W) to control the PEC etching process in n-type silicon. The silicon wafer surface was patterned with notches through a lithography process and KOH etching. Then, PEC etching was introduced by illuminating the backside of the silicon wafer to enhance depth, resulting in high-aspect ratio structures. The effect of the PEC etching process was optimized by varying light intensities and electrolyte concentrations. This work was focused on determining and optimizing this PEC etching technique on silicon, with the goal of expanding the method to a variety of materials including GaN and SiC that are used in designing optoelectronic and electronic devices, sensors and energy harvesting devices.

  13. Surface Phenomena During Plasma-Assisted Atomic Layer Etching of SiO2.

    PubMed

    Gasvoda, Ryan J; van de Steeg, Alex W; Bhowmick, Ranadeep; Hudson, Eric A; Agarwal, Sumit

    2017-09-13

    Surface phenomena during atomic layer etching (ALE) of SiO 2 were studied during sequential half-cycles of plasma-assisted fluorocarbon (CF x ) film deposition and Ar plasma activation of the CF x film using in situ surface infrared spectroscopy and ellipsometry. Infrared spectra of the surface after the CF x deposition half-cycle from a C 4 F 8 /Ar plasma show that an atomically thin mixing layer is formed between the deposited CF x layer and the underlying SiO 2 film. Etching during the Ar plasma cycle is activated by Ar + bombardment of the CF x layer, which results in the simultaneous removal of surface CF x and the underlying SiO 2 film. The interfacial mixing layer in ALE is atomically thin due to the low ion energy during CF x deposition, which combined with an ultrathin CF x layer ensures an etch rate of a few monolayers per cycle. In situ ellipsometry shows that for a ∼4 Å thick CF x film, ∼3-4 Å of SiO 2 was etched per cycle. However, during the Ar plasma half-cycle, etching proceeds beyond complete removal of the surface CF x layer as F-containing radicals are slowly released into the plasma from the reactor walls. Buildup of CF x on reactor walls leads to a gradual increase in the etch per cycle.

  14. [Influence of different surface treatments on porcelain surface topography].

    PubMed

    Tai, Yinxia; Zhu, Xianchun; Sen, Yan; Liu, Chang; Zhang, Xian; Shi, Xueming

    2013-02-01

    To evaluate the influence of different surface treatments on porcelain surface topography. Metal ceramic prostheses in 6 groups were treated according to the different surface treatment methods, and the surface topography was observed through scanning electron microscope (SEM). Group A was the control one (untreated), group B was etched by 9.6% hydrofluoric acid(HF), group C was deglazed by grinding and then etched by 9.6% HF, group D was treated with Nd: YAG laser irradiation(0.75 W) and HF etching, group E was treated with Nd: YAG laser irradiation (1.05 W) and HF etching, and group F was treated with laser irradiation (1.45 W) and HF etching. Surface topography was different in different groups. A lot of inerratic cracks with the shapes of rhombuses and grid, and crater with a shape of circle were observed on the ceramic surface after treatment with energy parameters of 1.05 W Nd: YAG laser irradiation and 9.6% HF etching (group E). Surface topography showed a lot of concaves on the inner wall of the cracks, and the concaves with diameter of 1-5 microm could be observed on the inner wall of the holes, which had a diameter of 20 microm under SEM. The use of Nd: YAG laser irradiation with the energy parameters of 1.05 W and the HF with a concentration of 9.6% can evenly coarsen the porcelain surface, that is an effective surface treatment method.

  15. Model polymer etching and surface modification by a time modulated RF plasma jet: role of atomic oxygen and water vapor

    NASA Astrophysics Data System (ADS)

    Luan, P.; Knoll, A. J.; Wang, H.; Kondeti, V. S. S. K.; Bruggeman, P. J.; Oehrlein, G. S.

    2017-01-01

    The surface interaction of a well-characterized time modulated radio frequency (RF) plasma jet with polystyrene, poly(methyl methacrylate) and poly(vinyl alcohol) as model polymers is investigated. The RF plasma jet shows fast polymer etching but mild chemical modification with a characteristic carbonate ester and NO formation on the etched surface. By varying the plasma treatment conditions including feed gas composition, environment gaseous composition, and treatment distance, we find that short lived species, especially atomic O for Ar/1% O2 and 1% air plasma and OH for Ar/1% H2O plasma, play an essential role for polymer etching. For O2 containing plasma, we find that atomic O initiates polymer etching and the etching depth mirrors the measured decay of O atoms in the gas phase as the nozzle-surface distance increases. The etching reaction probability of an O atom ranging from 10-4 to 10-3 is consistent with low pressure plasma research. We also find that adding O2 and H2O simultaneously into Ar feed gas quenches polymer etching compared to adding them separately which suggests the reduction of O and OH density in Ar/O2/H2O plasma.

  16. Micromorphological characterization of adhesive interface of sound dentin and total-etch and self-etch adhesives.

    PubMed

    Drobac, Milan; Stojanac, Igor; Ramić, Bojana; Premović, Milica; Petrović, Ljubomir

    2015-01-01

    The ultimate goal in restorative dentistry has always been to achieve strong and permanent bond between the dental tissues and filling materials. It is not easy to achieve this task because the bonding process is different for enamel and dentin-dentin is more humid and more organic than enamel. It is moisture and organic nature of dentin that make this hard tissue very complex to achieve adhesive bond. One of the first and most widely used tools for examining the adhesive bond between hard dental tissues and composite restorative materials is scanning electron microscopy. The aim of this study was scanning electron microscopy analyzes the interfacial micro morphology of total-etch and self-etch adhesives. Micro morphological characteristics of interface between total-etch adhesive (Prime & Bond NT) in combination with the corresponding composite (Ceram X Mono) were compared with those of self-etching adhesive (AdheSE One) in, combination with the corresponding composite (Tetric EvoCeram). The specimens were observed under 1000 x magnification of scanning electron microscopy (JEOL, JSM-6460 Low Vacuum). Measurement of the thickness of the hybrid layer of the examined com posite systems was performed with the software of the device used (NIH Image Analyser). Micromorphological analysis of interface showed that the hybrid layer in sound dentin was well formed, its average thickness being 2.68 microm, with a large number of resin tags and a large amount of lateral branches for specimens with a composite system Prime & Bond NT-Ceram X Mono. However, the specimens' with composite systems Adhese One-Tetric EvoCeram did not show the presence of hybrid layer and the resin tags were poorly represented. The results of this study suggest that total-etch adhesives bond better with sound dentin than self-etch adhesive.

  17. Characterization of the porosity of human dental enamel and shear bond strength in vitro after variable etch times: initial findings using the BET method.

    PubMed

    Nguyen, Trang T; Miller, Arthur; Orellana, Maria F

    2011-07-01

    (1) To quantitatively characterize human enamel porosity and surface area in vitro before and after etching for variable etching times; and (2) to evaluate shear bond strength after variable etching times. Specifically, our goal was to identify the presence of any correlation between enamel porosity and shear bond strength. Pore surface area, pore volume, and pore size of enamel from extracted human teeth were analyzed by Brunauer-Emmett-Teller (BET) gas adsorption before and after etching for 15, 30, and 60 seconds with 37% phosphoric acid. Orthodontic brackets were bonded with Transbond to the samples with variable etch times and were subsequently applied to a single-plane lap shear testing system. Pore volume and surface area increased after etching for 15 and 30 seconds. At 60 seconds, this increase was less pronounced. On the contrary, pore size appears to decrease after etching. No correlation was found between variable etching times and shear strength. Samples etched for 15, 30, and 60 seconds all demonstrated clinically viable shear strength values. The BET adsorption method could be a valuable tool in enhancing our understanding of enamel characteristics. Our findings indicate that distinct quantitative changes in enamel pore architecture are evident after etching. Further testing with a larger sample size would have to be carried out for more definitive conclusions to be made.

  18. Post-processing of fused silica and its effects on damage resistance to nanosecond pulsed UV lasers.

    PubMed

    Ye, Hui; Li, Yaguo; Zhang, Qinghua; Wang, Wei; Yuan, Zhigang; Wang, Jian; Xu, Qiao

    2016-04-10

    HF-based (hydrofluoric acid) chemical etching has been a widely accepted technique to improve the laser damage performance of fused silica optics and ensure high-power UV laser systems at designed fluence. Etching processes such as acid concentration, composition, material removal amount, and etching state (etching with additional acoustic power or not) may have a great impact on the laser-induced damage threshold (LIDT) of treated sample surfaces. In order to find out the effects of these factors, we utilized the Taguchi method to determine the etching conditions that are helpful in raising the LIDT. Our results show that the most influential factors are concentration of etchants and the material etched away from the viewpoint of damage performance of fused silica optics. In addition, the additional acoustic power (∼0.6  W·cm-2) may not benefit the etching rate and damage performance of fused silica. Moreover, the post-cleaning procedure of etched samples is also important in damage performances of fused silica optics. Different post-cleaning procedures were, thus, experiments on samples treated under the same etching conditions. It is found that the "spraying + rinsing + spraying" cleaning process is favorable to the removal of etching-induced deposits. Residuals on the etched surface are harmful to surface roughness and optical transmission as well as laser damage performance.

  19. Ion beam sputter etching of orthopedic implanted alloy MP35N and resulting effects on fatigue

    NASA Technical Reports Server (NTRS)

    Wintucky, E. G.; Christopher, M.; Bahnuik, E.; Wang, S.

    1981-01-01

    The effects of two types of argon ion sputter etched surface structures on the tensile stress fatigue properties of orthopedic implant alloy MP35N were investigated. One surface structure was a natural texture resulting from direct bombardment by 1 keV argon ions. The other structure was a pattern of square holes milled into the surface by a 1 keV argon ion beam through a Ni screen mask. The etched surfaces were subjected to tensile stress only in fatigue tests designed to simulate the cyclic load conditions experienced by the stems of artificial hip joint implants. Both types of sputter etched surface structures were found to reduce the fatigue strength below that of smooth surface MP35N.

  20. The effect of dentinal stimulation on pulp nerve function and pulp morphology in the dog.

    PubMed

    Hirvonen, T J; Närhi, M V

    1986-11-01

    The effect of dentinal stimulation on pulpal nerve responses and pulp morphology has been studied in the dog. Canine tooth (n = 25) dentin was stimulated by drilling, probing, and air-blasting for from two to five hours. Acid-etching was used to open dentinal tubules. All test teeth showed disruption of the odontoblast layer and its separation from the predentin; also, dislocation of odontoblast nuclei into dentinal tubules was found in most cases. Single-fiber (n = 14, conduction velocity = 24.3 +/- 7.4 (SD) m/s) recordings of the responses of canine tooth pulpal nerves to dentinal stimulation were made in ten of the stimulated teeth. No changes in the sensitivity of the nerves to dentinal stimulation could be detected. It is concluded that pulpal nerve function and morphological changes of the pulp are not clearly correlated. The condition of the dentin surface seems to be the important factor.

  1. The dependence of carbide morphology on grain boundary character in the highly twinned Alloy 690

    NASA Astrophysics Data System (ADS)

    Li, Hui; Xia, Shuang; Zhou, Bangxin; Chen, Wenjue; Hu, Changliang

    2010-04-01

    The dependence of morphology of grain boundary carbides on grain boundary character in Alloy 690 (Ni-30Cr-10Fe, mass fraction, %) with high fraction of low Σ coincidence site lattice (CSL) grain boundaries was investigated by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Some of the surface grains were removed by means of deep etching. It was observed that carbides grow dendritically at grain boundaries. The carbide bars observed near incoherent twin boundaries and twin related Σ9 grain boundaries are actually secondary dendrites of the carbides on these boundaries. Higher order dendrites could be observed on random grain boundaries, however, no bar-like dendrites were observed near Σ27 grain boundaries and random grain boundaries. The morphology difference of carbides precipitated at grain boundaries with different characters is discussed based on the experimental results in this paper.

  2. Metal etching composition

    NASA Technical Reports Server (NTRS)

    Otousa, Joseph E. (Inventor); Thomas, Clark S. (Inventor); Foster, Robert E. (Inventor)

    1991-01-01

    The present invention is directed to a chemical etching composition for etching metals or metallic alloys. The composition includes a solution of hydrochloric acid, phosphoric acid, ethylene glycol, and an oxidizing agent. The etching composition is particularly useful for etching metal surfaces in preparation for subsequent fluorescent penetrant inspection.

  3. Bulk and Surface Morphologies of ABC Miktoarm Star Terpolymers Composed of PDMS, PI, and PMMA Arms

    DOE PAGES

    Chernyy, Sergey; Kirkensgaard, Jacob Judas Kain; Mahalik, Jyoti P.; ...

    2018-02-02

    DIM miktoarm star copolymers, composed of polydimethylsiloxane [D], poly(1,4-isoprene) [I], and poly(methyl methacrylate) [M], were synthesized using a newly developed linking methodology with 4-allyl-1,1-diphenylethylene as a linking agent. The equilibrium bulk morphologies of the DIM stars were found to range from [6.6.6] tiling patterns to alternating lamellar and alternating cylindrical morphologies, as determined experimentally by small-angle X-ray scattering and transmission electron microscopy and confirmed by dissipative particle dynamics and self-consistent field theory based arguments. The thin film morphologies, which differ from those found in the bulk, were identified by scanning electron microscopy, coupled with oxygen plasma etching. Finally, square arraysmore » of the PDMS nanodots and empty core cylinders were formed on silica after oxygen plasma removal of the poly(1,4-isoprene) and poly(methyl methacrylate) which generated nanostructured substrates decorated with these features readily observable.« less

  4. Bulk and Surface Morphologies of ABC Miktoarm Star Terpolymers Composed of PDMS, PI, and PMMA Arms

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Chernyy, Sergey; Kirkensgaard, Jacob Judas Kain; Mahalik, Jyoti P.

    DIM miktoarm star copolymers, composed of polydimethylsiloxane [D], poly(1,4-isoprene) [I], and poly(methyl methacrylate) [M], were synthesized using a newly developed linking methodology with 4-allyl-1,1-diphenylethylene as a linking agent. The equilibrium bulk morphologies of the DIM stars were found to range from [6.6.6] tiling patterns to alternating lamellar and alternating cylindrical morphologies, as determined experimentally by small-angle X-ray scattering and transmission electron microscopy and confirmed by dissipative particle dynamics and self-consistent field theory based arguments. The thin film morphologies, which differ from those found in the bulk, were identified by scanning electron microscopy, coupled with oxygen plasma etching. Finally, square arraysmore » of the PDMS nanodots and empty core cylinders were formed on silica after oxygen plasma removal of the poly(1,4-isoprene) and poly(methyl methacrylate) which generated nanostructured substrates decorated with these features readily observable.« less

  5. Characterizing fluorocarbon assisted atomic layer etching of Si using cyclic Ar/C4F8 and Ar/CHF3 plasma

    NASA Astrophysics Data System (ADS)

    Metzler, Dominik; Li, Chen; Engelmann, Sebastian; Bruce, Robert L.; Joseph, Eric A.; Oehrlein, Gottlieb S.

    2017-02-01

    With the increasing interest in establishing directional etching methods capable of atomic scale resolution for fabricating highly scaled electronic devices, the need for development and characterization of atomic layer etching processes, or generally etch processes with atomic layer precision, is growing. In this work, a flux-controlled cyclic plasma process is used for etching of SiO2 and Si at the Angstrom-level. This is based on steady-state Ar plasma, with periodic, precise injection of a fluorocarbon (FC) precursor (C4F8 and CHF3) and synchronized, plasma-based Ar+ ion bombardment [D. Metzler et al., J. Vac. Sci. Technol., A 32, 020603 (2014) and D. Metzler et al., J. Vac. Sci. Technol., A 34, 01B101 (2016)]. For low energy Ar+ ion bombardment conditions, physical sputter rates are minimized, whereas material can be etched when FC reactants are present at the surface. This cyclic approach offers a large parameter space for process optimization. Etch depth per cycle, removal rates, and self-limitation of removal, along with material dependence of these aspects, were examined as a function of FC surface coverage, ion energy, and etch step length using in situ real time ellipsometry. The deposited FC thickness per cycle is found to have a strong impact on etch depth per cycle of SiO2 and Si but is limited with regard to control over material etching selectivity. Ion energy over the 20-30 eV range strongly impacts material selectivity. The choice of precursor can have a significant impact on the surface chemistry and chemically enhanced etching. CHF3 has a lower FC deposition yield for both SiO2 and Si and also exhibits a strong substrate dependence of FC deposition yield, in contrast to C4F8. The thickness of deposited FC layers using CHF3 is found to be greater for Si than for SiO2. X-ray photoelectron spectroscopy was used to study surface chemistry. When thicker FC films of 11 Å are employed, strong changes of FC film chemistry during a cycle are seen whereas the chemical state of the substrate varies much less. On the other hand, for FC film deposition of 5 Å for each cycle, strong substrate surface chemical changes are seen during an etching cycle. The nature of this cyclic etching with periodic deposition of thin FC films differs significantly from conventional etching with steady-state FC layers since surface conditions change strongly throughout each cycle.

  6. Plasma processing of superconducting radio frequency cavities

    NASA Astrophysics Data System (ADS)

    Upadhyay, Janardan

    The development of plasma processing technology of superconducting radio frequency (SRF) cavities not only provides a chemical free and less expensive processing method, but also opens up the possibility for controlled modification of the inner surfaces of the cavity for better superconducting properties. The research was focused on the transition of plasma etching from two dimensional flat surfaces to inner surfaces of three dimensional (3D) structures. The results could be applicable to a variety of inner surfaces of 3D structures other than SRF cavities. Understanding the Ar/Cl2 plasma etching mechanism is crucial for achieving the desired modification of Nb SRF cavities. In the process of developing plasma etching technology, an apparatus was built and a method was developed to plasma etch a single cell Pill Box cavity. The plasma characterization was done with the help of optical emission spectroscopy. The Nb etch rate at various points of this cavity was measured before processing the SRF cavity. Cylindrical ring-type samples of Nb placed on the inner surface of the outer wall were used to measure the dependence of the process parameters on plasma etching. The measured etch rate dependence on the pressure, rf power, dc bias, temperature, Cl2 concentration and diameter of the inner electrode was determined. The etch rate mechanism was studied by varying the temperature of the outer wall, the dc bias on the inner electrode and gas conditions. In a coaxial plasma reactor, uniform plasma etching along the cylindrical structure is a challenging task due to depletion of the active radicals along the gas flow direction. The dependence of etch rate uniformity along the cylindrical axis was determined as a function of process parameters. The formation of dc self-biases due to surface area asymmetry in this type of plasma and its variation on the pressure, rf power and gas composition was measured. Enhancing the surface area of the inner electrode to reduce the asymmetry was studied by changing the contour of the inner electrode. The optimized contour of the electrode based on these measurements was chosen for SRF cavity processing.

  7. Cubic GaN quantum dots embedded in zinc-blende AlN microdisks

    NASA Astrophysics Data System (ADS)

    Bürger, M.; Kemper, R. M.; Bader, C. A.; Ruth, M.; Declair, S.; Meier, C.; Förstner, J.; As, D. J.

    2013-09-01

    Microresonators containing quantum dots find application in devices like single photon emitters for quantum information technology as well as low threshold laser devices. We demonstrate the fabrication of 60 nm thin zinc-blende AlN microdisks including cubic GaN quantum dots using dry chemical etching techniques. Scanning electron microscopy analysis reveals the morphology with smooth surfaces of the microdisks. Micro-photoluminescence measurements exhibit optically active quantum dots. Furthermore this is the first report of resonator modes in the emission spectrum of a cubic AlN microdisk.

  8. New silicon architectures by gold-assisted chemical etching.

    PubMed

    Mikhael, Bechelany; Elise, Berodier; Xavier, Maeder; Sebastian, Schmitt; Johann, Michler; Laetitia, Philippe

    2011-10-01

    Silicon nanowires (SiNWs) were produced by nanosphere lithography and metal assisted chemical etching. The combination of these methods allows the morphology and organization control of Si NWs on a large area. From the investigation of major parameters affecting the etching such as doping type, doping concentration of the substrate, we demonstrate the formation of new Si architectures consisting of organized Si NW arrays formed on a micro/mesoporous silicon layer with different thickness. These investigations will allow us to better understand the mechanism of Si etching to enable a wide range of applications such as molecular sensing, and for thermoelectric and photovoltaic devices. © 2011 American Chemical Society

  9. Selectively-etched nanochannel electrophoretic and electrochemical devices

    DOEpatents

    Surh, Michael P.; Wilson, William D.; Barbee, Jr., Troy W.; Lane, Stephen M.

    2004-11-16

    Nanochannel electrophoretic and electrochemical devices having selectively-etched nanolaminates located in the fluid transport channel. The normally flat surfaces of the nanolaminate having exposed conductive (metal) stripes are selectively-etched to form trenches and baffles. The modifications of the prior utilized flat exposed surfaces increase the amount of exposed metal to facilitate electrochemical redox reaction or control the exposure of the metal surfaces to analytes of large size. These etched areas variously increase the sensitivity of electrochemical detection devices to low concentrations of analyte, improve the plug flow characteristic of the channel, and allow additional discrimination of the colloidal particles during cyclic voltammetry.

  10. Selectively-etched nanochannel electrophoretic and electrochemical devices

    DOEpatents

    Surh, Michael P [Livermore, CA; Wilson, William D [Pleasanton, CA; Barbee, Jr., Troy W.; Lane, Stephen M [Oakland, CA

    2006-06-27

    Nanochannel electrophoretic and electrochemical devices having selectively-etched nanolaminates located in the fluid transport channel. The normally flat surfaces of the nanolaminate having exposed conductive (metal) stripes are selectively-etched to form trenches and baffles. The modifications of the prior utilized flat exposed surfaces increase the amount of exposed metal to facilitate electrochemical redox reaction or control the exposure of the metal surfaces to analytes of large size. These etched areas variously increase the sensitivity of electrochemical detection devices to low concentrations of analyte, improve the plug flow characteristic of the channel, and allow additional discrimination of the colloidal particles during cyclic voltammetry.

  11. DOE Office of Scientific and Technical Information (OSTI.GOV)

    Li, Chen; Metzler, Dominik; Oehrlein, Gottlieb S., E-mail: oehrlein@umd.edu

    Angstrom-level plasma etching precision is required for semiconductor manufacturing of sub-10 nm critical dimension features. Atomic layer etching (ALE), achieved by a series of self-limited cycles, can precisely control etching depths by limiting the amount of chemical reactant available at the surface. Recently, SiO{sub 2} ALE has been achieved by deposition of a thin (several Angstroms) reactive fluorocarbon (FC) layer on the material surface using controlled FC precursor flow and subsequent low energy Ar{sup +} ion bombardment in a cyclic fashion. Low energy ion bombardment is used to remove the FC layer along with a limited amount of SiO{sub 2} frommore » the surface. In the present article, the authors describe controlled etching of Si{sub 3}N{sub 4} and SiO{sub 2} layers of one to several Angstroms using this cyclic ALE approach. Si{sub 3}N{sub 4} etching and etching selectivity of SiO{sub 2} over Si{sub 3}N{sub 4} were studied and evaluated with regard to the dependence on maximum ion energy, etching step length (ESL), FC surface coverage, and precursor selection. Surface chemistries of Si{sub 3}N{sub 4} were investigated by x-ray photoelectron spectroscopy (XPS) after vacuum transfer at each stage of the ALE process. Since Si{sub 3}N{sub 4} has a lower physical sputtering energy threshold than SiO{sub 2}, Si{sub 3}N{sub 4} physical sputtering can take place after removal of chemical etchant at the end of each cycle for relatively high ion energies. Si{sub 3}N{sub 4} to SiO{sub 2} ALE etching selectivity was observed for these FC depleted conditions. By optimization of the ALE process parameters, e.g., low ion energies, short ESLs, and/or high FC film deposition per cycle, highly selective SiO{sub 2} to Si{sub 3}N{sub 4} etching can be achieved for FC accumulation conditions, where FC can be selectively accumulated on Si{sub 3}N{sub 4} surfaces. This highly selective etching is explained by a lower carbon consumption of Si{sub 3}N{sub 4} as compared to SiO{sub 2}. The comparison of C{sub 4}F{sub 8} and CHF{sub 3} only showed a difference in etching selectivity for FC depleted conditions. For FC accumulation conditions, precursor chemistry has a weak impact on etching selectivity. Surface chemistry analysis shows that surface fluorination and FC reduction take place during a single ALE cycle for FC depleted conditions. A fluorine rich carbon layer was observed on the Si{sub 3}N{sub 4} surface after ALE processes for which FC accumulation takes place. The angle resolved-XPS thickness calculations confirmed the results of the ellipsometry measurements in all cases.« less

  12. Spray-coating of superhydrophobic aluminum alloys with enhanced mechanical robustness.

    PubMed

    Zhang, Youfa; Ge, Dengteng; Yang, Shu

    2014-06-01

    A superhydrophobic aluminum alloy was prepared by one-step spray coating of an alcohol solution consisting of hydrophobic silica nanoparticles (15-40 nm) and methyl silicate precursor on etched aluminum alloy with pitted morphology. The as-sprayed metal surface showed a water contact angle of 155° and a roll-off angle of 4°. The coating was subjected to repeated mechanical tests, including high-pressure water jetting, sand particles impacting, and sandpaper shear abrasion. It remained superhydrophobic with a roll-off angle <10° up to three cycles of water jetting (25 kPa for 10 min) and sand particle impinging. After five cycles, the roll-off angle increased, but no more than 19° while the water contact angle remained greater than 150°. The superhydrophobic state was also maintained after three cycles of sandpaper abrasion. It was found that the micro-protrusion structures on the etched aluminum alloy played an important role to enhance the coating mechanical robustness, where the nanoparticles could grab on the rough surface, specifically in the groove structures, in comparison with the smooth glass substrates spray coated with the same materials. Further, we showed that the superhydrophobicity could be restored by spray a new cycle of the nanocomposite solution on the damaged surface. Copyright © 2014 Elsevier Inc. All rights reserved.

  13. Maskless and low-destructive nanofabrication on quartz by friction-induced selective etching

    PubMed Central

    2013-01-01

    A low-destructive friction-induced nanofabrication method is proposed to produce three-dimensional nanostructures on a quartz surface. Without any template, nanofabrication can be achieved by low-destructive scanning on a target area and post-etching in a KOH solution. Various nanostructures, such as slopes, hierarchical stages and chessboard-like patterns, can be fabricated on the quartz surface. Although the rise of etching temperature can improve fabrication efficiency, fabrication depth is dependent only upon contact pressure and scanning cycles. With the increase of contact pressure during scanning, selective etching thickness of the scanned area increases from 0 to 2.9 nm before the yield of the quartz surface and then tends to stabilise after the appearance of a wear. Refabrication on existing nanostructures can be realised to produce deeper structures on the quartz surface. Based on Arrhenius fitting of the etching rate and transmission electron microscopy characterization of the nanostructure, fabrication mechanism could be attributed to the selective etching of the friction-induced amorphous layer on the quartz surface. As a maskless and low-destructive technique, the proposed friction-induced method will open up new possibilities for further nanofabrication. PMID:23531381

  14. Reticulated shallow etch mesa isolation for controlling surface leakage in GaSb-based infrared detectors

    NASA Astrophysics Data System (ADS)

    Nolde, J. A.; Jackson, E. M.; Bennett, M. F.; Affouda, C. A.; Cleveland, E. R.; Canedy, C. L.; Vurgaftman, I.; Jernigan, G. G.; Meyer, J. R.; Aifer, E. H.

    2017-07-01

    Longwave infrared detectors using p-type absorbers composed of InAs-rich type-II superlattices (T2SLs) nearly always suffer from high surface currents due to carrier inversion on the etched sidewalls. Here, we demonstrate reticulated shallow etch mesa isolation (RSEMI): a structural method of reducing surface currents in longwave single-band and midwave/longwave dual-band detectors with p-type T2SL absorbers. By introducing a lateral shoulder to increase the separation between the n+ cathode and the inverted absorber surface, a substantial barrier to surface electron flow is formed. We demonstrate experimentally that the RSEMI process results in lower surface current, lower net dark current, much weaker dependence of the current on bias, and higher uniformity compared to mesas processed with a single deep etch. For the structure used, a shoulder width of 2 μm is sufficient to block surface currents.

  15. Influence of Hot-Etching Surface Treatment on Zirconia/Resin Shear Bond Strength

    PubMed Central

    Lv, Pin; Yang, Xin; Jiang, Ting

    2015-01-01

    This study was designed to evaluate the effect of hot-etching surface treatment on the shear bond strength between zirconia ceramics and two commercial resin cements. Ceramic cylinders (120 units; length: 2.5 mm; diameter: 4.7 mm) were randomly divided into 12 groups (n = 10) according to different surface treatments (blank control; airborne-particle-abrasion; hot-etching) and different resin cements (Panavia F2.0; Superbond C and B) and whether or not a thermal cycling fatigue test (5°–55° for 5000 cycles) was performed. Flat enamel surfaces, mounted in acrylic resin, were bonded to the zirconia discs (diameter: 4.7 mm). All specimens were subjected to shear bond strength testing using a universal testing machine with a crosshead speed of 1 mm/min. All data were statistically analyzed using one-way analysis of variance and multiple-comparison least significant difference tests (α = 0.05). Hot-etching treatment produced higher bond strengths than the other treatment with both resin cements. The shear bond strength of all groups significantly decreased after the thermal cycling test; except for the hot-etching group that was cemented with Panavia F2.0 (p < 0.05). Surface treatment of zirconia with hot-etching solution enhanced the surface roughness and bond strength between the zirconia and the resin cement. PMID:28793699

  16. Plasma processing of large curved surfaces for superconducting rf cavity modification

    DOE PAGES

    Upadhyay, J.; Im, Do; Popović, S.; ...

    2014-12-15

    In this study, plasma based surface modification of niobium is a promising alternative to wet etching of superconducting radio frequency (SRF) cavities. The development of the technology based on Cl 2/Ar plasma etching has to address several crucial parameters which influence the etching rate and surface roughness, and eventually, determine cavity performance. This includes dependence of the process on the frequency of the RF generator, gas pressure, power level, the driven (inner) electrode configuration, and the chlorine concentration in the gas mixture during plasma processing. To demonstrate surface layer removal in the asymmetric non-planar geometry, we are using a simplemore » cylindrical cavity with 8 ports symmetrically distributed over the cylinder. The ports are used for diagnosing the plasma parameters and as holders for the samples to be etched. The etching rate is highly correlated with the shape of the inner electrode, radio-frequency (RF) circuit elements, chlorine concentration in the Cl 2/Ar gas mixtures, residence time of reactive species and temperature of the cavity. Using cylindrical electrodes with variable radius, large-surface ring-shaped samples and d.c. bias implementation in the external circuit we have demonstrated substantial average etching rates and outlined the possibility to optimize plasma properties with respect to maximum surface processing effect.« less

  17. Process Development for Automated Solar Cell and Module Production. Task 4: Automated Array Assembly

    NASA Technical Reports Server (NTRS)

    1979-01-01

    A baseline sequence for the manufacture of solar cell modules was specified. Starting with silicon wafers, the process goes through damage etching, texture etching, junction formation, plasma edge etch, aluminum back surface field formation, and screen printed metallization to produce finished solar cells. The cells were then series connected on a ribbon and bonded into a finished glass tedlar module. A number of steps required additional developmental effort to verify technical and economic feasibility. These steps include texture etching, plasma edge etch, aluminum back surface field formation, array layup and interconnect, and module edge sealing and framing.

  18. Bonding performance of universal adhesives to er,cr:YSGG laser-irradiated enamel.

    PubMed

    Ayar, Muhammet Kerim; Erdemir, Fatih

    2017-04-01

    Universal adhesives have been recently introduced for use as self-etch or etch-and-rinse adhesives depending on the dental substrate and clinical condition. However, their bonding effectiveness to laser-irradiated enamel is still not well-known. Thus, the aim of this study was to compare the shear bond strength (SBS) of universal adhesives (Single Bond Universal; Nova Compo-B Plus) applied to Er,Cr:YSGG laser-irradiated enamel with SBS of the same adhesives applied in self-etch and acid-etching modes, respectively. Crown segments of sixty bovine incisors were embedded into standardized acrylic blocks. Flattened enamel surfaces were prepared. Specimens were divided into six groups according to universal adhesives and application modes randomly (n = 10), as follows: Single Bond Universal/acid-etching mode; Nova Compo-B Plus/acid-etching mode; Single Bond Universal/self-etching mode; Nova Compo-B Plus/self-etching mode; and Single Bond Universal/Er,Cr:YSGG Laser-etching mode; Nova Compo-B Plus/Er,Cr:YSGG Laser-etching mode. After surface treatments, universal adhesives were applied onto surfaces. SBS was determined after storage in water for 24 h using a universal testing machine with a crosshead speed of 0.5 mm min -1 . Failure modes were evaluated using a stereomicroscope. Data was analyzed using two-way of analyses of variances (ANOVA) (p = 0.05). Two-way ANOVA revealed that adhesive had no effect on SBS (p = 0.88), but application mode significantly influenced SBS (p = 0.00). Acid-etching significantly increased SBS, whereas there are no significant differences between self-etch mode and laser-etching for both adhesives. The bond strength of universal adhesives may depend on application mode. Acid etching may significantly increase bond strength, while laser etching may provide similar bond strength when compared to self-etch mode. © 2016 Wiley Periodicals, Inc.

  19. 76 FR 66609 - Airworthiness Directives; Bell Helicopter Textron Canada (Bell) Model 407 and 427 Helicopters

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-10-27

    ... surface. The AD also requires reidentifying the servo by metal-impression stamping or by vibro- etching... surface. The AD also requires reidentifying the servo by metal-impression stamping or by vibro-etching... metal-impression stamping or by vibro-etching ``67.01'' onto the modification plate. Before installing a...

  20. Shear bond strength of self-etch adhesives to enamel with additional phosphoric acid etching.

    PubMed

    Lührs, Anne-Katrin; Guhr, Silke; Schilke, Reinhard; Borchers, Lothar; Geurtsen, Werner; Günay, Hüsamettin

    2008-01-01

    This study evaluated the shear bond strength of self-etch adhesives to enamel and the effect of additional phosphoric acid etching. Seventy sound human molars were randomly divided into three test groups and one control group. The enamel surfaces of the control group (n=10) were treated with Syntac Classic (SC). Each test group was subdivided into two groups (each n=10). In half of each test group, ground enamel surfaces were coated with the self-etch adhesives AdheSe (ADH), Xeno III (XE) or Futurabond NR (FNR). In the remaining half of each test group, an additional phosphoric acid etching of the enamel surface was performed prior to applying the adhesives. The shear bond strength was measured with a universal testing machine at a crosshead speed of 1 mm/minute after storing the samples in distilled water at 37 degrees C for 24 hours. Fracture modes were determined by SEM examination. For statistical analysis, one-way ANOVA and the two-sided Dunnett Test were used (p>0.05). Additional phosphoric etching significantly increased the shear bond strength of all the examined self-etch adhesives (p<0.001). The highest shear bond strength was found for FNR after phosphoric acid etching. Without phosphoric acid etching, only FNR showed no significant differences compared to the control (SC). SEM evaluations showed mostly adhesive fractures. For all the self-etch adhesives, a slight increase in mixed fractures occurred after conditioning with phosphoric acid. An additional phosphoric acid etching of enamel should be considered when using self-etch adhesives. More clinical studies are needed to evaluate the long-term success of the examined adhesives.

