Green Synthesis of Magnetite (Fe3O4) Nanoparticles Using Seaweed ( Kappaphycus alvarezii) Extract

NASA Astrophysics Data System (ADS)

Yew, Yen Pin; Shameli, Kamyar; Miyake, Mikio; Kuwano, Noriyuki; Bt Ahmad Khairudin, Nurul Bahiyah; Bt Mohamad, Shaza Eva; Lee, Kar Xin

2016-06-01

In this study, a simple, rapid, and eco-friendly green method was introduced to synthesize magnetite nanoparticles (Fe3O4-NPs) successfully. Seaweed Kappaphycus alvarezii ( K. alvarezii) was employed as a green reducing and stabilizing agents. The synthesized Fe3O4-NPs were characterized with X-ray diffraction (XRD), ultraviolet-visible spectroscopy (UV-Vis), Fourier transform infrared (FT-IR), and transmission electron microscopy (TEM) techniques. The X-ray diffraction planes at (220), (311), (400), (422), (511), (440), and (533) were corresponding to the standard Fe3O4 patterns, which showed the high purity and crystallinity of Fe3O4-NPs had been synthesized. Based on FT-IR analysis, two characteristic absorption peaks were observed at 556 and 423 cm-1, which proved the existence of Fe3O4 in the prepared nanoparticles. TEM image displayed the synthesized Fe3O4-NPs were mostly in spherical shape with an average size of 14.7 nm.

Green Synthesis of Magnetite (Fe3O4) Nanoparticles Using Seaweed (Kappaphycus alvarezii) Extract.

PubMed

Yew, Yen Pin; Shameli, Kamyar; Miyake, Mikio; Kuwano, Noriyuki; Bt Ahmad Khairudin, Nurul Bahiyah; Bt Mohamad, Shaza Eva; Lee, Kar Xin

2016-12-01

In this study, a simple, rapid, and eco-friendly green method was introduced to synthesize magnetite nanoparticles (Fe3O4-NPs) successfully. Seaweed Kappaphycus alvarezii (K. alvarezii) was employed as a green reducing and stabilizing agents. The synthesized Fe3O4-NPs were characterized with X-ray diffraction (XRD), ultraviolet-visible spectroscopy (UV-Vis), Fourier transform infrared (FT-IR), and transmission electron microscopy (TEM) techniques. The X-ray diffraction planes at (220), (311), (400), (422), (511), (440), and (533) were corresponding to the standard Fe3O4 patterns, which showed the high purity and crystallinity of Fe3O4-NPs had been synthesized. Based on FT-IR analysis, two characteristic absorption peaks were observed at 556 and 423 cm(-1), which proved the existence of Fe3O4 in the prepared nanoparticles. TEM image displayed the synthesized Fe3O4-NPs were mostly in spherical shape with an average size of 14.7 nm.

Micro-Raman and FT-IR spectroscopic studies of ceramic shards excavated from ancient Stratonikeia city at Eskihisar village in West-South Turkey

NASA Astrophysics Data System (ADS)

Bahçeli, Semiha; Güleç, Gamze; Erdoğan, Hasan; Söğüt, Bilal

2016-02-01

In this study, micro-Raman and Fourier transformed infrared (FT-IR) spectroscopies, X-ray diffraction (XRD) and scanning electron microscope with energy dispersive X-ray (SEM-EDX) were used to characterize the mineralogical structures of pigments of four ceramic fragments in which one of them belongs to Hellenistic period (1st - IVth century BC) and other three ceramic shards belong to Early Rome (IVth century BC- 1st century AD) excavated from Stratonikeia ancient city. In the results of investigations on these four ceramic fragments, the various phases were identified: quartz, kaolinite, albit (or Na-feldspar), calcite, anastase, hematite and magnetite. Furthermore, the obtained findings indicate that firing temperature is about 800-850 °C for all the shards.

A novel method for the elaboration of hydroxyapatite with high purity by sol-gel using the albumin and comparison with the classical methods

NASA Astrophysics Data System (ADS)

Mohammed, Eddya; Bouazza, Tbib; Khalil, El-Hami

2018-02-01

In this paper, we report the first synthesis of hydroxyapatite (Hap) by sol-gel using the albumin (egg white) compared with the four classical elaboration methods such as co-precipitation, solid state, and solid-liquid samples of hydroxyapatite. We use a reference sample of hydroxyapatite bought from Fluka Chemika company (Lot and Filling code 385330/1 14599). All samples are characterized by X-ray diffraction (XRD), Uv-visible spectroscopy (Uv-Vis), and Fourier transforms infrared spectroscopy (FT-IR). The XRD study showed the existence of a Hexagonal phase for all our samples prepared in our laboratory and an orthorhombic phase for the Fulka Chemika sample of Hap (Lot and Filling code 385330/1 14599). The study by Uv-visible spectroscopy was performed to determine and compare the optical gap and the disorder of each sample of Hap. The FT-IR spectroscopy demonstrated that all our Hap samples had a similar mode of vibration of the chemical bonds (OH-) and (PO4)3-.

Thermal, structural, functional, optical and magnetic studies of pure and Ba doped CdO nanoparticles.

PubMed

Sivakumar, S; Venkatesan, A; Soundhirarajan, P; Khatiwada, Chandra Prasad

2015-12-05

In this research, a chemical precipitation method was used to synthesize undoped and doped cadmium oxide nanoparticles and studied by TG-DTA, XRD, FT-IR, SEM, with EDX and antibacterial activities, respectively. The melting points, thermal stability and the kinetic parameters like entropy (ΔS), enthalpy (ΔH), Gibb's energy (ΔG), activation energy (E), frequency factor (A) were evaluated from TG-DTA measurements. X-ray diffraction analysis (XRD) brought out the information about the synthesized products exist in spherical in shape with cubic structure. The functional groups and band area of the samples were established by Fourier transform infrared (FT-IR) spectroscopy. The direct and indirect band gap energy of pure and doped samples were determined by UV-Vis-DRS. The surface morphological, elemental compositions and particles sizes were evaluated by scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS). Finally, antibacterial activities indicated the Gram-positive and Gram-negative bacteria are more active in transporter, dehydrogenize and periplasmic enzymatic activities of pure and doped samples. Copyright © 2015 Elsevier B.V. All rights reserved.

One-step synthesis and characterizations of cerium oxide nanoparticles in an ambient temperature via Co-precipitation method

NASA Astrophysics Data System (ADS)

Pujar, Malatesh S.; Hunagund, Shirajahammad M.; Desai, Vani R.; Patil, Shivaprasadgouda; Sidarai, Ashok H.

2018-04-01

We report the simple Co-precipitation method for the synthesis of Cerium oxide (CeO2) nanoparticles (NPs) in an ambient temperature. We have taken the Cerium (III) nitrate hexahydrate (Ce(NO3)3.6H2O) and Sodium hydroxide (NaOH) as the precursors. The obtained NPs were analyzed using the UV-Vis spectrophotometer, Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD). The obtained results signify that UV-Vis spectrum exhibited a well-defined absorption peak at 274 nm and the estimated energy gap (Eg) is 4.05 eV. The FT-IR analysis provides the supporting evidence for the presence of bonding of O-H, nitrates, alcohols and O-Ce-O vibrations. The XRD result reveals that the synthesized CeO2 NPs was crystallite with cubic phase structure and the estimated average crystallite size of CeO2 NPs using Scherer's and W-H method was significantly different due to their assumptions. Further, it is purposed to study their photocatalytic biological activities.

Synthesis, molecular structure, FT-IR and XRD investigations of 2-(4-chlorophenyl)-2-oxoethyl 2-chlorobenzoate: a comparative DFT study.

PubMed

Chidan Kumar, C S; Fun, Hoong Kun; Tursun, Mahir; Ooi, Chin Wei; Chandraju, Siddegowda; Quah, Ching Kheng; Parlak, Cemal

2014-04-24

2-(4-Chlorophenyl)-2-oxoethyl 2-chlorobenzoate has been synthesized, its structural and vibrational properties have been reported using FT-IR and single-crystal X-ray diffraction (XRD) studies. The conformational analysis, optimized geometric parameters, normal mode frequencies and corresponding vibrational assignments of the synthesized compound (C15H10Cl2O3) have been examined by means of Becke-3-Lee-Yang-Parr (B3LYP) density functional theory (DFT) method together with 6-31++G(d,p) basis set. Furthermore, reliable conformational investigation and vibrational assignments have been made by the potential energy surface (PES) and potential energy distribution (PED) analyses, respectively. Calculations are performed with two possible conformations. The title compound crystallizes in orthorhombic space group Pbca with the unit cell dimensions a=12.312(5) Å, b=8.103(3) Å, c=27.565(11) Å, V=2750.0(19) Å(3). B3LYP method provides satisfactory evidence for the prediction of vibrational wavenumbers and structural parameters. Copyright © 2014 Elsevier B.V. All rights reserved.

XRD and FTIR studies the effect of heat treatment and doping the transition metal oxide on LiNbO3 and LiNb3O8 nano-crystallite phases in lithium borate glass system.

PubMed

Kashif, Ismail; Soliman, Ashia A; Sakr, Elham M; Ratep, Asmaa

2013-09-01

Glasses of various compositions in the system 90 Li2B4O7-10 Nb2O5 mixed with T.M ions (where T.M is the transition metal) were prepared by quenching technique. Heat-treatment of the parent glasses was performed at 540, 570 and 620 °C, for 5 and 16 h. The glass structure evolution during the controlled crystallization was examined by XRD and FT-IR spectroscopy analysis. The crystalline phases present in the glass ceramics were identified via X-ray diffraction as a function of heat treatment. The FT-IR data propose for these glasses and heat-treated glass network structures mainly built by: di-, tri-, tetra-, penta-and ortho-borate groups. It was found that the quantitative evolution of these various borate species in the glass structures is influenced by the transition metal. A detailed discussion relating to the N4 evolution with the T.M content was made. Copyright © 2013 Elsevier B.V. All rights reserved.

Synthesis and characterization of fluorapatite-titania (FAp-TiO 2) nanocomposite via mechanochemical process

NASA Astrophysics Data System (ADS)

Ebrahimi-Kahrizsangi, Reza; Nasiri-Tabrizi, Bahman; Chami, Akbar

2010-09-01

In this paper, synthesis of bionanocomposite of fluorapatite-titania (FAp-TiO 2) was studied by using one step mechanochemical process. Characterization of the products was accomplished by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, energy dispersive X-ray spectroscopy (EDX), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) techniques. Based on XRD patterns and FT-IR spectroscopy, correlation between the structural features of the nanostructured FAp-TiO 2 and the process conditions was discussed. Variations in crystallite size, lattice strain, and volume fraction of grain boundary were investigated during milling and the following heat treatment. Crystallization of the nanocomposite occurred after thermal treatment at 650 °C. Morphological features of powders were influenced by the milling time. The resulting FAp-20 wt.%TiO 2 nanocomposite powder exhibited an average particle size of 15 nm after 20 h of milling. The results show that the one step mechanosynthesis technique is an effective route to prepare FAp-based nanocomposites with excellent morphological and structural features.

Polyaniline-Cadmium Ferrite Nanostructured Composite for Room-Temperature Liquefied Petroleum Gas Sensing

NASA Astrophysics Data System (ADS)

Kotresh, S.; Ravikiran, Y. T.; Tiwari, S. K.; Vijaya Kumari, S. C.

2017-08-01

We introduce polyaniline-cadmium ferrite (PANI-CdFe2O4) nanostructured composite as a room-temperature-operable liquefied petroleum gas (LPG) sensor. The structure of PANI and the composite prepared by chemical polymerization was characterized by Fourier-transform infrared (FT-IR) spectroscopy, x-ray diffraction (XRD) analysis, and field-emission scanning electron microscopy. Comparative XRD and FT-IR analysis confirmed CdFe2O4 embedded in PANI matrix with mutual interfacial interaction. The nanostructure of the composite was confirmed by transmission electron microscopy. A simple LPG sensor operable at room temperature, exclusively based on spin-coated PANI-CdFe2O4 nanocomposite, was fabricated with maximum sensing response of 50.83% at 1000 ppm LPG. The response and recovery time of the sensor were 50 s and 110 s, respectively, and it was stable over a period of 1 month with slight degradation of 4%. The sensing mechanism is discussed on the basis of the p- n heterojunction barrier formed at the interface of PANI and CdFe2O4.