  1. Control of dental-derived induced pluripotent stem cells through modified surfaces for dental application.

    PubMed

    Choi, Hyunmin; Park, Kyu-Hyung; Lee, Ah-Reum; Mun, Chin Hee; Shin, Yong Dae; Park, Yong-Beom; Park, Young-Bum

    2017-07-01

    The aim of this study is to investigate the behaviour of iPSc derived from dental stem cells in terms of initial adhesion, differentiation potential on differently surface-treated titanium disc. iPSc derived from human gingival fibroblasts (hGFs) were established using 4-reprogramming factors transduction with Sendai virus. The hGF-iPSc established in this study exhibited the morphology and growth properties similar to human embryonic stem (ES) cells and expressed pluripotency makers. Alkaline Phosphatase (AP) staining, Embryoid Body (EB) formation and in vitro differentiation and karyotyping further confirmed pluripotency of hGF-iPSc. Then, hGF-iPSc were cultured on machined- and Sandblasted and acid etched (SLA)-treated titanium discs with osteogenic induction medium and their morphological as well as quantitative changes according to different surface types were investigated using Alizrin Red S staining, Scanning electron microscopy (SEM), Flow cytometry and RT-PCR. Time-dependent and surface-dependent morphological changes as well as quantitative change in osteogenic differentiation of hGF-iPSc were identified and osteogenic gene expression of hGF-iPSc cultured on SLA-treated titanium disc found to be greater than machined titanium disc, suggesting the fate of hGF-iPSc may be determined by the characteristics of surface to which hGF-iPSc first adhere. iPSc derived from dental stem cell can be one of the most promising and practical cell sources for personalized regenerative dentistry and their morphological change as well as quantitative change in osteogenic differentiation according to different surface types may be further utilized for future clinical application incorporated with dental implant.

  2. Effect of Coating Thickness on the Properties of TiN Coatings Deposited on Tool Steels Using Cathodic Arc Pvd Technique

    NASA Astrophysics Data System (ADS)

    Mubarak, A.; Akhter, Parvez; Hamzah, Esah; Mohd Toff, Mohd Radzi Hj.; Qazi, Ishtiaq A.

    Titanium nitride (TiN) widely used as hard coating material, was coated on tool steels, namely on high-speed steel (HSS) and D2 tool steel by physical vapor deposition method. The study concentrated on cathodic arc physical vapor deposition (CAPVD), a technique used for the deposition of hard coatings for tooling applications, and which has many advantages. The main drawback of this technique, however, is the formation of macrodroplets (MDs) during deposition, resulting in films with rougher morphology. Various standard characterization techniques and equipment, such as electron microscopy, atomic force microscopy, hardness testing machine, scratch tester, and pin-on-disc machine, were used to analyze and quantify the following properties and parameters: surface morphology, thickness, hardness, adhesion, and coefficient of friction (COF) of the deposited coatings. Surface morphology revealed that the MDs produced during the etching stage, protruded through the TiN film, resulting in film with deteriorated surface features. Both coating thickness and indentation loads influenced the hardness of the deposited coatings. The coatings deposited on HSS exhibit better adhesion compared to those on D2 tool steel. Standard deviation indicates that the coating deposited with thickness around 6.7 μm showed the most stable trend of COF versus sliding distance.

  3. DOE Office of Scientific and Technical Information (OSTI.GOV)

    Metzler, Dominik; Li, Chen; Engelmann, Sebastian

    With the increasing interest in establishing directional etching methods capable of atomic scale resolution for fabricating highly scaled electronic devices, the need for development and characterization of atomic layer etching (ALE) processes, or generally etch processes with atomic layer precision, is growing. In this work, a flux-controlled cyclic plasma process is used for etching of SiO 2 and Si at the Angstrom-level. This is based on steady-state Ar plasma, with periodic, precise injection of a fluorocarbon (FC) precursor (C 4F 8 and CHF 3), and synchronized, plasma-based Ar+ ion bombardment [D. Metzler et al., J Vac Sci Technol A 32,more » 020603 (2014), and D. Metzler et al., J Vac Sci Technol A 34, 01B101 (2016)]. For low energy Ar+ ion bombardment conditions, physical sputter rates are minimized, whereas material can be etched when FC reactants are present at the surface. This cyclic approach offers a large parameter space for process optimization. Etch depth per cycle, removal rates, and self-limitation of removal, along with material dependence of these aspects, were examined as a function of FC surface coverage, ion energy, and etch step length using in situ real time ellipsometry. The deposited FC thickness per cycle is found to have a strong impact on etch depth per cycle of SiO 2 and Si, but is limited with regard to control over material etching selectivity. Ion energy over the 20 to 30 eV range strongly impacts material selectivity. The choice of precursor can have a significant impact on the surface chemistry and chemically enhanced etching. CHF 3 has a lower FC deposition yield for both SiO 2 and Si, and also exhibits a strong substrate dependence of FC deposition yield, in contrast to C4F 8. The thickness of deposited FC layers using CHF 3 is found to be greater for Si than for SiO 2. X-ray photoelectron spectroscopy was used to study surface chemistry. When thicker FC films of 11 Å are employed, strong changes of FC film chemistry during a cycle are seen whereas the chemical state of the substrate varies much less. On the other hand, for FC film deposition of 5 Å for each cycle, strong substrate surface chemical changes are seen during an etching cycle. The nature of this cyclic etching with periodic deposition of thin FC films differs significantly from conventional etching with steady-state FC layers since surface conditions change strongly throughout each cycle.« less

  4. Comparison of Self-Etch Primers with Conventional Acid Etching System on Orthodontic Brackets

    PubMed Central

    Zope, Amit; Zope-Khalekar, Yogita; Chitko, Shrikant S.; Kerudi, Veerendra V.; Patil, Harshal Ashok; Jaltare, Pratik; Dolas, Siddhesh G

    2016-01-01

    Introduction The self-etching primer system consists of etchant and primer dispersed in a single unit. The etching and priming are merged as a single step leading to fewer stages in bonding procedure and reduction in the number of steps that also reduces the chance of introduction of error, resulting in saving time for the clinician. It also results in smaller extent of enamel decalcification. Aim To compare the Shear Bond Strength (SBS) of orthodontic bracket bonded with Self-Etch Primers (SEP) and conventional acid etching system and to study the surface appearance of teeth after debonding; etching with conventional acid etch and self-etch priming, using stereomicroscope. Materials and Methods Five Groups (n=20) were created randomly from a total of 100 extracted premolars. In a control Group A, etching of enamel was done with 37% phosphoric acid and bonding of stainless steel brackets with Transbond XT (3M Unitek, Monrovia, California). Enamel conditioning in left over four Groups was done with self-etching primers and adhesives as follows: Group B-Transbond Plus (3M Unitek), Group C Xeno V+ (Dentsply), Group D-G-Bond (GC), Group E-One-Coat (Coltene). The Adhesive Remnant Index (ARI) score was also evaluated. Additionally, the surface roughness using profilometer were observed. Results Mean SBS of Group A was 18.26±7.5MPa, Group B was 10.93±4.02MPa, Group C was 6.88±2.91MPa while of Group D was 7.78±4.13MPa and Group E was 10.39±5.22MPa respectively. In conventional group ARI scores shows that over half of the adhesive was remaining on the surface of tooth (score 1 to 3). In self-etching primer groups ARI scores show that there was no or minor amount of adhesive remaining on the surface of tooth (score 4 and 5). SEP produces a lesser surface roughness on the enamel than conventional etching. However, statistical analysis shows significant correlation (p<0.001) of bond strength with surface roughness of enamel. Conclusion All groups might show clinically useful SBS values and Transbond XT can be successfully used for bracket bonding after enamel conditioning with any of the SEPs tested. The SEPs used in Groups C (Xeno V+) and D (G-Bond) have significantly lowered SBS. Although, the values might still be clinically acceptable. PMID:28208997

  5. Porous silicon formation during Au-catalyzed etching

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Algasinger, Michael; Bernt, Maximilian; Koynov, Svetoslav

    2014-04-28

    The formation of “black” nano-textured Si during the Au-catalyzed wet-chemical etch process was investigated with respect to photovoltaic applications. Cross-sectional scanning electron microscopy (SEM) images recorded at different stages of the etch process exhibit an evolution of a two-layer structure, consisting of cone-like Si hillocks covered with a nano-porous Si (np-Si) layer. Optical measurements confirm the presence of a np-Si phase which appears after the first ∼10 s of the etch process and continuously increases with the etch time. Furthermore, the etch process was investigated on Si substrates with different doping levels (∼0.01–100 Ω cm). SEM images show a transition frommore » the two-layer morphology to a structure consisting entirely of np-Si for higher doping levels (<0.1 Ω cm). The experimental results are discussed on the basis of the model of a local electrochemical etch process. A better understanding of the metal-catalyzed etch process facilitates the fabrication of “black” Si on various Si substrates, which is of significant interest for photovoltaic applications.« less

  6. Determination of Etch Rate Behavior of 4H-SiC Using Chlorine Trifluoride Gas

    NASA Astrophysics Data System (ADS)

    Miura, Yutaka; Habuka, Hitoshi; Katsumi, Yusuke; Oda, Satoko; Fukai, Yasushi; Fukae, Katsuya; Kato, Tomohisa; Okumura, Hajime; Arai, Kazuo

    2007-12-01

    The etch rate of single-crystalline 4H-SiC is studied using chlorine trifluoride gas at 673-973 K and atmospheric pressure in a cold wall horizontal reactor. The 4H-SiC etch rate can be higher than 10 μm/min at substrate temperatures higher than 723 K. The etch rate increases with the chlorine trifluoride gas flow rate. The etch rate is calculated by taking into account the transport phenomena in the reactor including the chemical reaction at the substrate surface. The flat etch rate at the higher substrate temperatures is caused mainly by the relationship between the transport rate and the surface chemical reaction rate of chlorine trifluoride gas.

  7. Influence of surface treatment of yttria-stabilized tetragonal zirconia polycrystal with hot isostatic pressing on cyclic fatigue strength.

    PubMed

    Iijima, Toshihiko; Homma, Shinya; Sekine, Hideshi; Sasaki, Hodaka; Yajima, Yasutomo; Yoshinari, Masao

    2013-01-01

    Hot isostatic pressing processed yttria-stabilized tetragonal zirconia polycrystal (HIP Y-TZP) has the potential for application to implants due to its high mechanical performance. The aim of this study was to investigate the influence of surface treatment of HIP Y-TZP on cyclic fatigue strength. HIP Y-TZP specimens were subjected to different surface treatments. Biaxial flexural strength was determined by both static and cyclic fatigue testing. In the cyclic fatigue test, the load was applied at a frequency of 10 Hz for 10(6) cycles in distilled water at 37°C. The surface morphology, roughness, and crystal phase of the surfaces were also evaluated. The cyclic fatigue strength (888 MPa) of HIP Y-TZP with sandblasting and acid-etching was more than twice that of Y-TZP as specified in ISO 13356 for surgical implants (320 MPa), indicating the clinical potential of this material.

  8. Enhanced performance of solar cells with optimized surface recombination and efficient photon capturing via anisotropic-etching of black silicon

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Chen, H. Y.; Peng, Y., E-mail: gdyuan@semi.ac.cn, E-mail: py@usst.edu.cn; Hong, M.

    2014-05-12

    We report an enhanced conversion efficiency of femtosecond-laser treated silicon solar cells by surface modification of anisotropic-etching. The etching improves minority carrier lifetime inside modified black silicon area substantially; moreover, after the etching, an inverted pyramids/upright pyramids mixed texture surface is obtained, which shows better photon capturing capability than that of conventional pyramid texture. Combing of these two merits, the reformed solar cells show higher conversion efficiency than that of conventional pyramid textured cells. This work presents a way for fabricating high performance silicon solar cells, which can be easily applied to mass-production.

  9. Surface modification with alumina blasting and H2SO4-HCl etching for bonding two resin-composite veneers to titanium.

    PubMed

    Taira, Yohsuke; Egoshi, Takafumi; Kamada, Kohji; Sawase, Takashi

    2014-02-01

    The purpose of this study was to investigate the effect of an experimental surface treatment with alumina blasting and acid etching on the bond strengths between each of two resin composites and commercially pure titanium. The titanium surface was blasted with alumina and then etched with 45wt% H2SO4 and 15wt% HCl (H2SO4-HCl). A light- and heat-curing resin composite (Estenia) and a light-curing resin composite (Ceramage) were used with adjunctive metal primers. Veneered specimens were subjected to thermal cycling between 4 and 60°C for 50,000 cycles, and the shear bond strengths were determined. The highest bond strengths were obtained for Blasting/H2SO4-HCl/Estenia (30.2 ± 4.5 MPa) and Blasting/Etching/Ceramage (26.0 ± 4.5 MPa), the values of which were not statistically different, followed by Blasting/No etching/Estenia (20.4 ± 2.4 MPa) and Blasting/No etching/Ceramage (0.8 ± 0.3 MPa). Scanning electron microscopy observations revealed that alumina blasting and H2SO4-HCl etching creates a number of micro- and nanoscale cavities on the titanium surface, which contribute to adhesive bonding. © 2013 Eur J Oral Sci.

  10. Micromirror arrays using KOH:H[sub 2]O micromachining of silicon for lens templates, geodesic lenses, and other applications

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Kendall, D.L.; Eaton, W.P.; Manginell, R.

    Micromirrors having diameters from a few micrometers to several millimeters have been produced on (100) silicon by wet-chemical etching in KOH:H[sub 2]O. The f/[number sign]'s range from about 2.5 to at least 10. The microroughness of an etched mirror with diameter 550 [mu]m and 9.6-[mu]m sagitta is less than 5 nm and its surface figure is within 0.5 [mu]m of a perfect sphere. Data over a wide range of diameters are presented and a semiempirical model is developed to explain the behavior. The concordance of the normalized etched profiles for all diameter mirrors demonstrates that the etching is dominated bymore » surface reaction rather than diffusion limitation. Design and fabrication schemes are presented for making a wide range of mirror diameters and focal lengths, for both single micromirrors and arrays. The etched depressions can be used as templates for microlenses and as substrates for geodesic waveguide lenses and arrays. Chem-mechanical polishing on the etched structures reduces the edge curvature and produces oblate spheroidal surfaces, both of which should improve geodesic lens behavior. The etched structures can also be used as variable crystal orientation substrates for epitaxial nucleation and various surface analysis studies.« less

  11. Micromirror arrays using KOH:H2O micromachining of silicon for lens templates, geodesic lenses, and other applications

    NASA Astrophysics Data System (ADS)

    Kendall, Don L.; Eaton, William P.; Manginell, Ronald P.; Digges, Thomas G.

    1994-11-01

    Micromirrors having diameters from a few micrometers to several millimeters have been produced on (100) silicon by wet-chemical etching in KOH:H2O. The f/#'s range from about 2.5 to at least 10. The microroughness of an etched mirror with diameter 550 micrometers and 9.6-micrometers sagitta is less than 5 nm and its surface figure is within 0.5 micrometers of a perfect sphere. Data over a wide range of diameters are presented and a semiempirical model is developed to explain the behavior. The concordance of the normalized etched profiles for all diameter mirrors demonstrates that the etching is dominated by surface reaction rather than diffusion limitation. Design and fabrication schemes are presented for making a wide range of mirror diameters and focal lengths, for both single micromirrors and arrays. The etched depressions can be used as templates for microlenses and as substrates for geodesic waveguide lenses and arrays. Chem-mechanical polishing on the etched structures reduces the edge curvature and produces oblate spheroidal surfaces, both of which should improve geodesic lens behavior. The etched structures can also be used as variable crystal orientation substrates for epitaxial nucleation and various surface analysis studies.

  12. Effect of different atmospheres on the electrical contact performance of electronic components under fretting wear

    NASA Astrophysics Data System (ADS)

    Liu, Xin-Long; Cai, Zhen-Bing; Cui, Ye; Liu, Shan-Bang; Xu, Xiao-Jun; Zhu, Min-Hao

    2018-04-01

    The effects of oxide etch on the surface morphology of metals for industrial application is a common cause of electrical contacts failure, and it has becomes a more severe problem with the miniaturization of modern electronic devices. This study investigated the effects of electrical contact resistance on the contactor under three different atmospheres (oxygen, air, and nitrogen) based on 99.9% copper/pogo pins contacts through fretting experiments. The results showed the minimum and stable electrical contact resistance value when shrouded in the nitrogen environment and with high friction coefficient. The rich oxygen environment promotes the formation of cuprous oxide, thereby the electrical contact resistance increases. Scanning electron microscope microscopy and electron probe microanalysis were used to analyze the morphology and distribution of elements of the wear area, respectively. The surface product between contacts was investigated by x-ray photoelectron spectroscopy analysis to explain the different electrical contact properties of the three tested samples during fretting.

  13. Highly selective SiO2 etching over Si3N4 using a cyclic process with BCl3 and fluorocarbon gas chemistries

    NASA Astrophysics Data System (ADS)

    Matsui, Miyako; Kuwahara, Kenichi

    2018-06-01

    A cyclic process for highly selective SiO2 etching with atomic-scale precision over Si3N4 was developed by using BCl3 and fluorocarbon gas chemistries. This process consists of two alternately performed steps: a deposition step using BCl3 mixed-gas plasma and an etching step using CF4/Ar mixed-gas plasma. The mechanism of the cyclic process was investigated by analyzing the surface chemistry at each step. BCl x layers formed on both SiO2 and Si3N4 surfaces in the deposition step. Early in the etching step, the deposited BCl x layers reacted with CF x radicals by forming CCl x and BF x . Then, fluorocarbon films were deposited on both surfaces in the etching step. We found that the BCl x layers formed in the deposition step enhanced the formation of the fluorocarbon films in the CF4 plasma etching step. In addition, because F radicals that radiated from the CF4 plasma reacted with B atoms while passing through the BCl x layers, the BCl x layers protected the Si3N4 surface from F-radical etching. The deposited layers, which contained the BCl x , CCl x , and CF x components, became thinner on SiO2 than on Si3N4, which promoted the ion-assisted etching of SiO2. This is because the BCl x component had a high reactivity with SiO2, and the CF x component was consumed by the etching reaction with SiO2.

  14. Effect of surface acid etching on the biaxial flexural strength of two hot-pressed glass ceramics.

    PubMed

    Hooshmand, Tabassom; Parvizi, Shaghayegh; Keshvad, Alireza

    2008-07-01

    The purpose of this study was to assess the effect of surface acid etching on the biaxial flexural strength of two hot-pressed glass ceramics reinforced by leucite or lithium disilicate crystals. Forty glass ceramic disks (14-mm diameter, 2-mm thick) consisting of 20 leucite-based ceramic disks (IPS Empress) and 20 lithia disilicate-based ceramic (IPS Empress 2) were produced by hot-pressing technique. All specimens were polished and then cleaned ultrasonically in distilled water. Ten specimens of each ceramic group were then etched with 9% hydrofluoric (HF) acid gel for 2 minutes and cleaned ultrasonically again. The biaxial flexural strength was measured by the piston-on-three-ball test in a universal testing machine. Data based on ten specimens in each group were analyzed by two-way ANOVA (alpha= 0.05). Microstructure of ceramic surfaces before and after acid etching was also examined by a scanning electron microscope. The mean biaxial flexural strength values for each group tested were (in MPa): nonetched IPS Empress = 118.6 +/- 25.5; etched IPS Empress = 102.9 +/- 15.4; nonetched IPS Empress 2 = 283.0 +/- 48.5; and etched IPS Empress 2 = 250.6 +/- 34.6. The results showed that the etching process reduced the biaxial flexural strengths significantly for both ceramic types (p= 0.025). No significant interaction between the ceramic type and etching process was found (p= 0.407). From the results, it was concluded that surface HF acid etching could have a weakening effect on hot-pressed leucite or lithia disilicate-based glass ceramic systems.

  15. Characterizing Fluorocarbon Assisted Atomic Layer Etching of Si Using Cyclic Ar/C 4F 8 and Ar/CHF 3 Plasma

    DOE PAGES

    Metzler, Dominik; Li, Chen; Engelmann, Sebastian; ...

    2016-09-08

    With the increasing interest in establishing directional etching methods capable of atomic scale resolution for fabricating highly scaled electronic devices, the need for development and characterization of atomic layer etching (ALE) processes, or generally etch processes with atomic layer precision, is growing. In this work, a flux-controlled cyclic plasma process is used for etching of SiO 2 and Si at the Angstrom-level. This is based on steady-state Ar plasma, with periodic, precise injection of a fluorocarbon (FC) precursor (C 4F 8 and CHF 3), and synchronized, plasma-based Ar+ ion bombardment [D. Metzler et al., J Vac Sci Technol A 32,more » 020603 (2014), and D. Metzler et al., J Vac Sci Technol A 34, 01B101 (2016)]. For low energy Ar+ ion bombardment conditions, physical sputter rates are minimized, whereas material can be etched when FC reactants are present at the surface. This cyclic approach offers a large parameter space for process optimization. Etch depth per cycle, removal rates, and self-limitation of removal, along with material dependence of these aspects, were examined as a function of FC surface coverage, ion energy, and etch step length using in situ real time ellipsometry. The deposited FC thickness per cycle is found to have a strong impact on etch depth per cycle of SiO 2 and Si, but is limited with regard to control over material etching selectivity. Ion energy over the 20 to 30 eV range strongly impacts material selectivity. The choice of precursor can have a significant impact on the surface chemistry and chemically enhanced etching. CHF 3 has a lower FC deposition yield for both SiO 2 and Si, and also exhibits a strong substrate dependence of FC deposition yield, in contrast to C4F 8. The thickness of deposited FC layers using CHF 3 is found to be greater for Si than for SiO 2. X-ray photoelectron spectroscopy was used to study surface chemistry. When thicker FC films of 11 Å are employed, strong changes of FC film chemistry during a cycle are seen whereas the chemical state of the substrate varies much less. On the other hand, for FC film deposition of 5 Å for each cycle, strong substrate surface chemical changes are seen during an etching cycle. The nature of this cyclic etching with periodic deposition of thin FC films differs significantly from conventional etching with steady-state FC layers since surface conditions change strongly throughout each cycle.« less

  16. Effect of Mucoprotein on the Bond Strength of Resin Composite to Human Dentin

    PubMed Central

    Pinzon, Lilliam M; Powers, John M; O'Keefe, Kathy; Dusevish, Vladimir; Spencer, Paulette; Marshall, Grayson W

    2010-01-01

    The purpose of this study was to test the bond strength and analyze the morphology of the dentin-adhesive interface of two etch and rinse and two self-etch adhesive systems with two kinds of artificial saliva (with and without 450 mg/L mucin) contamination under different conditions of decontaminating the interface. Bonded specimens were sectioned perpendicularly to the bonded surface in 1-mm thick slabs. These 1-mm thick slabs were remounted in acrylic blocks and sectioned in sticks perpendicular to the bonding interfaces with a 1-mm2 area. Nine specimens from each condition were tested after 24 hours on a testing machine (Instron) at a speed of 0.5 mm/min for a total of 360 specimens. Means and standard deviations of bond strength (MPa) were calculated. ANOVA showed significant differences as well as Fisher's PLSD intervals (p<0.05). Different groups results ranges: Control group 34-60 MPa, saliva without mucin 0-52 MPa, and saliva with mucin 0-57 MPa. Failure sites were mixed, adhesive failure was common for the low bond strength results. P&BNT with ideal conditions and following the manufacturer's instructions (control) had the highest bond strengths and the dentin-adhesive interface exhibited an ideal morphology of a etch and rinse system. SEM gave complementary visual evidence of the effect in the dentin/adhesive interface structure with some contaminated conditions compared to their respective control groups. This in-vitro artificial saliva model with and without mucin showed that an organic component of saliva could increase or decrease the bond strength depending on the specific bonding agent and decontamination procedure. PMID:14505182

  17. Non-chapped, vertically well aligned titanium dioxide nanotubes fabricated by electrochemical etching

    NASA Astrophysics Data System (ADS)

    Loan Nguyen, Thu; Dieu Thuy Ung, Thi; Liem Nguyen, Quang

    2014-06-01

    This paper reports on the fabrication of non-chapped, vertically well aligned titanium dioxide nanotubes (TONTs) by using electrochemical etching method and further heat treatment. Very highly ordered metallic titanium nanotubes (TNTs) were formed by directly anodizing titanium foil at room temperature in an electrolyte composed of ammonium fluoride (NH4F), ethylene glycol (EG), and water. The morphology of as-formed TNTs is greatly dependent on the applied voltage, NH4F content and etching time. Particularly, we have found two interesting points related to the formation of TNTs: (i) the smooth surface without chaps of the largely etched area was dependent on the crystalline orientation of the titanium foil; and (ii) by increasing the anodizing potential from 15 V to 20 V, the internal diameter of TNT was increased from about 50 nm to 60 nm and the tube density decreased from 403 tubes μm-2 down to 339 tubes μm-2, respectively. For the anodizing duration from 1 h to 5 h, the internal diameter of each TNT was increased from ˜30 nm to 60 nm and the tube density decreased from 496 tubes μm-2 down to 403 tubes μm-2. After annealing at 400 °C in open air for 1 h, the TNTs were transformed into TONTs in anatase structure; further annealing at 600 °C showed the structural transformation from anatase to rutile as determined by Raman scattering spectroscopy.

  18. Modeling Cl2/O2/Ar inductively coupled plasmas used for silicon etching: effects of SiO2 chamber wall coating

    NASA Astrophysics Data System (ADS)

    Tinck, S.; Boullart, W.; Bogaerts, A.

    2011-08-01

    In this paper, simulations are performed to gain a better insight into the properties of a Cl2/Ar plasma, with and without O2, during plasma etching of Si. Both plasma and surface properties are calculated in a self-consistent manner. Special attention is paid to the behavior of etch products coming from the wafer or the walls, and how the chamber walls can affect the plasma and the resulting etch process. Two modeling cases are considered. In the first case, the reactor walls are defined as clean (Al2O3), whereas in the second case a SiO2 coating is introduced on the reactor walls before the etching process, so that oxygen will be sputtered from the walls and introduced into the plasma. For this reason, a detailed reaction set is presented for a Cl2/O2/Ar plasma containing etched species, as well as an extensive reaction set for surface processes, including physical and chemical sputtering, chemical etching and deposition processes. Density and flux profiles of various species are presented for a better understanding of the bulk plasma during the etching process. Detailed information is also given on the composition of the surfaces at various locations of the reactor, on the etch products in the plasma and on the surface loss probabilities of the plasma species at the walls, with different compositions. It is found that in the clean chamber, walls are mostly chlorinated (Al2Cl3), with a thin layer of etch products residing on the wall. In the coated chamber, an oxy-chloride layer is grown on the walls for a few nanometers during the etching process. The Cl atom wall loss probability is found to decrease significantly in the coated chamber, hence increasing the etch rate. SiCl2, SiCl4 and SiCl3 are found to be the main etch products in the plasma, with the fraction of SiCl2 being always slightly higher. The simulation results compare well with experimental data available from the literature.

  19. Anisotropic Etching of Hexagonal Boron Nitride and Graphene: Question of Edge Terminations.

    PubMed

    Stehle, Yijing Y; Sang, Xiahan; Unocic, Raymond R; Voylov, Dmitry; Jackson, Roderick K; Smirnov, Sergei; Vlassiouk, Ivan

    2017-12-13

    Chemical vapor deposition (CVD) has been established as the most effective way to grow large area two-dimensional materials. Direct study of the etching process can reveal subtleties of this competing with the growth reaction and thus provide the necessary details of the overall growth mechanism. Here we investigate hydrogen-induced etching of hBN and graphene and compare the results with the classical kinetic Wulff construction model. Formation of the anisotropically etched holes in the center of hBN and graphene single crystals was observed along with the changes in the crystals' circumference. We show that the edges of triangular holes in hBN crystals formed at regular etching conditions are parallel to B-terminated zigzags, opposite to the N-terminated zigzag edges of hBN triangular crystals. The morphology of the etched hBN holes is affected by a disbalance of the B/N ratio upon etching and can be shifted toward the anticipated from the Wulff model N-terminated zigzag by etching in a nitrogen buffer gas instead of a typical argon. For graphene, etched hexagonal holes are terminated by zigzag, while the crystal circumference is gradually changing from a pure zigzag to a slanted angle resulting in dodecagons.

  20. Effect of oxygen plasma etching on pore size-controlled 3D polycaprolactone scaffolds for enhancing the early new bone formation in rabbit calvaria.

    PubMed

    Kook, Min-Suk; Roh, Hee-Sang; Kim, Byung-Hoon

    2018-05-02

    This study was to investigate the effects of O 2 plasma-etching of the 3D polycaprolactone (PCL) scaffold surface on preosteoblast cell proliferation and differentiation, and early new bone formation. The PCL scaffolds were fabricated by 3D printing technique. After O 2 plasma treatment, surface characterizations were examined by scanning electron microscopy, atomic force microscopy, and contact angle. MTT assay was used to determine cell proliferation. To investigate the early new bone formation, rabbits were sacrificed at 2 weeks for histological analyses. As the O 2 plasma etching time is increased, roughness and hydrophilicity of the PCL scaffold surface increased. The cell proliferation and differentiation on plasma-etched samples was significantly increased than on untreated samples. At 2 weeks, early new bone formation in O 2 plasma-etched PCL scaffolds was the higher than that of untreated scaffolds. The O 2 plasma-etched PCL scaffolds showed increased preosteoblast differentiation as well as increased new bone formation.

  1. Self-etching ceramic primer versus hydrofluoric acid etching: Etching efficacy and bonding performance.

    PubMed

    El-Damanhoury, Hatem M; Gaintantzopoulou, Maria D

    2018-01-01

    This study assessed the effect of pretreatment of hybrid and glass ceramics using a self-etching primer on the shear bond strength (SBS) and surface topography, in comparison to pretreatment with hydrofluoric acid and silane. 40 rectangular discs from each ceramic material (IPS e.max CAD;EM, Vita Mark II;VM, Vita Enamic;VE), were equally divided (n=10) and assigned to one of four surface pretreatment methods; etching with 4.8% hydrofluoric acid followed by Monobond plus (HFMP), Monobond etch & prime (Ivoclar Vivadent) (MEP), No treatment (NT) as negative control and Monobond plus (Ivoclar Vivadent) with no etching (MP) as positive control. SBS of resin cement (Multilink-N, Ivoclar Vivadent) to ceramic surfaces was tested following a standard protocol. Surface roughness was evaluated using an Atomic force microscope (AFM). Surface topography and elemental analysis were analyzed using SEM/EDX. Data were analyzed with two-way analysis of variance (ANOVA) and post-hoc Bonferroni test at a significance level of α=0.05. Pretreatment with HFMP resulted in higher SBS and increased surface roughness in comparison to MEP and MP. Regardless the method of surface pretreatment, the mean SBS values of EM ceramic was significantly higher (p<0.05) than those recorded for VM and VE, except when VE was treated with MEP, where the difference was statistically insignificant. Traces of fluoride ion were detected when MEP was used with VE and VM. Under limited conditions, using MEP resulted in comparable SBS results to HFMP; meanwhile HFMP remains the gold standard for pretreatment of glass ceramics for resin-luting cementation. Copyright © 2017 Japan Prosthodontic Society. Published by Elsevier Ltd. All rights reserved.

  2. Electronegativity-dependent tin etching from thin films

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Pachecka, M., E-mail: m.pachecka@utwente.nl; Sturm, J. M.; Kruijs, R. W. E. van de

    2016-07-15

    The influence of a thin film substrate material on the etching of a thin layer of deposited tin (Sn) by hydrogen radicals was studied. The amount of remaining Sn was quantified for materials that cover a range of electronegativities. We show that, for metals, etching depends on the relative electronegativity of the surface material and Sn. Tin is chemically etched from surfaces with an electronegativity smaller than Sn, while incomplete Sn etching is observed for materials with an electronegativity larger than Sn. Furthermore, the amount of remaining Sn increases as the electronegativity of the surface material increases. We speculate, that,more » due to Fermi level differences in the material’s electronic structure, the energy of the two conduction bands shift such that the availability of electrons for binding with hydrogen is significantly reduced.« less

  3. Plasmaless cleaning process of silicon surface using chlorine trifluoride

    NASA Astrophysics Data System (ADS)

    Saito, Yoji; Yamaoka, Osamu; Yoshida, Akira

    1990-03-01

    Plasmaless etching using ClF3 gas around room temperature has been investigated for the silicon substrates with the various thicknesses of native oxide. The native oxide can be removed with ClF3 gas. A specular surface is obtained by ultraviolet light irradiation which remarkably accelerates the removal of the native oxide without changing the etch rate of silicon. The etched surface is analyzed with Auger electron measurement, indicating the existence of Cl atoms on it.

  4. Low damage dry etch for III-nitride light emitters

    NASA Astrophysics Data System (ADS)

    Nedy, Joseph G.; Young, Nathan G.; Kelchner, Kathryn M.; Hu, Yanling; Farrell, Robert M.; Nakamura, Shuji; DenBaars, Steven P.; Weisbuch, Claude; Speck, James S.

    2015-08-01

    We have developed a dry etch process for the fabrication of lithographically defined features close to light emitting layers in the III-nitride material system. The dry etch was tested for its effect on the internal quantum efficiency of c-plane InGaN quantum wells using the photoluminescence of a test structure with two active regions. No change was observed in the internal quantum efficiency of the test active region when the etched surface was greater than 71 nm away. To demonstrate the application of the developed dry etch process, surface-etched air gaps were fabricated 275 nm away from the active region of an m-plane InGaN/GaN laser diode and served as the waveguide upper cladding. Electrically injected lasing was observed without the need for regrowth or recovery anneals. This dry etch opens up a new design tool that can be utilized in the next generation of GaN light emitters.

  5. Influence of low concentration acid treatment on lithium disilicate core/veneer ceramic bond strength

    PubMed Central

    Garcia, Rudan P.; Conti, Paulo CR.; Pereira, Jefferson R.; Valle, Accácio Ld.

    2013-01-01

    Objective: This study evaluated the influence of low concentration acid treatment on the shear bond strength between lithium disilicate (LD) infrastructure and veneering porcelain. The surface morphology characteristic after this acid treatment was also examined. Study Design: LD reinforced ceramic cylinders (n=10) (IPS e.max Press, Ivoclar-Vivadent, Schaan, Liechtenstein) were treated (LD-treated) with a low concentration acid solution (Invex Liquid – Ivoclar-Vivadent, Schaan, Liechtenstein) or not treated with the acid solution (LD-untreated). They were veneered with a glass ceramic (IPS e.max Ceram, Ivoclar-Vivadent, Schaan, Liechtenstein). A metal ceramic group (CoCr) was tested as control. Shear bond strength (SBS) was conducted using a universal testing machine at 0.5 mm/min. Surface morphology characteristics after acid treatment were analyzed using scanning electron microscopy. Results: The acid treatment at low concentrations did not influence the SBS of the LD/veneering porcelain interface. The CoCr group showed the significant higher SBS value (35.59 ± 5.97 MPa), followed by LD-untreated group (27.76 ± 3.59 MPa) and LD-treated (27.02 ± 4.79 MPa). The fracture modes were predominantly adhesive for CoCr group and cohesive within the infrastructure for DL groups. Scanning Electron Microscopy (SEM) analysis showed no morphological differences between treated and untreated LD surfaces. Conclusions: Low concentration acid treatment did not improved SBS of veneering ceramic to LD and did not cause morphological changes on the LD surface. Key words:Lithium disilicate, glass ceramics, acid etching, shear bond strength, scanning electron microscopy. PMID:24455073

  6. Effect of surface treatments on the flexural properties and adhesion of glass fiber-reinforced composite post to self-adhesive luting agent and radicular dentin.

    PubMed

    Elnaghy, Amr M; Elsaka, Shaymaa E

    2016-01-01

    This study evaluated the effect of different surface treatments on the flexural properties and adhesion of glass fiber post to self-adhesive luting agent and radicular dentin. Seventy-five single-rooted human teeth were prepared to receive a glass fiber post (Reblida). The posts were divided into five groups according to the surface treatment: Gr C (control; no treatment), Gr S (silanization for 60 s), Gr AP (airborne-particle abrasion), Gr HF (etching with 9 % hydrofluoric acid for 1 min), and Gr M10 (etching with CH2Cl2 for 10 min). Dual-cure self-adhesive luting agent (Rely X Unicem) was applied to each group for testing the adhesion using micropush-out test. Failure types were examined with stereomicroscope and surface morphology of the posts was characterized using a scanning electron microscopy (SEM). Flexural properties of posts were assessed using a three-point bending test. Data were analyzed using ANOVA and Tukey's HSD test. Statistical significance was set at the 0.05 probability level. Groups treated with M10 showed significantly higher bond strength than those obtained with other surface treatments (P < 0.05). In general, improvements in bond strength (MPa) were found in the following order: M10 > C > S > AP > HF. Most failure modes were adhesive type of failures between dentin and luting agent (48.2%). SEM analysis revealed that the fiber post surfaces were modified after surface treatments. The surface treatments did not compromise the flexural properties of fiber posts. Application of M10 to the fiber post surfaces enhanced the adhesion to self-adhesive luting agent and radicular dentin.

  7. Polyimide-Based Capacitive Humidity Sensor

    PubMed Central

    Steinmaßl, Matthias; Endres, Hanns-Erik; Drost, Andreas; Eisele, Ignaz; Kutter, Christoph; Müller-Buschbaum, Peter

    2018-01-01

    The development of humidity sensors with simple transduction principles attracts considerable interest by both scientific researchers and industrial companies. Capacitive humidity sensors, based on polyimide sensing material with different thickness and surface morphologies, are prepared. The surface morphology of the sensing layer is varied from flat to rough and then to nanostructure called nanograss by using an oxygen plasma etch process. The relative humidity (RH) sensor selectively responds to the presence of water vapor by a capacitance change. The interaction between polyimide and water molecules is studied by FTIR spectroscopy. The complete characterization of the prepared capacitive humidity sensor performance is realized using a gas mixing setup and an evaluation kit. A linear correlation is found between the measured capacitance and the RH level in the range of 5 to 85%. The morphology of the humidity sensing layer is revealed as an important parameter influencing the sensor performance. It is proved that a nanograss-like structure is the most effective for detecting RH, due to its rapid response and recovery times, which are comparable to or even better than the ones of commercial polymer-based sensors. This work demonstrates the readiness of the developed RH sensor technology for industrialization. PMID:29751632

  8. Surface modification of traditional and bioresorbable metallic implant materials for improved biocompatibility

    NASA Astrophysics Data System (ADS)

    Walker, Emily K.

    Due to their strength, elasticity, and durability, a variety of metal alloys are commonly used in medical implants. Traditionally, corrosion-resistant metals have been preferred. These permanent materials can cause negative systemic and local tissue effects in the long-term. Permanent stenting can lead to late-stent thrombosis and in-stent restenosis. Metallic pins and screws for fracture fixation can corrode and fail, cause loss of bone mass, and contribute to inflammation and pain at the implant site, requiring reintervention. Corrodible metallic implants have the potential to prevent many of these complications by providing transient support to the affected tissue, dissolving at a rate congruent with the healing of the tissue. Alloys of iron and manganese (FeMn) exhibit similar fatigue strength, toughness, and elasticity compared with 316L stainless steel, making them very attractive candidates for bioresorbable stents and temporary fracture fixation devices. Much attention in recent years has been given to creating alloys with ideal mechanical properties for various applications. Little work has been done on determining the blood compatibility of these materials or on examining how their surfaces can be improved to improve cell adhesion, however. We examined thethrombogenic response of blood exposed to various resorbable ferrous stent materials through contact with porcine blood. The resorbable materials induced comparable or lower levels of several coagulation factors compared with 316L stainless steel. Little platelet adhesion was observed on any of the tested materials. Endothelialization is an important process after the implantation of a vascular stent, as it prevents damage to the vessel wall that can accelerate neointimal hyperplasia. Micromotion can lead to the formation of fibrous tissue surrounding an orthopedic implant, loosening, and ultimately failure of the implant. Nanoscale features were created on the surfaces of noble metal coatings, silicon, and bioabsorbable materials through ion beam irradiation in order to improve endothelialzation and bone cell adhesion. Gold, palladium, silicon, and iron manganese surfaces were patterned through ion beam irradiation using argon ions. The surface morphology of the samples was examined using atomic force microscopy (AFM) and scanning electron microscopy (SEM), while surface chemistry was examined through x-ray photoelectron spectroscopy (XPS) and contact angle goniometry measurements. It was not possible to create nanoscale surface features on the surfaces of the gold and palladium films. At near normal incidence, irradiation produced ripples on the surfaces of Si(100), while oblique incidence irradiation produced nanoislands in the presence of impurities on the surface. Iron manganese irradiation resulted in the formation of blade-shaped structures for ion energies between 500eV and 1000eV, and significant iron enrichment at the surface. Chemical treatment can also be used to create surface features that will enhance cell adhesion. Ti6Al4V is one of the most commonly used alloys for permanent orthopedic devices. The creation of a porous surface in order to improve osteoblast adhesion was achieved through chemical etching using acid-peroxide solutions. While phosphoric acid etched the grain boundaries, sulfuric and nitric acid preferentially etched grains of particular orientations, creating a spongy, porous morphology that has the potential to aid in osseointegration.

  9. Containerless processing of single crystals in low-G environment

    NASA Technical Reports Server (NTRS)

    Walter, H. U.

    1974-01-01

    Experiments on containerless crystal growth from the melt were conducted during Skylab missions SL3 and SL4 (Skylab Experiment M-560). Six samples of InSb were processed, one of them heavily doped with selenium. The concept of the experiment is discussed and related to general crystal growth methods and their merits as techniques for containerless processing in space. The morphology of the crystals obtained is explained in terms of volume changes associated with solidification and wetting conditions during solidification. All samples exhibit extremely well developed growth facets. Analysis by X-ray topographical methods and chemical etching shows that the crystals are of high structural perfection. Average dislocation density as revealed by etching is of the order of 100 per sq cm; no dislocation clusters could be observed in the space-grown samples. A sequence of striations that is observed in the first half of the selenium-doped sample is explained as being caused by periodic surface breakdown.

  10. Fabrication of high reflectivity nanoporous distributed Bragg reflectors by controlled electrochemical etching of GaN

    NASA Astrophysics Data System (ADS)

    Lee, Seung-Min; Kang, Jin-Ho; Lee, June Key; Ryu, Sang-Wan

    2016-09-01

    The nanoporous medium is a valuable feature of optical devices because of its variable optical refractive index with porosity. One important application is in a GaN-based vertical cavity surface emitting laser having a distributed Bragg reflector (DBR) composed of alternating nanoporous and bulk GaNs. However, optimization of the fabrication process for high reflectivity DBRs having wellcontrolled high reflection bands has not been studied yet. We used electrochemical etching to study the fabrication process of a nanoporous GaN DBR and analyzed the relationship between the morphology and optical reflectivity. Several electrolytes were examined for the formation of the optimized nanoporous structure. A highly reflective DBRs having reflectivity of ~100% were obtained over a wide wavelength range of 450-750 nm. Porosification of semiconductors into nanoporous layers could provide a high reflectivity DBR due to controlled index-contrast, which would be advantages for the construction of a high-Q optical cavity.

  11. DOE Office of Scientific and Technical Information (OSTI.GOV)

    Kafka, Kyle R. P.; Hoffman, Brittany N.; Papernov, Semyon

    The laser-induced damage threshold of fused-silica samples processed via magnetorheological finishing is investigated for polishing compounds depending on the type of abrasive material and the post-polishing surface roughness. The effectiveness of laser conditioning is examined using a ramped pre-exposure with the same 351-nm, 3-ns Gaussian pulses. Lastly, we examine chemical etching of the surface and correlate the resulting damage threshold to the etching protocol. A combination of etching and laser conditioning is found to improve the damage threshold by a factor of ~3, while maintaining <1-nm surface roughness.

  12. Process For Patterning Dispenser-Cathode Surfaces

    NASA Technical Reports Server (NTRS)

    Garner, Charles E.; Deininger, William D.

    1989-01-01

    Several microfabrication techniques combined into process cutting slots 100 micrometer long and 1 to 5 micrometer wide into tungsten dispenser cathodes for traveling-wave tubes. Patterned photoresist serves as mask for etching underlying aluminum. Chemically-assisted ion-beam etching with chlorine removes exposed parts of aluminum layer. Etching with fluorine or chlorine trifluoride removes tungsten not masked by aluminum layer. Slots enable more-uniform low-work function coating dispensed to electron-emitting surface. Emission of electrons therefore becomes more uniform over cathode surface.

  13. Method of making tapered capillary tips with constant inner diameters

    DOEpatents

    Kelly, Ryan T [West Richland, WA; Page, Jason S [Kennewick, WA; Tang, Keqi [Richland, WA; Smith, Richard D [Richland, WA

    2009-02-17

    Methods of forming electrospray ionization emitter tips are disclosed herein. In one embodiment, an end portion of a capillary tube can be immersed into an etchant, wherein the etchant forms a concave meniscus on the outer surface of the capillary. Variable etching rates in the meniscus can cause an external taper to form. While etching the outer surface of the capillary wall, a fluid can be flowed through the interior of the capillary tube. Etching continues until the immersed portion of the capillary tube is completely etched away.

  14. Influence of laser etching on enamel and dentin bond strength of Silorane System Adhesive.

    PubMed

    Ustunkol, Ildem; Yazici, A Ruya; Gorucu, Jale; Dayangac, Berrin

    2015-02-01

    The aim of this in vitro study was to evaluate the shear bond strength (SBS) of Silorane System Adhesive to enamel and dentin surfaces that had been etched with different procedures. Ninety freshly extracted human third molars were used for the study. After the teeth were embedded with buccal surfaces facing up, they were randomly divided into two groups. In group I, specimens were polished with a 600-grit silicon carbide (SiC) paper to obtain flat exposed enamel. In group II, the overlying enamel layer was removed and exposed dentin surfaces were polished with a 600-grit SiC paper. Then, the teeth in each group were randomly divided into three subgroups according to etching procedures: etched with erbium, chromium:yttrium-scandium-gallium-garnet laser (a), etched with 35% phosphoric acid (b), and non-etched (c, control). Silorane System Adhesive was used to bond silorane restorative to both enamel and dentin. After 24-h storage in distilled water at room temperature, a SBS test was performed using a universal testing machine at a crosshead speed of 1 mm/min. The data were analyzed using two-way ANOVA and Bonferroni tests (p < 0.05). The highest SBS was found after additional phosphoric acid treatment in dentin groups (p < 0.05). There were no statistically significant differences between the laser-etched and non-etched groups in enamel and dentin (p > 0.05). The SBS of self-etch adhesive to dentin was not statistically different from enamel (p > 0.05). Phosphoric acid treatment seems the most promising surface treatment for increasing the enamel and dentin bond strength of Silorane System Adhesive.

  15. Influence of the doping level on the porosity of silicon nanowires prepared by metal-assisted chemical etching

    NASA Astrophysics Data System (ADS)

    Geyer, Nadine; Wollschläger, Nicole; Fuhrmann, Bodo; Tonkikh, Alexander; Berger, Andreas; Werner, Peter; Jungmann, Marco; Krause-Rehberg, Reinhard; Leipner, Hartmut S.

    2015-06-01

    A systematic method to control the porosity of silicon nanowires is presented. This method is based on metal-assisted chemical etching (MACE) and takes advantage of an HF/H2O2 etching solution and a silver catalyst in the form of a thin patterned film deposited on a doped silicon wafer. It is found that the porosity of the etched nanowires can be controlled by the doping level of the wafer. For low doping concentrations, the wires are primarily crystalline and surrounded by only a very thin layer of porous silicon (pSi) layer, while for highly doped silicon, they are porous in their entire volume. We performed a series of controlled experiments to conclude that there exists a well-defined critical doping concentration separating the crystalline and porous regimes. Furthermore, transmission electron microscopy investigations showed that the pSi has also a crystalline morphology on a length scale smaller than the pore size, determined from positron annihilation lifetime spectroscopy to be mesoscopic. Based on the experimental evidence, we devise a theoretical model of the pSi formation during MACE and apply it for better control of the nanowire morphology.

  16. Deterministic Nanopatterning of Diamond Using Electron Beams.

    PubMed

    Bishop, James; Fronzi, Marco; Elbadawi, Christopher; Nikam, Vikram; Pritchard, Joshua; Fröch, Johannes E; Duong, Ngoc My Hanh; Ford, Michael J; Aharonovich, Igor; Lobo, Charlene J; Toth, Milos

    2018-03-27

    Diamond is an ideal material for a broad range of current and emerging applications in tribology, quantum photonics, high-power electronics, and sensing. However, top-down processing is very challenging due to its extreme chemical and physical properties. Gas-mediated electron beam-induced etching (EBIE) has recently emerged as a minimally invasive, facile means to dry etch and pattern diamond at the nanoscale using oxidizing precursor gases such as O 2 and H 2 O. Here we explain the roles of oxygen and hydrogen in the etch process and show that oxygen gives rise to rapid, isotropic etching, while the addition of hydrogen gives rise to anisotropic etching and the formation of topographic surface patterns. We identify the etch reaction pathways and show that the anisotropy is caused by preferential passivation of specific crystal planes. The anisotropy can be controlled by the partial pressure of hydrogen and by using a remote RF plasma source to radicalize the precursor gas. It can be used to manipulate the geometries of topographic surface patterns as well as nano- and microstructures fabricated by EBIE. Our findings constitute a comprehensive explanation of the anisotropic etch process and advance present understanding of electron-surface interactions.

  17. DOE Office of Scientific and Technical Information (OSTI.GOV)

    Gray, D.C.; Tepermeister, I.; Sawin, H.H.

    A multiple beam apparatus has been constructed to facilitate the study of ion-enhanced fluorine chemistry on undoped polysilicon and silicon dioxide surfaces by allowing the fluxes of fluorine (F) atoms and argon (Ar{sup +}) ions to be independently varied over several orders of magnitude. The chemical nature of the etching surfaces has been investigated following the vacuum transfer of the sample dies to an adjoining x-ray photoelectron spectroscopy facility. The etching {open_quotes}enhancement{close_quotes} effect of normally incident Ar{sup +} ions has been quantified over a wide range of ion energy through the use of Kaufman and electron cyclotron resonance-type ion sources.more » The increase in per ion etching yield of fluorine saturated silicon and silicon dioxide surfaces with increasing ion energy (E{sub ion}) was found to scale as (E{sub ion}{sup 1/2}-E{sub th}{sup 1/2}), where E{sub th} is the etching threshold energy for the process. Simple near-surface site occupation models have been proposed for the quantification of the ion-enhanced etching kinetics in these systems. Acceptable agreement has been found in comparison of these Ar{sup +}/F etching model predictions with similar Ar{sup +}/XeF{sub 2} studies reported in the literature, as well as with etching rate measurements made in F-based plasmas of gases such as SF{sub 6} and NF{sub 3}. 69 refs., 12 figs., 6 tabs.« less

  18. Evaluating the shear bond strength of enamel and dentin with or without etching: A comparative study between dimethacrylate-based and silorane-based adhesives

    PubMed Central

    Hajizadeh, Hila; Nasseh, Atefeh; Rahmanpour, Naim

    2015-01-01

    Background Silorane-based composites and their specific self-etch adhesive were introduced to conquest the polymerization shrinkage of methacrylate-based composites. It has been shown that additional etching of enamel and dentin can improve the bond strength of self-etch methacrylate-based adhesives but this claim is not apparent about silorane-based adhesives. Our objective was to compare the shear bond strength (SBS) of enamel and dentin between silorane-based adhesive resin and a methacrylate-based resin with or without additional etching. Material and Methods 40 sound human premolars were prepared and divided into two groups: 1- Filtek P60 composite and Clearfil SE Bond adhesive; 2- Filtek P90 composite and Silorane adhesive. Each group divided into two subgroups: with or without additional etching. For additional etching, 37% acid phosphoric was applied before bonding procedure. A cylinder of the composite was bonded to the surface. After 24 hours storage and 500 thermo cycling between 5-55°C, shear bond strength was assessed with the cross head speed of 0.5 mm/min. Then, bonded surfaces were observed under stereomicroscope to determine the failure mode. Data were analyzed with two-way ANOVA and Fischer exact test. Results Shear bond strength of Filtek P60 composite was significantly higher than Filtek P90 composite both in enamel and dentin surfaces (P<0.05). However, additional etching had no significant effect on shear bond strength in enamel or dentin for each of the composites (P>0.05). There was no interaction between composite type and additional etching (P>0.05). Failure pattern was mainly adhesive and no significant correlation was found between failure and composite type or additional etching (P>0.05). Conclusions Shear bond strength of methacrylate-based composite was significantly higher than silorane-based composite both in enamel and dentin surfaces and additional etching had no significant effect on shear bond strength in enamel or dentin for each of the composites. The mode of failure had no meaningful relation to the type of composite and etching factor. Key words:Shear bond strength, adhesive, composite resin, silorane, methacrylate. PMID:26644830

  19. Influence of Application Time and Etching Mode of Universal Adhesives on Enamel Adhesion.

    PubMed

    Sai, Keiichi; Takamizawa, Toshiki; Imai, Arisa; Tsujimoto, Akimasa; Ishii, Ryo; Barkmeier, Wayne W; Latta, Mark A; Miyazaki, Masashi

    2018-01-01

    To investigate the influence of application time and etching mode of universal adhesives on enamel adhesion. Five universal adhesives, Adhese Universal, Bondmer Lightless, Clearfil Universal Bond Quick, G-Premio Bond, and Scotchbond Universal, were used. Bovine incisors were prepared and divided into four groups of ten teeth each. SBS, Ra, and SFE were determined after the following procedures: 1. self-etch mode with immediate air blowing after application (IA); 2. self-etch mode with prolonged application time (PA); 3. etch-and-rinse mode with IA; 4. etch-and-rinse mode with PA. After 24-h water storage, the bonded assemblies were subjected to shear bond strength (SBS) tests. For surface roughness (Ra) and surface free energy (SFE) measurements, the adhesives were simply applied to the enamel and rinsed with acetone and water before the measurements were carried out. Significantly higher SBS and Ra values were obtained with etch-and-rinse mode than with self-etch mode regardless of the application time or type of adhesive. Although most adhesives showed decreased SFE values with increased application time in self-etch mode, SFE values in etch-and-rinse mode were dependent on the adhesive type and application time. Etching mode, application time, and type of adhesive significantly influenced the SBS, Ra, and SFE values.

  20. Etching nano-holes in silicon carbide using catalytic platinum nano-particles

    NASA Astrophysics Data System (ADS)

    Moyen, E.; Wulfhekel, W.; Lee, W.; Leycuras, A.; Nielsch, K.; Gösele, U.; Hanbücken, M.

    2006-09-01

    The catalytic reaction of platinum during a hydrogen etching process has been used to perform controlled vertical nanopatterning of silicon carbide substrates. A first set of experiments was performed with platinum powder randomly distributed on the SiC surface. Subsequent hydrogen etching in a hot wall reactor caused local atomic hydrogen production at the catalyst resulting in local SiC etching and hole formation. Secondly, a highly regular and monosized distribution of Pt was obtained by sputter deposition of Pt through an Au membrane serving as a contact mask. After the lift-off of the mask, the hydrogen etching revealed the onset of well-controlled vertical patterned holes on the SiC surface.

  1. Formation of Micro- and Nanostructures on the Nanotitanium Surface by Chemical Etching and Deposition of Titania Films by Atomic Layer Deposition (ALD)

    PubMed Central

    Nazarov, Denis V.; Zemtsova, Elena G.; Valiev, Ruslan Z.; Smirnov, Vladimir M.

    2015-01-01

    In this study, an integrated approach was used for the preparation of a nanotitanium-based bioactive material. The integrated approach included three methods: severe plastic deformation (SPD), chemical etching and atomic layer deposition (ALD). For the first time, it was experimentally shown that the nature of the etching medium (acidic or basic Piranha solutions) and the etching time have a significant qualitative impact on the nanotitanium surface structure both at the nano- and microscale. The etched samples were coated with crystalline biocompatible TiO2 films with a thickness of 20 nm by Atomic Layer Deposition (ALD). Comparative study of the adhesive and spreading properties of human osteoblasts MG-63 has demonstrated that presence of nano- and microscale structures and crystalline titanium oxide on the surface of nanotitanium improve bioactive properties of the material. PMID:28793716

  2. Removal and deposition efficiencies of the long-lived 222Rn daughters during etching of germanium surfaces

    NASA Astrophysics Data System (ADS)

    Zuzel, G.; Wójcik, M.; Majorovits, B.; Lampert, M. O.; Wendling, P.

    2012-06-01

    Removal and deposition efficiencies of the long-lived 222Rn daughters during etching from and onto surfaces of standard and high purity germanium were investigated. The standard etching procedure of Canberra-France used during production of high purity n-type germanium diodes was applied to germanium discs, which have been exposed earlier to a strong radon source for deposition of its progenies. An uncontaminated sample was etched in a solution containing 210Pb, 210Bi and 210Po. All isotopes were measured before and after etching with appropriate detectors. In contrast to copper and stainless steel, they were removed from germanium very efficiently. However, the reverse process was also observed. Considerable amounts of radioactive lead, bismuth and polonium isotopes present initially in the artificially polluted etchant were transferred to the clean high purity surface during processing of the sample.

  3. Overlapping double etch technique for evaluation of metallic alloys to stress corrosion cracking

    DOEpatents

    Steeves, Arthur F.; Stewart, James C.

    1981-01-01

    A double overlapping etch zone technique for evaluation of the resistance of metallic alloys to stress corrosion cracking. The technique involves evaluating the metallic alloy along the line of demarcation between an overlapping double etch zone and single etch zone formed on the metallic alloy surface.

  4. Feasibility of Plasma Treated Clay in Clay/Polymer Nanocomposites Powders for use Laser Sintering (LS)

    NASA Astrophysics Data System (ADS)

    Almansoori, Alaa; Seabright, Ryan; Majewski, C.; Rodenburg, C.

    2017-05-01

    The addition of small quantities of nano-clay to nylon is known to improve mechanical properties of the resulting nano-composite. However, achieving a uniform dispersion and distribution of the clay within the base polymer can prove difficult. A demonstration of the fabrication and characterization of plasma-treated organoclay/Nylon12 nanocomposite was carried out with the aim of achieving better dispersion of clay platelets on the Nylon12 particle surface. Air-plasma etching was used to enhance the compatibility between clays and polymers to ensure a uniform clay dispersion in composite powders. Downward heat sintering (DHS) in a hot press is used to process neat and composite powders into tensile and XRD specimens. Morphological studies using Low Voltage Scanning Electron Microscopy (LV-SEM) were undertaken to characterize the fracture surfaces and clay dispersion in powders and final composite specimens. Thermogravimetric analysis (TGA) testing performed that the etched clay (EC) is more stable than the nonetched clay (NEC), even at higher temperatures. The influence of the clay ratio and the clay plasma treatment process on the mechanical properties of the nanocomposites was studied by tensile testing. The composite fabricated from (3% EC/N12) powder showed ~19 % improvement in elastic modulus while the composite made from (3% NEC/N12) powder was improved by only 14%). Most notably however is that the variation between tests is strongly reduced when etch clay is used in the composite. We attribute this to a more uniform distribution and better dispersion of the plasma treated clay within polymer powders and ultimately the composite.

  5. Effect of enamel etching time on roughness and bond strength.

    PubMed

    Barkmeier, Wayne W; Erickson, Robert L; Kimmes, Nicole S; Latta, Mark A; Wilwerding, Terry M

    2009-01-01

    The current study examined the effect of different enamel conditioning times on surface roughness and bond strength using an etch-and-rinse system and four self-etch adhesives. Surface roughness (Ra) and composite to enamel shear bond strengths (SBS) were determined following the treatment of flat ground human enamel (4000 grit) with five adhesive systems: (1) Adper Single Bond Plus (SBP), (2) Adper Prompt L-Pop (PLP), (3) Clearfil SE Bond (CSE), (4) Clearfil S3 Bond (CS3) and (5) Xeno IV (X4), using recommended treatment times and an extended treatment time of 60 seconds (n = 10/group). Control groups were also included for Ra (4000 grit surface) and SBS (no enamel treatment and Adper Scotchbond Multi-Purpose Adhesive). For surface roughness measurements, the phosphoric acid conditioner of the SBP etch-and-rinse system was rinsed from the surface with an air-water spray, and the other four self-etch adhesive agents were removed with alternating rinses of water and acetone. A Proscan 2000 non-contact profilometer was used to determine Ra values. Composite (Z100) to enamel bond strengths (24 hours) were determined using Ultradent fixtures and they were debonded with a crosshead speed of 1 mm/minute. The data were analyzed with ANOVA and Fisher's LSD post-hoc test. The etch-and- rinse system (SBP) produced the highest Ra (microm) and SBS (MPa) using both the recommended treatment time (0.352 +/- 0.028 microm and 40.5 +/- 6.1 MPa) and the extended treatment time (0.733 +/- 0.122 microm and 44.2 +/- 8.2 MPa). The Ra and SBS of the etch-and-rinse system were significantly greater (p < 0.05) than all the self-etch systems and controls. Increasing the treatment time with phosphoric acid (SBP) and PLP produced greater surface roughness (p < 0.05) but did not result in significantly higher bond strengths (p > 0.05).

  6. Chemical Etching of Zinc Oxide for Thin-Film Silicon Solar Cells

    PubMed Central

    Hüpkes, Jürgen; Owen, Jorj I; Pust, Sascha E; Bunte, Eerke

    2012-01-01

    Abstract Chemical etching is widely applied to texture the surface of sputter-deposited zinc oxide for light scattering in thin-film silicon solar cells. Based on experimental findings from the literature and our own results we propose a model that explains the etching behavior of ZnO depending on the structural material properties and etching agent. All grain boundaries are prone to be etched to a certain threshold, that is defined by the deposition conditions and etching solution. Additionally, several approaches to modify the etching behavior through special preparation and etching steps are provided. PMID:22162035

  7. Trench formation in <110> silicon for millimeter-wave switching device

    NASA Astrophysics Data System (ADS)

    Datta, P.; Kumar, Praveen; Nag, Manoj; Bhattacharya, D. K.; Khosla, Y. P.; Dahiya, K. K.; Singh, D. V.; Venkateswaran, R.; Kumar, Devender; Kesavan, R.

    1999-11-01

    Anisotropic etching using alkaline solution has been adopted to form trenches in silicon while fabricating surface oriented bulk window SPST switches. An array pattern has been etched on silicon with good control on depth of trenches. KOH-water solution is seen to yield a poor surface finish. Use of too much of additive like isopropyl alcohol improves the surface condition but distorts the array pattern due to loss of anisotropy. However, controlled use of this additive during the last phase of trench etching is found to produce trenched arrays with desired depth, improved surface finish and minimum distortion of lateral dimensions.

  8. Nanoscale Etching and Indentation of Silicon(001) Surface with Carbon Nanotube Tips

    NASA Technical Reports Server (NTRS)

    Dzegilenko, Fendor N.; Srivastava, Deepak; Saini, Subhash

    1998-01-01

    The possibility of nanoscale etching and indentation of Si(001)(2x1) surface by (8,0) and (10,10) carbon nanotube tips is demonstrated, for the first time, by classical molecular dynamics simulations employing Tersoff's many-body potential for a mixed C/Si/Ge system. In the nanotube tip barely touching the surface scenario atomistic etching is observed, where as in the nanoindentation scenario nanotube tip penetrates the surface without much hindrance. The results are explained in terms of the relative strength of C-C, C-Si, and Si-Si bonds.

  9. Enhanced photo-response of porous silicon photo-detectors by embeddingTitanium-dioxide nano-particles

    NASA Astrophysics Data System (ADS)

    Ali, Hiba M.; Makki, Sameer A.; Abd, Ahmed N.

    2018-05-01

    Porous silicon (n-PS) films can be prepared by photoelectochemical etching (PECE) Silicon chips n - types with 15 (mA / cm2), in 15 minutes etching time on the fabrication nano-sized pore arrangement. By using X-ray diffraction measurement and atomic power microscopy characteristics (AFM), PS was investigated. It was also evaluated the crystallites size from (XRD) for the PS nanoscale. The atomic force microscopy confirmed the nano-metric size chemical fictionalization through the electrochemical etching that was shown on the PS surface chemical composition. The atomic power microscopy checks showed the roughness of the silicon surface. It is also notified (TiO2) preparation nano-particles that were prepared by pulse laser eradication in ethanol (PLAL) technique through irradiation with a Nd:YAG laser pulses TiO2 target that is sunk in methanol using 400 mJ of laser energy. It has been studied the structural, optical and morphological of TiO2NPs. It has been detected that through XRD measurement, (TiO2) NPs have been Tetragonal crystal structure. While with AFM measurements, it has been realized that the synthesized TiO2 particles are spherical with an average particle size in the (82 nm) range. It has been determined that the energy band gap of TiO2 NPs from optical properties and set to be in (5eV) range.The transmittance and reflectance spectra have determined the TiO2 NPs optical constants. It was reported the effectiveness of TiO2 NPs expansion on the PS Photodetector properties which exposes the benefits in (Al/PS/Si/Al). The built-in tension values depend on the etching time current density and laser flounce. Al/TiO2/PS/Si/Al photo-detector heterojunction have two response peaks that are situated at 350 nm and (700 -800nm) with max sensitivity ≈ 0.7 A/W. The maximum given detectivity is 9.38at ≈ 780 nm wavelength.

  10. Nanowall formation by maskless wet-etching on a femtosecond laser irradiated silicon surface

    NASA Astrophysics Data System (ADS)

    Lee, Siwoo; Jo, Kukhyun; Keum, Hee-sung; Chae, Sangmin; Kim, Yonghyeon; Choi, Jiyeon; Lee, Hyun Hwi; Kim, Hyo Jung

    2018-04-01

    We found that micro-cells surrounded by nanowalls can be formed by a maskless wet-etching process on Si (100) surfaces possessing Laser Induced Periodic Surface Structure (LIPSS) by femtosecond laser irradiation. The LIPSS process could produce periodic one-dimensional micron scale ripples on a Si surface, which could be developed into micro-cells by a subsequent etching process. The solution etching conditions strongly affected both the micro-cell and nanowall shapes such as the height and the thickness of nanowalls. The tetramethylammonium hydroxide solution created thin nanowalls and the resulting micro-cells with a well-flattened bottom while the KOH solution formed thick walls and incomplete micro-cells. The bottoms of micro-cells surrounded by the nanowalls were considerably flat with a 3.10 nm surface roughness. A pentacene layer was deposited on the micro-cells of a Si surface to evaluate the film properties by grazing incidence wide angle x-ray scattering measurements. The pentacene film on the micro-cell Si surface showed a strong film phase, which was comparable to the film phase grown on the atomically flat Si surface.

  11. Changes in boron fiber strength due to surface removal by chemical etching

    NASA Technical Reports Server (NTRS)

    Smith, R. J.

    1976-01-01

    The effects of chemical etching on the tensile strength of commercial boron/tungsten fibers were investigated. Fibers with as-received diameters of 203, 143, and 100 micrometers were etched to diameters as small as 43 micrometers. The etching generally resulted in increasing fiber tensile strength with decreasing fiber diameter. And for the 203 micrometer fibers there was an accompanying significant decrease in the coefficient of variation of the tensile strength for diameters down to 89 micrometers. Heat treating these fibers above 1,173 K in a vacuum caused a marked decrease in the average tensile strength of at least 80 percent. But after the fibers were etched, their strengths exceeded the as-received strengths. The tensile strength behavior is explained in terms of etching effects on surface flaws and the residual stress pattern of the as-received fibers.

  12. Mechanisms of Hydrocarbon Based Polymer Etch

    NASA Astrophysics Data System (ADS)

    Lane, Barton; Ventzek, Peter; Matsukuma, Masaaki; Suzuki, Ayuta; Koshiishi, Akira

    2015-09-01

    Dry etch of hydrocarbon based polymers is important for semiconductor device manufacturing. The etch mechanisms for oxygen rich plasma etch of hydrocarbon based polymers has been studied but the mechanism for lean chemistries has received little attention. We report on an experimental and analytic study of the mechanism for etching of a hydrocarbon based polymer using an Ar/O2 chemistry in a single frequency 13.56 MHz test bed. The experimental study employs an analysis of transients from sequential oxidation and Ar sputtering steps using OES and surface analytics to constrain conceptual models for the etch mechanism. The conceptual model is consistent with observations from MD studies and surface analysis performed by Vegh et al. and Oehrlein et al. and other similar studies. Parameters of the model are fit using published data and the experimentally observed time scales.