Green synthesis of silver nanoparticles using tannins

NASA Astrophysics Data System (ADS)

Raja, Pandian Bothi; Rahim, Afidah Abdul; Qureshi, Ahmad Kaleem; Awang, Khalijah

2014-09-01

Colloidal silver nanoparticles were prepared by rapid green synthesis using different tannin sources as reducing agent viz. chestnut (CN), mangrove (MG) and quebracho (QB). The aqueous silver ions when exposed to CN, MG and QB tannins were reduced which resulted in formation of silver nanoparticles. The resultant silver nanoparticles were characterized using UV-Visible, X-ray diffraction (XRD), scanning electron microscopy (SEM/EDX), and transmission electron microscopy (TEM) techniques. Furthermore, the possible mechanism of nanoparticles synthesis was also derived using FT-IR analysis. Spectroscopy analysis revealed that the synthesized nanoparticles were within 30 to 75 nm in size, while XRD results showed that nanoparticles formed were crystalline with face centered cubic geometry.

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

Zhang Hui; Zou Kang; Guo Shaohuan

A nanostructural drug-inorganic clay composite involving a pharmaceutically active compound captopril (Cpl) intercalated Mg-Al-layered double hydroxides (Cpl-LDHs) with Mg/Al molar ratio of 2.06 has been assembled by coprecipitation method. Powder X-ray diffraction (XRD), Fourier transform infrared spectra (FT-IR) and Raman spectra analysis indicate a successful intercalation of Cpl between the layers with a vertical orientation of Cpl disulphide-containing S-S linkage. SEM photo indicates that as-synthesized Cpl-LDHs possess compact and non-porous structure with approximately and linked elliptical shape particles of ca. 50 nm. TG-DTA analyses suggest that the thermal stability of intercalated organic species is largely enhanced due to host-guest interactionmore » involving the hydrogen bond compared to pure form before intercalation. The in vitro release studies show that both the release rate and release percentages markedly decrease with increasing pH from 4.60 to 7.45 due to possible change of release mechanism during the release process. The kinetic simulation for the release data, and XRD and FT-IR analyses for samples recovered from release media indicate that the dissolution mechanism is mainly responsible for the release behaviour of Cpl-LDHs at pH 4.60, while the ion-exchange one is responsible for that at pH 7.45. - Graphical abstract: Based on XRD, FT-IR and Raman spectra analyses, it is suggested that captopril (Cpl) exists as its disulphide metabolites in the interlayer of Mg-Al-LDHs via hydrogen bonding between guest carboxylate function and hydroxyl group of the host layers. A schematic supramolecular structure of Cpl intercalates involving a vertical orientation of Cpl disulphide-containing S-S bond between the layers with carboxylate anions pointing to both hydroxide layers is presented.« less

The functionalization and characterization of multi-walled carbon nanotubes (MWCNTs)

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

Abdullah, Mohd Pauzi; Center of Water Analysis and Research; Zulkepli, Siti Aminah

2015-09-25

Functionalization is the process of introducing chemical functional groups on the surface of the material. In this study, a multi-walled carbon nanotube (MWCNTs) was functionalized by oxidation treatment using concentrated nitric acid. The functionalized and pristine MWCNTs were analyzed by using Fourier Transform Infrared Spectroscopy (FT-IR) and X-Ray Diffraction (XRD). The XRD patterns exhibit the graphitic properties for all samples. Besides, the XRD results also demonstrate that the percent of crystallinity of MWCNTs increases as the duration of acid treatment increases. The percent of crystallinity increases from 66% to 80% when the pristine MWCNT treated for 12 hours with additionalmore » 12 hours reflux process with nitric acid. The IR spectrum for the 12 hours-treated MWCNTs shows the formation of carboxyl functional group. Additional 12 hours reflux process with nitric acid on the 12 hours-treated MWCNTs have shown the loss of existing carboxyl group and only hydroxyl group formed.« less

The study of the changes in the biochemical and mineral contents of bones of Catla catla due to lead intoxication.

PubMed

Palaniappan, P L R M; Krishnakumar, N; Vadivelu, M; Vijayasundaram, V

2010-02-01

In the present study, an attempt has been made to analyze the changes in the biochemical and mineral contents of lead-intoxicated bones of Catla catla at subchronic (15.5 ppm) exposure, and also to determine whether the effects of Pb intoxication can be reversed with the chelating agent meso 2, 3-dimercaptosuccinic acid (DMSA) on the bones of freshwater fingerlings Catla catla by using Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), and atomic absorption spectrophotometer techniques. The FT-IR spectra of the lead-exposed bones show significant alteration in the biochemical constituents. The XRD analysis showed a decrease in crystallinity due to lead exposure. Further, the Ca, Mg, and P contents of the lead-exposed bones were less than those of the control group, and there was an increase in the mineral contents of the bones after DMSA treatment. In conclusion, the present study suggests that the subchronic lead exposure results in severe loss of bone minerals. The overall decrease in the FT-IR band intensity of Pb-exposed bones relative to the control indicates a decrease in the biochemical constituents like proteins and lipids. The increase in the band intensity after treatment with chelating agent DMSA indicates increased biochemical constituents, showing that the subchronic effects of lead can be reversed by DMSA. The amide I bands observed at 1654 cm(-1) in the present study suggest that the protein is dominated by alpha-helical structure.

Structure, spectra and thermal, mechanical, Faraday rotation properties of novel diamagnetic SeO2-PbO-Bi2O3-B2O3 glasses

NASA Astrophysics Data System (ADS)

Chen, Qiuling; Su, Kai; Li, Yantao; Zhao, Zhiwei

2018-06-01

Faraday rotation diamagnetic glass has attracted research attentions in photonics, sensing and magneto optical devices due to their high refractive index, wide transmittance in UV and Fourier transform infrared (FT-IR) range and temperature independent Faraday rotation. Selenite modified heavy metal oxides glasses with composition of xSeO2-(10-x) B2O3-45PbO-45Bi2O3 (x = 0, 1, 5 and 10mol%) and 15%SeO2-40%PbO-45%Bi2O3 have been fabricated by melt-quenching method in present study. The influence of SeO2 on glass forming ability, thermal, mechanical properties and Faraday rotation were evaluated through X-ray Diffraction (XRD), Fourier transforms infrared spectra (FT-IR), Raman, X-ray photoelectron spectroscopy (XPS), differential scanning calorimetry (DSC), Vicker's hardness and Verdet constant measurements. XRD spectra reveal that the good vitrification was achieved for glass with SeO2 amounts ≤10% even without B2O3. FT-IR, Raman and XPS spectra ascertain the existence of characteristic vibration of SeO4, SeO3, PbO4, BiO3 and BO3 units. The incorporation of SeO2 increases the connectivity of glassy network by increasing the Tg, thermal stability and mechanical hardness. The small band gap, high polarizable Se4+ ions and isolated SeO3 units contribute to Faraday rotation improvement.

Green synthesis of silver nanoparticles using marine algae Caulerpa racemosa and their antibacterial activity against some human pathogens

NASA Astrophysics Data System (ADS)

Kathiraven, T.; Sundaramanickam, A.; Shanmugam, N.; Balasubramanian, T.

2015-04-01

We present the synthesis and antibacterial activity of silver nanoparticles using Caulerpa racemosa, a marine algae. Fresh C. racemosa was collected from the Gulf of Mannar, Southeast coast of India. The seaweed extract was used for the synthesis of AgNO3 at room temperature. UV-visible spectrometry study revealed surface plasmon resonance at 413 nm. The characterization of silver nanoparticle was carried out using Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD) and transmission electron microscope (TEM). FT-IR measurements revealed the possible functional groups responsible for reduction and stabilization of the nanoparticles. X-ray diffraction analysis showed that the particles were crystalline in nature with face-centered cubic geometry.TEM micrograph has shown the formation of silver nanoparticles with the size in the range of 5-25 nm. The synthesized AgNPs have shown the best antibacterial activity against human pathogens such as Staphylococcus aureus and Proteus mirabilis. The above eco-friendly synthesis procedure of AgNPs could be easily scaled up in future for the industrial and therapeutic needs.

A novel method for the functionalization of aminoacids L-glycine, L-glutamic acid and L-arginine on maghemite/magnetite nanoparticles

NASA Astrophysics Data System (ADS)

Bruno, A. J.; Correa, J. R.; Peláez-Abellán, E.; Urones-Garrote, E.

2018-06-01

Nanoparticles of maghemite/magnetite functionalized with L-glycine, L-glutamic acid and L-arginine were synthesized by a novel method. The novel procedure consists in an alternative of that reported by Massart for the precipitation of magnetite in which the aminoacid is added in the carboxylate form. The amounts of aminoacid in the initial molar concentrations were 35%, 45% and 65% with respect to the ferrophase. The obtained nanoparticles were characterized by several techniques: X-ray diffraction (XRD), Fourier transform IR spectroscopy (FT-IR), transmission electron microscopy (TEM), Electron energy-loss spectroscopy (EELS) and magnetometry. The IR spectroscopy confirmed that the selected aminoacids were functionalized on the surface of iron oxide. XRD and EELS confirm that iron oxide consists of a maghemite-magnetite intermediate phase with an average particle size about 6 nm, which was measured by transmission electron microscopy. The superparamagnetic character of the nanoparticles was evaluated by magnetometry.

Synthesis and characterization of some metal oxide nanocrystals by microwave irradiation

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

Rashad, M.; Gaber, A.; Abdelrahim, M. A.

2013-12-16

Copper oxide and cobalt oxide (CuO, Co3O4) nanocrystals (NCs) have been successfully prepared in a short time using microwave irradiation. The resulted powders of nanocrystals (NCs) were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). Thermogravimetric analysis (TGA) measurements are also studied. Fourier-transform infrared (FT-IR) and UV–visible absorption spectroscopy of both kind of nanoparticels are illustrated. Optical absorption analysis indicated the direct band gap for both kinds of nanocrystals.

Adsorption of malachite green dye from aqueous solution on the bamboo leaf ash

NASA Astrophysics Data System (ADS)

Kuntari, Priwidyanjati, Dessyntha Anggiani

2017-12-01

Bamboo leaf ash has been developed as an adsorbent material for removal malachite green from aqueous solution. Adsorption parameters have studied are contact time and initial pH. The effect of contact time and pH were examined in the batch adsorption processes. The physicochemical characters of bamboo leaf ash were investigated by using X-Ray Diffraction (XRD) and FT-IR spectroscopy. Malachite green concentration was determined by UV-Vis spectrophotometer. FT-IR spectrogram of bamboo leaf ash shows that typical fingerprint of adsorbent material with Si-O-Si or Al-O-Al group. The X-ray diffractograms of bamboo leaf ash show that adsorbent material has a highly amorphous nature. The percentage of adsorption was showed raised with increasing contact time. The optimum removal of malachite green when the initial dye concentration, initial pH, weight of adsorbent and contact time was 20 mg/L, 7, 0.25 g and 75 minutes respectively.

A study on the stability and green synthesis of silver nanoparticles using Ziziphora tenuior (Zt) extract at room temperature.

PubMed

Sadeghi, Babak; Gholamhoseinpoor, F

2015-01-05

Biomolecules present in plant extracts can be used to reduce metal ions to nanoparticles in a single-step green synthesis process. This biogenic reduction of metal ion to base metal is quite rapid, readily conducted at room temperature and pressure, and easily scaled up. Mediated Synthesis by plant extracts is environmentally benign. The involved reducing agents include the various water soluble plant metabolites (e.g. alkaloids, phenolic compounds, terpenoids) and co-enzymes. Silver (Ag) nanoparticles have the particular focus of plant-based syntheses. Extracts of a diverse range of Ziziphora tenuior (Zt) have been successfully used in making nanoparticles. The aim of this study was to investigate the antioxidant properties of this plant and its ability to synthesize silver nanoparticles. Z.tenuior leaves were used to prepare the aqueous extract for this study. Silver nanoparticles were characterized with different techniques such as UV-vis spectroscopy, Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), Scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Transmission electron microscopy experiments showed that these nanoparticles are spherical and uniformly distributed and its size is from 8 to 40 nm. FT-IR spectroscopy revealed that silver nanoparticles were functionalized with biomolecules that have primary amine group (NH₂), carbonyl group, -OH groups and other stabilizing functional groups. X-ray diffraction pattern showed high purity and face centered cubic structure of silver nanoparticles with size of 38 nm. In addition to plant extracts, live plants can be used for the synthesis. Here were view the methods of making nanoparticles using plant extracts. The scanning electron microscopy (SEM) implies the right of forming silver nanoparticles. The results of TEM, SEM, FT-IR, UV-VIS and XRD confirm that the leaves extract of Zt can synthesis silver nanoparticles. Copyright © 2014 Elsevier B.V. All rights reserved.