  13. Effect of bracket bonding with Er: YAG laser on nanomechanical properties of enamel.

    PubMed

    Alavi, Shiva; Birang, Reza; Hajizadeh, Fatemeh; Banimostafaee, Hamed

    2014-01-01

    The aim of this study was to compare the effects of conventional acid etching and laser etching on the nano-mechanical properties of the dental enamel using nano-indentation test. In this experimental in vitro study, buccal surfaces of 10 premolars were divided into three regions. One of the regions was etched with 37% phosphoric acid and another etched with Er:YAG laser, the third region was not etched. The brackets were bonded to both of etched regions. After thermocycling for 500 cycles, the brackets were removed and the teeth were decoronated from the bracket bonding area. Seven nano-indentations were applied at 1-31 μm depth from the enamel surface in each region. Mean values of the hardness and elastic modulus were analyzed with repeated measures analysis of variance and Tukey HSD tests, using the SPSS software (SPSS Inc., version16.0, Chicago, Il, USA). P < 0.05 was considered as significant. The hardness up to 21 μm in depth and elastic modulus up to 6 μm in depth from the enamel surface for laser-etched enamel had significantly higher values than control enamel and the hardness up to 11 μm in depth and elastic modulus up to 6 μm in depth for acid-etched enamel had significantly lower values than the control enamel. The mechanical properties of the enamel were decreased after bracket bonding with conventional acid etching and increased after bonding with Er:YAG laser.

  14. Improvement of enamel bond strengths for conventional and resin-modified glass ionomers: acid-etching vs. conditioning*

    PubMed Central

    Zhang, Ling; Tang, Tian; Zhang, Zhen-liang; Liang, Bing; Wang, Xiao-miao; Fu, Bai-ping

    2013-01-01

    Objective: This study deals with the effect of phosphoric acid etching and conditioning on enamel micro-tensile bond strengths (μTBSs) of conventional and resin-modified glass ionomer cements (GICs/RMGICs). Methods: Forty-eight bovine incisors were prepared into rectangular blocks. Highly-polished labial enamel surfaces were either acid-etched, conditioned with liquids of cements, or not further treated (control). Subsequently, two matching pre-treated enamel surfaces were cemented together with one of four cements [two GICs: Fuji I (GC), Ketac Cem Easymix (3M ESPE); two RMGICs: Fuji Plus (GC), RelyX Luting (3M ESPE)] in preparation for μTBS tests. Pre-treated enamel surfaces and cement-enamel interfaces were analyzed by scanning electron microscopy (SEM). Results: Phosphoric acid etching significantly increased the enamel μTBS of GICs/RMGICs. Conditioning with the liquids of the cements produced significantly weaker or equivalent enamel μTBS compared to the control. Regardless of etching, RMGICs yielded stronger enamel μTBS than GICs. A visible hybrid layer was found at certain enamel-cement interfaces of the etched enamels. Conclusions: Phosphoric acid etching significantly increased the enamel μTBSs of GICs/RMGICs. Phosphoric acid etching should be recommended to etch the enamel margins before the cementation of the prostheses such as inlays and onlays, using GICs/RMGICs to improve the bond strengths. RMGICs provided stronger enamel bond strength than GICs and conditioning did not increase enamel bond strength. PMID:24190447

  15. Nanosecond laser-induced back side wet etching of fused silica with a copper-based absorber liquid

    NASA Astrophysics Data System (ADS)

    Lorenz, Pierre; Zehnder, Sarah; Ehrhardt, Martin; Frost, Frank; Zimmer, Klaus; Schwaller, Patrick

    2014-03-01

    Cost-efficient machining of dielectric surfaces with high-precision and low-roughness for industrial applications is still challenging if using laser-patterning processes. Laser induced back side wet etching (LIBWE) using UV laser pulses with liquid heavy metals or aromatic hydrocarbons as absorber allows the fabrication of well-defined, nm precise, free-form surfaces with low surface roughness, e.g., needed for optical applications. The copper-sulphatebased absorber CuSO4/K-Na-Tartrate/NaOH/formaldehyde in water is used for laser-induced deposition of copper. If this absorber can also be used as precursor for laser-induced ablation, promising industrial applications combining surface structuring and deposition within the same setup could be possible. The etching results applying a KrF excimer (248 nm, 25 ns) and a Nd:YAG (1064 nm, 20 ns) laser are compared. The topography of the etched surfaces were analyzed by scanning electron microscopy (SEM), white light interferometry (WLI) as well as laser scanning microscopy (LSM). The chemical composition of the irradiated surface was studied by energy-dispersive X-ray spectroscopy (EDX) and Fourier transform infrared spectroscopy (FT-IR). For the discussion of the etching mechanism the laser-induced heating was simulated with finite element method (FEM). The results indicate that the UV and IR radiation allows micro structuring of fused silica with the copper-based absorber where the etching process can be explained by the laser-induced formation of a copper-based absorber layer.

  16. Ultrastructure of the surface of dental enamel with molar incisor hypomineralization (MIH) with and without acid etching.

    PubMed

    Bozal, Carola B; Kaplan, Andrea; Ortolani, Andrea; Cortese, Silvina G; Biondi, Ana M

    2015-01-01

    The aim of the present work was to analyze the ultrastructure and mineral composition of the surface of the enamel on a molar with MIH, with and without acid etching. A permanent tooth without clinical MIH lesions (control) and a tooth with clinical diagnosis of mild and moderate MIH, with indication for extraction, were processed with and without acid etching (H3PO4 37%, 20") for observation with scanning electron microscope (SEM) ZEISS (Supra 40) and mineral composition analysis with an EDS detector (Oxford Instruments). The control enamel showed normal prismatic surface and etching pattern. The clinically healthy enamel on the tooth with MIH revealed partial loss of prismatic pattern. The mild lesion was porous with occasional cracks. The moderate lesion was more porous, with larger cracks and many scales. The mineral composition of the affected surfaces had lower Ca and P content and higher O and C. On the tooth with MIH, even on normal looking enamel, the demineralization does not correspond to an etching pattern, and exhibits exposure of crystals with rods with rounded ends and less demineralization in the inter-prismatic spaces. Acid etching increased the presence of cracks and deep pores in the adamantine structure of the enamel with lesion. In moderate lesions, the mineral composition had higher content of Ca, P and Cl. Enamel with MIH, even on clinically intact adamantine surfaces, shows severe alterations in the ultrastructure and changes in ionic composition, which affect the acid etching pattern and may interfere with adhesion.

  17. Correlation between border traps and exposed surface properties in gate recessed normally-off Al2O3/GaN MOSFET

    NASA Astrophysics Data System (ADS)

    Yin, Ruiyuan; Li, Yue; Sun, Yu; Wen, Cheng P.; Hao, Yilong; Wang, Maojun

    2018-06-01

    We report the effect of the gate recess process and the surface of as-etched GaN on the gate oxide quality and first reveal the correlation between border traps and exposed surface properties in normally-off Al2O3/GaN MOSFET. The inductively coupled plasma (ICP) dry etching gate recess with large damage presents a rough and active surface that is prone to form detrimental GaxO validated by atomic force microscopy and X-ray photoelectron spectroscopy. Lower drain current noise spectral density of the 1/f form and less dispersive ac transconductance are observed in GaN MOSFETs fabricated with oxygen assisted wet etching compared with devices based on ICP dry etching. One decade lower density of border traps is extracted in devices with wet etching according to the carrier number fluctuation model, which is consistent with the result from the ac transconductance method. Both methods show that the density of border traps is skewed towards the interface, indicating that GaxO is of higher trap density than the bulk gate oxide. GaxO located close to the interface is the major location of border traps. The damage-free oxidation assisted wet etching gate recess technique presents a relatively smooth and stable surface, resulting in lower border trap density, which would lead to better MOS channel quality and improved device reliability.

  18. Ridge-width dependence of the threshold of long wavelength (λ ≈ 14 µm) Quantum Cascade lasers with sloped and vertical sidewalls.

    PubMed

    Huang, Xue; Chiu, Yenting; Charles, William O; Gmachl, Claire

    2012-01-30

    We investigate the ridge-width dependence of the threshold of Quantum Cascade lasers fabricated by wet and dry etching, respectively. The sloped sidewalls resulting from wet etching affect the threshold in two ways as the ridge gets narrower. First, the transverse modes are deeper in the substrate, hence reducing the optical confinement factor. Second, more important, a non-negligible field exists in the lossy SiO2 insulation layer, as a result of transverse magnetic mode coupling to the surface plamon mode at the insulator/metal surface, which increases the waveguide loss. By contrast, dry etching is anisotropic and leads to waveguides with vertical sidewalls, which avoids the shift of the modes to the substrate layer and coupling to the surface plasmons, resulting in improved threshold compared with wet-etched lasers, e.g., for narrow ridge widths below 20 µm, the threshold of a 14 µm wide λ ≈ 14 µm laser by dry etching is ~60% lower than that of a wet-etched laser of the same width, at 80 K.

  19. Anisotropic Etching of Hexagonal Boron Nitride and Graphene: Question of Edge Terminations

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Stehle, Yijing Y.; Sang, Xiahan; Unocic, Raymond R.

    Here, chemical vapor deposition (CVD) has been established as the most effective way to grow large area two-dimensional materials. Direct study of the etching process can reveal subtleties of this competing with the growth reaction and thus provide the necessary details of the overall growth mechanism. Here we investigate hydrogen-induced etching of hBN and graphene and compare the results with the classical kinetic Wulff construction model. Formation of the anisotropically etched holes in the center of hBN and graphene single crystals was observed along with the changes in the crystals' circumference. We show that the edges of triangular holes inmore » hBN crystals formed at regular etching conditions are parallel to B-terminated zigzags, opposite to the N-terminated zigzag edges of hBN triangular crystals. The morphology of the etched hBN holes is affected by a disbalance of the B/N ratio upon etching and can be shifted toward the anticipated from the Wulff model N-terminated zigzag by etching in a nitrogen buffer gas instead of a typical argon. For graphene, etched hexagonal holes are terminated by zigzag, while the crystal circumference is gradually changing from a pure zigzag to a slanted angle resulting in dodecagons.« less

  20. Anisotropic Etching of Hexagonal Boron Nitride and Graphene: Question of Edge Terminations

    DOE PAGES

    Stehle, Yijing Y.; Sang, Xiahan; Unocic, Raymond R.; ...

    2017-11-14

    Here, chemical vapor deposition (CVD) has been established as the most effective way to grow large area two-dimensional materials. Direct study of the etching process can reveal subtleties of this competing with the growth reaction and thus provide the necessary details of the overall growth mechanism. Here we investigate hydrogen-induced etching of hBN and graphene and compare the results with the classical kinetic Wulff construction model. Formation of the anisotropically etched holes in the center of hBN and graphene single crystals was observed along with the changes in the crystals' circumference. We show that the edges of triangular holes inmore » hBN crystals formed at regular etching conditions are parallel to B-terminated zigzags, opposite to the N-terminated zigzag edges of hBN triangular crystals. The morphology of the etched hBN holes is affected by a disbalance of the B/N ratio upon etching and can be shifted toward the anticipated from the Wulff model N-terminated zigzag by etching in a nitrogen buffer gas instead of a typical argon. For graphene, etched hexagonal holes are terminated by zigzag, while the crystal circumference is gradually changing from a pure zigzag to a slanted angle resulting in dodecagons.« less

  1. Self-formation of a nanonet of fluorinated carbon nanowires on the Si surface by combined etching in fluorine-containing plasma

    NASA Astrophysics Data System (ADS)

    Amirov, I. I.; Gorlachev, E. S.; Mazaletskiy, L. A.; Izyumov, M. O.; Alov, N. V.

    2018-03-01

    In this work, we report a technique of the self-formation of a nanonet of fluorinated carbon nanowires on the Si surface using a combined etching in fluorine-containing C4F8/Ar and SF6 plasmas. Using scanning electron microscopy, atomic force microscopy and x-ray photoelectron spectroscopy, we show that after the etching of Si in the C4F8/Ar plasma, a fluorinated carbon film of nanometer-scale thickness is formed on its surface and its formation accelerates at elevated temperatures. After a subsequent short-term etching in the SF6 plasma, the film is modified into a nanonet of self-formed fluorinated carbon nanowires.

  2. Wet-chemical dissolution of TRISO-coated simulated high-temperature-reactor fuel particles

    NASA Astrophysics Data System (ADS)

    Skolo, K. P.; Jacobs, P.; Venter, J. H.; Klopper, W.; Crouse, P. L.

    2012-01-01

    Chemical etching with different mixtures of acidic solutions has been investigated to disintegrate the two outermost coatings from tri-structural isotropic coated particles containing zirconia kernels, which are used in simulated particles instead of uranium dioxide. A scanning electron microscope (SEM) was used to study the morphology of the particles after the first etching step as well as at different stages of the second etching step. SEM examination shows that the outer carbon layer can be readily removed with a CrO 3-HNO 3/H 2SO 4 solution. This finding was verified by energy dispersive spectroscopy (EDS) analysis. Etching of the silicon carbide layer in a hydrofluoric-nitric solution yielded partial removal of the coating and localized attack of the underlying coating layers. The SEM results provide evidence that the etching of the silicon carbide layer is strongly influenced by its microstructure.

  3. Heterogeneous processes in CF4/O2 plasmas probed using laser-induced fluorescence of CF2

    NASA Astrophysics Data System (ADS)

    Hansen, S. G.; Luckman, G.; Nieman, George C.; Colson, Steven D.

    1990-09-01

    Laser-induced fluorescence of CF2 is used to monitor heterogeneous processes in ≊300 mTorr CF4/O2 plasmas. CF2 is rapidly removed at fluorinated copper and silver surfaces in 13.56-MHz rf discharges as judged by a distinct dip in its spatial distribution. These metals, when employed as etch masks, are known to accelerate plasma etching of silicon, and the present results suggest catalytic dehalogenation of CF2 is involved in this process. In contrast, aluminum and silicon dioxide exhibit negligible reactivity with CF2, which suggests that aluminum masks will not appreciably accelerate silicon etching and that ground state CF2 does not efficiently etch silicon dioxide. Measurement of CF2 decay in a pulsed discharge coupled with direct laser sputtering of metal into the gas phase indicates the interaction between CF2 and the active metals is purely heterogeneous. Aluminum does, however, exhibit homogeneous reactivity with CF2. Redistribution of active metal by plasma sputtering readily occurs; silicon etch rates may also be enhanced by the metal's presence on the silicon surface. Polymers contribute CF2 to the plasma as they etch. The observation of an induction period suggests fluorination of the polymer surface is the first step in its degradation. Polymeric etch masks can therefore depress the silicon etch rate by removal of F atoms, the primary etchants.

  4. Quadrilateral Micro-Hole Array Machining on Invar Thin Film: Wet Etching and Electrochemical Fusion Machining

    PubMed Central

    Choi, Woong-Kirl; Kim, Seong-Hyun; Choi, Seung-Geon; Lee, Eun-Sang

    2018-01-01

    Ultra-precision products which contain a micro-hole array have recently shown remarkable demand growth in many fields, especially in the semiconductor and display industries. Photoresist etching and electrochemical machining are widely known as precision methods for machining micro-holes with no residual stress and lower surface roughness on the fabricated products. The Invar shadow masks used for organic light-emitting diodes (OLEDs) contain numerous micro-holes and are currently machined by a photoresist etching method. However, this method has several problems, such as uncontrollable hole machining accuracy, non-etched areas, and overcutting. To solve these problems, a machining method that combines photoresist etching and electrochemical machining can be applied. In this study, negative photoresist with a quadrilateral hole array pattern was dry coated onto 30-µm-thick Invar thin film, and then exposure and development were carried out. After that, photoresist single-side wet etching and a fusion method of wet etching-electrochemical machining were used to machine micro-holes on the Invar. The hole machining geometry, surface quality, and overcutting characteristics of the methods were studied. Wet etching and electrochemical fusion machining can improve the accuracy and surface quality. The overcutting phenomenon can also be controlled by the fusion machining. Experimental results show that the proposed method is promising for the fabrication of Invar film shadow masks. PMID:29351235

  5. Overlapping double etch technique for evaluation of metallic alloys to stress corrosion cracking

    DOEpatents

    Not Available

    1980-05-28

    A double overlapping etch zone technique for evaluation of the resistance of metallic alloys to stress corrosion cracking is described. The technique involves evaluating the metallic alloy along the line of demarcation between an overlapping double etch zone and single etch zone formed on the metallic alloy surface.

  6. Etching of enamel for direct bonding with a thulium fiber laser

    NASA Astrophysics Data System (ADS)

    Kabaş Sarp, Ayşe S.; Gülsoy, Murat

    2011-03-01

    Background: Laser etching of enamel for direct bonding can decrease the risk of surface enamel loss and demineralization which are the adverse effects of acid etching technique. However, in excess of +5.5°C can cause irreversible pulpal responses. In this study, a 1940- nm Thulium Fiber Laser in CW mode was used for laser etching. Aim: Determination of the suitable Laser parameters of enamel surface etching for direct bonding of ceramic brackets and keeping that intrapulpal temperature changes below the threshold value. Material and Method: Polycrystalline ceramic orthodontic brackets were bonded on bovine teeth by using 2 different kinds of etching techniques: Acid and Laser Etching. In addition to these 3 etched groups, there was also a group which was bonded without etching. Brackets were debonded with a material testing machine. Breaking time and the load at the breaking point were measured. Intrapulpal temperature changes were recorded by a K-type Thermocouple. For all laser groups, intrapulpal temperature rise was below the threshold value of 5.5°C. Results and Conclusion: Acid-etched group ( 11.73 MPa) significantly required more debonding force than 3- second- irradiated ( 5.03 MPa) and non-etched groups ( 3.4 MPa) but the results of acid etched group and 4- second- irradiated group (7.5 MPa) showed no significant difference. Moreover, 4- second irradiated group was over the minimum acceptable value for clinical use. Also, 3- second lasing caused a significant reduction in time according to acid-etch group. As a result, 1940- nm laser irradiation is a promising method for laser etching.

  7. Chemical etching of nitinol stents.

    PubMed

    Katona, Bálint; Bognár, Eszter; Berta, Balázs; Nagy, Péter; Hirschberg, Kristóf

    2013-01-01

    At present the main cause of death originates from cardiovascular diseases. Primarily the most frequent cause is vessel closing thus resulting in tissue damage. The stent can help to avoid this. It expands the narrowed vessel section and allows free blood flow. The good surface quality of stents is important. It also must have adequate mechanical characteristics or else it can be damaged which can easily lead to the fracture of the implant. Thus, we have to consider the importance of the surface treatment of these implants. In our experiments the appropriate design was cut from a 1.041 mm inner diameter and 0.100 mm wall thickness nitinol tube by using Nd:YAG laser device. Then, the stent was subjected to chemical etching. By doing so, the burr created during the laser cutting process can be removed and the surface quality refined. In our research, we changed the time of chemical etching and monitored the effects of this parameter. The differently etched stents were subjected to microscopic analysis, mass measurement and in vivo environment tests. The etching times that gave suitable surface and mechanical features were identified.

  8. Fabrication mechanism of friction-induced selective etching on Si(100) surface

    PubMed Central

    2012-01-01

    As a maskless nanofabrication technique, friction-induced selective etching can easily produce nanopatterns on a Si(100) surface. Experimental results indicated that the height of the nanopatterns increased with the KOH etching time, while their width increased with the scratching load. It has also found that a contact pressure of 6.3 GPa is enough to fabricate a mask layer on the Si(100) surface. To understand the mechanism involved, the cross-sectional microstructure of a scratched area was examined, and the mask ability of the tip-disturbed silicon layer was studied. Transmission electron microscope observation and scanning Auger nanoprobe analysis suggested that the scratched area was covered by a thin superficial oxidation layer followed by a thick distorted (amorphous and deformed) layer in the subsurface. After the surface oxidation layer was removed by HF etching, the residual amorphous and deformed silicon layer on the scratched area can still serve as an etching mask in KOH solution. The results may help to develop a low-destructive, low-cost, and flexible nanofabrication technique suitable for machining of micro-mold and prototype fabrication in micro-systems. PMID:22356699

  9. Fabrication mechanism of friction-induced selective etching on Si(100) surface.

    PubMed

    Guo, Jian; Song, Chenfei; Li, Xiaoying; Yu, Bingjun; Dong, Hanshan; Qian, Linmao; Zhou, Zhongrong

    2012-02-23

    As a maskless nanofabrication technique, friction-induced selective etching can easily produce nanopatterns on a Si(100) surface. Experimental results indicated that the height of the nanopatterns increased with the KOH etching time, while their width increased with the scratching load. It has also found that a contact pressure of 6.3 GPa is enough to fabricate a mask layer on the Si(100) surface. To understand the mechanism involved, the cross-sectional microstructure of a scratched area was examined, and the mask ability of the tip-disturbed silicon layer was studied. Transmission electron microscope observation and scanning Auger nanoprobe analysis suggested that the scratched area was covered by a thin superficial oxidation layer followed by a thick distorted (amorphous and deformed) layer in the subsurface. After the surface oxidation layer was removed by HF etching, the residual amorphous and deformed silicon layer on the scratched area can still serve as an etching mask in KOH solution. The results may help to develop a low-destructive, low-cost, and flexible nanofabrication technique suitable for machining of micro-mold and prototype fabrication in micro-systems.

  10. Chemical etching and organometallic chemical vapor deposition on varied geometries of GaAs

    NASA Technical Reports Server (NTRS)

    Bailey, Sheila G.; Landis, Geoffrey A.; Wilt, David M.

    1989-01-01

    Results of micron-spaced geometries produced by wet chemical etching and subsequent OMCVD growth on various GaAs surfaces are presented. The polar lattice increases the complexity of the process. The slow-etch planes defined by anisotropic etching are not always the same as the growth facets produced during MOCVD deposition, especially for deposition on higher-order planes produced by the hex groove etching.

  11. Selective protection of poly(tetra-fluoroethylene) from effects of chemical etching

    DOEpatents

    Martinez, Robert J.; Rye, Robert R.

    1991-01-01

    A photolithographic method for treating an article formed of polymeric material comprises subjecting portions of a surface of the polymeric article to ionizing radiation; and then subjecting the surface to chemical etching. The ionizing radiation treatment according to the present invention minimizes the effect of the subseuent chemical etching treatment. Thus, selective protection from the effects of chemical etching can be easily provided. The present invention has particular applicability to articles formed of fluorocarbons, such as PTFE. The ionizing radiation employed in the method may comprise Mg(k.alpha.) X-rays or lower-energy electrons.

  12. Metal-assisted chemical etching using sputtered gold: a simple route to black silicon

    NASA Astrophysics Data System (ADS)

    Kurek, Agnieszka; Barry, Seán T.

    2011-08-01

    We report an accessible and simple method of producing 'black silicon' with aspect ratios as high as 8 using common laboratory equipment. Gold was sputtered to a thickness of 8 nm using a low-vacuum sputter coater. The structures were etched into silicon substrates using an aqueous H2O2/HF solution, and the gold was then removed using aqua regia. Ultrasonication was necessary to produce columnar structures, and an etch time of 24 min gave a velvety, non-reflective surface. The surface features after 24 min etching were uniformly microstructured over an area of square centimetres.

  13. Edge morphology evolution of graphene domains during chemical vapor deposition cooling revealed through hydrogen etching.

    PubMed

    Zhang, Haoran; Zhang, Yanhui; Zhang, Yaqian; Chen, Zhiying; Sui, Yanping; Ge, Xiaoming; Yu, Guanghui; Jin, Zhi; Liu, Xinyu

    2016-02-21

    During cooling, considerable changes such as wrinkle formation and edge passivation occur in graphene synthesized on the Cu substrate. Wrinkle formation is caused by the difference in the thermal expansion coefficients of graphene and its substrate. This work emphasizes the cooling-induced edge passivation. The graphene-edge passivation can limit the regrowth of graphene at the domain edge. Our work shows that silicon-containing particles tend to accumulate at the graphene edge, and the formation of these particles is related to cooling. Furthermore, a clear curvature can be observed at the graphene edge on the Cu substrate, indicating the sinking of the graphene edge into the Cu substrate. Both the sinking of the graphene edge and the accumulation of silicon-containing particles are responsible for edge passivation. In addition, two kinds of graphene edge morphologies are observed after etching, which were explained by different etching mechanisms that illustrate the changes of the graphene edge during cooling.

  14. Reduction of chlorine radical chemical etching of GaN under simultaneous plasma-emitted photon irradiation

    NASA Astrophysics Data System (ADS)

    Liu, Zecheng; Imamura, Masato; Asano, Atsuki; Ishikawa, Kenji; Takeda, Keigo; Kondo, Hiroki; Oda, Osamu; Sekine, Makoto; Hori, Masaru

    2017-08-01

    Surface chemical reactions on the GaN surface with Cl radicals are thermally enhanced in the high-temperature Cl2 plasma etching of GaN, resulting in the formation of etch pits and thereby, a roughened surface. Simultaneous irradiation of ultraviolet (UV) photons in Cl2 plasma emissions with wavelengths of 258 and 306 nm reduces the surface chemical reactions because of the photodissociation of both Ga and N chlorides, which leads to a suppression of the increase in surface roughness. Compared with Si-related materials, we point out that photon-induced reactions should be taken into account during the plasma processing of wide-bandgap semiconductors.

  15. [Effect of hydrofluoric acid etching time on the resin bond durability of glass ceramic].

    PubMed

    Meng, Xiang-feng; Zhou, Xiao-lu; Luo, Xiao-ping

    2010-05-01

    To analyze the effect of hydrofluoric acid (HFA) etching time on the resin bond durability of glass ceramic. Three groups of samples of machinable glass ceramic (ProCAD) were etched by 4.8% HFA for 0, 30 and 60 s respectively. The roughness parameters (Ra, Sm, S) and surface area of the samples, were measured with a 3D-laser scanning microscope. Then the ceramic surfaces were bonded with four resin cements (silane coupler/resin cement), which were Monobond S/Variolink II, Clearfil Ceramic Primer/Clearfil Esthetic Cement, GC Ceramic Primer/Linkmax HV, and Porcelain Liner M/SuperBond. The micro-bond strengths between the ceramic and the resin were tested at baseline and after the samples had been treated in 30000 thermal cycles. The Ra [(3.89+/-1.94), (12.53+/-0.80), (13.58+/-1.10) microm] and surface area [(7.81+/-2.96), (30.18+/-2.05), (34.16+/-1.97) mm2] of ceramic increased with the increase of HFA etching time. The thermal cycling test reduced the bond strength of all test groups. The bond strength of Monobond S/Variolink II group [(3.59+/-3.51), (16.18+/-2.62), (20.33+/-2.45) MPa] and Clearfil Ceramic Primer/Clearfil Esthetic Cement group [(4.74+/-2.08), (7.77+/-1.55), (13.45+/-3.75) MPa] increased with the increase of HFA etching time; 30 s HFA etching group of Porcelain Liner M/SuperBond had higher bond strength [(22.00+/-1.64) MPa] than its 0 s HFA etching group [(12.96+/-4.17) MPa], and no significant difference was found between the 30 s and 60 s HFA etching groups of Porcelain Liner M/SuperBond [(20.42+/-3.01) MPa]. HFA etching time had no effect on the bond strength of GC Ceramic Primer/Linkmax HV. HFA etching can improve the resin bond durability of glass ceramic, and the etching time is not only related to the change of ceramic surface roughness and area, but also to the characteristics of resins.

  16. Anisotropic etching of silicon in solutions containing tensioactive compounds

    NASA Astrophysics Data System (ADS)

    Zubel, Irena

    2016-12-01

    The results of investigations concerning anisotropic etching in 3M KOH and 25% TMAH solutions modified by tensioactive compounds such as alcohols, diols and a typical surfactant Triton X100 have been compared. Etching anisotropy was assessed on the basis of etch rates ratio V(110)/V(100). It was stated that the relation between surface tension of the solutions and etch rates of particular planes depend not only on the kind of surfactant but also on the kind of etching solution (KOH, TMAH). It points out an important role of TMA+ ions in the etching process, probably in the process of forming an adsorption layer, consisting of the molecules of tensioactive compounds on Si surface, which decides about etch rate. We have observed that this phenomenon occurs only at high concentration of TMA+ ions (25% TMAH). Reduction of TMAH concentration changes the properties of surfactant containing TMAH solutions. From all investigated solutions, the solutions that assured developing of (110) plane inclined at the angle of 45° to (100) substrate were selected. Such planes can be used as micromirrors in MOEMS structures. The solutions provide the etch rate ratio V(110)/V(100)<0.7, thus they were selected from hydroxide solutions containing surfactants. A simple way for etch rate anisotropy V(110)/V(100) assessment based on microscopic images etched structures has been proposed.

  17. Fabrication of 3D surface structures using grayscale lithography

    NASA Astrophysics Data System (ADS)

    Stilson, Christopher; Pal, Rajan; Coutu, Ronald A.

    2014-03-01

    The ability to design and develop 3D microstructures is important for microelectromechanical systems (MEMS) fabrication. Previous techniques used to create 3D devices included tedious steps in direct writing and aligning patterns onto a substrate followed by multiple photolithography steps using expensive, customized equipment. Additionally, these techniques restricted batch processing and placed limits on achievable shapes. Gray-scale lithography enables the fabrication of a variety of shapes using a single photolithography step followed by reactive ion etching (RIE). Micromachining 3D silicon structures for MEMS can be accomplished using gray-scale lithography along with dry anisotropic etching. In this study, we investigated: using MATLAB for mask designs; feasibility of using 1 μm Heidelberg mask maker to direct write patterns onto photoresist; using RIE processing to etch patterns into a silicon substrate; and the ability to tailor etch selectivity for precise fabrication. To determine etch rates and to obtain desired etch selectivity, parameters such as gas mixture, gas flow, and electrode power were studied. This process successfully demonstrates the ability to use gray-scale lithography and RIE for use in the study of micro-contacts. These results were used to produce a known engineered non-planer surface for testing micro-contacts. Surface structures are between 5 μm and 20 μm wide with varying depths and slopes based on mask design and etch rate selectivity. The engineered surfaces will provide more insight into contact geometries and failure modes of fixed-fixed micro-contacts.

  18. Etch pit investigation of free electron concentration controlled 4H-SiC

    NASA Astrophysics Data System (ADS)

    Kim, Hong-Yeol; Shin, Yun Ji; Kim, Jung Gon; Harima, Hiroshi; Kim, Jihyun; Bahng, Wook

    2013-04-01

    Etch pits were investigated using the molten KOH selective etching method to examine dependence of etch pit shape and size on free electron concentration. The free electron concentrations of highly doped 4H-silicon carbide (SiC) were controlled by proton irradiation and thermal annealing, which was confirmed by a frequency shift in the LO-phonon-plasmon-coupled (LOPC) mode on micro-Raman spectroscopy. The proton irradiated sample with 5×1015 cm-2 fluence and an intrinsic semi-insulating sample showed clearly classified etch pits but different ratios of threading screw dislocation (TSD) and threading edge dislocation (TED) sizes. Easily classified TEDs and TSDs on proton irradiated 4H-SiC were restored as highly doped 4H-SiC after thermal annealing due to the recovered carrier concentrations. The etched surface of proton irradiated 4H-SiC and boron implanted SiC showed different surface conditions after activation.

  19. Comparative Evaluation of the Etching Pattern of Er,Cr:YSGG & Acid Etching on Extracted Human Teeth-An ESEM Analysis

    PubMed Central

    Mazumdar, Dibyendu; Ranjan, Shashi; Krishna, Naveen Kumar; Kole, Ravindra; Singh, Priyankar; Lakiang, Deirimika; Jayam, Chiranjeevi

    2016-01-01

    Introduction Etching of enamel and dentin surfaces increases the surface area of the substrate for better bonding of the tooth colored restorative materials. Acid etching is the most commonly used method. Recently, hard tissue lasers have been used for this purpose. Aim The aim of the present study was to evaluate and compare the etching pattern of Er,Cr:YSGG and conventional etching on extracted human enamel and dentin specimens. Materials and Methods Total 40 extracted non-diseased teeth were selected, 20 anterior and 20 posterior teeth each for enamel and dentin specimens respectively. The sectioned samples were polished by 400 grit Silicon Carbide (SiC) paper to a thickness of 1.0 ± 0.5 mm. The enamel and dentin specimens were grouped as: GrE1 & GrD1 as control specimens, GrE2 & GrD2 were acid etched and GrE3 & GrD3 were lased. Acid etching was done using Conditioner 36 (37 % phosphoric acid) according to manufacturer instructions. Laser etching was done using Er,Cr:YSGG (Erbium, Chromium : Ytrium Scandium Gallium Garnet) at power settings of 3W, air 70% and water 20%. After surface treatment with assigned agents the specimens were analyzed under ESEM (Environmental Scanning Electron Microscope) at X1000 and X5000 magnification. Results Chi Square and Student “t” statistical analysis was used to compare smear layer removal and etching patterns between GrE2-GrE3. GrD2 and GrD3 were compared for smear layer removal and diameter of dentinal tubule opening using the same statistical analysis. Chi-square test for removal of smear layer in any of the treated surfaces i.e., GrE2-E3 and GrD2-D3 did not differ significantly (p>0.05). While GrE2 showed predominantly type I etching pattern (Chi-square=2.78, 0.05

    0.10) and GrE3 showed type III etching (Chi-square=4.50, p<0.05). The tubule diameters were measured using GSA (Gesellschaft fur Softwareentwicklung und Analytik, Germany) image analyzer and the ‘t’ value of student ‘t’ test was 18.10 which was a highly significant result (p<.001). GrD2 had a mean dentinal tubule diameter of 2.78μm and GrD3 of 1.09μm. Conclusion The present study revealed type I etching pattern after acid etching, while type III etching pattern in enamel after laser etching. The lased dentin showed preferential removal of intertubular dentin while acid etching had more effect on the peritubular dentin. No significant differences was observed in removal of smear layer between the acid etched and lased groups. Although diameter of the exposed dentinal tubules was lesser after lased treatment in comparison to acid etching, further long term in vivo studies are needed with different parameters to establish the usage of Er,Cr:YSGG as a sole etching agent. PMID:27437337

  20. Impact of recess etching and surface treatments on ohmic contacts regrown by molecular-beam epitaxy for AlGaN/GaN high electron mobility transistors

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Joglekar, S.; Azize, M.; Palacios, T.

    Ohmic contacts fabricated by regrowth of n{sup +} GaN are favorable alternatives to metal-stack-based alloyed contacts in GaN-based high electron mobility transistors. In this paper, the influence of reactive ion dry etching prior to regrowth on the contact resistance in AlGaN/GaN devices is discussed. We demonstrate that the dry etch conditions modify the surface band bending, dangling bond density, and the sidewall depletion width, which influences the contact resistance of regrown contacts. The impact of chemical surface treatments performed prior to regrowth is also investigated. The sensitivity of the contact resistance to the surface treatments is found to depend uponmore » the dangling bond density of the sidewall facets exposed after dry etching. A theoretical model has been developed in order to explain the observed trends.« less

  1. Optical-diffraction method for determining crystal orientation

    DOEpatents

    Sopori, B.L.

    1982-05-07

    Disclosed is an optical diffraction technique for characterizing the three-dimensional orientation of a crystal sample. An arbitrary surface of the crystal sample is texture etched so as to generate a pseudo-periodic diffraction grating on the surface. A laser light beam is then directed onto the etched surface, and the reflected light forms a farfield diffraction pattern in reflection. Parameters of the diffraction pattern, such as the geometry and angular dispersion of the diffracted beam are then related to grating shape of the etched surface which is in turn related to crystal orientation. This technique may be used for examining polycrystalline silicon for use in solar cells.

  2. Cyclic etching of tin-doped indium oxide using hydrogen-induced modified layer

    NASA Astrophysics Data System (ADS)

    Hirata, Akiko; Fukasawa, Masanaga; Nagahata, Kazunori; Li, Hu; Karahashi, Kazuhiro; Hamaguchi, Satoshi; Tatsumi, Tetsuya

    2018-06-01

    The rate of etching of tin-doped indium oxide (ITO) and the effects of a hydrogen-induced modified layer on cyclic, multistep thin-layer etching were investigated. It was found that ITO cyclic etching is possible by precisely controlling the hydrogen-induced modified layer. Highly selective etching of ITO/SiO2 was also investigated, and it was suggested that cyclic etching by selective surface adsorption of Si can precisely control the etch rates of ITO and SiO2, resulting in an almost infinite selectivity for ITO over SiO2 and in improved profile controllability.

  3. Free-standing mesoporous carbon thin films with highly ordered pore architectures for nanodevices.

    PubMed

    Feng, Dan; Lv, Yingying; Wu, Zhangxiong; Dou, Yuqian; Han, Lu; Sun, Zhenkun; Xia, Yongyao; Zheng, Gengfeng; Zhao, Dongyuan

    2011-09-28

    We report for the first time the synthesis of free-standing mesoporous carbon films with highly ordered pore architecture by a simple coating-etching approach, which have an intact morphology with variable sizes as large as several square centimeters and a controllable thickness of 90 nm to ∼3 μm. The mesoporous carbon films were first synthesized by coating a resol precursors/Pluronic copolymer solution on a preoxidized silicon wafer and forming highly ordered polymeric mesostructures based on organic-organic self-assembly, followed by carbonizing at 600 °C and finally etching of the native oxide layer between the carbon film and the silicon substrate. The mesostructure of this free-standing carbon film is confirmed to be an ordered face-centered orthorhombic Fmmm structure, distorted from the (110) oriented body-centered cubic Im3̅m symmetry. The mesoporosity of the carbon films has been evaluated by nitrogen sorption, which shows a high specific BET surface area of 700 m(2)/g and large uniform mesopores of ∼4.3 nm. Both mesostructures and pore sizes can be tuned by changing the block copolymer templates or the ratio of resol to template. These free-standing mesoporous carbon films with cracking-free uniform morphology can be transferred or bent on different surfaces, especially with the aid of the soft polymer layer transfer technique, thus allowing for a variety of potential applications in electrochemistry and biomolecule separation. As a proof of concept, an electrochemical supercapacitor device directly made by the mesoporous carbon thin films shows a capacitance of 136 F/g at 0.5 A/g. Moreover, a nanofilter based on the carbon films has shown an excellent size-selective filtration of cytochrome c and bovine serum albumin.

  4. Amelogenin-assisted ex vivo remineralization of human enamel: effects of supersaturation degree and fluoride concentration

    PubMed Central

    Fan, Yuwei; Nelson, James R.; Alvarez, Jason R.; Hagan, Joseph; Berrier, Allison; Xu, Xiaoming

    2011-01-01

    The formation of organized nanocrystals that resemble enamel is crucial for successful enamel remineralization. Calcium, phosphate and fluoride ions and amelogenin are important ingredients for the formation of organized hydroxyapatite (HAP) crystals in vitro. However, the effects of these remineralization agents on the enamel crystal morphology have not been thoroughly studied. The objective of this study was to investigate the effects of fluoride ions, supersaturation degree and amelogenin on the crystal morphology and organization of ex vivo remineralized human enamel. Extracted third molars were sliced thin and acid-etched to provide the enamel surface for immersion in different remineralization solutions. The crystal morphology and mineral phase of the remineralized enamel surface were analyzed by FE-SEM, ATR-FTIR and XRD. The concentration of fluoride and supersaturation degree of hydroxyapatite had significant effects on the crystal morphology and crystal organization, which varied from plate-like loose crystals to rod-like densely packed nanocrystal arrays. Densely packed arrays of fluoridated hydroxyapatite nanorods were observed under the following conditions: σ(HAP) = 10.2±2.0 with fluoride 1.5±0.5 mg/L and amelogenin 40±10 µg/mL, pH 6.8±0.4. A phase diagram summarized the conditions that form dense or loose hydroxyapatite nanocrystal structures. This study provides the basis for the development of novel dental materials for caries management. PMID:21256987

  5. The improvement of adhesive properties of PEEK through different pre-treatments

    NASA Astrophysics Data System (ADS)

    Hallmann, Lubica; Mehl, Albert; Sereno, Nuno; Hämmerle, Christoph H. F.

    2012-07-01

    The purpose of this in vitro study was the evaluation of the bond strength of the adhesives/composite resin to Poly Ether Ether Ketone (PEEK) based dental polymer after using different surface conditioning methods. PEEK blanks were cut into discs. All disc specimens were polished with 800 grit SiC paper and divided into 6 main groups. Main groups were divided into 2 subgroups. The main groups of 32 specimens each were treated as follow: (1) control specimens (no treatment), (2) piranha solution etching, (3) abraded with 50 μm alumina particles and chemical etching, (4) abraded with 110 μm alumina particles and chemical etching, (5) abraded with 30 μm silica-coated alumina particles and chemical etching, (6) abraded with 110 μm silica-coated alumina particles and chemical etching. Plexiglas tubes filled with a composite resin (RelyX Unicem) were bonded to the specimens. The adhesives used were Heliobond and Clearfil Ceramic Primer. Each specimen was stored in distilled water (37 °C) for 3 days. Tensile bond strength was measured in a universal testing machine and failure methods were evaluated. Abraded surface with 50 μm alumina particles followed by etching with piranha solution lead to the highest bond strength of 21.4 MPa when Heliobond like adhesive was used. Tribochemical silica coated/etched PEEK surfaces did not have an effect on the bond strength. Non-treated PEEK surface was not able to establish a bond with composite resin. The proper choice of adhesive/composite resin system leads to a strong bond. ConclusionAirborne particle abrasion in combination with piranha solution etching improves the adhesive properties of PEEK.

  6. Comparing the shear bond strength of direct and indirect composite inlays in relation to different surface conditioning and curing techniques

    PubMed Central

    Zorba, Yahya Orcun; Ilday, Nurcan Ozakar; Bayındır, Yusuf Ziya; Demirbuga, Sezer

    2013-01-01

    Objective: The aim of this study was to test the null hypothesis that different surface conditioning (etch and rinse and self-etch) and curing techniques (light cure/dual cure) had no effect on the shear bond strength of direct and indirect composite inlays. Materials and Methods: A total of 112 extracted human molar teeth were horizontally sectioned and randomly divided into two groups according to restoration technique (direct and indirect restorations). Each group was further subdivided into seven subgroups (n = 8) according to bonding agent (etch and rinse adhesives Scotchbond multi-purpose plus, All-Bond 3, Adper Single Bond and Prime Bond NT; and self-etch adhesives Clearfil Liner Bond, Futurabond DC and G bond). Indirect composites were cemented to dentin surfaces using dual-curing luting cement. Shear bond strength of specimens was tested using a Universal Testing Machine. Two samples from each subgroup were evaluated under Scanning electron microscopy to see the failing modes. Data was analyzed using independent sample t-tests and Tukey's tests. Results: Surface conditioning and curing of bonding agents were all found to have significant effects on shear bond strength (P < 0.05) of both direct and indirect composite inlays. With direct restoration, etch and rinse systems and dual-cured bonding agents yielded higher bond strengths than indirect restoration, self-etch systems and light-cured bonding agents. Conclusions: The results of the present study indicated that direct restoration to be a more reliable method than indirect restoration. Although etch and rinse bonding systems showed higher shear bond strength to dentin than self-etch systems, both systems can be safely used for the adhesion of direct as well as indirect restorations. PMID:24932118

  7. Shear bond strength of composite bonded with three adhesives to Er,Cr:YSGG laser-prepared enamel.

    PubMed

    Türkmen, Cafer; Sazak-Oveçoğlu, Hesna; Günday, Mahir; Güngör, Gülşad; Durkan, Meral; Oksüz, Mustafa

    2010-06-01

    To assess in vitro the shear bond strength of a nanohybrid composite resin bonded with three adhesive systems to enamel surfaces prepared with acid and Er,Cr:YSGG laser etching. Sixty extracted caries- and restoration-free human maxillary central incisors were used. The teeth were sectioned 2 mm below the cementoenamel junction. The crowns were embedded in autopolymerizing acrylic resin with the labial surfaces facing up. The labial surfaces were prepared with 0.5-mm reduction to receive composite veneers. Thirty specimens were etched with Er,Cr:YSGG laser. This group was also divided into three subgroups, and the following three bonding systems were then applied on the laser groups and the other three unlased groups: (1) 37% phosphoric acid etch + Bond 1 primer/adhesive (Pentron); (2) Nano-bond self-etch primer (Pentron) + Nano-bond adhesive (Pentron); and (3) all-in-one adhesive-single dose (Futurabond NR, Voco). All of the groups were restored with a nanohybrid composite resin (Smile, Pentron). Shear bond strength was measured with a Zwick universal test device with a knife-edge loading head. The data were analyzed with two-factor ANOVA. There were no significant differences in shear bond strength between self-etch primer + adhesive and all-in-one adhesive systems for nonetched and laser-etched enamel groups (P > .05). However, bond strength values for the laser-etched + Bond 1 primer/adhesive group (48.00 +/- 13.86 MPa) were significantly higher than the 37% phosphoric acid + Bond 1 primer/adhesive group (38.95 +/- 20.07 MPa) (P < .05). The Er,Cr:YSGG laser-powered hydrokinetic system etched the enamel surface more effectively than 37% phosphoric acid for subsequent attachment of composite material.

  8. An evaluation of shear bond strength of self-etch adhesive on pre-etched enamel: an in vitro study.

    PubMed

    Rao, Bhadra; Reddy, Satti Narayana; Mujeeb, Abdul; Mehta, Kanchan; Saritha, G

    2013-11-01

    To determine the shear bond strength of self-etch adhesive G-bond on pre-etched enamel. Thirty caries free human mandibular premolars extracted for orthodontic purpose were used for the study. Occlusal surfaces of all the teeth were flattened with diamond bur and a silicon carbide paper was used for surface smoothening. The thirty samples were randomly grouped into three groups. Three different etch systems were used for the composite build up: group 1 (G-bond self-etch adhesive system), group 2 (G-bond) and group 3 (Adper single bond). Light cured was applied for 10 seconds with a LED unit for composite buildup on the occlusal surface of each tooth with 8 millimeters (mm) in diameter and 3 mm in thickness. The specimens in each group were tested in shear mode using a knife-edge testing apparatus in a universal testing machine across head speed of 1 mm/ minute. Shear bond strength values in Mpa were calculated from the peak load at failure divided by the specimen surface area. The mean shear bond strength of all the groups were calculated and statistical analysis was carried out using one-way Analysis of Variance (ANOVA). The mean bond strength of group 1 is 15.5 Mpa, group 2 is 19.5 Mpa and group 3 is 20.1 Mpa. Statistical analysis was carried out between the groups using one-way ANOVA. Group 1 showed statistically significant lower bond strength when compared to groups 2 and 3. No statistical significant difference between groups 2 and 3 (p < 0.05). Self-etch adhesive G-bond showed increase in shear bond strength on pre-etched enamel.

  9. Comparing the shear bond strength of direct and indirect composite inlays in relation to different surface conditioning and curing techniques.

    PubMed

    Zorba, Yahya Orcun; Ilday, Nurcan Ozakar; Bayındır, Yusuf Ziya; Demirbuga, Sezer

    2013-10-01

    The aim of this study was to test the null hypothesis that different surface conditioning (etch and rinse and self-etch) and curing techniques (light cure/dual cure) had no effect on the shear bond strength of direct and indirect composite inlays. A total of 112 extracted human molar teeth were horizontally sectioned and randomly divided into two groups according to restoration technique (direct and indirect restorations). Each group was further subdivided into seven subgroups (n = 8) according to bonding agent (etch and rinse adhesives Scotchbond multi-purpose plus, All-Bond 3, Adper Single Bond and Prime Bond NT; and self-etch adhesives Clearfil Liner Bond, Futurabond DC and G bond). Indirect composites were cemented to dentin surfaces using dual-curing luting cement. Shear bond strength of specimens was tested using a Universal Testing Machine. Two samples from each subgroup were evaluated under Scanning electron microscopy to see the failing modes. Data was analyzed using independent sample t-tests and Tukey's tests. Surface conditioning and curing of bonding agents were all found to have significant effects on shear bond strength (P < 0.05) of both direct and indirect composite inlays. With direct restoration, etch and rinse systems and dual-cured bonding agents yielded higher bond strengths than indirect restoration, self-etch systems and light-cured bonding agents. The results of the present study indicated that direct restoration to be a more reliable method than indirect restoration. Although etch and rinse bonding systems showed higher shear bond strength to dentin than self-etch systems, both systems can be safely used for the adhesion of direct as well as indirect restorations.

  10. Effect of bracket bonding with Er: YAG laser on nanomechanical properties of enamel

    PubMed Central

    Alavi, Shiva; Birang, Reza; Hajizadeh, Fatemeh; Banimostafaee, Hamed

    2014-01-01

    Background: The aim of this study was to compare the effects of conventional acid etching and laser etching on the nano-mechanical properties of the dental enamel using nano-indentation test. Materials and Methods: In this experimental in vitro study, buccal surfaces of 10 premolars were divided into three regions. One of the regions was etched with 37% phosphoric acid and another etched with Er:YAG laser, the third region was not etched. The brackets were bonded to both of etched regions. After thermocycling for 500 cycles, the brackets were removed and the teeth were decoronated from the bracket bonding area. Seven nano-indentations were applied at 1-31 μm depth from the enamel surface in each region. Mean values of the hardness and elastic modulus were analyzed with repeated measures analysis of variance and Tukey HSD tests, using the SPSS software (SPSS Inc., version16.0, Chicago, Il, USA). P < 0.05 was considered as significant. Results: The hardness up to 21 μm in depth and elastic modulus up to 6 μm in depth from the enamel surface for laser-etched enamel had significantly higher values than control enamel and the hardness up to 11 μm in depth and elastic modulus up to 6 μm in depth for acid-etched enamel had significantly lower values than the control enamel. Conclusion: The mechanical properties of the enamel were decreased after bracket bonding with conventional acid etching and increased after bonding with Er:YAG laser. PMID:24688560

  11. Enamel Deproteinization using Papacarie and 10% Papain Gel on Shear Bond Strength of Orthodontic Brackets Before and After Acid Etching.

    PubMed

    Agarwal, R M; Yeluri, R; Singh, C; Munshi, A K

    2015-01-01

    To suggest Papacarie(®) as a new deproteinizing agent in comparison with indigenously prepared 10% papain gel before and after acid etching that may enhance the quality of the bond between enamel surface and composite resin complex. One hundred and twenty five extracted human premolars were utilized and divided into five groups: In the group 1, enamel surface was etched and primer was applied. In group 2, treatment with papacarie(®) for 60 seconds followed by etching and primer application. In group 3, etching followed by treatment with papacarie(®) for 60 seconds and primer application. In group 4, treatment with 10% papain gel for 60 seconds followed by etching and primer application. In group 5, etching followed by treatment with 10% papain gel for 60 seconds and primer application . After bonding the brackets, the mechanical testing was performed using a Universal testing machine. The failure mode was analyzed using an adhesive remnant index. The etching patterns before and after application of papacarie(®) and 10% papain gel was also evaluated using SEM. The values obtained for shear bond strength were submitted to analysis of variance and Tukey test (p < 0.05). It was observed that group 2 and group 4 had the highest shear bond strength and was statistically significant from other groups (p=0.001). Regarding Adhesive remnant index no statistical difference was seen between the groups (p=0.538). Papacarie(®) or 10% papain gel can be used to deproteinize the enamel surface before acid etching to enhance the bond strength of orthodontic brackets.

  12. Large-scale and highly efficient synthesis of micro- and nano-fibers with controlled fiber morphology by centrifugal jet spinning for tissue regeneration

    NASA Astrophysics Data System (ADS)

    Ren, Liyun; Pandit, Vaibhav; Elkin, Joshua; Denman, Tyler; Cooper, James A.; Kotha, Shiva P.

    2013-02-01

    PLLA fibrous tissue scaffolds with controlled fiber nanoscale surface roughness are fabricated with a novel centrifugal jet spinning process. The centrifugal jet spinning technique is a highly efficient synthesis method for micron- to nano-sized fibers with a production rate up to 0.5 g min-1. During the centrifugal jet spinning process, a polymer solution jet is stretched by the centrifugal force of a rotating chamber. By engineering the rheological properties of the polymer solution, solvent evaporation rate and centrifugal force that are applied on the solution jet, polyvinylpyrrolidone (PVP) and poly(l-lactic acid) (PLLA) composite fibers with various diameters are fabricated. Viscosity measurements of polymer solutions allowed us to determine critical polymer chain entanglement limits that allow the generation of continuous fiber as opposed to beads or beaded fibers. Above a critical concentration at which polymer chains are partially or fully entangled, lower polymer concentrations and higher centrifugal forces resulted in thinner fibers. Etching of PVP from the PLLA-PVP composite fibers doped with increasing PVP concentrations yielded PLLA fibers with increasing nano-scale surface roughness and porosity, which increased the fiber hydrophilicity dramatically. Scanning electron micrographs of the etched composite fibers suggest that PVP and PLLA were co-contiguously phase separated within the composite fibers during spinning and nano-scale roughness features were created after the partial etching of PVP. To study the tissue regeneration efficacy of the engineered PLLA fiber matrix, human dermal fibroblasts are used to simulate partial skin graft. Fibers with increased PLLA surface roughness and porosity demonstrated a trend towards higher cell attachment and proliferation.PLLA fibrous tissue scaffolds with controlled fiber nanoscale surface roughness are fabricated with a novel centrifugal jet spinning process. The centrifugal jet spinning technique is a highly efficient synthesis method for micron- to nano-sized fibers with a production rate up to 0.5 g min-1. During the centrifugal jet spinning process, a polymer solution jet is stretched by the centrifugal force of a rotating chamber. By engineering the rheological properties of the polymer solution, solvent evaporation rate and centrifugal force that are applied on the solution jet, polyvinylpyrrolidone (PVP) and poly(l-lactic acid) (PLLA) composite fibers with various diameters are fabricated. Viscosity measurements of polymer solutions allowed us to determine critical polymer chain entanglement limits that allow the generation of continuous fiber as opposed to beads or beaded fibers. Above a critical concentration at which polymer chains are partially or fully entangled, lower polymer concentrations and higher centrifugal forces resulted in thinner fibers. Etching of PVP from the PLLA-PVP composite fibers doped with increasing PVP concentrations yielded PLLA fibers with increasing nano-scale surface roughness and porosity, which increased the fiber hydrophilicity dramatically. Scanning electron micrographs of the etched composite fibers suggest that PVP and PLLA were co-contiguously phase separated within the composite fibers during spinning and nano-scale roughness features were created after the partial etching of PVP. To study the tissue regeneration efficacy of the engineered PLLA fiber matrix, human dermal fibroblasts are used to simulate partial skin graft. Fibers with increased PLLA surface roughness and porosity demonstrated a trend towards higher cell attachment and proliferation. Electronic supplementary information (ESI) available. See DOI: 10.1039/c3nr33423f

  13. Influence of Si wafer thinning processes on (sub)surface defects

    NASA Astrophysics Data System (ADS)

    Inoue, Fumihiro; Jourdain, Anne; Peng, Lan; Phommahaxay, Alain; De Vos, Joeri; Rebibis, Kenneth June; Miller, Andy; Sleeckx, Erik; Beyne, Eric; Uedono, Akira

    2017-05-01

    Wafer-to-wafer three-dimensional (3D) integration with minimal Si thickness can produce interacting multiple devices with significantly scaled vertical interconnections. Realizing such a thin 3D structure, however, depends critically on the surface and subsurface of the remaining backside Si after the thinning processes. The Si (sub)surface after mechanical grinding has already been characterized fruitfully for a range of few dozen of μm. Here, we expand the characterization of Si (sub)surface to 5 μm thickness after thinning process on dielectric bonded wafers. The subsurface defects and damage layer were investigated after grinding, chemical mechanical polishing (CMP), wet etching and plasma dry etching. The (sub)surface defects were characterized using transmission microscopy, atomic force microscopy, and positron annihilation spectroscopy. Although grinding provides the fastest removal rate of Si, the surface roughness was not compatible with subsequent processing. Furthermore, mechanical damage such as dislocations and amorphous Si cannot be reduced regardless of Si thickness and thin wafer handling systems. The CMP after grinding showed excellent performance to remove this grinding damage, even though the removal amount is 1 μm. For the case of Si thinning towards 5 μm using grinding and CMP, the (sub)surface is atomic scale of roughness without vacancy. For the case of grinding + dry etch, vacancy defects were detected in subsurface around 0.5-2 μm. The finished surface after wet etch remains in the nm scale in the strain region. By inserting a CMP step in between grinding and dry etch it is possible to significantly reduce not only the roughness, but also the remaining vacancies at the subsurface. The surface of grinding + CMP + dry etching gives an equivalent mono vacancy result as to that of grinding + CMP. This combination of thinning processes allows development of extremely thin 3D integration devices with minimal roughness and vacancy surface.

  14. Low-damage direct patterning of silicon oxide mask by mechanical processing

    PubMed Central

    2014-01-01

    To realize the nanofabrication of silicon surfaces using atomic force microscopy (AFM), we investigated the etching of mechanically processed oxide masks using potassium hydroxide (KOH) solution. The dependence of the KOH solution etching rate on the load and scanning density of the mechanical pre-processing was evaluated. Particular load ranges were found to increase the etching rate, and the silicon etching rate also increased with removal of the natural oxide layer by diamond tip sliding. In contrast, the local oxide pattern formed (due to mechanochemical reaction of the silicon) by tip sliding at higher load was found to have higher etching resistance than that of unprocessed areas. The profile changes caused by the etching of the mechanically pre-processed areas with the KOH solution were also investigated. First, protuberances were processed by diamond tip sliding at lower and higher stresses than that of the shearing strength. Mechanical processing at low load and scanning density to remove the natural oxide layer was then performed. The KOH solution selectively etched the low load and scanning density processed area first and then etched the unprocessed silicon area. In contrast, the protuberances pre-processed at higher load were hardly etched. The etching resistance of plastic deformed layers was decreased, and their etching rate was increased because of surface damage induced by the pre-processing. These results show that etching depth can be controlled by controlling the etching time through natural oxide layer removal and mechanochemical oxide layer formation. These oxide layer removal and formation processes can be exploited to realize low-damage mask patterns. PMID:24948891

  15. Bond strength of one-step self-etch adhesives and their predecessors to ground versus unground enamel

    PubMed Central

    Yazici, A. Ruya; Yildirim, Zeren; Ertan, Atila; Ozgunaltay, Gül; Dayangac, Berrin; Antonson, Sibel A; Antonson, Donald E

    2012-01-01

    Objective The aim of this study was to compare the shear bond strength of several self-etch adhesives to their two-step predecessors to ground and unground enamel. Methods: Seventy-five extracted, non-carious human third molar teeth were selected for this study. The buccal surfaces of each tooth were mechanically ground to obtain flat enamel surfaces (ground enamel), while the lingual surfaces were left intact (unground enamel). The teeth were randomly divided into five groups according to the adhesive systems (n=15): one-step self-etch adhesive - Clearfil S3 Bond, its two-step predecessor - Clearfil SE Bond, one-step self-etch adhesive - AdheSE One, and its two-step predecessor - AdheSE, and a two-step etch-and-rinse adhesive - Adper Single Bond 2(control). After application of the adhesives to the buccal and lingual enamel surfaces of each tooth, a cylindrical capsule filled with a hybrid composite resin (TPH) was seated against the surfaces. The specimens were stored in distilled water at 37°C for 24 hours, followed by thermocy-cling (5°C–55°C/500 cycles). They were subjected to shear bond strength test in a universal testing machine at a crosshead speed of 1.0 mm/minute. The data were compared using a two-way ANOVA, followed by Bonferroni test at P<.05. Results: All adhesives exhibited statistically similar bond strengths to ground and unground enamel except for the etch-and-rinse adhesive that showed significantly higher bond strengths than the self-etch adhesives (P<.05). No significant differences in bond strength values were observed between ground and unground enamel for any of the adhesives tested (P=.17). Conclusion: Similar bond strengths to ground and unground enamel were achieved with one-step self-etch adhesives and their predecessors. Enamel preparation did not influence the bonding performance of the adhesives tested. PMID:22904656

  16. Bond strength of one-step self-etch adhesives and their predecessors to ground versus unground enamel.

    PubMed

    Yazici, A Ruya; Yildirim, Zeren; Ertan, Atila; Ozgunaltay, Gül; Dayangac, Berrin; Antonson, Sibel A; Antonson, Donald E

    2012-07-01

    The aim of this study was to compare the shear bond strength of several self-etch adhesives to their two-step predecessors to ground and unground enamel. Seventy-five extracted, non-carious human third molar teeth were selected for this study. The buccal surfaces of each tooth were mechanically ground to obtain flat enamel surfaces (ground enamel), while the lingual surfaces were left intact (unground enamel). The teeth were randomly divided into five groups according to the adhesive systems (n=15): one-step self-etch adhesive - Clearfil S3 Bond, its two-step predecessor - Clearfil SE Bond, one-step self-etch adhesive - AdheSE One, and its two-step predecessor - AdheSE, and a two-step etch-and-rinse adhesive - Adper Single Bond 2(control). After application of the adhesives to the buccal and lingual enamel surfaces of each tooth, a cylindrical capsule filled with a hybrid composite resin (TPH) was seated against the surfaces. The specimens were stored in distilled water at 37°C for 24 hours, followed by thermocy-cling (5°C-55°C/500 cycles). They were subjected to shear bond strength test in a universal testing machine at a crosshead speed of 1.0 mm/minute. The data were compared using a two-way ANOVA, followed by Bonferroni test at P<.05. All adhesives exhibited statistically similar bond strengths to ground and unground enamel except for the etch-and-rinse adhesive that showed significantly higher bond strengths than the self-etch adhesives (P<.05). No significant differences in bond strength values were observed between ground and unground enamel for any of the adhesives tested (P=.17). Similar bond strengths to ground and unground enamel were achieved with one-step self-etch adhesives and their predecessors. Enamel preparation did not influence the bonding performance of the adhesives tested.

  17. Thermal atomic layer etching of crystalline aluminum nitride using sequential, self-limiting hydrogen fluoride and Sn(acac){sub 2} reactions and enhancement by H{sub 2} and Ar plasmas

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Johnson, Nicholas R.; Sun, Huaxing; Sharma, Kashish

    2016-09-15

    Thermal atomic layer etching (ALE) of crystalline aluminum nitride (AlN) films was demonstrated using sequential, self-limiting reactions with hydrogen fluoride (HF) and tin(II) acetylacetonate [Sn(acac){sub 2}] as the reactants. Film thicknesses were monitored versus number of ALE reaction cycles at 275 °C using in situ spectroscopic ellipsometry (SE). A low etch rate of ∼0.07 Å/cycle was measured during etching of the first 40 Å of the film. This small etch rate corresponded with the AlO{sub x}N{sub y} layer on the AlN film. The etch rate then increased to ∼0.36 Å/cycle for the pure AlN films. In situ SE experiments established the HF and Sn(acac){submore » 2} exposures that were necessary for self-limiting surface reactions. In the proposed reaction mechanism for thermal AlN ALE, HF fluorinates the AlN film and produces an AlF{sub 3} layer on the surface. The metal precursor, Sn(acac){sub 2}, then accepts fluorine from the AlF{sub 3} layer and transfers an acac ligand to the AlF{sub 3} layer in a ligand-exchange reaction. The possible volatile etch products are SnF(acac) and either Al(acac){sub 3} or AlF(acac){sub 2}. Adding a H{sub 2} plasma exposure after each Sn(acac){sub 2} exposure dramatically increased the AlN etch rate from 0.36 to 1.96 Å/cycle. This enhanced etch rate is believed to result from the ability of the H{sub 2} plasma to remove acac surface species that may limit the AlN etch rate. The active agent from the H{sub 2} plasma is either hydrogen radicals or radiation. Adding an Ar plasma exposure after each Sn(acac){sub 2} exposure increased the AlN etch rate from 0.36 to 0.66 Å/cycle. This enhanced etch rate is attributed to either ions or radiation from the Ar plasma that may also lead to the desorption of acac surface species.« less

  18. Single clay sheets inside electrospun polymer nanofibers

    NASA Astrophysics Data System (ADS)

    Sun, Zhaohui

    2005-03-01

    Nanofibers were prepared from polymer solution with clay sheets by electrospinning. Plasma etching, as a well controlled process, was used to supply electrically excited gas molecules from a glow discharge. To reveal the structure and arrangement of clay layers in the polymer matrix, plasma etching was used to remove the polymer by controlled gasification to expose the clay sheets due to the difference in reactivity. The shape, flexibility, and orientation of clay sheets were studied by transmission and scanning electron microscopy. Additional quantitative information on size distribution and degree of exfoliation of clay sheets were obtained by analyzing electron micrograph of sample after plasma etching. Samples in various forms including fiber, film and bulk, were thinned by plasma etching. Morphology and dispersion of inorganic fillers were studied by electron microscopy.

  19. Effect of different surface treatments on roughness of IPS Empress 2 ceramic.

    PubMed

    Kara, Haluk Baris; Dilber, Erhan; Koc, Ozlem; Ozturk, A Nilgun; Bulbul, Mehmet

    2012-03-01

    The aim of this study was to evaluate the influence of different surface treatments (air abrasion, acid etching, laser irradiation) on the surface roughness of a lithium-disilicate-based core ceramic. A total of 40 discs of lithium disilicate-based core ceramic (IPS Empress 2; Ivoclar Vivadent, Schaan, Liechtenstein) were prepared (10 mm in diameter and 1 mm in thickness) according to the manufacturer's instructions. Specimens were divided into four groups (n = 10), and the following treatments were applied: air abrasion with alumina particles (50 μm), acid etching with 5% hydrofluoric acid, Nd:YAG laser irradiation (1 mm distance, 100 mJ, 20 Hz, 2 W) and Er:YAG laser irradiation (1 mm distance, 500 mJ, 20 Hz, 10 W). Following determination of surface roughness (R(a)) by profilometry, specimens were examined with atomic force microscopy. The data were analysed by one-way analysis of variance (ANOVA) and Tukey HSD test (α = 0.05). One-way ANOVA indicated that surface roughness following air abrasion was significantly different from the surface roughness following laser irradiation and acid etching (P < 0.001). The Tukey HSD test indicated that the air abrasion group had a significantly higher mean value of roughness (P < 0.05) than the other groups. No significant difference was found between the acid etching and laser irradiation (both Er:YAG and Nd:YAG) groups (P > 0.05). Air abrasion increased surface roughness of lithium disilicate-based core ceramic surfaces more effectively than acid-etching and laser irradiation.

  20. Enhanced in vitro biocompatibility of ultrafine-grained biomedical NiTi alloy with microporous surface

    NASA Astrophysics Data System (ADS)

    Zheng, C. Y.; Nie, F. L.; Zheng, Y. F.; Cheng, Y.; Wei, S. C.; Valiev, R. Z.

    2011-08-01

    Bulk ultrafine-grained Ni 50.8Ti 49.2 alloy (UFG-NiTi) was successfully fabricated by equal-channel angular pressing (ECAP) technique in the present study, and to further improve its surface biocompatibility, surface modification techniques including sandblasting, acid etching and alkali treatment were employed to produce either irregularly roughened surface or microporous surface or hierarchical porous surface with bioactivity. The effect of the above surface treatments on the surface roughness, wettability, corrosion behavior, ion release, apatite forming ability and cytocompatibility of UFG-NiTi alloy were systematically investigated with the coarse-grained NiTi alloy as control. The pitting corrosion potential ( Epit) was increased from 393 mV (SCE) to 704 mV (SCE) with sandblasting and further increased to 1539 mV (SCE) with following acid etching in HF/HNO 3 solution. All the above surface treatment increased the apatite forming ability of UFG-NiTi in varying degrees when soaked them in simulated body fluid (SBF). Meanwhile, both sandblasting and acid etching could promote the cytocompatibility for osteoblasts: sandblasting enhanced cell attachment and acid etching increased cell proliferation. The different corrosion behavior, apatite forming ability and cellular response of UFG-NiTi after different surface modifications are attributed to the topography and wettability of the resulting surface oxide layer.

  1. The research on conformal acid etching process of glass ceramic

    NASA Astrophysics Data System (ADS)

    Wang, Kepeng; Guo, Peiji

    2014-08-01

    A series of experiments have been done to explore the effect of different conditions on the hydrofluoric acid etching. The hydrofluoric acid was used to etch the glass ceramic called "ZERODUR", which is invented by SCHOTT in Germany. The glass ceramic was processed into cylindrical samples. The hydrofluoric acid etching was done in a plastic beaker. The concentration of hydrofluoric acid and the etching time were changed to measure the changes of geometric tolerance and I observed the surface using a microscope in order to find an appropriate condition of hydrofluoric acid etching.

  2. Influence of Etching Mode on Enamel Bond Durability of Universal Adhesive Systems.

    PubMed

    Suzuki, T; Takamizawa, T; Barkmeier, W W; Tsujimoto, A; Endo, H; Erickson, R L; Latta, M A; Miyazaki, M

    2016-01-01

    The purpose of this study was to determine the enamel bond durability of three universal adhesives in different etching modes through fatigue testing. The three universal adhesives used were Scotchbond Universal, Prime&Bond Elect universal dental adhesive, and All-Bond Universal light-cured dental adhesive. A single-step self-etch adhesive, Clearfil S 3 Bond Plus was used as a control. The shear bond strength (SBS) and shear fatigue strength (SFS) to human enamel were evaluated in total-etch mode and self-etch mode. A stainless steel metal ring with an internal diameter of 2.4 mm was used to bond the resin composite to the flat-ground (4000-grit) tooth surfaces for determination of both SBS and SFS. For each enamel surface treatment, 15 specimens were prepared for SBS and 30 specimens for SFS. The staircase method for fatigue testing was then used to determine the SFS of the resin composite bonded to the enamel using 10-Hz frequencies for 50,000 cycles or until failure occurred. Scanning electron microscopy was used to observe representative debonded specimen surfaces and the resin-enamel interfaces. A two-way analysis of variance and the Tukey post hoc test were used for analysis of the SBS data, whereas a modified t-test with Bonferroni correction was used for the SFS data. All adhesives in total-etch mode showed significantly higher SBS and SFS values than those in self-etch mode. Although All-Bond Universal in self-etch mode showed a significantly lower SBS value than the other adhesives, there was no significant difference in SFS values among the adhesives in this mode. All adhesives showed higher SFS:SBS ratios in total-etch mode than in self-etch mode. With regard to the adhesive systems used in this study, universal adhesives showed higher enamel bond strengths in total-etch mode. Although the influence of different etching modes on the enamel-bonding performance of universal adhesives was found to be dependent on the adhesive material, total-etch mode effectively increased the enamel bond strength and durability, as measured by fatigue testing.