The photoluminescent properties of Y2O3:Bi3+, Eu3+, Dy3+ phosphors for white-light-emitting diodes.

PubMed

Han, Xiumei; Feng, Xu; Qi, Xiwei; Wang, Xiaoqiang; Li, Mingya

2014-05-01

Bi3+, Eu3+, Dy3+ activated Y2O3 phosphors were prepared through the sol-gel process. X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectra, and photoluminescence (PL) spectra were used to characterize the resulting phosphors. The XRD patterns show the refined crystal structure of Y2O3. The energy transfer processes of Bi(3+)-Eu3+ occurred in the host lattices. The thermal stability of Y2O3:Bi3+, Eu3+, Dy3+ phosphors was studied. Under short wavelength UV excitation, the phosphors show excellent characteristic red, blue, and yellow emission with medium intensity.

Preparation and Characterization of Polyurethanes with Cross-Linked Siloxane in the Side Chain by Sol-Gel Reactions

PubMed Central

Zhao, Hui; Hao, Tong-Hui; Hu, Guo-Hua; Shi, Dean; Huang, Da; Jiang, Tao; Zhang, Qun-Chao

2017-01-01

A series of novel polyurethanes containing cross-linked siloxane in the side chain (SPU) were successfully synthesized through a sol-gel process. The SPU was composed of 0%–20% N-(n-butyl)-3-aminopropyltriethoxysilane (HDI-T) modified hexamethylene diisocynate homopolymer. The effects of HDI-T content on both the structure and properties of SPU were investigated by Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), mechanical properties tests, gel content test, water contact angle measurement and water absorption test. FT-IR, XPS and XRD results confirmed the successful incorporation of HDI-T onto polyurethanes and the formation of Si–O–Si. The surface roughness and the Si content of SPU enhanced with the increase of HDI-T content. Both crystallization and melting temperature shifted to a lower point after the incorporation of HDI-T. The hydrophobicity, tensile strength, Young’s modulus and pencil hardness overall increased with the increasing of HDI-T content, whereas the thermal stability and the elongation at break of SPU slightly decreased. PMID:28772607

A novel route for synthesis of nanocrystalline hydroxyapatite from eggshell waste.

PubMed

Siva Rama Krishna, D; Siddharthan, A; Seshadri, S K; Sampath Kumar, T S

2007-09-01

The eggshell waste has been value engineered to a nanocrystalline hydroxyapatite (HA) by microwave processing. To highlight the advantages of eggshell as calcium precursor in the synthesis of HA (OHA), synthetic calcium hydroxide was also used to form HA (SHA) following similar procedure and were compared with a commercially available pure HA (CHA). All the HAs were characterized by X-ray powder diffraction (XRD) method, Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and specific surface area measurements. Nanocrystalline nature of OHA is revealed through characteristic broad peaks in XRD patterns, platelets of length 33-50 nm and width 8-14 nm in TEM micrograph and size calculations from specific surface area measurements. FT-IR spectra showed characteristic bands of HA and additionally peaks of carbonate ions. The cell parameter calculations suggest the formation of carbonated HA of B-type. The OHA exhibits superior sinterability in terms of hardness and density than both SHA and CHA may be due to larger surface area of its spherulite structure. The in vitro dissolution study shows longer stability in phosphate buffer and cell culture test using osteoblast cells establishes biocompatibility of OHA.

Development of solid dispersions of artemisinin for transdermal delivery.

PubMed

Shahzad, Yasser; Sohail, Sadia; Arshad, Muhammad Sohail; Hussain, Talib; Shah, Syed Nisar Hussain

2013-11-30

Solid dispersions of the poorly soluble drug artemisinin were developed using polymer blends of polyvinylpyrrolidone (PVP) and polyethylene glycol (PEG) with the aim of enhancing solubility and in vitro permeation of artemisinin through skin. Formulations were characterised using a combination of molecular dynamics (MD) simulations, differential scanning calorimetry (DSC), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR). Solubility of artemisinin was determined in two solvents: de-ionised water and phosphate buffered saline (PBS; pH 7.4), while in vitro drug permeation studies were carried out using rabbit skin as a model membrane. MD simulations revealed miscibility between the drug and polymers. DSC confirmed the molecular dispersion of the drug in the polymer blend. Decrease in crystallinity of artemisinin with respect to polymer content and the absence of specific drug-polymer interactions were confirmed using XRD and FT-IR, respectively. The solubility of artemisinin was dramatically enhanced for the solid dispersions, as was the permeation of artemisinin from saturated solid-dispersion vehicles relative to that from saturated solutions of the pure drug. The study suggests that high energy solid forms of artemisinin could possibly enable transdermal delivery of artemisinin. Copyright © 2013 Elsevier B.V. All rights reserved.

Preparation and characterization of cross-linked poly (vinyl alcohol)-graphene oxide nanocomposites as an interlayer for Schottky barrier diodes

NASA Astrophysics Data System (ADS)

Badrinezhad, Lida; Bilkan, Çigdem; Azizian-Kalandaragh, Yashar; Nematollahzadeh, Ali; Orak, Ikram; Altindal, Şemsettin

2018-01-01

Cross-linked polyvinyl alcohol (PVA) graphene oxide (GO) nanocomposites were prepared by simple solution-mixing route and characterized by Raman, UV-visible and fourier transform infrared (FT-IR) spectroscopy analysis, X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques. The XRD pattern and SEM analysis showed significant changes in the nanocomposite structures, and the FT-IR spectroscopy results confirmed the chemical interaction between the GO filler and the PVA matrix. After these morphological characterizations, PVA-GO-based diodes were fabricated and their electrical properties were characterized using current-voltage (I-V) and impedance-voltage-frequency (Z-V-f) measurements at room temperature. Semilogarithmic I-V characteristics of diode showed a good rectifier behavior. The values of C and G/ω increased with decreasing frequency due to the surface/interface states (Nss) which depend on the relaxation time and the frequency of the signal. The voltage, dependent profiles of Nss and series resistance (Rs) were obtained from the methods of high-low frequency capacitance and Nicollian and Brews, respectively. The obtained values of Nss and Rs were attributed to the use of cross-linked PVA-GO interlayer at the Au/n-Si interface.

Size-dependent photocatalytic activity of La0.8Sr0.2MnO3 nanoparticles prepared by hydrothermal synthesis

NASA Astrophysics Data System (ADS)

Rahmani Afje, F.; Ehsani, M. H.

2018-04-01

Synthesize of La0.8Sr0.2MnO3 (LSMO) manganite were carried out in different particle sizes by hydrothermal method. Structural and optical properties of the prepared specimens were studied by x-ray diffraction (XRD), Fourier transform infra-red (FT-IR) spectroscopy, field emission scanning electron microscopy (FESEM), and UV–vis spectroscopy. The XRD study, coupled with the Rietveld refinement, exhibited rhombohedral structure with R-3C space group. Using the FT-IR and FESEM analyses, the perovskite structure of the samples with Nano-rod-like morphologies were inferred. Furthermore, the average sizes of 48.11, 70.99 and 111.45 nm were obtained for the ones sintered at 800, 900, and 1000 °C temperatures, respectively. The optical research showed that band gap energy is about 2.13 eV, being suitable in visible-light photocatalytic activity for water purification from dyes and toxic organic materials. The photo-degradation efficiency for decolorizing methyl orange solution (10 ppm) for various samples (100 ppm) were systematically probed and a strong relation is concluded between particle size and photocatalytic activity.

Eco-friendly synthesis of cuprous oxide (Cu2O) nanoparticles and improvement of their solar photocatalytic activities

NASA Astrophysics Data System (ADS)

Kerour, A.; Boudjadar, S.; Bourzami, R.; Allouche, B.

2018-07-01

In this work, we have synthesized cuprous oxide (Cu2O) nanoparticles with octahedral and spherical like shapes by an ecofriendly, simple and coast effective method, by using the aqueous extract of Aloe vera and copper sulfate as solvent and precursor respectively. The effect of Aloe vera aqueous extract concentration on the morphological, structural and optical properties of as synthesized nanoparticles was studied by Scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform (FT-IR) spectroscopy and UV-visible diffuse reflectance. The SEM images showing octahedral and spherical agglomeration of nanoparticles. The cubic structure of Cu2O was confirmed by XRD analysis, the crystallites size depends to the concentration of Aloe vera aqueous extract with an average size ranged between 24 and 61 nm. The FT-IR vibration measurements valid the presence of pure Cu2O in the samples. The UV-visible spectra show that the prepared cuprous oxide (Cu2O) has a gap energy estimated from 2.5 to 2.62 eV. The photocatalytic activities of the as-prepared material were highly improvement by the fast degradation of methylene blue in aqueous solution at room temperature under solar simulator irradiation.

Green synthesis and characterization of graphene nanosheets

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

Tavakoli, Farnosh; Salavati-Niasari, Masoud, E-mail: salavati@kashanu.ac.ir; Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran

Highlights: • For the first time, we have synthesized graphene nanosheets in the presence of pomegranate juice. • Here pomegranate juice was used not only as reductant but also as capping agent. • FT-IR, XRD, SEM, EDS and TEM were used to characterize the samples. • According to TEM image, graphene nanosheet is individually exfoliated after stirring for 24 h. • As shown in the TEM image, graphene monolayer is obtained. - Abstract: For the first time, we have successfully synthesized graphene nanosheets in the presence of pomegranate juice. In this approach, pomegranate juice was used not only as reductantmore » but also as capping agent to form graphene nanosheets. At first, the improved Hummer method to oxidize graphite for the synthesis of graphene oxide (GO) was applied, and then the as-produced graphene oxide was reduced by pomegranate juice to form graphene nanosheets. Fourier transformed infrared (FT-IR), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), high resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM) and raman were used to characterize the samples. The results obtained from the characterization techniques proved high purity of the final products.« less

Piper betle-mediated green synthesis of biocompatible gold nanoparticles

NASA Astrophysics Data System (ADS)

Punuri, Jayasekhar Babu; Sharma, Pragya; Sibyala, Saranya; Tamuli, Ranjan; Bora, Utpal

2012-08-01

Here, we report the novel use of the ethonolic leaf extract of Piper betle for gold nanoparticle (AuNP) synthesis. The successful formation of AuNPs was confirmed by UV-visible spectroscopy, and different parameters such as leaf extract concentration (2%), gold salt concentration (0.5 mM), and time (18 s) were optimized. The synthesized AuNPs were characterized with different biophysical techniques such as transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), and energy-dispersive X-ray spectroscopy (EDX). TEM experiments showed that nanoparticles were of various shapes and sizes ranging from 10 to 35 nm. FT-IR spectroscopy revealed that AuNPs were functionalized with biomolecules that have primary amine group -NH2, carbonyl group, -OH groups, and other stabilizing functional groups. EDX showed the presence of the elements on the surface of the AuNPs. FT-IR and EDX together confirmed the presence of biomolecules bounded on the AuNPs. Cytotoxicity of the AuNPs was tested on HeLa and MCF-7 cancer cell lines, and they were found to be nontoxic, indicating their biocompatibility. Thus, synthesized AuNPs have potential for use in various biomedical applications.