  3. Nanoscale Ge fin etching using F- and Cl-based etchants for Ge-based multi-gate devices

    NASA Astrophysics Data System (ADS)

    Zhang, Bingxin; An, Xia; Li, Ming; Hao, Peilin; Zhang, Xing; Huang, Ru

    2018-04-01

    In this paper, nanoscale germanium (Ge) fin etching with inductively coupled plasma equipment with SF6/CHF3/Ar and Cl2/BCl3/Ar gas mixes are experimentally demonstrated. The impact of the gas ratio on etching induced Ge surface flatness, etch rate and sidewall steepness are comprehensively investigated and compared for these two kinds of etchants and the optimized gas ratio is provided. By using silicon oxide as a hard mask, nanoscale Ge fin with a flat surface and sharp sidewall is experimentally illustrated, which indicates great potential for use in nanoscale Ge-based multi-gate MOSFETs.

  4. Etching of semiconductor cubic crystals: Determination of the dissolution slowness surfaces

    NASA Astrophysics Data System (ADS)

    Tellier, C. R.

    1990-03-01

    Equations of the representative surface of dissolution slowness for cubic crystals are determined in the framework of a tensorial approach of the orientation-dependent etching process. The independent dissolution constants are deduced from symmetry considerations. Using previous data on the chemical etching of germanium and gallium arsenide crystals, some possible polar diagrams of the dissolution slowness are proposed. A numerical and graphical simulation method is used to obtain the derived dissolution shapes. The influence of extrema in the dissolution slowness on the successive dissolution shapes is also examined. A graphical construction of limiting shapes of etched crystals appears possible using the tensorial representation of the dissolution slowness.

  5. Rapid recipe formulation for plasma etching of new materials

    NASA Astrophysics Data System (ADS)

    Chopra, Meghali; Zhang, Zizhuo; Ekerdt, John; Bonnecaze, Roger T.

    2016-03-01

    A fast and inexpensive scheme for etch rate prediction using flexible continuum models and Bayesian statistics is demonstrated. Bulk etch rates of MgO are predicted using a steady-state model with volume-averaged plasma parameters and classical Langmuir surface kinetics. Plasma particle and surface kinetics are modeled within a global plasma framework using single component Metropolis Hastings methods and limited data. The accuracy of these predictions is evaluated with synthetic and experimental etch rate data for magnesium oxide in an ICP-RIE system. This approach is compared and superior to factorial models generated from JMP, a software package frequently employed for recipe creation and optimization.

  6. Acid-etching technique of non-decalcified bone samples for visualizing osteocyte-lacuno-canalicular network using scanning electron microscope.

    PubMed

    Lampi, Tiina; Dekker, Hannah; Ten Bruggenkate, Chris M; Schulten, Engelbert A J M; Mikkonen, Jopi J W; Koistinen, Arto; Kullaa, Arja M

    2018-01-01

    The aim of this study was to define the acid-etching technique for bone samples embedded in polymethyl metacrylate (PMMA) in order to visualize the osteocyte lacuno-canalicular network (LCN) for scanning electron microscopy (SEM). Human jaw bone tissue samples (N = 18) were collected from the study population consisting of patients having received dental implant surgery. After collection, the bone samples were fixed in 70% ethanol and non-decalcified samples embedded routinely into polymethyl metacrylate (PMMA). The PMMA embedded specimens were acid-etched in either 9 or 37% phosphoric acid (PA) and prepared for SEM for further analysis. PMMA embedded bone specimens acid-etched by 9% PA concentration accomplishes the most informative and favorable visualization of the LCN to be observed by SEM. Etching of PMMA embedded specimens is recommendable to start with 30 s or 40 s etching duration in order to find the proper etching duration for the samples examined. Visualizing osteocytes and LCN provides a tool to study bone structure that reflects changes in bone metabolism and diseases related to bone tissue. By proper etching protocol of non-decalcified and using scanning electron microscope it is possible to visualize the morphology of osteocytes and the network supporting vitality of bone tissue.

  7. Experimental visualization of the cathode layer in AC surface dielectric barrier discharge

    NASA Astrophysics Data System (ADS)

    Kim, Sang-You; Lho, Taihyeop; Chung, Kyu-Sun

    2018-06-01

    A narrow etched polyimide line at the bottom edge of a biased electrode (BE) and a non-etched dielectric surface near the biased electrode were observed in an atmospheric AC flexible surface dielectric barrier discharge of polyimide dielectric. These findings are attributed to the bombardment of positive oxygen ions on the bottom edge of the BE and the electron breakdown trajectory not contacting the polyimide surface following the electric field lines formed between the BE edge and the surface charge layer on the dielectric. The length of the non-etched dielectric surface during the first micro-discharge was observed as 22 μm. This occurred, regardless of three different operating durations, which is in good agreement with the length of the cathode layer according to Paschen's law.

  8. Flower-like Rh/Cu superhydrophobic coating via electrodeposition and its self-cleaning property

    NASA Astrophysics Data System (ADS)

    Zhao, N.; Lu, S. X.; Xu, W. G.; Cheng, X. L.

    2017-01-01

    Rh/Cu superhydrophobic coatings with textured flower-like dual micro-nano structures were fabricated on copper substrates via electrodesposition of Rh followed by annealing treatment. The scanning electron microscopy and X-ray diffraction pattern were conducted to analyse the morphology and chemical composition of the coating surfaces, respectively. The water drops exhibited a water contact angle of 168±1° and a sliding angle of 0±1° on the coating surfaces which were obtained by etching in concentrated hydrochloric acid and nitric acid, electrodeposited at -1.0 V for 30 min and annealing in an oven at 180°C for 60 min. The prepared superhydrophobic coatings showed excellent water repellence and self-cleaning property due to its extremely high water contact angle.

  9. Effect of surface etching and electrodeposition of copper on nitinol

    NASA Astrophysics Data System (ADS)

    Ramos-Moore, E.; Rosenkranz, A.; Matamala, L. F.; Videla, A.; Durán, A.; Ramos-Grez, J.

    2017-10-01

    Nitinol-based materials are very promising for medical and dental applications since those materials can combine shape memory, corrosion resistance, biocompatibility and antibacterial properties. In particular, surface modifications and coating deposition can be used to tailor and to unify those properties. We report preliminary results on the study of the effect of surface etching and electrodeposition of Copper on Nitinol using optical, chemical and thermal techniques. The results show that surface etching enhances the surface roughness of Nitinol, induces the formation of Copper-based compounds at the Nitinol-Copper interface, reduces the austenitic-martensitic transformations enthalpies and reduces the Copper coating roughness. Further studies are needed in order to highlight the influence of the electrodeposited Copper on the memory shape properties of NiTi.

  10. Method for surface treatment of a cadmium zinc telluride crystal

    DOEpatents

    James, Ralph; Burger, Arnold; Chen, Kuo-Tong; Chang, Henry

    1999-01-01

    A method for treatment of the surface of a CdZnTe (CZT) crystal that reduces surface roughness (increases surface planarity) and provides an oxide coating to reduce surface leakage currents and thereby, improve resolution. A two step process is disclosed, etching the surface of a CZT crystal with a solution of lactic acid and bromine in ethylene glycol, following the conventional bromine/methanol etch treatment, and after attachment of electrical contacts, oxidizing the CZT crystal surface.

  11. Effects of morphology parameters on anti-icing performance in superhydrophobic surfaces

    NASA Astrophysics Data System (ADS)

    Nguyen, Thanh-Binh; Park, Seungchul; Lim, Hyuneui

    2018-03-01

    In this paper, we report the contributions of actual ice-substrate contact area and nanopillar height to passive anti-icing performance in terms of adhesion force and freezing time. Well-textured nanopillars with various parameters were fabricated via colloidal lithography and a dry etching process. The nanostructured quartz surface was coated with low-energy material to confer water-repellent properties. These superhydrophobic surfaces were investigated to determine the parameters essential for reducing adhesion strength and delaying freezing time. A well-textured surface with nanopillars of very small top diameter, regardless of height, could reduce adhesion force and delay freezing time in a subsequent de-icing process. Small top diameters of nanopillars also ensured the metastable Cassie-Baxter state based on energy barrier calculations. The results demonstrated the important role of areal fraction in anti-icing efficiency, and the negligible contribution of texture height. This insight into icing phenomena should lead to design of improved ice-phobic surfaces in the future.

  12. Method for forming suspended micromechanical structures

    DOEpatents

    Fleming, James G.

    2000-01-01

    A micromachining method is disclosed for forming a suspended micromechanical structure from {111} crystalline silicon. The micromachining method is based on the use of anisotropic dry etching to define lateral features of the structure which are etched down into a {111}-silicon substrate to a first etch depth, thereby forming sidewalls of the structure. The sidewalls are then coated with a protection layer, and the substrate is dry etched to a second etch depth to define a spacing of the structure from the substrate. A selective anisotropic wet etchant (e.g. KOH, EDP, TMAH, NaOH or CsOH) is used to laterally undercut the structure between the first and second etch depths, thereby forming a substantially planar lower surface of the structure along a {111} crystal plane that is parallel to an upper surface of the structure. The lateral extent of undercutting by the wet etchant is controlled and effectively terminated by either timing the etching, by the location of angled {111}-silicon planes or by the locations of preformed etch-stops. This present method allows the formation of suspended micromechanical structures having large vertical dimensions and large masses while allowing for detailed lateral features which can be provided by dry etch definition. Additionally, the method of the present invention is compatible with the formation of electronic circuitry on the substrate.

  13. Methods for improving the damage performance of fused silica polished by magnetorheological finishing

    DOE PAGES

    Kafka, Kyle R. P.; Hoffman, Brittany N.; Papernov, Semyon; ...

    2017-12-11

    The laser-induced damage threshold of fused-silica samples processed via magnetorheological finishing is investigated for polishing compounds depending on the type of abrasive material and the post-polishing surface roughness. The effectiveness of laser conditioning is examined using a ramped pre-exposure with the same 351-nm, 3-ns Gaussian pulses. Lastly, we examine chemical etching of the surface and correlate the resulting damage threshold to the etching protocol. A combination of etching and laser conditioning is found to improve the damage threshold by a factor of ~3, while maintaining <1-nm surface roughness.

  14. Methods for improving the damage performance of fused silica polished by magnetorheological finishing

    NASA Astrophysics Data System (ADS)

    Kafka, K. R. P.; Hoffman, B.; Papernov, S.; DeMarco, M. A.; Hall, C.; Marshall, K. L.; Demos, S. G.

    2017-12-01

    The laser-induced damage threshold of fused-silica samples processed via magnetorheological finishing is investigated for polishing compounds depending on the type of abrasive material and the post-polishing surface roughness. The effectiveness of laser conditioning is examined using a ramped pre-exposure with the same 351-nm, 3-ns Gaussian pulses. Finally, we examine chemical etching of the surface and correlate the resulting damage threshold to the etching protocol. A combination of etching and laser conditioning is found to improve the damage threshold by a factor of 3, while maintaining <1-nm surface roughness.

  15. A Twice Electrochemical-Etching Method to Fabricate Superhydrophobic-Superhydrophilic Patterns for Biomimetic Fog Harvest.

    PubMed

    Yang, Xiaolong; Song, Jinlong; Liu, Junkai; Liu, Xin; Jin, Zhuji

    2017-08-18

    Superhydrophobic-superhydrophilic patterned surfaces have attracted more and more attention due to their great potential applications in the fog harvest process. In this work, we developed a simple and universal electrochemical-etching method to fabricate the superhydrophobic-superhydrophilic patterned surface on metal superhydrophobic substrates. The anti-electrochemical corrosion property of superhydrophobic substrates and the dependence of electrochemical etching potential on the wettability of the fabricated dimples were investigated on Al samples. Results showed that high etching potential was beneficial for efficiently producing a uniform superhydrophilic dimple. Fabrication of long-term superhydrophilic dimples on the Al superhydrophobic substrate was achieved by combining the masked electrochemical etching and boiling-water immersion methods. A long-term wedge-shaped superhydrophilic dimple array was fabricated on a superhydrophobic surface. The fog harvest test showed that the surface with a wedge-shaped pattern array had high water collection efficiency. Condensing water on the pattern was easy to converge and depart due to the internal Laplace pressure gradient of the liquid and the contact angle hysteresis contrast on the surface. The Furmidge equation was applied to explain the droplet departing mechanism and to control the departing volume. The fabrication technique and research of the fog harvest process may guide the design of new water collection devices.

  16. Beam Simulation Studies of Plasma-Surface Interactions in Fluorocarbon Etching of Silicon and Silicon Dioxide

    NASA Astrophysics Data System (ADS)

    Gray, David C.

    1992-01-01

    A molecular beam apparatus has been constructed which allows the synthesis of dominant species fluxes to a wafer surface during fluorocarbon plasma etching. These species include atomic F as the primary etchant, CF _2 as a potential polymer forming precursor, and Ar^{+} or CF _{rm x}^{+} type ions. Ionic and neutral fluxes employed are within an order of magnitude of those typical of fluorocarbon plasmas and are well characterized through the use of in -situ probes. Etching yields and product distributions have been measured through the use of in-situ laser interferometry and line-of-sight mass spectrometry. XPS studies of etched surfaces were performed to assess surface chemical bonding states and average surface stoichiometry. A useful design guide was developed which allows optimal design of straight -tube molecular beam dosers in the collisionally-opaque regime. Ion-enhanced surface reaction kinetics have been studied as a function of the independently variable fluxes of free radicals and ions, as well as ion energy and substrate temperature. We have investigated the role of Ar ^{+} ions in enhancing the chemistries of F and CF_2 separately, and in combination on undoped silicon and silicon dioxide surfaces. We have employed both reactive and inert ions in the energy range most relevant to plasma etching processes, 20-500 eV, through the use of Kaufman and ECR type ion sources. The effect of increasing ion energy on the etching of fluorine saturated silicon and silicon dioxide surfaces was quantified through extensions of available low energy physical sputtering theory. Simple "site"-occupation models were developed for the quantification of the ion-enhanced fluorine etching kinetics in these systems. These models are suitable for use in topography evolution simulators (e.g. SAMPLE) for the predictive modeling of profile evolution in non-depositing fluorine-based plasmas such as NF_3 and SF_6. (Copies available exclusively from MIT Libraries, Rm. 14-0551, Cambridge, MA 02139-4307. Ph. 617 -253-5668; Fax 617-253-1690.) (Abstract shortened with permission of school.).

  17. Synthesis of Dispersible Mesoporous Nitrogen-Doped Hollow Carbon Nanoplates with Uniform Hexagonal Morphologies for Supercapacitors.

    PubMed

    Cao, Jie; Jafta, Charl J; Gong, Jiang; Ran, Qidi; Lin, Xianzhong; Félix, Roberto; Wilks, Regan G; Bär, Marcus; Yuan, Jiayin; Ballauff, Matthias; Lu, Yan

    2016-11-02

    In this study, dispersible mesoporous nitrogen-doped hollow carbon nanoplates have been synthesized as a new anisotropic carbon nanostructure using gibbsite nanoplates as templates. The gibbsite-silica core-shell nanoplates were first prepared before the gibbsite core was etched away. Dopamine as carbon precursor was self-polymerized on the hollow silica nanoplates surface assisted by sonification, which not only favors a homogeneous polymer coating on the nanoplates but also prevents their aggregation during the polymerization. Individual silica-polydopamine core-shell nanoplates were immobilized in a silica gel in an insulated state via a silica nanocasting technique. After pyrolysis in a nanoconfine environment and elimination of silica, discrete and dispersible hollow carbon nanoplates are obtained. The resulted hollow carbon nanoplates bear uniform hexagonal morphology with specific surface area of 460 m 2 ·g -1 and fairly accessible small mesopores (∼3.8 nm). They show excellent colloidal stability in aqueous media and are applied as electrode materials for symmetric supercapacitors. When using polyvinylimidazolium-based nanoparticles as a binder in electrodes, the hollow carbon nanoplates present superior performance in parallel to polyvinylidene fluoride (PVDF) binder.

  18. High-temperature morphological evolution of lithographically introduced cavities in silicon carbide

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Narushima, Takayuki; Glaeser, Andreas M.

    2000-12-01

    Internal cavities of controlled geometry and crystallography were introduced in 6H silicon carbide single crystals by combining lithographic methods, ion beam etching, and solid-state diffusion bonding. The morphological evolution of these internal cavities (negative crystals) in response to anneals of up to 128 h duration at 1900 degrees C was examined using optical microscopy. Surface energy anisotropy and faceting have a strong influence on both the geometric and kinetic characteristics of evolution. Decomposition of 12{bar 1}0 cavity edges into 101{bar 0} facets was observed after 16 h anneals, indicating that 12{bar 1}0 faces are not components of the Wulff shape.more » The shape evolution kinetics of penny-shaped cavities were also investigated. Experimentally observed evolution rates decreased much more rapidly with those predicted by a model in which surface diffusion is assumed to be rate-limiting. This suggests that the development of facets, and the associated loss of ledges and terraces during the initial stages of evolution results in an evolution process limited by the nucleation rate of attachment/detachment sites (ledges) on the facets.« less

  19. Comparative evaluation of surface topography of tooth prepared using erbium, chromium: Yttrium, scandium, gallium, garnet laser and bur and its clinical implications.

    PubMed

    Verma, Mahesh; Kumari, Pooja; Gupta, Rekha; Gill, Shubhra; Gupta, Ankur

    2015-01-01

    Erbium, chromium: Yttrium, scandium, gallium, garnet (Er, Cr: YSGG) laser has been successfully used in the ablation of dental hard and soft tissues. It has been reported that this system is also useful for preparing tooth surfaces and etching, but no consensus exist in the literature regarding the advantage of lasers over conventional tooth preparation technique. Labial surfaces of 25 extracted human maxillary central incisors were divided into two halves. Right half was prepared with diamond bur and left half with Er, Cr; YSGG laser and a reduction of 0.3-0.5 mm was carried out. Topography of prepared surfaces of five teeth were examined under scanning electron microscope (SEM). The remaining samples were divided into 4 groups of 10 specimens each based on the surface treatment received: One group was acid etched and other was nonetched. Composite resin cylinders were bonded on prepared surfaces and shear bond strength was assessed using a universal testing machine. The SEM observation revealed that the laser prepared surfaces were clean, highly irregular and devoid of a smear layer. Bur prepared surfaces were relatively smooth but covered with smear layer. Highest bond strength was shown by laser prepared acid etched group, followed by bur prepared the acid etched group. The bur prepared nonacid etched group showed least bond strength. Er, Cr: YSGG laser can be used for preparing tooth and bond strength value achieved by laser preparation alone without surface treatment procedure lies in the range of clinical acceptability.

  20. On the influence of etch pits in the overall dissolution rate of apatite basal sections

    NASA Astrophysics Data System (ADS)

    Alencar, Igor; Guedes, Sandro; Palissari, Rosane; Hadler, Julio C.

    2015-09-01

    Determination of efficiencies for particle detection plays a central role for proper estimation of reaction rates. If chemical etching is employed in the revelation of latent particle tracks in solid-state detectors, dissolution rates and etchable lengths are important factors governing the revelation and observation. In this work, the mask method, where a reference part of the sample is protected during dissolution, was employed to measure step heights in basal sections of apatite etched with a nitric acid, HNO, solution at a concentration of 1.1 M and a temperature of 20 °C. We show a drastic increase in the etching velocity as the number of etch pits in the surface augments, in accordance with the dissolution stepwave model, where the outcrop of each etch pit generates a continuous sequence of stepwaves. The number of etch pits was varied by irradiation with neutrons and perpendicularly incident heavy ions. The size dependence of the etch-pit opening with etching duration for ion (200-300 MeV 152Sm and 238U) tracks was also investigated. There is no distinction for the etch pits between the different ions, and the dissolution seems to be governed by the opening velocity when a high number of etch pits are present in the surface. Measurements of the etchable lengths of these ion tracks show an increase in these lengths when samples are not pre-annealed before irradiation. We discuss the implications of these findings for fission-track modelling.

  1. Smoothing single-crystalline SiC surfaces by reactive ion etching using pure NF{sub 3} and NF{sub 3}/Ar mixture gas plasmas

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Tasaka, Akimasa, E-mail: aki-tasaka-load@yahoo.co.jp; Kotaka, Yuki; Oda, Atsushi

    2014-09-01

    In pure NF{sub 3} plasma, the etching rates of four kinds of single-crystalline SiC wafer etched at NF{sub 3} pressure of 2 Pa were the highest and it decreased with an increase in NF{sub 3} pressure. On the other hand, they increased with an increase in radio frequency (RF) power and were the highest at RF power of 200 W. A smooth surface was obtained on the single-crystalline 4H-SiC after reactive ion etching at NF{sub 3}/Ar gas pressure of 2 Pa and addition of Ar to NF{sub 3} plasma increased the smoothness of SiC surface. Scanning electron microscopy observation revealed that the numbermore » of pillars decreased with an increase in the Ar-concentration in the NF{sub 3}/Ar mixture gas. The roughness factor (R{sub a}) values were decreased from 51.5 nm to 25.5 nm for the As-cut SiC, from 0.25 nm to 0.20 nm for the Epi-SiC, from 5.0 nm to 0.7 nm for the Si-face mirror-polished SiC, and from 0.20 nm to 0.16 nm for the C-face mirror-polished SiC by adding 60% Ar to the NF{sub 3} gas. Both the R{sub a} values of the Epi- and the C-face mirror-polished wafer surfaces etched using the NF{sub 3}/Ar (40:60) plasma were similar to that treated with mirror polishing, so-called the Catalyst-Referred Etching (CARE) method, with which the lowest roughness of surface was obtained among the chemical mirror polishing methods. Etching duration for smoothing the single-crystalline SiC surface using its treatment was one third of that with the CARE method.« less

  2. Does active application of universal adhesives to enamel in self-etch mode improve their performance?

    PubMed

    Loguercio, Alessandro D; Muñoz, Miguel Angel; Luque-Martinez, Issis; Hass, Viviane; Reis, Alessandra; Perdigão, Jorge

    2015-09-01

    To evaluate the effect of adhesion strategy on the enamel microshear bond strengths (μSBS), etching pattern, and in situ degree of conversion (DC) of seven universal adhesives. 84 extracted third molars were sectioned in four parts (buccal, lingual, proximal) and divided into 21 groups, according to the combination of the main factors adhesive (AdheSE Universal [ADU], All-Bond Universal [ABU], Clearfil Universal [CFU], Futurabond U [FBU], G-Bond Plus [GBP], Prime&Bond Elect (PBE), and Scotchbond Universal Adhesive [SBU]), and adhesion strategy (etch-and-rinse, active self-etch, and passive self-etch). Specimens were stored in water (37°C/24h) and tested at 1.0mm/min (μSBS). Enamel-resin interfaces were evaluated for DC using micro-Raman spectroscopy. The enamel-etching pattern was evaluated under a field-emission scanning electron microscope (direct and replica techniques). Data were analyzed with two-way ANOVA and Tukey's test (α=0.05). Active self-etch application increased μSBS and DC for five out of the seven universal adhesives when compared to passive application (p<0.001). A deeper enamel-etching pattern was observed for all universal adhesives in the etch-and-rinse strategy. A slight improvement in etching ability was observed in active self-etch application compared to that of passive self-etch application. Replicas of GBP and PBE applied in active self-etch mode displayed morphological features compatible with water droplets. The DC of GBP and PBE were not affected by the application/strategy mode. In light of the improved performance of universal adhesives when applied actively in SE mode, selective enamel etching with phosphoric acid may not be crucial for their adhesion to enamel. The active application of universal adhesives in self-etch mode may be a practical alternative to enamel etching in specific clinical situations. Copyright © 2015 Elsevier Ltd. All rights reserved.

  3. Comparative evaluation of self-etching primers and phosphoric acid effectiveness on composite to enamel bond: an in vitro study.

    PubMed

    Patil, Basanagouda S; Rao, Bk Raghavendra; Sharathchandra, Sm; Hegde, Reshma; Kumar, G Vinay

    2013-09-01

    The aim of the present study was to investigate the effectiveness of the one total-etch self-priming adhesive, one two-step self-etching primer adhesive, and one 'all-in-one' self-etching adhesive system on the adhesion of a resin composite to enamel. Thirty-six freshly extracted human mandibular molars were selected for this study. A fat area about 5 mm in diameter was created on the exposed mesial surface of enamel of each tooth by moist grinding with 320, 420 and 600 grit silicon carbide paper. Twelve teeth were randomly assigned into three groups. In group 1, Adper Easy One (3M ESPE), a one step self-etching primer adhesive was applied and light curing unit for 10 seconds. In group 2, Adper SE Plus, a two-step self-etching primer with bottle A containing the aqueous primer and bottle B containing the acidic adhesive was applied and light cured for 10 seconds. Group 3 (control)-etchant 37% phosphoric acid is applied to the surface for 15 seconds and rinsed with water and air dried and adhesive (single bond 2) is applied to the surface and tube is placed and light cured for 20 seconds. Composite material (Z350) was placed in the tube and light cured for 40 seconds in all the groups. Bond strength testing was done using universal testing machine at the enamel-composite interface. The debonded enamel surface was evaluated in stereomicroscope to assess the cohesive, adhesive or mixed fracture. Data was statistically analyzed by one way analysis of variance (ANOVA). Group 1 performed least among all groups with a mean score of 19.46 MPa. Group 2 had a mean score of 25.67 MPa. Group 3 had a mean score of 27.16 MPa. Under the conditions of this in vitro study, the bond strength values of the two-step self-etching primer systems tested were similar to the total-etch. And, one step self-etching primers have lower bond strength compared to the total-etch.

  4. Topology assisted self-organization of colloidal nanoparticles: application to 2D large-scale nanomastering.

    PubMed

    Kadiri, Hind; Kostcheev, Serguei; Turover, Daniel; Salas-Montiel, Rafael; Nomenyo, Komla; Gokarna, Anisha; Lerondel, Gilles

    2014-01-01

    Our aim was to elaborate a novel method for fully controllable large-scale nanopatterning. We investigated the influence of the surface topology, i.e., a pre-pattern of hydrogen silsesquioxane (HSQ) posts, on the self-organization of polystyrene beads (PS) dispersed over a large surface. Depending on the post size and spacing, long-range ordering of self-organized polystyrene beads is observed wherein guide posts were used leading to single crystal structure. Topology assisted self-organization has proved to be one of the solutions to obtain large-scale ordering. Besides post size and spacing, the colloidal concentration and the nature of solvent were found to have a significant effect on the self-organization of the PS beads. Scanning electron microscope and associated Fourier transform analysis were used to characterize the morphology of the ordered surfaces. Finally, the production of silicon molds is demonstrated by using the beads as a template for dry etching.

  5. Tunable laser interference lithography preparation of plasmonic nanoparticle arrays tailored for SERS.

    PubMed

    Gisbert Quilis, Nestor; Lequeux, Médéric; Venugopalan, Priyamvada; Khan, Imran; Knoll, Wolfgang; Boujday, Souhir; Lamy de la Chapelle, Marc; Dostalek, Jakub

    2018-05-23

    The facile preparation of arrays of plasmonic nanoparticles over a square centimeter surface area is reported. The developed method relies on tailored laser interference lithography (LIL) that is combined with dry etching and it offers means for the rapid fabrication of periodic arrays of metallic nanostructures with well controlled morphology. Adjusting the parameters of the LIL process allows for the preparation of arrays of nanoparticles with a diameter below hundred nanometers independently of their lattice spacing. Gold nanoparticle arrays were precisely engineered to support localized surface plasmon resonance (LSPR) with different damping at desired wavelengths in the visible and near infrared part of the spectrum. The applicability of these substrates for surface enhanced Raman scattering is demonstrated where cost-effective, uniform and reproducible substrates are of paramount importance. The role of deviations in the spectral position and the width of the LSPR band affected by slight variations of plasmonic nanostructures is discussed.

  6. Mechanism of wiggling enhancement due to HBr gas addition during amorphous carbon etching

    NASA Astrophysics Data System (ADS)

    Kofuji, Naoyuki; Ishimura, Hiroaki; Kobayashi, Hitoshi; Une, Satoshi

    2015-06-01

    The effect of gas chemistry during etching of an amorphous carbon layer (ACL) on wiggling has been investigated, focusing especially on the changes in residual stress. Although the HBr gas addition reduces critical dimension loss, it enhances the surface stress and therefore increases wiggling. Attenuated total reflectance Fourier transform infrared spectroscopy revealed that the increase in surface stress was caused by hydrogenation of the ACL surface with hydrogen radicals. Three-dimensional (3D) nonlinear finite element method analysis confirmed that the increase in surface stress is large enough to cause the wiggling. These results also suggest that etching with hydrogen compound gases using an ACL mask has high potential to cause the wiggling.

  7. Multi-Functional, Micro Electromechanical Silicon Carbide Accelerometer

    NASA Technical Reports Server (NTRS)

    Okojie, Robert S. (Inventor)

    2004-01-01

    A method of bulk manufacturing SiC sensors is disclosed and claimed. Materials other than SiC may be used as the substrate material. Sensors requiring that the SiC substrate be pierced are also disclosed and claimed. A process flow reversal is employed whereby the metallization is applied first before the recesses are etched into or through the wafer. Aluminum is deposited on the entire planar surface of the metallization. Photoresist is spun onto the substantially planar surface of the Aluminum which is subsequently masked (and developed and removed). Unwanted Aluminum is etched with aqueous TMAH and subsequently the metallization is dry etched. Photoresist is spun onto the still substantially planar surface of Aluminum and oxide and then masked (and developed and removed) leaving the unimidized photoresist behind. Next, ITO is applied over the still substantially planar surface of Aluminum, oxide and unimidized photoresist. Unimidized and exposed photoresist and ITO directly above it are removed with Acetone. Next, deep reactive ion etching attacks exposed oxide not protected by ITO. Finally, hot phosphoric acid removes the Al and ITO enabling wires to connect with the metallization. The back side of the SiS wafer may be also etched.

  8. Multi-functional micro electromechanical devices and method of bulk manufacturing same

    NASA Technical Reports Server (NTRS)

    Okojie, Robert S. (Inventor)

    2004-01-01

    A method of bulk manufacturing SiC sensors is disclosed and claimed. Materials other than SiC may be used as the substrate material. Sensors requiring that the SiC substrate be pierced are also disclosed and claimed. A process flow reversal is employed whereby the metallization is applied first before the recesses are etched into or through the wafer. Aluminum is deposited on the entire planar surface of the metallization. Photoresist is spun onto the substantially planar surface of the Aluminum which is subsequently masked (and developed and removed). Unwanted Aluminum is etched with aqueous TMAH and subsequently the metallization is dry etched. Photoresist is spun onto the still substantially planar surface of Aluminum and oxide and then masked (and developed and removed) leaving the unimidized photoresist behind. Next, ITO is applied over the still substantially planar surface of Aluminum, oxide and unimidized photoresist. Unimidized and exposed photoresist and ITO directly above it are removed with Acetone. Next, deep reactive ion etching attacks exposed oxide not protected by ITO. Finally, hot phosphoric acid removes the Al and ITO enabling wires to connect with the metallization. The back side of the SiC wafer may be also be etched.

  9. Self-terminated etching of GaN with a high selectivity over AlGaN under inductively coupled Cl2/N2/O2 plasma with a low-energy ion bombardment

    NASA Astrophysics Data System (ADS)

    Zhong, Yaozong; Zhou, Yu; Gao, Hongwei; Dai, Shujun; He, Junlei; Feng, Meixin; Sun, Qian; Zhang, Jijun; Zhao, Yanfei; DingSun, An; Yang, Hui

    2017-10-01

    Etching of GaN/AlGaN heterostructure by O-containing inductively coupled Cl2/N2 plasma with a low-energy ion bombardment can be self-terminated at the surface of the AlGaN layer. The estimated etching rates of GaN and AlGaN were 42 and 0.6 nm/min, respectively, giving a selective etching ratio of 70:1. To study the mechanism of the etching self-termination, detailed characterization and analyses were carried out, including X-ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectroscopy (TOF-SIMS). It was found that in the presence of oxygen, the top surface of the AlGaN layer was converted into a thin film of (Al,Ga)Ox with a high bonding energy, which effectively prevented the underlying atoms from a further etching, resulting in a nearly self-terminated etching. This technique enables a uniform and reproducible fabrication process for enhancement-mode high electron mobility transistors with a p-GaN gate.

  10. Pulsed laser micro-scribing of copper thin films on polyimide substrate in NaCl solution

    NASA Astrophysics Data System (ADS)

    Shiby, Sooraj; Nammi, Srinagalakshmi; Vasa, Nilesh J.; Krishnan, Sivarama

    2018-02-01

    Recently, there is an increasing interest to create micro-channels on metal thin films for diverse applications, such as biomedical, micro channel heat exchangers, chemical separation processes and microwave antenna. Nanosecond (ns) Nd3+:YAG laser has been studied for generating micro-channels on Cu thin film (35 μm) deposited on polyimide substrate (50 μm). A pulsed Nd3+:YAG laser (532 nm / 355 nm) based scribing was performed in air and water ambiancePlasma shielding phenomenon is observed to influence the depth of microchannel at higher energies. A novel pump-probe experiment has been conducted for verifying the plasma shielding effect in air. In underwater scribing the recast layer was reduced significantly as compared to that in air. Laser scribing of Cu thin film followed by chemical etching using FeCl3 was studied. However, the approach of chemical etching resulted in undercut and thinning of Cu film. Alternatively, laser material processing in NaCl solution was studied. Cl- ions present in the solution reacts with Cu which is removed from the sample via laser ablation and forms CuCl2. Formation of CuCl2 in turn improved the surface morphology of the channel through localized etching. The surface roughness parameter Ra was less than 400 nm for NaCl solution based scribing which is smaller compared to air and underwater based methods which are typically around 800 nm or above. Preliminary studies using femtosecond (fs) laser based Cu scribing in air with the fluence of 0.5 J/cm2 resulted in a crated depth of 3 μm without any recast layer.

  11. In situ nanoscale observations of gypsum dissolution by digital holographic microscopy.

    PubMed

    Feng, Pan; Brand, Alexander S; Chen, Lei; Bullard, Jeffrey W

    2017-06-01

    Recent topography measurements of gypsum dissolution have not reported the absolute dissolution rates, but instead focus on the rates of formation and growth of etch pits. In this study, the in situ absolute retreat rates of gypsum (010) cleavage surfaces at etch pits, at cleavage steps, and at apparently defect-free portions of the surface are measured in flowing water by reflection digital holographic microscopy. Observations made on randomly sampled fields of view on seven different cleavage surfaces reveal a range of local dissolution rates, the local rate being determined by the topographical features at which material is removed. Four characteristic types of topographical activity are observed: 1) smooth regions, free of etch pits or other noticeable defects, where dissolution rates are relatively low; 2) shallow, wide etch pits bounded by faceted walls which grow gradually at rates somewhat greater than in smooth regions; 3) narrow, deep etch pits which form and grow throughout the observation period at rates that exceed those at the shallow etch pits; and 4) relatively few, submicrometer cleavage steps which move in a wave-like manner and yield local dissolution fluxes that are about five times greater than at etch pits. Molar dissolution rates at all topographical features except submicrometer steps can be aggregated into a continuous, mildly bimodal distribution with a mean of 3.0 µmolm -2 s -1 and a standard deviation of 0.7 µmolm -2 s -1 .

  12. Fabrication of superhydrophobic surface with improved corrosion inhibition on 6061 aluminum alloy substrate

    NASA Astrophysics Data System (ADS)

    Li, Xuewu; Zhang, Qiaoxin; Guo, Zheng; Shi, Tian; Yu, Jingui; Tang, Mingkai; Huang, Xingjiu

    2015-07-01

    This work has developed a simple and low-cost method to render 6061 aluminum alloy surface superhydrophobicity and excellent corrosion inhibition. The superhydrophobic aluminum alloy surface has been fabricated by hydrochloric acid etching, potassium permanganate passivation and fluoroalkyl-silane modification. Meanwhile, the effect of the etching and passivation time on the wettability and corrosion inhibition of the fabricated surface has also been investigated. Results show that with the etching time of 6 min and passivation time of 180 min the fabricated micro/nano-scale terrace-like hierarchical structures accompanying with the nanoscale coral-like network bulge structures after being modified can result in superhydrophobicity with a water contact angle (CA) of 155.7°. Moreover, an extremely weak adhesive force to droplets as well as an outstanding self-cleaning behavior of the superhydrophobic surface has also been proved. Finally, corrosion inhibition in seawater of the as-prepared aluminum alloy surface is characterized by potentiodynamic polarization curves and electrochemical impedance spectroscopy. Evidently, the fabricated superhydrophobic surface attained an improved corrosion inhibition efficiency of 83.37% compared with the traditional two-step processing consisting of etching and modification, which will extend the further applications of aluminum alloy especially in marine engineering fields.

  13. Single Crystals Grown Under Unconstrained Conditions

    NASA Astrophysics Data System (ADS)

    Sunagawa, Ichiro

    Based on detailed investigations on morphology (evolution and variation in external forms), surface microtopography of crystal faces (spirals and etch figures), internal morphology (growth sectors, growth banding and associated impurity partitioning) and perfection (dislocations and other lattice defects) in single crystals, we can deduce how and by what mechanism the crystal grew and experienced fluctuation in growth parameters through its growth and post-growth history under unconstrained condition. The information is useful not only in finding appropriate way to growing highly perfect and homogeneous single crystals, but also in deciphering letters sent from the depth of the Earth and the Space. It is also useful in discriminating synthetic from natural gemstones. In this chapter, available methods to obtain molecular information are briefly summarized, and actual examples to demonstrate the importance of this type of investigations are selected from both natural minerals (diamond, quartz, hematite, corundum, beryl, phlogopite) and synthetic crystals (SiC, diamond, corundum, beryl).

  14. Evaluation of microshear bond strength of resin composites to enamel of dental adhesive systems associated with Er,Cr:YSGG laser

    NASA Astrophysics Data System (ADS)

    Cassimiro-Silva, Patricia F.; Zezell, Denise M.; Monteiro, Gabriela Q. d. M.; Benetti, Carolina; de Paula Eduardo, Carlos; Gomes, Anderson S. L.

    2016-02-01

    The aim of this in vitro study was to evaluate the microshear bond strength (μSBS) of resin composite to enamel etching by Er,Cr:YSGG laser with the use of two differents adhesives systems. Fifty freshly extracted human molars halves were embedded in acrylic resin before preparation for the study, making a total of up to 100 available samples. The specimens were randomly assigned into six groups (η=10) according to substrate pre-treatment and adhesive system on the enamel. A two-step self-etching primer system (Clearfil SE Bond) and a universal adhesive used as an etch-andrinse adhesive (Adper Single Bond Universal) were applied to the nonirradiated enamel surface according to manufacturer's instructions, as control groups (Control CF and Control SB, respectively). For the other groups, enamel surfaces were previously irradiated with the Er,Cr:YSGG laser with 0.5 W, 75 mJ and 66 J/cm2 (CF 5 Hz and SB 5 Hz) and 1.25 W, 50 mJ and 44 J/cm2 (CF 15 Hz and SB 15 Hz). Irradiation was performed under air (50%) and water (50%) cooling. An independent t-test was performed to compare the adhesive systems. Mean μSBS ± sd (MPa) for each group was 16.857 +/- 2.61, 17.87 +/- 5.83, 12.23 +/- 2.02, 9.88 +/- 2.26, 15.94 +/- 1.98, 17.62 +/- 2.10, respectively. The control groups and the 50 mJ laser groups showed no statistically significant differences, regardless of the adhesive system used. The results obtained lead us to affirm that the bonding interaction of adhesives to enamel depends not only on the morphological aspects of the dental surface, but also on the characteristics of the adhesive employed and the parameters of the laser.

  15. Surface photovoltage studies of p-type AlGaN layers after reactive-ion etching

    NASA Astrophysics Data System (ADS)

    McNamara, J. D.; Phumisithikul, K. L.; Baski, A. A.; Marini, J.; Shahedipour-Sandvik, F.; Das, S.; Reshchikov, M. A.

    2016-10-01

    The surface photovoltage (SPV) technique was used to study the surface and electrical properties of Mg-doped, p-type AlxGa1-xN (0.06 < x < 0.17) layers. SPV measurements reveal significant deviation from previous SPV studies on p-GaN:Mg thin films and from the predictions of a thermionic model for the SPV behavior. In particular, the SPV of the p-AlGaN:Mg layers exhibited slower-than-expected transients under ultraviolet illumination and delayed restoration to the initial dark value. The slow transients and delayed restorations can be attributed to a defective surface region which interferes with normal thermionic processes. The top 45 nm of the p-AlGaN:Mg layer was etched using a reactive-ion etch which caused the SPV behavior to be substantially different. From this study, it can be concluded that a defective, near-surface region is inhibiting the change in positive surface charge by allowing tunneling or hopping conductivity of holes from the bulk to the surface, or by the trapping of electrons traveling to the surface by a high concentration of defects in the near-surface region. Etching removes the defective layer and reveals a region of presumably higher quality, as evidenced by substantial changes in the SPV behavior.

  16. Method for surface treatment of a cadmium zinc telluride crystal

    DOEpatents

    James, R.; Burger, A.; Chen, K.T.; Chang, H.

    1999-08-03

    A method for treatment of the surface of a CdZnTe (CZT) crystal is disclosed that reduces surface roughness (increases surface planarity) and provides an oxide coating to reduce surface leakage currents and thereby, improve resolution. A two step process is disclosed, etching the surface of a CZT crystal with a solution of lactic acid and bromine in ethylene glycol, following the conventional bromine/methanol etch treatment, and after attachment of electrical contacts, oxidizing the CZT crystal surface. 3 figs.

  17. Lateral electrochemical etching of III-nitride materials for microfabrication

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Han, Jung

    Conductivity-selective lateral etching of III-nitride materials is described. Methods and structures for making vertical cavity surface emitting lasers with distributed Bragg reflectors via electrochemical etching are described. Layer-selective, lateral electrochemical etching of multi-layer stacks is employed to form semiconductor/air DBR structures adjacent active multiple quantum well regions of the lasers. The electrochemical etching techniques are suitable for high-volume production of lasers and other III-nitride devices, such as lasers, HEMT transistors, power transistors, MEMs structures, and LEDs.

  18. Optimization and characterization of bulk hexagonal boron nitride single crystals grown by the nickel-chromium flux method

    NASA Astrophysics Data System (ADS)

    Hoffman, Tim

    Hexagonal boron nitride (hBN) is a wide bandgap III-V semiconductor that has seen new interest due to the development of other III-V LED devices and the advent of graphene and other 2-D materials. For device applications, high quality, low defect density materials are needed. Several applications for hBN crystals are being investigated, including as a neutron detector and interference-less infrared-absorbing material. Isotopically enriched crystals were utilized for enhanced propagation of phonon modes. These applications exploit the unique physical, electronic and nanophotonics applications for bulk hBN crystals. In this study, bulk hBN crystals were grown by the flux method using a molten Ni-Cr solvent at high temperatures (1500°C) and atmospheric pressures. The effects of growth parameters, source materials, and gas environment on the crystals size, morphology and purity were established and controlled, and the reliability of the process was greatly improved. Single-crystal domains exceeding 1mm in width and 200microm in thickness were produced and transferred to handle substrates for analysis. Grain size dependence with respect to dwell temperature, cooling rate and cooling temperature were analyzed and modeled using response surface morphology. Most significantly, crystal grain width was predicted to increase linearly with dwell temperature, with single-crystal domains exceeding 2mm in at 1700°C. Isotopically enriched 10B and 11B hBN crystal were produced using a Ni-Cr-B flux method, and their properties investigated. 10B concentration was evaluated using SIMS and correlated to the shift in the Raman peak of the E2g mode. Crystals with enrichment of 99% 10B and >99% 11B were achieved, with corresponding Raman shift peaks at 1392.0 cm-1 and 1356.6 cm-1, respectively. Peak FWHM also decreased as isotopic enrichment approached 100%, with widths as low as 3.5 cm-1 achieved, compared to 8.0 cm-1 for natural abundance samples. Defect selective etching was performed using a molten NaOH-KOH etchant at 425°C-525°C, to quantify the quality of the crystals. Three etch pit shapes were identified and etch pit width was investigated as a function of temperature. Etch pit density and etch pit activation energy was estimated at 5x107 cm-2 and 60 kJ/mol, respectively. Screw and mixed-type dislocations were identified using diffraction-contrast TEM imaging.

  19. Ge quantum dot arrays grown by ultrahigh vacuum molecular-beam epitaxy on the Si(001) surface: nucleation, morphology, and CMOS compatibility.

    PubMed

    Yuryev, Vladimir A; Arapkina, Larisa V

    2011-09-05

    Issues of morphology, nucleation, and growth of Ge cluster arrays deposited by ultrahigh vacuum molecular beam epitaxy on the Si(001) surface are considered. Difference in nucleation of quantum dots during Ge deposition at low (≲600°C) and high (≳600°C) temperatures is studied by high resolution scanning tunneling microscopy. The atomic models of growth of both species of Ge huts--pyramids and wedges-- are proposed. The growth cycle of Ge QD arrays at low temperatures is explored. A problem of lowering of the array formation temperature is discussed with the focus on CMOS compatibility of the entire process; a special attention is paid upon approaches to reduction of treatment temperature during the Si(001) surface pre-growth cleaning, which is at once a key and the highest-temperature phase of the Ge/Si(001) quantum dot dense array formation process. The temperature of the Si clean surface preparation, the final high-temperature step of which is, as a rule, carried out directly in the MBE chamber just before the structure deposition, determines the compatibility of formation process of Ge-QD-array based devices with the CMOS manufacturing cycle. Silicon surface hydrogenation at the final stage of its wet chemical etching during the preliminary cleaning is proposed as a possible way of efficient reduction of the Si wafer pre-growth annealing temperature.

  20. Factors affecting the shear bond strength of metal and ceramic brackets bonded to different ceramic surfaces.

    PubMed

    Abu Alhaija, Elham S J; Abu AlReesh, Issam A; AlWahadni, Ahed M S

    2010-06-01

    The aims of this study were to evaluate the shear bond strength (SBS) of metal and ceramic brackets bonded to two different all-ceramic crowns, IPS Empress 2 and In-Ceram Alumina, to compare the SBS between hydrofluoric acid (HFA), phosphoric acid etched, and sandblasted, non-etched all-ceramic surfaces. Ninety-six all-ceramic crowns were fabricated resembling a maxillary left first premolar. The crowns were divided into eight groups: (1) metal brackets bonded to sandblasted 9.6 per cent HFA-etched IPS Empress 2 crowns; (2) metal brackets bonded to sandblasted 9.6 per cent HFA-etched In-Ceram crowns; (3) ceramic brackets bonded to sandblasted 9.6 per cent HFA-etched IPS Empress 2 crowns; (4) ceramic brackets bonded to sandblasted 9.6 per cent HFA-etched In-Ceram crowns; (5) metal brackets bonded to sandblasted 37 per cent phosphoric acid-etched IPS Empress 2 crowns; (6) metal brackets bonded to sandblasted 37 per cent phosphoric acid-etched In-Ceram crowns; (7) metal brackets bonded to sandblasted, non-etched IPS Empress 2 crowns; and (8) metal brackets bonded to sandblasted, non-etched In-Ceram crowns. Metal and ceramic orthodontic brackets were bonded using a conventional light polymerizing adhesive resin. An Instron universal testing machine was used to determine the SBS at a crosshead speed of 0.1 mm/minute. Comparison between groups was performed using a univariate general linear model and chi-squared tests. The highest mean SBS was found in group 3 (120.15 +/- 45.05 N) and the lowest in group 8 (57.86 +/- 26.20 N). Of all the variables studied, surface treatment was the only factor that significantly affected SBS (P < 0.001). Acid etch application to sandblasted surfaces significantly increased the SBS in groups 1, 2, 5, and 6. The SBS of metal brackets debonded from groups 1, 3, and 5 were not significantly different from those of groups 2, 4, and 6. All debonded metal brackets revealed a similar pattern of bond failure at the adhesive-restorative interface. However, ceramic brackets had a significantly different adhesive failure pattern with dominant failure at the adhesive-bracket interface. Ceramic fractures after bracket removal were found more often in groups 1-4. No significant difference in ceramic fracture was observed between the IPS Empress 2 and In-Ceram groups.

  1. Aggressiveness of contemporary self-etching adhesives. Part II: etching effects on unground enamel.

    PubMed

    Pashley, D H; Tay, F R

    2001-09-01

    The aggressiveness of three self-etching adhesives on unground enamel was investigated. Ultrastructural features and microtensile bond strength were examined, first using these adhesives as both the etching and resin-infiltration components, and then examining their etching efficacy alone through substitution of the proprietary resins with the same control resins. For SEM examination, buccal, mid-coronal, unground enamel from human extracted bicuspids were etched with either Clearfil Mega Bond (Kuraray), Non-Rinse Conditioner (NRC; Dentsply DeTrey) or Prompt L-Pop (ESPE). Those in the control group were etched with 32% phosphoric acid (Bisco) for 15s. They were all rinsed off prior to examination of the etching efficacy. For TEM examination, the self-etching adhesives were used as recommended. Unground enamel treated with NRC were further bonded using Prime&Bond NT (Dentsply), while those in the etched, control group were bonded using All-Bond 2 (Bisco). Completely demineralized, resin replicas were embedded in epoxy resin for examination of the extent of resin infiltration. For microtensile bond strength evaluation, specimens were first etched and bonded using the self-etching adhesives. A second group of specimens were etched with the self-etching adhesives, rinsed but bonded using a control adhesive. Following restoration with Z100 (3M Dental Products), they were sectioned into beams of uniform cross-sectional areas and stressed to failure. Etching patterns of aprismatic enamel, as revealed by SEM, and the subsurface hybrid layer morphology, as revealed by TEM, varied according to the aggressiveness of the self-etching adhesives. Clearfil Mega Bond exhibited the mildest etching patterns, while Prompt L-Pop produced an etching effect that approached that of the total-etch control group. Microtensile bond strength of the three experimental groups were all significantly lower than the control group, but not different from one another. When the self-etching adhesives were replaced with the control adhesive after etching, bond strengths of NRC/Prime&Bond NT and Prompt L-Pop were not significantly different from that of the control group, but were significantly higher than that of Clearfil Mega Bond. Both etching efficacy and strength of the resins are important contributing factors in bonding of self-etching adhesives to unground enamel.

  2. Crystal defects observed by the etch-pit method and their effects on Schottky-barrier-diode characteristics on (\\bar{2}01) β-Ga2O3

    NASA Astrophysics Data System (ADS)

    Kasu, Makoto; Oshima, Takayoshi; Hanada, Kenji; Moribayashi, Tomoya; Hashiguchi, Akihiro; Oishi, Toshiyuki; Koshi, Kimiyoshi; Sasaki, Kohei; Kuramata, Akito; Ueda, Osamu

    2017-09-01

    A pixel array of vertical Schottky-barrier diodes (SBDs) was fabricated and measured on the surface of a (\\bar{2}01) β-Ga2O3 single crystal. Subsequently, etch pits and patterns were observed on the same surface. Three types of etch pits were discovered: (1) a line-shaped etch pattern originating from a void and extending toward the [010] direction, (2) an arrow-shaped etch pit whose arrow’s head faces toward the [102] direction and, (3) a gourd-shaped etch pit whose point head faces toward the [102] direction. Their average densities were estimated to be 5 × 102, 7 × 104, and 9 × 104 cm-2, respectively. We confirmed no clear relationship between the leakage current in SBDs and these crystalline defects. Such results are obtained because threading dislocations run mainly in the [010] growth direction and do not go through the (\\bar{2}01) sample plate.

  3. Wet etch methods for InAs nanowire patterning and self-aligned electrical contacts

    NASA Astrophysics Data System (ADS)

    Fülöp, G.; d'Hollosy, S.; Hofstetter, L.; Baumgartner, A.; Nygård, J.; Schönenberger, C.; Csonka, S.

    2016-05-01

    Advanced synthesis of semiconductor nanowires (NWs) enables their application in diverse fields, notably in chemical and electrical sensing, photovoltaics, or quantum electronic devices. In particular, indium arsenide (InAs) NWs are an ideal platform for quantum devices, e.g. they may host topological Majorana states. While the synthesis has been continously perfected, only a few techniques have been developed to tailor individual NWs after growth. Here we present three wet chemical etch methods for the post-growth morphological engineering of InAs NWs on the sub-100 nm scale. The first two methods allow the formation of self-aligned electrical contacts to etched NWs, while the third method results in conical shaped NW profiles ideal for creating smooth electrical potential gradients and shallow barriers. Low temperature experiments show that NWs with etched segments have stable transport characteristics and can serve as building blocks of quantum electronic devices. As an example we report the formation of a single electrically stable quantum dot between two etched NW segments.

  4. Selective etching of injection molded zirconia-toughened alumina: Towards osseointegrated and antibacterial ceramic implants.

    PubMed

    Flamant, Quentin; Caravaca, Carlos; Meille, Sylvain; Gremillard, Laurent; Chevalier, Jérôme; Biotteau-Deheuvels, Katia; Kuntz, Meinhard; Chandrawati, Rona; Herrmann, Inge K; Spicer, Christopher D; Stevens, Molly M; Anglada, Marc

    2016-12-01

    Due to their outstanding mechanical properties and excellent biocompatibility, zirconia-toughened alumina (ZTA) ceramics have become the gold standard in orthopedics for the fabrication of ceramic bearing components over the last decade. However, ZTA is bioinert, which hampers its implantation in direct contact with bone. Furthermore, periprosthetic joint infections are now the leading cause of failure for joint arthroplasty prostheses. To address both issues, an improved surface design is required: a controlled micro- and nano-roughness can promote osseointegration and limit bacterial adhesion whereas surface porosity allows loading and delivery of antibacterial compounds. In this work, we developed an integrated strategy aiming to provide both osseointegrative and antibacterial properties to ZTA surfaces. The micro-topography was controlled by injection molding. Meanwhile a novel process involving the selective dissolution of zirconia (selective etching) was used to produce nano-roughness and interconnected nanoporosity. Potential utilization of the porosity for loading and delivery of antibiotic molecules was demonstrated, and the impact of selective etching on mechanical properties and hydrothermal stability was shown to be limited. The combination of injection molding and selective etching thus appears promising for fabricating a new generation of ZTA components implantable in direct contact with bone. Zirconia-toughened alumina (ZTA) is the current gold standard for the fabrication of orthopedic ceramic components. In the present work, we propose an innovative strategy to provide both osseointegrative and antibacterial properties to ZTA surfaces: we demonstrate that injection molding allows a flexible design of surface micro-topography and can be combined with selective etching, a novel process that induces nano-roughness and surface interconnected porosity without the need for coating, avoiding reliability issues. These surface modifications have the potential to improve osseointegration. Furthermore, our results show that the porosity can be used for drug delivery and suggest that the etched surface could reduce bacterial adhesion. Copyright © 2016 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

  5. Homogeneous alignment of nematic liquid crystals by ion beam etched surfaces

    NASA Technical Reports Server (NTRS)

    Wintucky, E. G.; Mahmood, R.; Johnson, D. L.

    1979-01-01

    A wide range of ion beam etch parameters capable of producing uniform homogeneous alignment of nematic liquid crystals on SiO2 films are discussed. The alignment surfaces were generated by obliquely incident (angles of 5 to 25 deg) argon ions with energies in the range of 0.5 to 2.0 KeV, ion current densities of 0.1 to 0.6 mA sq cm and etch times of 1 to 9 min. A smaller range of ion beam parameters (2.0 KeV, 0.2 mA sq cm, 5 to 10 deg and 1 to 5 min.) were also investigated with ZrO2 films and found suitable for homogeneous alignment. Extinction ratios were very high (1000), twist angles were small ( or = 3 deg) and tilt-bias angles very small ( or = 1 deg). Preliminary scanning electron microscopy results indicate a parallel oriented surface structure on the ion beam etched surfaces which may determine alignment.

  6. Fabrication of broadband quasi-omnidirectional antireflective surface on glass for photovoltaic application

    NASA Astrophysics Data System (ADS)

    Kumar, Arvind; Kumar, Praveen; Srinivas, G.; Jakeer Khan G., H.; Siju, Barshilia, Harish C.

    2016-05-01

    In this paper, we have demonstrated a simple and cost effective HF-vapor phase etching method to fabricate the broadband quasi-omnidirectional antireflective surface on glass substrate. Both-sides etched sodalime glass substrates under optimized conditions showed a broadband enhancement in the transmittance spectra with maximum transmittance as high as ~97% at 598 nm. FESEM results confirmed the formation of a graded nanoporous surface, which lowers it refractive index. The etched surface exhibited excellent AR property over a wide range of incidence angles (8°-48°), which is attributed due to the formation of graded porosity. Silicon solar cell covered with plain glass showed Isc of 0.123A and efficiency of 8.76%, while it showed Isc of 0.130A and efficiency of 9.2% when it was covered by etched glass. Furthermore, it exhibited an excellent anti-soiling property as compared to plain glass. All these results show its strong potential in the photovoltaic application.

  7. High-Temperature Isothermal Capacitance Transient Spectroscopy Study on Inductively Coupled Plasma Etching Damage for p-GaN Surfaces

    NASA Astrophysics Data System (ADS)

    Aoki, Toshichika; Wakayama, Hisashi; Kaneda, Naoki; Mishima, Tomoyoshi; Nomoto, Kazuki; Shiojima, Kenji

    2013-11-01

    The effects of the inductively coupled plasma (ICP) etching damage on the electrical characteristics of low-Mg-doped p-GaN Schottky contacts were evaluated by high-temperature isothermal capacitance transient spectroscopy. A large single peak for an acceptor-type surface state was dominantly detected for as-grown samples. The energy level and state density were obtained to be 1.18 eV above the valence band, which is close to a Ga vacancy (VGa), and 1.5×1013 cm-2, respectively. It was speculated that a small portion of Ga atoms were missing from the surface, and a high VGa density was observed in a few surface layers. The peak intensity decreased by 60% upon annealing at 800 °C, and further decrease was found by ICP etching. This decrease is consistent with the suppression of the memory effect in current-voltage characteristics. Upon annealing and ICP etching, since the VGa structure might be disordered, the peak intensity decreased.

  8. Plastic deformation of a magnesium oxide 001-plane surface produced by cavitation

    NASA Technical Reports Server (NTRS)

    Hattori, S.; Miyoshi, K.; Buckley, D. H.; Okada, T.

    1986-01-01

    An investigation was conducted to examine plastic deformation of a cleaved single-crystal magnesium oxide 001-plane surface exposed to cavitation. Cavitation damage experiments were carried out in distilled water at 25 C by using a magnetostrictive oscillator in close proximity (2 mm) to the surface of the cleaved specimen. The dislocation-etch-pit patterns induced by cavitation were examined and compared with that of microhardness indentations. The results revealed that dislocation-etch-pit patterns around hardness indentations contain both screw and edge dislocations, while the etch-pit patterns on the surface exposed to cavitation contain only screw dislocations. During cavitation, deformation occurred in a thin surface layer, accompanied by work-hardening of the ceramic. The row of screw dislocations underwent a stable growth, which was analyzed crystallographically.

  9. Fabrication and Atomic Force Microscopy Characterization of Molecular Composites of Fullerenes in Aerogel Matrix for Optical Limiting

    NASA Technical Reports Server (NTRS)

    Lu, W. J .; Sunkara, H. B.; Shi, D.; Morgan, S. H.; Penn, B.; Frazier, D.; Collins, W. E.

    1998-01-01

    An optical limiter is a device which exhibits a decrease in the transmittance in a material with an increase in intensity of light. Sol-gel techniques offer many advantages in the fabrication of materials. These materials possess many desirable properties for nonlinear optical (NLO) device applications which include transparency, high thermal and chemical stabilities, very low refractive index and dielectric constants. C60 shows a higher excited state absorption cross section than the ground state absorption cross section over the complete visible spectrum, and the spectrum of the excited state absorption of C60 has the same general shape as the ground state absorption. This fact suggests that fullerenes are ideal optical limiting materials. Aerogels are fabricated by sol-gel processing. One of the key issues is the dispersion of fullerenes into small and uniform pores of silica aerogel host matrices. The aerogel network was characterized by Raman spectroscopy. Atomic force microscopy is a technique with many advantages to characterize the aerogel materials. The morphology of the cleaved surface for a C60/aerogel sample shows that there are long paralleled shaped stripes with 20-30 nm in width and about 500 nm in length on the cleaved surface. The cleaved surface also was etched by 5% HF solution for one minutes, and it became smoother after HF etching. The main feature in on the surface is the spherical particles with the size of few nanometers, and no aggregated fullerenes appear. The fullerenes are well dispersed in the aerogel matrices.

  10. Dynamic Pattern Formation in Electron-Beam-Induced Etching [Emergent formation of dynamic topographic patterns in electron beam induced etching

    DOE PAGES

    Martin, Aiden A.; Bahm, Alan; Bishop, James; ...

    2015-12-15

    Here, we report highly ordered topographic patterns that form on the surface of diamond, span multiple length scales, and have a symmetry controlled by the precursor gas species used in electron-beam-induced etching (EBIE). The pattern formation dynamics reveals an etch rate anisotropy and an electron energy transfer pathway that is overlooked by existing EBIE models. Therefore, we, modify established theory such that it explains our results and remains universally applicable to EBIE. Furthermore, the patterns can be exploited in controlled wetting, optical structuring, and other emerging applications that require nano- and microscale surface texturing of a wide band-gap material.

  11. Direct observation for atomically flat and ordered vertical {111} side-surfaces on three-dimensionally figured Si(110) substrate using scanning tunneling microscopy

    NASA Astrophysics Data System (ADS)

    Yang, Haoyu; Hattori, Azusa N.; Ohata, Akinori; Takemoto, Shohei; Hattori, Ken; Daimon, Hiroshi; Tanaka, Hidekazu

    2017-11-01

    A three-dimensional Si{111} vertical side-surface structure on a Si(110) wafer was fabricated by reactive ion etching (RIE) followed by wet-etching and flash-annealing treatments. The side-surface was studied with scanning tunneling microscopy (STM) in atomic scale for the first time, in addition to atomic force microscopy (AFM), scanning electron microscopy (SEM), and low-energy electron diffraction (LEED). AFM and SEM showed flat and smooth vertical side-surfaces without scallops, and STM proved the realization of an atomically-flat 7 × 7-reconstructed structure, under optimized RIE and wet-etching conditions. STM also showed that a step-bunching occurred on the produced {111} side-surface corresponding to a reversely taped side-surface with a tilt angle of a few degrees, but did not show disordered structures. Characteristic LEED patterns from both side- and top-reconstructed surfaces were also demonstrated.

  12. Research on subsurface deformed layer in ultra-precision cutting of single crystal copper by focused ion beam etching method

    NASA Astrophysics Data System (ADS)

    Chen, Y.; Huang, X. J.; Kong, J. X.

    2018-03-01

    In this paper, the focused ion beam was used to study the subsurface deformed layer of single crystal copper caused by the nanoscale single-point diamond fly cutting, and the possibility of using nanometer ultra-precision cutting to remove the larger deformation layer caused by traditional rough cutting process was explored. The maximum cutting thickness of single-point diamond cutting was about 146 nm, and the surface of the single-crystal copper after cutting was etched and observed by using the focused ion beam method. It was found that the morphology of the near-surface layer and the intermediate layer of the copper material were larger differences: the near-surface of the material was smaller and more compact, and the intermediate material layer of the material was more coarse sparse. The results showed that the traditional precision cutting would residual significant subsurface deformed layer and the thickness was on micron level. Even more, the subsurface deformed layer was obviously removed from about 12μm to 5μm after single-point diamond fly cutting in this paper. This paper proved that the large-scale subsurface deformed layer caused by traditional cutting process could be removed by nanometer ultra-precision cutting. It was of great significance to further establish the method that control of the deformation of weak rigid components by reducing the depth of the subsurface deformed layers.

  13. Influence of Er,Cr:YSGG laser treatment on the microtensile bond strength of adhesives to dentin.

    PubMed

    Cardoso, Marcio Vivan; Coutinho, Edurado; Ermis, R Banu; Poitevin, André; Van Landuyt, Kirsten; De Munck, Jan; Carvalho, Rubens C R; Lambrechts, Paul; Van Meerbeek, Bart

    2008-02-01

    In light of the concept of minimally invasive dentistry, erbium lasers have been considered as an alternative technique to the use of diamond burs for cavity preparation. The purpose of this study was to assess the bonding effectiveness of adhesives to Er,Cr:YSGG laser-irradiated dentin using irradiation settings specific for cavity preparation. Fifty-four midcoronal dentin surfaces, obtained from sound human molars, were irradiated with an Er,Cr:YSGG laser or prepared with a diamond bur using a high-speed turbine. One etch-and-rinse (Optibond FL/Kerr) and three self-etching adhesives (Adper Prompt L-Pop/3M ESPE, Clearfil SE Bond/Kuraray, and Clearfil S3 Bond/Kuraray) were used to bond the composite to dentin. The microtensile bond strength (microTBS) was determined after 24 h of storage in water at 37 degrees C. The Kruskal-Wallis test was used to determine pairwise statistical differences (p < 0.05). Prepared dentin surfaces, adhesive interfaces, and failure patterns were analyzed using a stereomicroscope and Field-emission gun Scanning Electron Microscopy (Feg-SEM). Significantly lower microTBS was observed to laser-irradiated than to bur-cut dentin (p < 0.05), irrespective of the adhesive employed. Feg-SEM photomicrographs of lased dentin revealed an imbricate patterned substrate and the presence of microcracks at the dentin surface. Morphological alterations produced by Er,Cr:YSGG laser-irradiation adversely influence the bonding effectiveness of adhesives to dentin.

  14. An easy and environmentally-friendly approach to superamphiphobicity of aluminum surfaces

    NASA Astrophysics Data System (ADS)

    Deng, R.; Hu, Y. M.; Wang, L.; Li, Zh. H.; Shen, T.; Zhu, Y.; Xiang, J. Zh.

    2017-04-01

    Superamphiphobic Al surfaces were achieved via an easy and environmentally-friendly approach. Aqueous mixed solution of 0.7 M CuSO4 and 1 M NaCl was used to etch polished Al surfaces to fabricate a rough morphology distributed with microscale step-like pits. The uniformly distributed nanoscale petals covered on the microscale pits were obtained by subsequent 96 °C hot deionized water bathing for 13 min. Thus, the hierarchical micro/nanometer scale roughness was formed which provided the structural basic of superamphiphobic Al surfaces. By 1H, 1H, 2H, 2H-Perfluorodecyl-triethoxysilane (PFDTS) derivatization, desirable superamphiphobic Al surfaces were achieved with the highest static contact angles of 162° for water, 156° for peanut oil, respectively. Meanwhile, the sliding angles were lower than 10° for both water and peanut oil droplets. The as-prepared Al surfaces were investigated by field-emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), and optical contact angle measurements. The FE-SEM images of as-prepared Al surfaces showed a hierarchical micro/nanometer scale morphology. XPS analyses demonstrated the PFDTS derivitization on Al surfaces. The superamphiphobic Al surfaces presented good mechanical durability and chemical stability which have a wide range of applications in fields such as self-cleaning, anti-icing, anti-corrosion, oil transportation, energy harvesting, microfluidics, and so forth. The approach reported in this paper may easily realize the industrial production of superamphiphobic Al surfaces owing to the advantage of facile, low cost and environmentally-friendly.