Study on antibacterial alginate-stabilized copper nanoparticles by FT-IR and 2D-IR correlation spectroscopy

PubMed Central

Díaz-Visurraga, Judith; Daza, Carla; Pozo, Claudio; Becerra, Abraham; von Plessing, Carlos; García, Apolinaria

2012-01-01

Background The objective of this study was to clarify the intermolecular interaction between antibacterial copper nanoparticles (Cu NPs) and sodium alginate (NaAlg) by Fourier transform infrared spectroscopy (FT-IR) and to process the spectra applying two-dimensional infrared (2D-IR) correlation analysis. To our knowledge, the addition of NaAlg as a stabilizer of copper nanoparticles has not been previously reported. It is expected that the obtained results will provide valuable additional information on: (1) the influence of reducing agent ratio on the formation of copper nanoparticles in order to design functional nanomaterials with increased antibacterial activity, and (2) structural changes related to the incorporation of Cu NPs into the polymer matrix. Methods Cu NPs were prepared by microwave heating using ascorbic acid as reducing agent and NaAlg as stabilizing agent. The characterization of synthesized Cu NPs by ultraviolet visible spectroscopy, transmission electron microscopy (TEM), electron diffraction analysis, X-ray diffraction (XRD), and semiquantitative analysis of the weight percentage composition indicated that the average particle sizes of Cu NPs are about 3–10 nm, they are spherical in shape, and consist of zerovalent Cu and Cu2O. Also, crystallite size and relative particle size of stabilized Cu NPs were calculated by XRD using Scherrer’s formula and FT from the X-ray diffraction data. Thermogravimetric analysis, differential thermal analysis, differential scanning calorimetry (DSC), FT-IR, second-derivative spectra, and 2D-IR correlation analysis were applied to studying the stabilization mechanism of Cu NPs by NaAlg molecules. The minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) of stabilized Cu NPs against five bacterial strains (Staphylococccus aureus ATCC 6538P, Escherichia coli ATCC 25922 and O157: H7, and Salmonella enterica serovar Typhimurium ATCC 13311 and 14028) were evaluated with macrodilution, agar dilution plate count, and well-diffusion methods. Results On the basis of the semiquantitative analysis, there was a direct correlation between the reducing agent ratio and the percentage of zerovalent Cu. This was confirmed with the statistical analysis of population of Cu NPs from TEM micrographs. At lower reducing agent ratios, two phases coexist (Cu2O and zerovalent Cu) due to incomplete reduction of copper ions by the reducing agent; however, at higher reducing agent ratios, the Cu NPs consist mainly of zerovalent Cu. Crystallite size and relative particle size of stabilized Cu NPs showed considerable differences in results and tendencies in respect to TEM analysis. However, the relative particle size values obtained from FT of XRD data agreed well with the histograms from the TEM observations. From FT results, the relative particle size and reducing agent ratio of stabilized Cu NPs showed an inverse correlation. The incomplete reduction of copper ions at lower reducing agent ratios was also confirmed by DSC studies. FT-IR and 2D-IR correlation spectra analysis suggested the first event involved in the stabilization of Cu NPs is their electrostatic interaction with –C=O of carboxylate groups of NaAlg, followed by the interaction with the available O–C–O−, and finally with the –OH groups. Bacterial susceptibility to stabilized nanoparticles was found to vary depending on the bacterial strains. The lowest MIC and MBC of stabilized Cu NPs ranged between 2 mg/L and 8 mg/L for all studied strains. Disk-diffusion studies with both E. coli strains revealed greater effectiveness of the stabilized Cu NPs compared to the positive controls (cloxacillin, amoxicillin, and nitrofurantoin). S. aureus showed the highest sensitivity to stabilized Cu NPs compared to the other studied strains. Conclusion Cu NPs were successfully synthesized via chemical reduction assisted with microwave heating. Average particle size, polydispersity, and phase composition of Cu NPs depended mainly on the reducing agent ratio. Likewise, thermal stability and antibacterial activity of stabilized Cu NPs were affected by their phase composition. Because of the carboxylate groups in polymer chains, the structural changes of stabilized Cu NPs are different from those of NaAlg. NaAlg acted as a size controller and stabilizing agent of Cu NPs, due to their ability to bind strongly to the metal surface. Our study on the stabilizing agent–dependent structural changes of stabilized NPs is helpful for wide application of NaAlg as an important biopolymer. PMID:22848180

Development of functionalized hydroxyapatite/poly(vinyl alcohol) composites

NASA Astrophysics Data System (ADS)

Stipniece, Liga; Salma-Ancane, Kristine; Rjabovs, Vitalijs; Juhnevica, Inna; Turks, Maris; Narkevica, Inga; Berzina-Cimdina, Liga

2016-06-01

Based on the well-known pharmaceutical excipient potential of poly(vinyl alcohol) (PVA) and clinical success of hydroxyapatite (HAp), the objective of this work was to fabricate functionalized composite microgranules. PVA was modified with succinic anhydride to introduce carboxyl groups (-COOH), respectively, by reaction between the -OH groups of PVA and succinic anhydride, for attachment of drug molecules. For the first time, the functionalized composite microgranules containing HAp/PVA in the ratio of 1:1 were prepared through in situ precipitation of HAp in modified PVA aqueous solutions followed by spray drying of obtained suspensions. The microgranules were characterized by Fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and differential scanning calorimetry (DSC). The presence of -COOH groups was verified by FT-IR, and the amount of functional groups added to PVA molecules (averaging 15 mol%) was determined by nuclear magnetic resonance spectroscopy (NMR). DSC results showed that modification with -COOH groups slightly decreased the thermal stability of PVA. FT-IR and XRD analysis confirmed that the resulting composites contain mainly nanocrystalline HAp and PVA. Moreover, the images taken by FE-SEM revealed that the microgranules consisted of nanosized HAp crystallites homogenously embedded in the PVA matrix. DSC measurements indicated that decomposition mechanism of the HAp/PVA differs from that of pure PVA and occurs at lower temperatures. However, the presence of HAp had minor influence on the thermal decomposition of the PVA modified with succinic anhydride. The investigation of composite microgranules confirmed interaction and integration between the HAp and PVA.

Preparation and characterization of NiW-nHA composite catalyst for hydrocracking

NASA Astrophysics Data System (ADS)

Zhou, Gang; Hou, Yongzhao; Liu, Lei; Liu, Hongru; Liu, Can; Liu, Jing; Qiao, Huiting; Liu, Wenyong; Fan, Yubo; Shen, Shituan; Rong, Long

2012-11-01

The synthesis, characterization and catalytic capability of the NiW-nano-hydroxyapatite (NiW-nHA) composite were investigated in this paper. The NiW-nHA catalyst was prepared by a co-precipitation method. Then Fourier transform infrared (FT-IR) spectroscopy, transmission electron microscopy (TEM), X-ray diffraction (XRD) and energy dispersive spectroscopy (EDX) were used to analyze this material. In addition, the catalytic capacity of the NiW-nHA composite was also examined by FT-IR and gas chromatography (GC). The results of FT-IR analysis indicated that Ni, W and nHA combined closely. TEM observation revealed that this catalyst was needle shaped and the crystal retained a nanometer size. XRD data also suggested that a new phase of CaWO4 appeared and the lattice parameters of nHA changed in this system. nHA was the carrier of metals. The rates of Ni/W-loading were 73.24% and 65.99% according to the EDX data, respectively. Furthermore, the conversion of 91.88% Jatropha oil was achieved at 360 °C and 3 MPa h-1 over NiW-nHA catalyst. The straight chain alkanes ranging from C15 to C18 were the main components in the production. The yield of C15-C18 alkanes was up to 83.56 wt%. The reaction pathway involved hydrocracking of the C&z.dbd;C bonds of these triglycerides from Jatropha oil. This paper developed a novel non-sulfided catalyst to obtain a ``green biofuel'' from vegetable oil.

Process Parameters on the Crystallization and Morphology of Hydroxyapatite Powders Prepared by a Hydrolysis Method

NASA Astrophysics Data System (ADS)

Wang, Moo-Chin; Hon, Min-Hsiung; Chen, Hui-Ting; Yen, Feng-Lin; Hung, I.-Ming; Ko, Horng-Huey; Shih, Wei-Jen

2013-07-01

The effects of process parameters on the crystallization and morphology of hydroxyapatite (Ca10(PO4)6(OH)2, HA) powders synthesized from dicalcium phosphate dihydrate (CaHPO4·2H2O, DCPD) using a hydrolysis method have been investigated. X-ray diffraction (XRD), Fourier-transform infrared (FT-IR) spectra, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED) were used to characterize the synthesized powders. When DCPD underwent hydrolysis in 2.5 NaOH solution (Na(aq)) at 303 K to 348 K (30 °C to 75 °C) for 1 hour, the XRD results revealed that HA was obtained for all the as-dried samples. The SEM morphology of the HA powders for DCPD hydrolysis produced at 348 K (75 °C) shows regular alignment and a short rod shape with a size of 200 nm in length and 50 nm in width. With DCPD hydrolysis in 2.5 M NaOH(aq) holding at 348 K (75 °C) for 1 to 24 hours, XRD results demonstrated that all samples were HA and no other phases could be detected. Moreover, the XRD results also show that all the as-dried powders still maintained the HA structure when DCPD underwent hydrolysis in 0.1 to 5 M NaOH(aq) at 348 K (75 °C) for 1 hour. Otherwise, the full transformation from HA to octa-calcium phosphate (OCP, Ca8H2(PO4)6·5H2O) occurred when hydrolysis happened in 10 M NaOH(aq). FT-IR spectra analysis revealed that some carbonated HA (Ca10(PO4)6(CO3), CHA) had formed. The SEM morphology results show that the 60 to 65 nm width of the uniformly long rods with regular alignment formed in the HA powder aggregates when DCPD underwent hydrolysis in 2.5 M NaOH(aq) at 348 K (75 °C) for 1 hour.

The effect of chemical modification on the physico-chemical characteristics of halloysite: FTIR, XRF, and XRD studies

NASA Astrophysics Data System (ADS)

Szczepanik, Beata; Słomkiewicz, Piotr; Garnuszek, Magdalena; Czech, Kamil; Banaś, Dariusz; Kubala-Kukuś, Aldona; Stabrawa, Ilona

2015-03-01

The effect of chemical modification of halloysite from a Polish strip mine "Dunino" on the chemical composition and structure of this clay mineral was studied using infrared spectroscopy (ATR FT-IR), wavelength dispersive X-ray fluorescence (WDXRF), and X-ray powder diffraction (XRPD) methods. The results obtained by the WDXRF technique confirm that the content of silica and alumina was the highest for bleached halloysite samples and the lowest for acid-treated halloysite. A higher content of Fe2O3 in comparison to halloysite samples coming from other countries was observed for raw halloysite samples. XRPD diffraction pattern obtained for raw halloysite confirmed the presence of halloysite, kaolinite, hematite, and calcite minerals in the sample. Bleaching the halloysite removes (or significantly reduces) the content of other minerals present in the raw halloysite. The FT-IR spectra of the studied halloysite samples show in the 3700-3600 cm-1 region well-defined hydroxyl stretching bands characteristic for the kaolin-group minerals and bands associated with the vibrations of the aluminium-silicon skeleton in the 1400-1000 cm-1 region. Modifying halloysite with 4-chloro-aniline causes successive incorporation of amine into the BH sample.

Grafted chromium 13-membered dioxo-macrocyclic complex into aminopropyl-based nanoporous SBA-15

NASA Astrophysics Data System (ADS)

Tarlani, Aliakbar; Joharian, Monika; Narimani, Khashayar; Muzart, Jacques; Fallah, Mahtab

2013-07-01

In a new approach, chromium (III) tetraaza dioxo ligand was grafted onto functionalized SBA-15 after four step reactions by using coordinating ability of anchored amino functionalized SBA-15. After the termination of each step, the obtained product was characterized by FT-IR, low-angle X-ray diffraction (LA-XRD), N2 adsorption-desorption isotherms (Brunauer-Emmett-Teller (BET)-Barret-Joyner-Halenda (BJH)) and thermogravimetric analysis (TGA), and used as catalyst for the efficient and regioselective alcoholysis of styrene oxide to 2-alkoxy-1-phenylethanol product at ambient temperature.