  15. Acid Etching and Plasma Sterilization Fail to Improve Osseointegration of Grit Blasted Titanium Implants

    PubMed Central

    Saksø, Mikkel; Jakobsen, Stig S; Saksø, Henrik; Baas, Jørgen; Jakobsen, Thomas; Søballe, Kjeld

    2012-01-01

    Interaction between implant surface and surrounding bone influences implant fixation. We attempted to improve the bone-implant interaction by 1) adding surface micro scale topography by acid etching, and 2) removing surface-adherent pro-inflammatory agents by plasma cleaning. Implant fixation was evaluated by implant osseointegration and biomechanical fixation. The study consisted of two paired animal sub-studies where 10 skeletally mature Labrador dogs were used. Grit blasted titanium alloy implants were inserted press fit in each proximal tibia. In the first study grit blasted implants were compared with acid etched grit blasted implants. In the second study grit blasted implants were compared with acid etched grit blasted implants that were further treated with plasma sterilization. Implant performance was evaluated by histomorphometrical investigation (tissue-to-implant contact, peri-implant tissue density) and mechanical push-out testing after four weeks observation time. Neither acid etching nor plasma sterilization of the grit blasted implants enhanced osseointegration or mechanical fixation in this press-fit canine implant model in a statistically significant manner. PMID:22962567

  16. Effect of phosphate treatment of Acid-etched implants on mineral apposition rates near implants in a dog model.

    PubMed

    Foley, Christine Hyon; Kerns, David G; Hallmon, William W; Rivera-Hidalgo, Francisco; Nelson, Carl J; Spears, Robert; Dechow, Paul C; Opperman, Lynne A

    2010-01-01

    This study evaluated the effects of phosphate coating of acid-etched titanium on the mineral apposition rate (MAR) and new bone-to-implant contact (BIC) in a canine model. Titanium implants (2.2 3 4 mm) with acid-etched surfaces that were electrolytically phosphated or not were placed in 48 mandibular sites in six foxhounds. Tetracycline and calcein dyes were administered 1 week after implant placement and 1 week before sacrifice. At 12 weeks after implant placement, the animals were sacrificed. MAR and BIC were evaluated using fluorescence microscopy. Light microscopic and histologic evaluations were performed on undecalcified sections. Microscopic evaluation showed the presence of healthy osteoblasts lining bone surfaces near implants. Similar BIC was observed in phosphated and nonphosphated titanium implant sites. MAR was significantly higher around the nonphosphated titanium implant surfaces than around the phosphated titanium samples. No significant differences were found between dogs or implant sites. Acid-etched implants showed significantly higher MARs compared to acid-etched, phosphate-coated implants. Int J Maxillofac Implants 2010;25:278-286.

  17. Nanotextured PDMS Substrates for Enhanced Roughness and Aptamer Immobilization for Cancer Cell Capture

    NASA Astrophysics Data System (ADS)

    Islam, Muhymin; Mahmood, Arif; Bellah, Md.; Kim, Young-Tae; Iqbal, Samir

    2014-03-01

    Detection of circulating tumor cells (CTCs) in the early stages of cancer is requires very sensitive approach. Nanotextured polydimethylsiloxane (PDMS) substrates were fabricated by micro reactive ion etching (Micro-RIE) to have better control on surface morphology and to improve the affinity of PDMS surfaces to capture cancer cells using surface immobilized aptamers. The aptamers were specific to epidermal growth factor receptors (EGFR) present in cell membranes, and overexpressed in tumor cells. We also investigated the effect of nano-scale features on cell capturing by implementing various surfaces of different roughnesses. Three different recipes were used to prepare nanotextured PDMS by micro-RIE using oxygen (O2) and carbon tetrafluoride (CF4). The measured average roughness of three nanotextured PDMS surfaces were found to impact average densities of captured cells. In all cases, nanotextured PDMS facilitated cell capturing possibly due to increased effective surface area of roughened substrates at nanoscale. It was also observed that cell capture efficiency was higher for higher surface roughness. The nanotextured PDMS substrates are thus useful for cancer cytology devices.

  18. Fracture surface analysis in composite and titanium bonding

    NASA Technical Reports Server (NTRS)

    Devilbiss, T. A.; Wightman, J. P.

    1985-01-01

    To understand the mechanical properties of fiber-reinforced composite materials, it is necessary to understand the mechanical properties of the matrix materials and of the reinforcing fibers. Another factor that can affect the mechanical properties of a composite material is the interaction between the fiber and the matrix. In general, composites with strong fiber matrix bonding will give higher modulus, lower toughness composites. Composites with weak bonding will have a lower modulus and more ductility. The situation becomes a bit more complex when all possibilities are examined. To be considered are the following: the properties of the surface layer on the fiber, the interactive forces between polymer and matrix, the surface roughness and porosity of the fiber, and the morphology of the matrix polymer at the fiber surface. In practice, the surface of the fibers is treated to enhance the mechanical properties of a composite. These treatments include anodization, acid etching, high temperature oxidation, and plasma oxidation, to name a few. The goal is to be able to predict the surface properties of carbon fibers treated in various ways, and then to relate surface properties to fiber matrix bonding.

  19. Effect of source frequency and pulsing on the SiO2 etching characteristics of dual-frequency capacitive coupled plasma

    NASA Astrophysics Data System (ADS)

    Kim, Hoe Jun; Jeon, Min Hwan; Mishra, Anurag Kumar; Kim, In Jun; Sin, Tae Ho; Yeom, Geun Young

    2015-01-01

    A SiO2 layer masked with an amorphous carbon layer (ACL) has been etched in an Ar/C4F8 gas mixture with dual frequency capacitively coupled plasmas under variable frequency (13.56-60 MHz)/pulsed rf source power and 2 MHz continuous wave (CW) rf bias power, the effects of the frequency and pulsing of the source rf power on the SiO2 etch characteristics were investigated. By pulsing the rf power, an increased SiO2 etch selectivity was observed with decreasing SiO2 etch rate. However, when the rf power frequency was increased, not only a higher SiO2 etch rate but also higher SiO2 etch selectivity was observed for both CW and pulse modes. A higher CF2/F ratio and lower electron temperature were observed for both a higher source frequency mode and a pulsed plasma mode. Therefore, when the C 1s binding states of the etched SiO2 surfaces were investigated using X-ray photoelectron spectroscopy (XPS), the increase of C-Fx bonding on the SiO2 surface was observed for a higher source frequency operation similar to a pulsed plasma condition indicating the increase of SiO2 etch selectivity over the ACL. The increase of the SiO2 etch rate with increasing etch selectivity for the higher source frequency operation appears to be related to the increase of the total plasma density with increasing CF2/F ratio in the plasma. The SiO2 etch profile was also improved not only by using the pulsed plasma but also by increasing the source frequency.

  20. Effect of Saliva on the Tensile Bond Strength of Different Generation Adhesive Systems: An In-Vitro Study.

    PubMed

    Gupta, Nimisha; Tripathi, Abhay Mani; Saha, Sonali; Dhinsa, Kavita; Garg, Aarti

    2015-07-01

    Newer development of bonding agents have gained a better understanding of factors affecting adhesion of interface between composite and dentin surface to improve longevity of restorations. The present study evaluated the influence of salivary contamination on the tensile bond strength of different generation adhesive systems (two-step etch-and-rinse, two-step self-etch and one-step self-etch) during different bonding stages to dentin where isolation is not maintained. Superficial dentin surfaces of 90 extracted human molars were randomly divided into three study Groups (Group A: Two-step etch-and-rinse adhesive system; Group B: Two-step self-etch adhesive system and Group C: One-step self-etch adhesive system) according to the different generation of adhesives used. According to treatment conditions in different bonding steps, each Group was further divided into three Subgroups containing ten teeth in each. After adhesive application, resin composite blocks were built on dentin and light cured subsequently. The teeth were then stored in water for 24 hours before sending for testing of tensile bond strength by Universal Testing Machine. The collected data were then statistically analysed using one-way ANOVA and Tukey HSD test. One-step self-etch adhesive system revealed maximum mean tensile bond strength followed in descending order by Two-step self-etch adhesive system and Two-step etch-and-rinse adhesive system both in uncontaminated and saliva contaminated conditions respectively. Unlike One-step self-etch adhesive system, saliva contamination could reduce tensile bond strength of the two-step self-etch and two-step etch-and-rinse adhesive system. Furthermore, the step of bonding procedures and the type of adhesive seems to be effective on the bond strength of adhesives contaminated with saliva.

  1. Effect of alloy addition and growth conditions on the formation of Mg-based bioabsorbable thin films

    NASA Astrophysics Data System (ADS)

    Pursel, Sean M.; Petrilli, John D.; Horn, Mark W.; Shaw, Barbara A.

    2008-08-01

    Magnesium is an essential mineral in the human body and has recently been studied as a bioabsorbable material for use in cardiac stents. New areas of application can be found in bone plates, bone screws, and orthopedic implants. Magnesium alone has a corrosion rate much too high for use in such applications and has been alloyed with various elements to improve corrosion resistance. The use of vapor deposition to create Mg alloys for the above applications has not been attempted although certain properties of non-equilibrium alloys, namely corrosion resistance, can be improved. Using vapor deposition the characterization of the growth of magnesium alloy thin films has been done utilizing various alloying elements, substrate temperatures, post-deposition treatments, and substrate positions. The results point towards a growth mode controlled by crystallization of the Mg. Mg Sculptured thin films (STFs) are used to demonstrate these effects and potential solutions while also providing a route to control nanoscale surface morphology to enhance cell growth, cell attachment, and absorption properties. The results of the study are presented in terms of x-ray diffraction data, microscopy analysis of growth evolution, and corrosion testing. This magnesium alloy research utilizes a dual source deposition method that has also provided insight about some of the growth modes of other alloy STFs. Engineering of surface morphology using dip coatings and etching has been used in biomedical materials to enhance certain application specific surface properties. STF technology potentially provides a path to merge the advantages of non-equilibrium alloy formation and engineering nanoscale surface morphology.

  2. Surface Passivation of CdZnTe Detector by Hydrogen Peroxide Solution Etching

    NASA Technical Reports Server (NTRS)

    Hayes, M.; Chen, H.; Chattopadhyay, K.; Burger, A.; James, R. B.

    1998-01-01

    The spectral resolution of room temperature nuclear radiation detectors such as CdZnTe is usually limited by the presence of conducting surface species that increase the surface leakage current. Studies have shown that the leakage current can be reduced by proper surface preparation. In this study, we try to optimize the performance of CdZnTe detector by etching the detector with hydrogen peroxide solution as function of concentration and etching time. The passivation effect that hydrogen peroxide introduces have been investigated by current-voltage (I-V) measurement on both parallel strips and metal-semiconductor-metal configurations. The improvements on the spectral response of Fe-55 and 241Am due to hydrogen peroxide treatment are presented and discussed.

  3. Electrical transport and low-frequency noise in chemical vapor deposited single-layer MoS2 devices.

    PubMed

    Sharma, Deepak; Amani, Matin; Motayed, Abhishek; Shah, Pankaj B; Birdwell, A Glen; Najmaei, Sina; Ajayan, Pulickel M; Lou, Jun; Dubey, Madan; Li, Qiliang; Davydov, Albert V

    2014-04-18

    We have studied temperature-dependent (77-300 K) electrical characteristics and low-frequency noise (LFN) in chemical vapor deposited (CVD) single-layer molybdenum disulfide (MoS2) based back-gated field-effect transistors (FETs). Electrical characterization and LFN measurements were conducted on MoS2 FETs with Al2O3 top-surface passivation. We also studied the effect of top-surface passivation etching on the electrical characteristics of the device. Significant decrease in channel current and transconductance was observed in these devices after the Al2O3 passivation etching. For passivated devices, the two-terminal resistance variation with temperature showed a good fit to the activation energy model, whereas for the etched devices the trend indicated a hopping transport mechanism. A significant increase in the normalized drain current noise power spectral density (PSD) was observed after the etching of the top passivation layer. The observed channel current noise was explained using a standard unified model incorporating carrier number fluctuation and correlated surface mobility fluctuation mechanisms. Detailed analysis of the gate-referred noise voltage PSD indicated the presence of different trapping states in passivated devices when compared to the etched devices. Etched devices showed weak temperature dependence of the channel current noise, whereas passivated devices exhibited near-linear temperature dependence.

  4. Method of plasma etching Ga-based compound semiconductors

    DOEpatents

    Qiu, Weibin; Goddard, Lynford L.

    2012-12-25

    A method of plasma etching Ga-based compound semiconductors includes providing a process chamber and a source electrode adjacent to the process chamber. The process chamber contains a sample comprising a Ga-based compound semiconductor. The sample is in contact with a platen which is electrically connected to a first power supply, and the source electrode is electrically connected to a second power supply. The method includes flowing SiCl.sub.4 gas into the chamber, flowing Ar gas into the chamber, and flowing H.sub.2 gas into the chamber. RF power is supplied independently to the source electrode and the platen. A plasma is generated based on the gases in the process chamber, and regions of a surface of the sample adjacent to one or more masked portions of the surface are etched to create a substantially smooth etched surface including features having substantially vertical walls beneath the masked portions.

  5. Method of plasma etching GA-based compound semiconductors

    DOEpatents

    Qiu, Weibin; Goddard, Lynford L.

    2013-01-01

    A method of plasma etching Ga-based compound semiconductors includes providing a process chamber and a source electrode adjacent thereto. The chamber contains a Ga-based compound semiconductor sample in contact with a platen which is electrically connected to a first power supply, and the source electrode is electrically connected to a second power supply. SiCl.sub.4 and Ar gases are flowed into the chamber. RF power is supplied to the platen at a first power level, and RF power is supplied to the source electrode. A plasma is generated. Then, RF power is supplied to the platen at a second power level lower than the first power level and no greater than about 30 W. Regions of a surface of the sample adjacent to one or more masked portions of the surface are etched at a rate of no more than about 25 nm/min to create a substantially smooth etched surface.

  6. Innovations in bonding to zirconia-based materials: Part I.

    PubMed

    Aboushelib, Moustafa N; Matinlinna, Jukka P; Salameh, Ziad; Ounsi, Hani

    2008-09-01

    Establishing a reliable bond to zirconia-based materials has proven to be difficult which is the major limitation against fabricating adhesive zirconia restorations. This bond could be improved using novel selective infiltration etching conditioning in combination with engineered zirconia primers. Aim of the work was to evaluate resin-to-zirconia bond strength using selective infiltration etching and novel silane-based zirconia primers. Zirconia discs (Procera Zirconia) received selective infiltration etching surface treatment followed by coating with either of five especially engineered experimental zirconia primers. Pre-aged resin-composite discs (Tetric Ivo Ceram) were bonded to the treated surface using an MDP-containing resin-composite (Panavia F 2.0). The bilayered specimens were cut into microbars and the microtensile bond strength (MTBS) was evaluated. 'As-sintered' zirconia discs served as a control (alpha=0.05). The broken microbars were examined using a scanning electron microscope (SEM). The combination of selective infiltration etching with experimental zirconia primers significantly improved (F=3805, P<0.0001) the MTBS values (41+/-5.8 MPa) compared to the 'as-sintered' surface using the same primers which demonstrated spontaneous failure and very low bond strength values (2.6+/-3.1 MPa). SEM analysis revealed that selective infiltration etching surface treatment resulted in a nano-retentive surface where the zirconia primers were able to penetrate and interlock which explained the higher MTBS values observed for the treated specimens.

  7. Cryo-Etched Black Silicon for Use as Optical Black

    NASA Technical Reports Server (NTRS)

    Yee, Karl Y.; White, Victor E.; Mouroulis, Pantazis; Eastwood, Michael L.

    2011-01-01

    Stray light reflected from the surface of imaging spectrometer components in particular, the spectrometer slit degrade the image quality. A technique has been developed for rapid, uniform, and cost-effective black silicon formation based on inductively coupled plasma (ICP) etching at cryogenic temperatures. Recent measurements show less than 1-percent total reflectance from 350 2,500 nm of doped black silicon formed in this way, making it an excellent option for texturing of component surfaces for reduction of stray light. Oxygen combines with SF6 + Si etch byproducts to form a passivation layer atop the Si when the etch is performed at cryogenic temperatures. Excess flow of oxygen results in micromasking and the formation of black silicon. The process is repeatable and reliable, and provides control over etch depth and sidewall profile. Density of the needles can be controlled to some extent. Regions to be textured can be patterned lithographically. Adhesion is not an issue as the nanotips are part of the underlying substrate. This is in contrast to surface growth/deposition techniques such as carbon nanotubes (CNTs). The black Si surface is compatible with wet processing, including processing with solvents, the textured surface is completely inorganic, and it does not outgas. In radiometry applications, optical absorbers are often constructed using gold black or CNTs. This black silicon technology is an improvement for these types of applications.

  8. Tuning of structural, light emission and wetting properties of nanostructured copper oxide-porous silicon matrix formed on electrochemically etched copper-coated silicon substrates

    NASA Astrophysics Data System (ADS)

    Naddaf, M.

    2017-01-01

    Matrices of copper oxide-porous silicon nanostructures have been formed by electrochemical etching of copper-coated silicon surfaces in HF-based solution at different etching times (5-15 min). Micro-Raman, X-ray diffraction and X-ray photoelectron spectroscopy results show that the nature of copper oxide in the matrix changes from single-phase copper (I) oxide (Cu2O) to single-phase copper (II) oxide (CuO) on increasing the etching time. This is accompanied with important variation in the content of carbon, carbon hydrides, carbonyl compounds and silicon oxide in the matrix. The matrix formed at the low etching time (5 min) exhibits a single broad "blue" room-temperature photoluminescence (PL) band. On increasing the etching time, the intensity of this band decreases and a much stronger "red" PL band emerges in the PL spectra. The relative intensity of this band with respect to the "blue" band significantly increases on increasing the etching time. The "blue" and "red" PL bands are attributed to Cu2O and porous silicon of the matrix, respectively. In addition, the water contact angle measurements reveal that the hydrophobicity of the matrix surface can be tuned from hydrophobic to superhydrophobic state by controlling the etching time.

  9. Suboxide/subnitride formation on Ta masks during magnetic material etching by reactive plasmas

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Li, Hu; Muraki, Yu; Karahashi, Kazuhiro

    2015-07-15

    Etching characteristics of tantalum (Ta) masks used in magnetoresistive random-access memory etching processes by carbon monoxide and ammonium (CO/NH{sub 3}) or methanol (CH{sub 3}OH) plasmas have been examined by mass-selected ion beam experiments with in-situ surface analyses. It has been suggested in earlier studies that etching of magnetic materials, i.e., Fe, Ni, Co, and their alloys, by such plasmas is mostly due to physical sputtering and etch selectivity of the process arises from etch resistance (i.e., low-sputtering yield) of the hard mask materials such as Ta. In this study, it is shown that, during Ta etching by energetic CO{sup +}more » or N{sup +} ions, suboxides or subnitrides are formed on the Ta surface, which reduces the apparent sputtering yield of Ta. It is also shown that the sputtering yield of Ta by energetic CO{sup +} or N{sup +} ions has a strong dependence on the angle of ion incidence, which suggests a correlation between the sputtering yield and the oxidation states of Ta in the suboxide or subnitride; the higher the oxidation state of Ta, the lower is the sputtering yield. These data account for the observed etch selectivity by CO/NH{sub 3} and CH{sub 3}OH plasmas.« less

  10. Effect of postoperative peroxide bleaching on the marginal seal of composite restorations bonded with self-etch adhesives.

    PubMed

    Roubickova, A; Dudek, M; Comba, L; Housova, D; Bradna, P

    2013-01-01

    The aim of this study was to determine the effect of peroxide bleaching on the marginal seal of composite restorations bonded with several adhesive systems. Combined cylindrical Class V cavities located half in enamel and half in dentin were prepared on the buccal and lingual surfaces of human molars. The cavities were bonded with the self-etch adhesives Clearfil SE-Bond (CLF), Adper Prompt (ADP), and iBond (IBO) and an etch-and-rinse adhesive Gluma Comfort Bond (GLU) and restored with a microhybrid composite Charisma. Experimental groups were treated 25 times for eight hours per day with a peroxide bleaching gel Opalescence PF 20, while the control groups were stored in distilled water for two months and then subjected to a microleakage test using a dye penetration method. Scanning electron microscopy was used to investigate the etching and penetration abilities of the adhesives and morphology of debonded restoration-enamel interfaces after the microleakage tests. Statistical analyses were performed using nonparametric Kruskal-Wallis, Mann-Whitney, and Wilcoxon tests at p=0.05. The microleakage of all GLU groups was low and not significantly affected by peroxide bleaching. Low microleakage was recorded for CLF control groups, but after bleaching, a small but significant increase in microleakage at the enamel margin indicated its sensitivity to peroxide bleaching. For ADP and IBO control groups, the microleakage at the enamel margins was significantly higher than for GLU and CLF and exceeded that at the dentin margins. Bleaching did not induce any significant changes in the microleakage. Electron microscopy analysis indicated that in our experimental setup, decreased adhesion and mechanical resistance of the ADP- and IBO-enamel interfaces could be more important than the chemical degradation effects induced by the peroxide bleaching gel.

  11. The role of surface implant treatments on the biological behavior of SaOS-2 osteoblast-like cells. An in vitro comparative study.

    PubMed

    Conserva, Enrico; Menini, Maria; Ravera, Giambattista; Pera, Paolo

    2013-08-01

    The aim of this study was an in vitro comparison of osteoblast adhesion, proliferation and differentiation related to six dental implants with different surface characteristics, and to determine if the interaction between cells and implant is influenced by surface structure and chemical composition. Six types of implants were tested, presenting four different surface treatments: turned, sandblasted, acid-etched, anodized. The implant macro- and microstructure were analyzed using SEM, and the surface chemical composition was investigated using energy-dispersive X-ray analysis. SaOS-2 osteoblasts were used for the evaluation of cell adhesion and proliferation by SEM, and cell viability in contact with the various surfaces was determined using cytotoxicity MTT assays. Alkaline phosphatase (ALP) enzymatic activity in contact with the six surfaces was evaluated. Data relative to MTT assay and ALP activity were statistically analyzed using Kruskal-Wallis not parametric test and Nemenyi-Damico-Wolfe-Dunn post hoc test. All the implants tested supported cell adhesion, proliferation and differentiation, revealing neither organic contaminants nor cytotoxicity effects. The industrial treatments investigated changed the implant surface microscopic aspect and SaOS-2 cell morphology appeared to be influenced by the type of surface treatment at 6, 24, and 72 h of growth. SaOS-2 cells spread more rapidly on sandblasted surfaces. Turned surfaces showed the lowest cell proliferation at SEM observation. Sandblasted surfaces showed the greatest ALP activity values per cell, followed by turned surfaces (P < 0.05). On the base of this in vitro investigation, differently surfaced implants affected osteoblast morphology, adhesion, proliferation, and differentiation. Sandblasted surfaces promoted the most suitable osteoblast behavior. © 2012 John Wiley & Sons A/S.

  12. Shear bond strength of one-step self-etch adhesives to enamel: effect of acid pretreatment.

    PubMed

    Poggio, Claudio; Scribante, Andrea; Della Zoppa, Federica; Colombo, Marco; Beltrami, Riccardo; Chiesa, Marco

    2014-02-01

    The purposes of this study were to evaluate the effect of surface pretreatment with phosphoric acid on the enamel bond strength of four-one-step self-etch adhesives with different pH values. One hundred bovine permanent mandibular incisors were used. The materials used in this study included four-one-step self-etch adhesives with different pH values: Adper(™) Easy Bond Self-Etch Adhesive (ph = 0,8-1), Futurabond NR (ph = 1,4), G-aenial Bond (ph = 1,5), Clearfil(3) S Bond (ph = 2,7). One two-step self-etch adhesive (Clearfil SE Bond/ph = 0,8-1) was used as control. The teeth were assigned into two subgroups according to bonding procedure. In the first subgroup (n = 50), no pretreatment agent was applied. In the second subgroup (n = 50), etching was performed using 37% phosphoric acid for 30 s. After adhesive systems application, a nanohybrid composite resin was inserted into the enamel surface. The specimens were placed in a universal testing machine (Model 3343, Instron Corp., Canton, Mass., USA). After the testing procedure, the fractured surfaces were examined with an optical microscope at a magnification of 10× to determine failure modes. The adhesive remnant index (ARI) was used to assess the amount of adhesive left on the enamel surface. Descriptive statistics of the shear bond strength and frequency distribution of ARI scores were calculated. Enamel pretreatment with phosphoric acid significantly increased bond strength values of all the adhesives tested. No significant differences in bond strength were detected among the four different one-step self-etch adhesives with different pH. Two-step self-etch adhesive showed the highest bond strength. © 2013 John Wiley & Sons A/S.

  13. Effect of hydrofluoric acid surface treatments on micro-shear bond strength of CAD/CAM ceramics

    PubMed Central

    Mokhtarpour, Faraneh; Alaghehmand, Homayoon; Khafri, Soraya

    2017-01-01

    Introduction Dental ceramics are appreciated as highly esthetic restorative materials that can simulate the appearance of natural dentition better than other materials. The aim of this study was to evaluate the effect of hydrofluoric acid concentration and etching time on micro-shear bond strength (μSBS) to IPS e.max CAD and Vita Mark II of a dual cured resin cement (Panavia F2.0). Methods This study was an experimental in vitro study, performed in the dental material research center of Babol University of Medical Sciences in 2016. Two hydrofluoric acid concentrations (5% and 10%) and three different etching times (20, 60 and 120 seconds) were used to etch the specimens respectively. A silane coupling agent (Clearfil porcelain activator) and priming and bonding agent (Clearfil SE bond) were used on the etched surfaces in accordance to the manufacturer’s instructions of use. Then resin cement was applied on the prepared ceramic surfaces and light cured. μSBS between resin cement and the porcelains were measured with a universal testing machine. Mode of failure was observed with 40× magnification by means of a Stereo microscope. Data were analyzed with ANOVA and independent-samples t-test and Chi-square tests. Results In both e.max and Vita Mark II groups, μSBS were not significantly different when different etching times (one-way ANOVA) and HF acid concentrations (Independent-samples t-test) were used (p>0.05), but the highest μSBS was shown in e.max specimens etched 60 s with 5% HF and Vita Mark II specimens etched 20 s with 10% HF. μSBS of e.max was significantly higher than Vita Mark II (p=0.00). Conclusion Best surface treatment for e.max and Vita Mark II ceramics is 20 s etch using 5 % hydrofluoric acid. PMID:29238488

  14. Plasma-Etching of Spray-Coated Single-Walled Carbon Nanotube Films for Biointerfaces

    NASA Astrophysics Data System (ADS)

    Kim, Joon Hyub; Lee, Jun-Yong; Min, Nam Ki

    2012-08-01

    We present an effective method for the batch fabrication of miniaturized single-walled carbon nanotube (SWCNT) film electrodes using oxygen plasma etching. We adopted the approach of spray-coating for good adhesion of the SWCNT film onto a pre-patterned Pt support and used O2 plasma patterning of the coated films to realize efficient biointerfaces between SWCNT surfaces and biomolecules. By these approaches, the SWCNT film can be easily integrated into miniaturized electrode systems. To demonstrate the effectiveness of plasma-etched SWCNT film electrodes as biointerfaces, Legionella antibody was selected as analysis model owing to its considerable importance to electrochemical biosensors and was detected using plasma-etched SWCNT film electrodes and a 3,3',5,5'-tetramethyl-benzidine dihydrochloride/horseradish peroxidase (TMB/HRP) catalytic system. The response currents increased with increasing concentration of Legionella antibody. This result indicates that antibodies were effectively immobilized on plasma-etched and activated SWCNT surfaces.

  15. Integration of Electrodeposited Ni-Fe in MEMS with Low-Temperature Deposition and Etch Processes

    PubMed Central

    Schiavone, Giuseppe; Murray, Jeremy; Perry, Richard; Mount, Andrew R.; Desmulliez, Marc P. Y.; Walton, Anthony J.

    2017-01-01

    This article presents a set of low-temperature deposition and etching processes for the integration of electrochemically deposited Ni-Fe alloys in complex magnetic microelectromechanical systems, as Ni-Fe is known to suffer from detrimental stress development when subjected to excessive thermal loads. A selective etch process is reported which enables the copper seed layer used for electrodeposition to be removed while preserving the integrity of Ni-Fe. In addition, a low temperature deposition and surface micromachining process is presented in which silicon dioxide and silicon nitride are used, respectively, as sacrificial material and structural dielectric. The sacrificial layer can be patterned and removed by wet buffered oxide etch or vapour HF etching. The reported methods limit the thermal budget and minimise the stress development in Ni-Fe. This combination of techniques represents an advance towards the reliable integration of Ni-Fe components in complex surface micromachined magnetic MEMS. PMID:28772683

  16. DOE Office of Scientific and Technical Information (OSTI.GOV)

    Saxena, Shailendra K., E-mail: phd1211512@iiti.ac.in; Sahu, Gayatri; Sagdeo, Pankaj R.

    Quantum confinement effect has been studied in cheese like silicon nano-structures (Ch-SiNS) fabricated by metal induced chemical etching using different etching times. Scanning electron microscopy is used for the morphological study of these Ch-SiNS. A visible photoluminescence (PL) emission is observed from the samples under UV excitation at room temperature due to quantum confinement effect. The average size of Silicon Nanostructures (SiNS) present in the samples has been estimated by bond polarizability model using Raman Spectroscopy from the red-shift observed from SiNSs as compared to its bulk counterpart. The sizes of SiNS present in the samples decreases as etching timemore » increase from 45 to 75 mintunes.« less

  17. Dry etching, surface passivation and capping processes for antimonide based photodetectors

    NASA Astrophysics Data System (ADS)

    Dutta, Partha; Langer, Jeffery; Bhagwat, Vinay; Juneja, Jasbir

    2005-05-01

    III-V antimonide based devices suffer from leakage currents. Surface passivation and subsequent capping of the surfaces are absolutely essential for any practical applicability of antimonide based devices. The quest for a suitable surface passivation technology is still on. In this paper, we will present some of the promising recent developments in this area based on dry etching of GaSb based homojunction photodiodes structures followed by various passivation and capping schemes. We have developed a damage-free, universal dry etching recipe based on unique ratios of Cl2/BCl3/CH4/Ar/H2 in ECR plasma. This novel dry plasma process etches all III-V compounds at different rates with minimal damage to the side walls. In GaSb based photodiodes, an order of magnitude lower leakage current, improved ideality factor and higher responsivity has been demonstrated using this recipe compared to widely used Cl2/Ar and wet chemical etch recipes. The dynamic zero bias resistance-area product of the Cl2/BCl3/CH4/Ar/H2 etched diodes (830 Ω cm2) is higher than the Cl2/Ar (300 Ω cm2) and wet etched (330 Ω cm2) diodes. Ammonium sulfide has been known to passivate surfaces of III-V compounds. In GaSb photodiodes, the leakage current density reduces by a factor of 3 upon sulfur passivation using ammonium sulfide. However, device performance degrades over a period of time in the absence of any capping or protective layer. Silicon Nitride has been used as a cap layer by various researchers. We have found that by using silicon nitride caps, the devices exhibit higher leakage than unpassivated devices probably due to plasma damage during SiNx deposition. We have experimented with various polymers for capping material. It has been observed that ammonium sulfide passivation when combined with parylene capping layer (150 Å), devices retain their improved performance for over 4 months.

  18. Catalytically-etched hexagonal boron nitride flakes and their surface activity

    NASA Astrophysics Data System (ADS)

    Kim, Do-Hyun; Lee, Minwoo; Ye, Bora; Jang, Ho-Kyun; Kim, Gyu Tae; Lee, Dong-Jin; Kim, Eok-Soo; Kim, Hong Dae

    2017-04-01

    Hexagonal boron nitride (h-BN) is a ceramic compound which is thermally stable up to 1000 °C in air. Due to this, it is a very challenging task to etch h-BN under air atmosphere at low temperature. In this study, we report that h-BN flakes can be easily etched by oxidation at 350 °C under air atmosphere in the presence of transition metal (TM) oxide. After selecting Co, Cu, and Zn elements as TM precursors, we simply oxidized h-BN sheets impregnated with the TM precursors at 350 °C in air. As a result, microscopic analysis revealed that an etched structure was created on the surface of h-BN flakes regardless of catalyst type. And, X-ray diffraction patterns indicated that the air oxidation led to the formation of Co3O4, CuO, and ZnO from each precursor. Thermogravimetric analysis showed a gradual weight loss in the temperature range where the weight of h-BN flakes increased by air oxidation. As a result of etching, pore volume and pore area of h-BN flakes were increased after catalytic oxidation in all cases. In addition, the surface of h-BN flakes became highly active when the h-BN samples were etched by Co3O4 and CuO catalysts. Based on these results, we report that h-BN flakes can be easily oxidized in the presence of a catalyst, resulting in an etched structure in the layered structure.

  19. Bond strength with various etching times on young permanent teeth

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Wang, W.N.; Lu, T.C.

    1991-07-01

    Tensile bond strengths of an orthodontic resin cement were compared for 15-, 30-, 60-, 90-, or 120-second etching times, with a 37% phosphoric acid solution on the enamel surfaces of young permanent teeth. Fifty extracted premolars from 9- to 16-year-old children were used for testing. An orthodontic composite resin was used to bond the bracket directly onto the buccal surface of the enamel. The tensile bond strengths were tested with an Instron machine. Bond failure interfaces between bracket bases and teeth surfaces were examined with a scanning electron microscope and calculated with mapping of energy-dispersive x-ray spectrometry. The results ofmore » tensile bond strength for 15-, 30-, 60-, or 90-second etching times were not statistically different. For the 120-second etching time, the decrease was significant. Of the bond failures, 43%-49% occurred between bracket and resin interface, 12% to 24% within the resin itself, 32%-40% between resin and tooth interface, and 0% to 4% contained enamel fragments. There was no statistical difference in percentage of bond failure interface distribution between bracket base and resin, resin and enamel, or the enamel detachment. Cohesive failure within the resin itself at the 120-second etching time was less than at other etching times, with a statistical significance. To achieve good retention, to decrease enamel loss, and to reduce moisture contamination in the clinic, as well as to save chairside time, a 15-second etching time is suggested for teenage orthodontic patients.« less

  20. An in vitro evaluation of the responses of human osteoblast-like SaOs-2 cells on SLA titanium surfaces irradiated by different powers of CO2 lasers.

    PubMed

    Ayubianmarkazi, Nader; Karimi, Mohammadreza; Koohkan, Shima; Sanasa, Armand; Foroutan, Tahereh

    2015-11-01

    Bacterial biofilms have been identified as the primary etiological factor for the development and progression of peri-implantitis. Lasers have been shown to remove bacterial plaque from titanium surfaces effectively and can restore its biocompatibility without damaging these surfaces. Therefore, the aim of this study was to evaluate the responses (i.e., the cell viability and morphology) of human osteoblast-like SaOs-2 cells to sandblasted, large grit, and acid-etched (SLA) titanium surfaces irradiated by CO2 lasers at two different power outputs. A total of 24 SLA disks were randomly radiated by CO2 lasers at either 6 W (group 1, 12 disks) or 8 W (group 2, 12 disks). Non-irradiated disks were used as a control group (four disks). The cell viability rates of the SaOs-2 cells in the control and study groups (6 and 8 W) were 0.33 ± 0.00, 0.24 ± 0.11, and 0.2372 ± 0.09, respectively (P < 0.6). Cells with cytoplasmic extensions and spreading morphology were most prominent in the control group (141.00 ± 29.00), while in the study groups (6 and 8 W), the number of cells with such morphology was 60.40 ± 26.00 and 35.20 ± 5.40, respectively (P < 0.005). Within the limits of this study, it may be concluded that the use of CO2 lasers with the aforementioned setting parameters could not be recommended for decontamination of SLA titanium surfaces.

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