A simple method to synthesize polyhedral hexagonal boron nitride nanofibers

NASA Astrophysics Data System (ADS)

Lin, Liang-xu; Zheng, Ying; Li, Zhao-hui; shen, Xiao-nv; Wei, Ke-mei

2007-12-01

Hexagonal boron nitride (h-BN) fibers with polyhedral morphology were synthesized with a simple-operational, large-scale and low-cost method. The sample obtained was studied by X-ray photoelectron spectrometer (XPS), electron energy lose spectroscopy (EELS), X-ray powder diffraction (XRD), Fourier transformation infrared spectroscopy (FT-IR), etc., which matched with h-BN. Environment scanning electron microscopy (ESEM) and transmission electron microscope (TEM) indicated that the BN fibers possess polyhedral morphology. The diameter of the BN fibers is mainly in the range of 100-500 nm.

Solvothermal synthesis of fusiform hexagonal prism SrCO{sub 3} microrods via ethylene glycol solution

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

Shi Liange; Du Fanglin

2007-08-07

Fusiform hexagonal prism SrCO{sub 3} microrods were prepared by a simple solvothermal route at 120 deg. C, and characterized by X-ray powder diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and Fourier transform infrared (FT-IR) spectroscopy. By controlling the content of ethylene glycol (EG), it was found that ethylene glycol (EG) played an important role in the formation of such SrCO{sub 3} microrods. Finally, effects of other solvents on the products, including 1,2-propanediol and glycerin, were also investigated.

Structure and thermal decomposition of sulfated β-cyclodextrin intercalated in a layered double hydroxide

NASA Astrophysics Data System (ADS)

Wang, Ji; Wei, Min; Rao, Guoying; Evans, David G.; Duan, Xue

2004-01-01

The sodium salt of hexasulfated β-cyclodextrin has been synthesized and intercalated into a magnesium-aluminum layered double hydroxide by ion exchange. The structure, composition and thermal decomposition behavior of the intercalated material have been studied by variable temperature X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), inductively coupled plasma emission spectroscopy (ICP), and thermal analysis (TG-DTA) and a model for the structure has been proposed. The thermal stability of the intercalated sulfated β-cyclodextrin is significantly enhanced compared with the pure form before intercalation.

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

Deus, R.C.; Cortés, J.A., E-mail: leandrosrr89@gmail.com; Ramirez, M.A.

Highlights: • CeO{sub 2} nanoparticles were obtained by microwave-hydrothermal method. • Rietveld refinement reveals a cubic structure. • KOH mineralizer agent exhibit weak agglomeration at low temperature and shorter time. - Abstract: The structural and photoluminescent properties at room temperature of CeO{sub 2} and La-doped CeO{sub 2} particles were undertaken. The obtained particles were synthesized by a microwave-assisted hydrothermal method (MAH) under different lanthanum contents. X-ray diffraction (XRD), Fourier transform infrared (FT-IR), Fourier transform Raman (FT-Raman), Ultra-violet spectroscopy (UV–vis) and photoluminescence (PL) measurements were carried out. XRD revealed that the powders are free of secondary phases and crystallize in themore » cubic structure. Raman data show that increasing La doping content increase oxygen vacancies due to lattice expansion. The UV/vis absorption spectroscopy suggested the presence of intermediate energy levels in the band gap of structurally ordered powders. Lanthanum addition creates oxygen vacancies and shifts the photoluminescence in the low energy range leading to intense PL emission.« less

Efficient synthesis of highly fluorescent nitrogen-doped carbon dots for cell imaging using unripe fruit extract of Prunus mume

NASA Astrophysics Data System (ADS)

Atchudan, Raji; Edison, Thomas Nesakumar Jebakumar Immanuel; Sethuraman, Mathur Gopalakrishnan; Lee, Yong Rok

2016-10-01

Highly fluorescent nitrogen-doped carbon dots (N-CDs) were synthesized using the extract of unripe Prunus mume (P. mume) fruit by a simple one step hydrothermal-carbonization method. The N-CDs were synthesized at different pH ranges, 2.3, 5, 7, and 9. The pH of the P. mume extract was adjusted using an aqueous ammonia solution (25%). The optical properties of N-CDs were examined by UV-vis and fluorescence spectroscopy. The N-CDs synthesized at pH 9 emitted high fluorescence intensity compared to other obtained N-CDs. The N-CDs synthesized at pH 9 was further characterized by high resolution transmission electron microscopy (HR-TEM), X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and Fourier transform-infra red (FT-IR) spectroscopy. HR-TEM showed that the average size of the synthesized N-CDs was approximately 9 nm and the interlayer distance was 0.21 nm, which was validated by XRD. The graphitic nature of the synthesized N-CDs were confirmed by Raman spectroscopy. XPS and FT-IR spectroscopy confirmed the doping of the nitrogen moiety over the synthesized CDs. The synthesized nitrogen doped CDs (N-CDs) were low toxicity and were used as a staining probe for fluorescence cell imaging.

Low temperature-fired Ni-Cu-Zn ferrite nanoparticles through auto-combustion method for multilayer chip inductor applications

PubMed Central

2012-01-01

Ferrite nanoparticles of basic composition Ni0.7-xZnxCu0.3Fe2O4 (0.0 ≤ x ≤ 0.2, x = 0.05) were synthesized through auto-combustion method and were characterized for structural properties using X-ray diffraction [XRD], scanning electron microscopy, transmission electron microscopy, and Fourier transform infrared spectroscopy [FT-IR]. XRD analysis of the powder samples sintered at 600°C for 4 h showed the cubic spinel structure for ferrites with a narrow size distribution from 28 to 32 nm. FT-IR showed two absorption bands (v1 and v2) that are attributed to the stretching vibration of tetrahedral and octahedral sites. The effect of Zn doping on the electrical properties was studied using dielectric and impedance spectroscopy at room temperature. The dielectric parameters (ε', ε″, tanδ, and σac) show their maximum value for 10% Zn doping. The dielectric constant and loss tangent decrease with increasing frequency of the applied field. The results are explained in the light of dielectric polarization which is similar to the conduction phenomenon. The complex impedance shows that the conduction process in grown nanoparticles takes place predominantly through grain boundary volume. PACS: 75.50.Gg; 78.20; 77.22.Gm. PMID:22316055

Chamomile flower extract-directed CuO nanoparticle formation for its antioxidant and DNA cleavage properties.

PubMed

Duman, Fatih; Ocsoy, Ismail; Kup, Fatma Ozturk

2016-03-01

In this study, we report the synthesis of copper oxide nanoparticles (CuO NPs) using a medicinal plant (Matricaria chamomilla) flower extract as both reducing and capping agent and investigate their antioxidant activity and interaction with plasmid DNA (pBR322).The CuO NPs were characterized using Uv-Vis spectroscopy, FT-IR (Fourier transform infrared spectroscopy), DLS (dynamic light scattering), XRD (X-ray diffraction), EDX (energy-dispersive X-ray) spectroscopy and SEM (scanning electron microscopy). The CuO NPs exhibited nearly mono-distributed and spherical shapes with diameters of 140 nm size. UV-Vis absorption spectrum of CuO NPs gave a broad peak around 285 and 320 nm. The existence of functional groups on the surface of CuO NPs was characterized with FT-IR analysis. XRD pattern showed that the NPs are in the form of a face-centered cubic crystal. Zeta potential value was measured as -20 mV due to the presence of negatively charged functional groups in plant extract. Additionally, we demonstrated concentration-dependent antioxidant activity of CuO NPs and their interaction with plasmid DNA. We assumed that the CuO NPs both cleave and break DNA double helix structure. Copyright © 2015 Elsevier B.V. All rights reserved.

Synthesis, characterizations and anti-bacterial activities of pure and Ag doped CdO nanoparticles by chemical precipitation method

NASA Astrophysics Data System (ADS)

Sivakumar, S.; Venkatesan, A.; Soundhirarajan, P.; Khatiwada, Chandra Prasad

2015-02-01

In the present study, synthesized pure and Ag (1%, 2%, and 3%) doped Cadmium Oxide (CdO) nanoparticles by chemical precipitation method. Then, the synthesized products were characterized by thermo gravimetric-differential thermal analysis (TG-DTA), X-ray diffraction (XRD) analysis, Fourier transform infrared (FT-IR) spectroscopy, Ultra violet-Vis diffused reflectance spectroscopy (UV-Vis-DRS), Scanning electron microscopy (SEM), Energy dispersive X-rays (EDX) spectroscopy, and anti-bacterial activities, respectively. The transition temperatures and phase transitions of Cd(OH)2 to CdO at 400 °C was confirmed by TG-DTA analysis. The XRD patterns show the cubic shape and average particle sizes are 21, 40, 34, and 37 nm, respectively for pure and Ag doped samples. FT-IR study confirmed the presence of CdO and Ag at 677 and 459 cm-1, respectively. UV-Vis-DRS study shows the variation on direct and indirect band gaps. The surface morphologies and elemental analysis have been confirmed from SEM and with EDX. In addition, the synthesized products have been characterized by antibacterial activities against Gram-positive and negative bacteria. Further, the present investigation suggests that CdO nanoparticles have the great potential applications on various industrial and medical fields of research.

Effect of reaction atmosphere on structural and optical properties of hexagonal molybdenum oxide (h-MoO{sub 3})

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

Doss, V. Arumai; Chithambararaj, A.; Bose, A. Chandra, E-mail: acbose@nitt.edu

2016-05-23

The present work aims to synthesize single phase h-MoO{sub 3} nanocrytals by chemical precipitation method exposed under different reaction atmospheres. The reaction atmosphere have been successfully tuned as air, nitrogen and argon and studied its effects on structural, functional, morphology and optical properties by using X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy and diffuse reflectance spectroscopy (DRS) measurements. The XRD result indicates that the sample exhibits characteristic hexagonal phase of MoO{sub 3}. The crystallite size is estimated by well known Scherrer’s method. The crystallite size is relative small in the case of sample prepared atmore » argon atmosphere. The functional groups such as Mo-O, N-H and O-H are identified from FT-IR spectroscopy. The particle exhibits rod like morphology with perfect hexagonal cross-section. The optical absorption observed at 420-450 nm corresponds to fundamental optical absorption by h-MoO{sub 3}. The band gap values are estimated using Kublka-Munk (K-M) function and found to be 2. 87 eV, 2.93 eV and 2.97 eV for samples synthesized under air, nitrogen and argon, respectively.« less

Optical and structural investigation of Dy3+-Nd3+ co-doped in magnesium lead borosilicate glasses.

PubMed

Rao, T G V M; Rupesh Kumar, A; Neeraja, K; Veeraiah, N; Rami Reddy, M

2014-01-24

MgO-PbO-B2O3-SiO2-Nd2O3-Dy2O3 glasses are prepared by melt-quenching technique. The samples are characterized by X-ray diffraction (XRD), optical absorption, luminescence and Fourier transform infrared (FT-IR) spectral studied. XRD analysis evidently indicates that the prepared samples are fully amorphous nature. From the optical absorption spectra, the bonding environment surrounding the Dy(3+) and their energy level scheme in glass network is analyzed. Enhancement of Dy(3+) emission by non-radiative energy transfers from Nd(3+) has been observed here. The samples emits intensive bluish yellow color from the (4)F9/2→(6)H15/2, (6)H13/2 transition of Dy(3+) ions in these glasses which are nearer to white light and it is also supported by the chromaticity color coordinates. The FT-IR spectra reveal that network connectivity is increased with replacement of bonds B-O-B, Si-O-Si by more resistant B-O-Si bonds with gradually increasing the content of Dy(3+) ions in the glass network. Along with spectroscopic parameters some physical parameters like density, refractive index etc. are measured for the glasses. Copyright © 2013 Elsevier B.V. All rights reserved.

Biological and catalytic applications of green synthesized fluorescent N-doped carbon dots using Hylocereus undatus.

PubMed

Arul, Velusamy; Edison, Thomas Nesakumar Jebakumar Immanuel; Lee, Yong Rok; Sethuraman, Mathur Gopalakrishnan

2017-03-01

In this work, a simple hydrothermal route for the synthesis of fluorescent nitrogen doped carbon dots (N-CDs) is reported. The Hylocereus undatus (H. undatus) extract and aqueous ammonia are used as carbon and nitrogen source, respectively. The optical properties of synthesized N-CDs are analyzed using UV-Visible (UV-Vis) and fluorescence spectroscopy. The surface morphology, elemental composition, crystallinity and functional groups present in the N-CDs are examined using high resolution transmission electron microscopy (HR-TEM) with energy dispersive spectroscopy (EDS), selected area electron diffraction (SAED), X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy, respectively. The synthesized N-CDs emit strong blue fluorescence at 400nm under the excitation of 320nm. Further, the excitation dependent emission properties are also observed from the fluorescence of synthesized N-CDs. The HR-TEM results reveal that synthesized N-CDs are in spherical shape with average diameter of 2.5nm. The XRD pattern exhibits, the graphitic nature of synthesized N-CDs. The doping of nitrogen is confirmed from the EDS and FT-IR studies. The cytotoxicity and biocompatibility of N-CDs are evaluated through MTT assay on L-929 (Lymphoblastoid-929) and MCF-7 (Michigan Cancer Foundation-7) cells. The results indicate that the fluorescent N-CDs show less cytotoxicity and good biocompatibility on both L-929 and MCF-7 cells. Moreover, the N-CDs show excellent catalytic activity towards the reduction of methylene blue by sodium borohydride. Copyright © 2017 Elsevier B.V. All rights reserved.

Preparation of a novel breviscapine-loaded halloysite nanotubes complex for controlled release of breviscapine

NASA Astrophysics Data System (ADS)

Gao, Min; Lu, Liqian; Wang, Xiaoyue; Lin, Houke; Zhou, Qingsong

2017-11-01

For sustain the release rate and prolong half-life of breviscapine in vivo, the breviscapine-loaded halloysite nanotubes complex was prepared. The breviscapine was encapsulated into halloysite nanotubes (HNTs) using a vacuum process. The complex were investigated by scanning electron microscopy (SEM), differential scanning calorimetry (DSC), transmission electron microscope (TEM), X-ray diffraction (XRD) and fourier transform infrared spectroscopy(FT-IR). The formation of breviscapine-loaded HNTs complex was proved by the test results of SEM, DSC, TEM and IR analysise. The results confirmed that breviscapine was successfully loaded in the halloysite nanotubes. Additionally, the in vitro drug release of breviscapine from breviscapine-loaded HNTs complex was investigated, the result indicated this complex has apparent sustained-release effect.

Synthesis and characterization of arsenic-doped cysteine-capped thoria-based nanoparticles

NASA Astrophysics Data System (ADS)

Pereira, F. J.; Díez, M. T.; Aller, A. J.

2013-09-01

Thoria materials have been largely used in the nuclear industry. Nonetheless, fluorescent thoria-based nanoparticles provide additional properties to be applied in other fields. Thoria-based nanoparticles, with and without arsenic and cysteine, were prepared in 1,2-ethanediol aqueous solutions by a simple precipitation procedure. The synthesized thoria-based nanoparticles were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (ED-XRS), Raman spectroscopy, Fourier transform infrared (FT-IR) spectroscopy and fluorescence microscopy. The presence of arsenic and cysteine, as well as the use of a thermal treatment facilitated fluorescence emission of the thoria-based nanoparticles. Arsenic-doped and cysteine-capped thoria-based nanoparticles prepared in 2.5 M 1,2-ethanediol solutions and treated at 348 K showed small crystallite sizes and strong fluorescence. However, thoria nanoparticles subjected to a thermal treatment at 873 K also produced strong fluorescence with a very narrow size distribution and much smaller crystallite sizes, 5 nm being the average size as shown by XRD and TEM. The XRD data indicated that, even after doping of arsenic in the crystal lattice of ThO2, the samples treated at 873 K were phase pure with the fluorite cubic structure. The Raman and FT-IR spectra shown the most characteristics vibrational peaks of cysteine together with other peaks related to the bonds of this molecule to thoria and arsenic when present.

Synthesis and characterization of nano-hydroxyapatite using Sapindus Mukorossi extract

NASA Astrophysics Data System (ADS)

Subha, B.; Prasath, P. Varun; Abinaya, R.; Kavitha, R. J.; Ravichandran, K.

2015-06-01

Nano-Hydroxyapatite (HAP) powders were successfully synthesised by hydrothermal method using Sapindus Mukorossi extract as an additive. The structural and morphological analyses of thus synthesised powders were carried out using FT-IR, XRD and FESEM/EDX. The FT-IR spectra confirm the presence of phosphate and hydroxyl groups corresponding to HAP. The XRD analysis reveals the formation of HAP phase and found to reduce the crystallite size with addition of Sapindus Mukorossi extract. The morphology changes from sphere to flake shape by the influence of extract.

[Free crystalline silica: a comparison of methods for its determination in total dust].

PubMed

Maciejewska, Aleksandra; Szadkowska-Stańczyk, Irena; Kondratowicz, Grzegorz

2005-01-01

The major objective of the study was to compare and investigate the usefulness of quantitative analyses of free crystalline silica (FCS) in the assessment of dust exposure in samples of total dust of varied composition, using three methods: chemical method in common use in Poland; infrared spectrometry; and x-ray powder diffraction. Mineral composition and FCS contents were investigated in 9 laboratory samples of raw materials, materials, and industrial wastes, containing from about 2 to over 80% of crystalline silica and reduced to particles of size corresponding with that of total dust. Sample components were identified using XRD and FT-IR methods. Ten independent determinations of FCS with each of the three study methods were performed in dust samples. An analysis of linear correlation was applied to investigate interrelationship between mean FCS determinations. In analyzed dust samples, along with silica dust there were numerous minerals interfering with silica during the quantitative analysis. Comparison of mean results of FCS determinations showed that the results obtained using the FT-IR method were by 12-13% lower than those obtained with two other methods. However, the differences observed were within the limits of changeability of results associated with their precision and dependence on reference materials used. Assessment of occupational exposure to dusts containing crystalline silica can be performed on the basis of quantitative analysis of FCS in total dusts using each of the compared methods. The FT-IR method is most appropriate for the FCS determination in samples of small amount of silica or collected at low dust concentrations; the XRD method for the analysis of multicomponent samples; and the chemical method in the case of medium and high FCS contents in samples or high concentrations of dusts in the work environment.

Zn(1-x)Cu(x)O (0.02 ≤ x ≤ 0.1) Nanomaterials Prepared by Ball Milling, Citrate Sol Gel, and Molten Salt Flux Methods.

PubMed

Balamurugan, S; Melba, K

2015-06-01

The Cu doped ZnO, (Zn(1-x)Cu(x))O (x = 0.02, 0.04, 0.06, 0.08, and 0.1) nanomaterials were prepared by ball milling technique (BMT), citrate sol gel (CSG), and molten salt flux (MSF) methods. The various as-prepared (Zn(1-x)Cu(x))O materials were analyzed by powder X-ray diffraction (pXRD), FT-IR, and SEM-EDX measurements in order to check the phase formation, purity, surface morphology and elements present in the annealed materials. Due to the preparation methods as well as doping of 'x' slight variations in cell parameters are seen. The average crystalline size of CSG method shows smaller size (25-35 nm) than BMT and MSF approaches. The materials obtained by MSF technique reveal the average crystalline size in the range of 32-72 nm whereas the BMT materials exhibit 36-50 nm for the composition, 0.02 ≤ x ≤ 0.1. The presence of functional groups and the chemical bonding in (Zn(1-x)Cu(x))O system is confirmed through FT-IR measurements. It is evident from the FT-IR data that bands seen at 400-500 cm(-1) are characteristics of M-O (M = metal ion) bonding in the studied materials. The micro images observed by SEM exhibiting polycrystalline character as compared with the crystallite size obtained from XRD. Among the three approaches employed in the present investigations, in terms of average particle size the CSG method may be concluded as an efficient method for the preparation of Zn(1-x)Cu(x)O nanomaterials.

H3PW12O40 Encapsulation by Nanoporous Metal Organic Framework HKUST-1: Synthesis, Characterization, Activity and Stability.

PubMed

Rafiee, Ezzat; Nobakht, Narges

2016-01-01

Hybrid composite material was obtained through encapsulation of H3PW12O40 (PW) into HKUST-1 (Cu3(BTC)2, BTC = 1,3,5-benzenetricarboxylic acid), in molar composition of 5 Cu(NO3)2 · 3H2O/2.8 BTC/0.3 PW/0.6 CTAB by adding solutions of PW and copper salts to mixture of BTC and surfactant. The catalyst was characterized by various techniques including powder X-ray diffraction (XRD), Fourier transform infrared (FT-IR), scanning electron microscopy (SEM), energy dispersive X-ray (EDX), laser particle size analyzer, Brunauer Emmett-Teller (BET). The acidity of the catalyst was measured by a potentiometric titration with n-butylamine and PW/HKUST-1 presented very strong acidic sites with Ei > 100 mV. This nano catalyst was successfully used for the synthesis of various β-keto enol ethers at 45 °C with 51-98% yield after 5-75 min. The catalyst was easily recycled and reused at least four times without significant loss of its activity (94% yield after forth run). The presence of the PW in PW/HKUST-1 and reused PW/HKUST-1 structure, eliminating any doubt about collapse of the HKUST-1 after catalytic reaction and can be followed by FT-IR, XRD and SEM techniques. Brönsted and Lewis acidity of the PW/HKUST-1 catalyst was distinguished by studying the FT-IR and determined by chemisorption of pyridine. The strength and dispersion of the protons on PW/HKUST-1 was considerably high and active surface protons became more available for reactant.

Preparation and characterization of biomimetic silk fibroin/chitosan composite nanofibers by electrospinning for osteoblasts culture.

PubMed

Chen, Jyh-Ping; Chen, Shih-Hsien; Lai, Guo-Jyun

2012-03-06

In this study, we have successfully fabricated electrospun bead-free silk fibroin [SF]/chitosan [CS] composite nanofibers [NFs] covering the whole range of CS content (0%, 25%, 50%, 75%, and 100%). SF/CS spinning solutions were prepared in a mixed solvent system of trifluoroacetic acid [TFA] and dichloromethane. The morphology of the NFs was observed by scanning electron microscope, and the average fiber diameter ranges from 215 to 478 nm. Confocal laser scanning microscopy confirms the uniform distribution of SF and CS within the composite NFs. To increase biocompatibility and preserve nanostructure when seeded with cells in culture medium, NFs were treated with an ethanol/ammonia aqueous solution to remove residual TFA and to change SF protein conformation. After the chemical treatment, SF/CS NFs could maintain the original structure for up to 54 days in culture medium. Properties of pristine and chemically treated SF/CS NFs were investigated by Fourier transform infrared spectroscopy [FT-IR], X-ray diffraction [XRD], and thermogravimetry/differential scanning calorimetry [TG/DSC]. Shift of absorption peaks in FT-IR spectra confirms the conformation change of SF from random coil to β-sheet by the action of ethanol, which is also consistent with the SF crystalline diffraction patterns measured by XRD. From TG/DSC analysis, the decomposition temperature peaks due to salt formation from TFA and protonated amines disappeared after chemical treatment, indicating complete removal of TFA by binding with ammonium ions during the treatment. This was also confirmed with the disappearance of F1s peak in X-ray photoelectron spectroscopy spectra and disappearance of TFA salt peaks in FT-IR spectra. The composite NFs could support the growth and osteogenic differentiation of human fetal osteoblastic [hFOB] cells, but each component in the composite NF shows distinct effect on cell behavior. SF promotes hFOB proliferation while CS enhances hFOB differentiation. The composite SF/CS NFs will be suitable for bone tissue engineering applications by choosing a suitable blend composition.PACS: 87.85.jf; 87.85.Rs; 68.37.Hk.

Synthesis and Thermal and Photo Behaviors of New Polyamide/Organocaly Nanocomposites Containing Para Phenylenediacrylic Moiety

NASA Astrophysics Data System (ADS)

Faghihi, Khalil; Soleimani, Masoumeh; Shabanian, Meisam; Abootalebi, Ashraf Sadat

2011-06-01

New type of aromatic polyamide/montmorillonite nanocomposites were produced using solution process in N-methyl-2-pyrolidone. Amide chains were synthesized from 4,4'-diaminodiphenyl sulfone and p-phenylenediacrylic acid in N-methyl-2-pyrolidone. The resulting nanocomposite films containing 5-15 mass % of organoclay were characterized for FT-IR, scanning electronmicroscopy (SEM), X-ray diffraction (XRD), thermogravimetric analysis (TGA), optical transparency and water absorption measurements. The distribution of organoclay and nanostructure of the composites were investigated by (XRD) and SEM analyses. Thermogravimetric analysis indicated an increase in thermal stability of nanocomposites as compared to pristine polyamide. The percentage optical transparency and water absorption of these hybrids was found to be much reduced upon the addition of modified layered silicate indicating decreased permeability.

Synthesis and characterization of high-quality cobalt vanadate crystals and their applications in lithium-ion batteries

NASA Astrophysics Data System (ADS)

Bhuiyan, Md. Tofajjol Hossen; Rahman, Md. Afjalur; Rahman, Md. Atikur; Sultana, Rajia; Mostafa, Md. Rakib; Tania, Asmaul Husna; Sarker, Md. Abdur Razzaque

2016-12-01

High-quality cobalt vanadate crystals have been synthesized by solid-state reaction route. Structure and morphology of the synthesized powders were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), and Fourier transform infrared (FT-IR) spectroscopy. The XRD patterns revealed that the as prepared materials are of high crystallinity and high quality. The SEM images showed that the crystalline CoV2O6 material is very uniform and well separated, with particle (of) area 252 μm. The electronic and optical properties were investigated by impedance analyzer and UV-visible spectrophotometer. Temperature-dependent electrical resistivity was measured using four-probe technique. The crystalline CoV2O6 material is a semiconductor and its activation energy is 0.05 eV.

Spectroscopic characterization of nanohydroxyapatite synthesized by molten salt method.

PubMed

Gopi, D; Indira, J; Kavitha, L; Kannan, S; Ferreira, J M F

2010-10-01

Hydroxyapatite (HAP) nanopowders were synthesized by molten salt method at 260 degrees C. The as-prepared powders were characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscope (SEM) and thermo gravimetric analysis (TGA). With the aid of the obtained results the effect of calcining time on the crystallinity, size and morphology of HAP nanopowders is presented. The HAP nanopowders synthesized by molten salt method consist of pure phase of HAP without any impurities and showed the rod-like morphology without detectable decomposition up to 1100 degrees C. Copyright 2010 Elsevier B.V. All rights reserved.

Fabrication of silica hollow particles using yeast cells as a template

NASA Astrophysics Data System (ADS)

Liao, Shenglan; Lin, Liqin; Chen, Xiaofang; Liu, Jingru; Zhang, Biao

2018-04-01

Inorganic hollow particles have attracted great interest in recent years. In this study, silica micro spheres were produced. Yeast cells were used as a biological template. The silica shell was synthesized by the hydrolysis of tetraethoxysilane (TEOS) in water-alcohol mixtures as solvent using ammonia as a catalyst according to the Stoeber process. Various approaches including X-ray diffraction (XRD), scanning electron microscopy (SEM) and Fourier transformed infrared (FT-IR) spectroscopy were used to characterize the products. The results showed that the thermally treated samples were SiO2 hollow microspheres with a diameter varying between 1-5μm.

FT-mid-IR spectroscopic investigation of fiber maturity and crystallinity at single boll level and a comparison with XRD approach

USDA-ARS?s Scientific Manuscript database

In previous study, we have reported the development of simple algorithms for determining fiber maturity and crystallinity from Fourier transform (FT) -mid-infrared (IR) measurement. Due to its micro-sampling feature, we were able to assess the fiber maturity and crystallinity at different portions o...

Green synthesis of gold nanoparticles using Stevia rebaudiana leaf extracts: Characterization and their stability.

PubMed

Sadeghi, Babak; Mohammadzadeh, M; Babakhani, B

2015-07-01

Various methods invented and developed for the synthesis of gold nanoparticles that increases daily consumed. According to this method, including potential environmental pollution problems and the complexity of the synthesis, in this study, the feasibility of using the leaves extract of Stevia rebaudiana (SR) for the reduction of gold ions to nanoparticles form have been studied. Stevia leaves were used to prepare the aqueous extract for this study. Gold nanoparticles were characterized with different techniques such as UV-vis spectroscopy, FT-IR spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Transmission electron microscopy experiments showed that these nanoparticles are spherical and uniformly distributed and its size is from 5 to 20 nm. FT-IR spectroscopy revealed that gold nanoparticles were functionalized with biomolecules that have primary amine group (NH2), carbonyl group, OH groups and other stabilizing functional groups. X-ray diffraction pattern showed high purity and face centered cubic structure of gold nanoparticles with size of 17 nm. The scanning electron microscopy (SEM) implies the right of forming gold nanoparticles. The results, confirm that gold nanoparticles have synthesized by the leaves extract of S. rebaudiana (SR). Copyright © 2015 Elsevier B.V. All rights reserved.

Preparation of thermally stable nanocrystalline hydroxyapatite by hydrothermal method.

PubMed

Prakash Parthiban, S; Elayaraja, K; Girija, E K; Yokogawa, Y; Kesavamoorthy, R; Palanichamy, M; Asokan, K; Narayana Kalkura, S

2009-12-01

Thermally stable hydroxyapatite (HAp) was synthesized by hydrothermal method in the presence of malic acid. X-ray diffraction (XRD), Fourier transform infra-red spectroscopy (FT-IR), Raman spectroscopy, scanning electron microscopy (SEM), differential thermal analysis (DTA), thermogravimetric analysis (TGA) was done on the synthesized powders. These analyses confirmed the sample to be free from impurities and other phases of calcium phosphates, and were of rhombus morphology along with nanosized particles. IR and Raman analyses indicated the adsorption of malic acid on HAp. Thermal stability of the synthesized HAp was confirmed by DTA and TGA. The synthesized powders were thermally stable upto 1,400 degrees C and showed no phase change. The proposed method might be useful for producing thermally stable HAp which is a necessity for high temperature coating applications.

Morphological and phase evolution of TiO 2 nanocrystals prepared from peroxotitanate complex aqueous solution: Influence of acetic acid

NASA Astrophysics Data System (ADS)

Chang, Jeong Ah; Vithal, Muga; Baek, In Chan; Seok, Sang Il

2009-04-01

Nanosized anatase and rutile TiO 2 having different shape, phase and size have been prepared from aqueous solutions of peroxo titanium complex starting from titanium(IV) isopropoxide (TTIP), acetic acid and hydrogen peroxide (H 2O 2) in water/isopropanol media by a facile sol-gel process. The TiO 2 nanocrystals are characterized by powder X-ray diffraction (XRD), Raman spectroscopy, FT-IR spectroscopy, TEM, high resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED) techniques. The influence of pH and the sequence of addition of reaction contents on the phase and morphology of TiO 2 are studied. The reasons for the observation of only anatase and/or mixture of anatase and rutile are given.

Effects of various polyoxyethylene sorbitan monooils (Tweens) and sodium dodecyl sulfate on reflux synthesis of copper nanoparticles

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

Zhang Xifeng; Yin Hengbo; Cheng Xiaonong

2006-11-09

Size-controlled synthesis of phase pure Cu nanoparticles was carried out by using copper sulfate pentahydrate as a precursor, ascorbic acid as a reductant, Tweens and sodium dodecyl sulfate (SDS) as modifiers in an aqueous solution at 80 deg. C. The as-prepared Cu nanoparticles were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and Fourier transform infrared (FT-IR). The stabilizing effects of SDS and Tweens on the Cu nanoparticles should be through the coordination between Cu nanoparticles and the respective sulfate group and oxygen-containing bond. The synergic effect of the composite SDS and Tweensmore » on Cu nanoparticles was different from those arising from the individuals.« less

Green synthesis of gold nanoparticles using a cheap Sphaeranthus indicus extract: Impact on plant cells and the aquatic crustacean Artemia nauplii.

PubMed

Balalakshmi, Chinnasamy; Gopinath, Kasi; Govindarajan, Marimuthu; Lokesh, Ravi; Arumugam, Ayyakannu; Alharbi, Naiyf S; Kadaikunnan, Shine; Khaled, Jamal M; Benelli, Giovanni

2017-08-01

The impact of green-fabricated gold nanoparticles on plant cells and non-target aquatic species is scarcely studied. In this research, we reported an environment friendly technique for the synthesis of gold nanoparticles (Au NPs) using the Sphaeranthus indicus leaf extract. The formation of the metal NPs was characterized by UV-Visible and FT-IR spectroscopy, XRD, SEM and TEM analyses. The UV-Visible spectra of Au NPs showed a surface plasmon resonance peak at 531nm. FT-IR analysis indicated functional bio-molecules associated with Au NPs formation. The crystalline nature of Au nanoparticles was confirmed by their XRD diffraction pattern. TEM revealed the spherical shape with a mean particle size of 25nm. Au NPs was tested at 0, 1, 3, 5, 7 and 10% doses in mitotic cell division assays, pollen germination experiments, and in vivo toxicity trials against the aquatic crustacean Artemia nauplii. Au NPs did not show any toxic effects on plant cells and aquatic invertebrates. Notably, Au NPs promoted mitotic cell division in Allium cepa root tip cells and germination of Gloriosa superba pollen grains. Au NPs showed no mortality on A. nauplii, all the tested animals showed 100% survivability. Therefore, these Au NPs have potential applications in the development of pollen germination media and plant tissue culture. Copyright © 2017 Elsevier B.V. All rights reserved.

Biocompatibility assessment of SiO2-TiO2 composite powder on MG63 osteoblast cell lines for orthopaedic applications.

PubMed

Chellappa, Maniickam; Thejaswini, Bezawada; Vijayalakshmi, Uthirapathy

2017-02-01

The objective of this study is to evaluate the biocompatibility of composite powder consisting of silica and titania (SiO 2 -TiO 2 ) for biomedical applications. The advancement of nanoscience and nanotechnology encourages researchers to actively participate in reinvention of existing materials with improved physical, chemical and biological properties. Hence, a composite/hybrid material has given birth of new materials with intriguing properties. In the present investigation, SiO 2 -TiO 2 composite powder was synthesised by sol-gel method and the prepared nanocomposite was characterised for its phase purity, functional groups, surface topography by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy. Furthermore, to understand the adverse effects of composite, biocompatibility test was analysed by cell culture method using MG63 osteoblast cell lines as a basic screening method. From the results, it was observed that typical Si-O-Ti peaks in FT-IR confirms the formation of composite and the crystallinity of the composite powder was analysed by XRD analysis. Further in vitro biocompatibility and acridine orange results have indicated better biocompatibility at different concentrations on osteoblast cell lines. On the basis of these observations, we envision that the prepared silica-titania nanocomposite is an intriguing biomaterial for better biomedical applications.

Effects of Synthesis Method on Electrical Properties of Graphene

NASA Astrophysics Data System (ADS)

Fuad, M. F. I. Ahmad; Jarni, H. H.; Shariffudin, W. N.; Othman, N. H.; Rahim, A. N. Che Abdul

2018-05-01

The aim of this study is to achieve the highest reduction capability and complete reductions of oxygen from graphene oxide (GO) by using different type of chemical methods. The modification of Hummer’s method has been proposed to produce GO, and hydrazine hydrate has been utilized in the GO’s reduction process into graphene. There are two types of chemical method are used to synthesize graphene; 1) Sina’s method and 2) Sasha’s method. Both GO and graphene were then characterized using X-Ray Powder Diffraction (XRD) and Fourier Transform Infrared Spectrometry (FT-IR). The graph patterns obtained from XRD showed that the values of graphene and GO are within their reliable ranges, FT-IR identified the comparison functional group between GO and graphene. Graphene was verified to experience the reduction process due to absent of functional group consist of oxygen has detected. Electrochemical impedance spectrometry (EIS) was then conducted to test the ability of conducting electricity of two batches (each weighted 1.6g) of graphene synthesized using different methods (Sina’s method and Sasha’s method). Sasha’s method was proven to have lower conductivity value compare to Sina’s method, with value of 6.2E+02 S/m and 8.1E+02 S/m respectively. These values show that both methods produced good graphene; however, by using Sina’s method, the graphene produced has better electrical properties.

Data on Molluscan Shells in parts of Nellore Coast, southeast coast of India.

PubMed

Lakshmanna, B; Jayaraju, N; Prasad, T Lakshmi; Sreenivasulu, G; Nagalakshmi, K; Kumar, M Pramod; Madakka, M

2018-02-01

X-ray diffraction (XRD), Scanning Electron Microscope-Energy Dispersive Spectroscopy (SEM-EDS), and Fourier Transform Infrared Spectroscopy (FT-IR), were applied to analyze the organic matrix of two Molluscan shells . The Mollusca shells are mineral structure and calcium carbonate crystallized as aragonite. The FT-IR spectra showed Alkyl Halide, Alkanes, Alcohols, Amides, Aromatic, and Hydroxyl groups in the organic matrix of the whole (organic and mineral) Molluscan shells. SEM images of particles of the two Molluscan shells at different magnifications were taken. The morphologies of the samples show a flake like structures with irregular grains, their sizes are at micrometric scale and the chemical analysis of EDS indicated that the major elements of Cardita and Gastropoda were C, O, and Ca, consistent with the results of XRD analysis. The results of the analysis of the EDS spectra of the shells showed that the content of most of the powder composition of shells is the element carbon, calcium oxygen, aluminium, and lead peaks that appear on the Cardita and Gastropoda and shells powders tap EDS spectra. The present work examined organic matrix of the selected shells of the heavily polluted and light polluted sites, along Nellore Coast, South East Coast of India. The heavily polluted sites have significantly thickened shells. The data demonstrated the sensitivity of this abundant and widely distributed intertidal fragile environment.

In vitro and in vivo studies on a novel solid dispersion of repaglinide using polyvinylpyrrolidone as the carrier.

PubMed

Yin, Li-Fang; Huang, Shi-Jing; Zhu, Chun-Li; Zhang, Shu-Hui; Zhang, Qiang; Chen, Xi-Jing; Liu, Qing-Wang

2012-11-01

In order to improve the dissolution and absorption of the water insoluble drug repaglinide, a solid dispersion was developed by solvent method using polyvinylpyrrolidone K30 (PVP K30) as the hydrophilic carrier for the first time. Studies indicated that both solubility and the dissolution rate of repaglinide were significantly increased in the solid dispersion system compared with that of repaglinide raw material or physical mixtures. The repaglinide solid dispersions with PVP K30 solid state was characterized by polarizing microscopy, differential scanning calorimetry (DSC), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FT-IR). DSC and XRD studies indicated that repaglinide existed in an amorphous form in the solid dispersion. FT-IR analysis demonstrated the presence of intermolecular hydrogen bonding between repaglinide and PVP K30 in the solid dispersion. In the in situ gastrointestinal perfusion experiment, solid dispersion was shown to remarkably enhance the absorption of repaglinide in stomach and all segments of intestine. In vivo pharmacokinetic study in rats showed that immediate and complete release of repaglinide from the solid dispersion resulted in rapid absorption that significantly increased the bioavailability and the maximum plasma concentration over repaglinide raw material. These results demonstrated PVP K30 was an appropriate carrier for solid dispersion of repaglinide, with increased dissolution and oral absorption.

Structural, optical and morphological characterization of Cu-doped α-Fe2O3 nanoparticles synthesized through co-precipitation technique

NASA Astrophysics Data System (ADS)

Lassoued, Abdelmajid; Lassoued, Mohamed Saber; Dkhil, Brahim; Gadri, Abdellatif; Ammar, Salah

2017-11-01

Pure and copper (Cu concentration varying from 2 to 8%) doped hematite (α-Fe2O3) nanocrystals were synthesized through co-precipitation method using simple equipment. X-ray Diffraction (XRD), Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), Fourier Transform Infra-Red (FT-IR), Raman spectroscopy, Differential Thermal Analysis (DTA), Thermo Gravimetric Analysis (TGA) and Ultraviolet-Visible (UV-Vis) techniques were used to characterize the synthesized samples. XRD measurements confirm that all the prepared nanocrystals consist only in nanocrystalline hematite phase. These results along with TEM and SEM show that the size of the nanoparticles decreases with Cu-doping down to 21 nm. FT-IR confirm the phase purity of the nanoparticles synthesized. The Raman spectroscopy was used not only to prove that we synthesized pure and Cu-doped hematite but also to identify their phonon modes. The TGA showed three mass losses, whereas DTA resulted in three endothermic peaks. The UV-Vis absorption measurements confirm that the decrease of particle size is accompanied by a decrease in the band gap value from 2.12 eV for pure α-Fe2O3 down to 1.91 eV for 8% Cu-doped α-Fe2O3. 8% Cu-doped hematite had the smallest size, the best crystallinity and the lowest band gap.

Insertion of bentonite with Organometallic [Fe3O(OOC6H5)6(H2O)3(NO3).nH2O] as Adsorbent of Congo Red

NASA Astrophysics Data System (ADS)

Said, Muhammad; Paluta Utami, Hasja; Hayati, Ferlina

2018-01-01

The adsorption of Congo red using bentonite inserted organometallic has been investigated. The insertion bentonite was characterized using FT-IR Spectrophotometer, XRD and XRF analysis. The FT-IR characterization showed the higher intensity of peak wavenumber at 470.6 cm-1 for Fe3O on the ratio 1:3. While the XRD characterization showed the shift of diffraction angle of 2θ was 5.2° and has a basal spacing of 16.8 Å. In the XRF characterization, the insertion process of organometallic occurred optimally with the percentage of metal oxide reached 71.75 %. The adsorption process of bentonite inserted organometallic compound [Fe3O(OOC6H5)6(H2O)3(NO3)·nH2O] showed the adsorption rate (k) is 0.050 min-1, the largest adsorption capacity (b) at 70°C is 4.48 mol/g, the largest adsorption energy at temperature 30°C which is 6.4 kJ/mol Organometallic compounds. The value of the enthalpy (ΔH) and entropy (ΔS) decreased with increasing concentrations of the Congo red. Effect of pH on the adsorption on at pH 3 shows the biggest of number Congo red absorbed is 19.52 mg/L for insertion of bentonite.

(2E)-1-(5-Chlorothiophen-2-yl)-3-{4-[(E)-2-phenylethenyl]phenyl}prop-2-en-1-one: Synthesis, XRD, FT-IR, Raman and DFT studies.

PubMed

Parlak, Cemal; Ramasami, Ponnadurai; Kumar, Chandraju Sadolalu Chidan; Tursun, Mahir; Quah, Ching Kheng; Rhyman, Lydia; Bilge, Metin; Fun, Hoong-Kun; Chandraju, Siddegowda

2015-01-01

A novel (2E)-1-(5-chlorothiophen-2-yl)-3-{4-[(E)-2-phenylethenyl]phenyl}prop-2-en-1-one [C21H15ClOS] compound has been synthesized and its structure has been characterized by FT-IR, Raman and single-crystal X-ray diffraction techniques. The conformational isomers, optimized geometric parameters, normal mode frequencies and corresponding vibrational assignments of the compound have been examined by means of HF, MP2, BP86, BLYP, BMK, B3LYP, B3PW91, B3P86 and M06-2X functionals. Reliable vibrational assignments and molecular orbitals have been investigated by the potential energy distribution and natural bonding orbital analyses, respectively. The compound crystallizes in the triclinic space group P-1 with the cis-trans-trans form. There is a good agreement between the experimentally determined structural parameters and vibrational frequencies of the compound and those predicted theoretically using the density functional theory with the BLYP and BP86 functionals. Copyright © 2015 Elsevier B.V. All rights reserved.

Electrosynthesis and characterization of zinc tungstate nanoparticles

NASA Astrophysics Data System (ADS)

Rahimi-Nasrabadi, Mehdi; Pourmortazavi, Seied Mahdi; Ganjali, Mohammad Reza; Hajimirsadeghi, Seiedeh Somayyeh; Zahedi, Mir Mahdi

2013-09-01

Zinc tungstate nanoparticles with different sizes are produced through an electrolysis process including a zinc plate anode in sodium tungstate solution. The shape and size of the product was found to be controlled by varying reaction parameters such as electrolysis voltage, stirring rate of electrolyte solution and temperature. The morphological (SEM) characterization analysis was performed on the product and UV-Vis spectrophotometry and FT-IR spectroscopy was utilized to characterize the electrodeposited nanoparticles. Study of the particle size of the product versus the electrolysis voltage showed that, increasing the voltage from 4 to 8 V, led to the particle size of zinc tungstate to decrease, but further increasing the voltage from 8 to 12 V, the particle size of the produced particles increased. The size and shape of the product was also found to be dependent on the stirring rate and temperature of the electrolyte solution. X-ray diffraction (XRD), scanning electron microscopy (SEM), FT-IR spectroscopy, and photoluminescence, were used to study the structure as well as composition of the nano-material prepared under optimum conditions.

3-Iodobenzaldehyde: XRD, FT-IR, Raman and DFT studies.

PubMed

Kumar, Chandraju Sadolalu Chidan; Parlak, Cemal; Tursun, Mahir; Fun, Hoong-Kun; Rhyman, Lydia; Ramasami, Ponnadurai; Alswaidan, Ibrahim A; Keşan, Gürkan; Chandraju, Siddegowda; Quah, Ching Kheng

2015-06-15

The structure of 3-iodobenzaldehyde (3IB) was characterized by FT-IR, Raman and single-crystal X-ray diffraction techniques. The conformational isomers, optimized geometric parameters, normal mode frequencies and corresponding vibrational assignments of 3IB were examined using density functional theory (DFT) method, with the Becke-3-Lee-Yang-Parr (B3LYP) functional and the 6-311+G(3df,p) basis set for all atoms except for iodine. The LANL2DZ effective core basis set was used for iodine. Potential energy distribution (PED) analysis of normal modes was performed to identify characteristic frequencies. 3IB crystallizes in monoclinic space group P21/c with the O-trans form. There is a good agreement between the theoretically predicted structural parameters, and vibrational frequencies and those obtained experimentally. In order to understand halogen effect, 3-halogenobenzaldehyde [XC6H4CHO; X=F, Cl and Br] was also studied theoretically. The free energy difference between the isomers is small but the rotational barrier is about 8kcal/mol. An atypical behavior of fluorine affecting conformational preference is observed. Copyright © 2015 Elsevier B.V. All rights reserved.

Effect of Heat Treatment Temperature on Chemical Compositions of Extracted Hydroxyapatite from Bovine Bone Ash

NASA Astrophysics Data System (ADS)

Younesi, M.; Javadpour, S.; Bahrololoom, M. E.

2011-11-01

This article presents the effect of heat treating temperature on chemical composition of hydroxyapatite (HA) that was produced by burning bovine bone, and then heat treating the obtained bone ash at different temperatures in range of 600-1100 °C in air. Bone ash and the resulting white powder from heat treating were characterized by Fourier transformed infrared spectroscopy (FT-IR) and x-ray diffractometry (XRD). The FT-IR spectra confirmed that heat treating of bone ash at temperature of 800 °C removed the total of organic substances. x-ray diffraction analysis showed that the white powder was HA and HA was the only crystalline phase indicated in heat treating product. x-ray fluorescence analyses revealed that calcium and phosphorous were the main elements and magnesium and sodium were minor impurities of produced powder at 800 °C. The results of the energy dispersive x-ray analysis showed that Ca/P ratio in produced HA varies in range of 1.46-2.01. The resulting material was found to be thermally stable up to 1100 °C.

One Step Synthesis of NiO Nanoparticles via Solid-State Thermal Decomposition at Low-Temperature of Novel Aqua(2,9-dimethyl-1,10-phenanthroline)NiCl2 Complex

PubMed Central

Barakat, Assem; Al-Noaimi, Mousa; Suleiman, Mohammed; Aldwayyan, Abdullah S.; Hammouti, Belkheir; Ben Hadda, Taibi; Haddad, Salim F.; Boshaala, Ahmed; Warad, Ismail

2013-01-01

[NiCl2(C14H12N2)(H2O)] complex has been synthesized from nickel chloride hexahydrate (NiCl2·6H2O) and 2,9-dimethyl-1,10-phenanthroline (dmphen) as N,N-bidentate ligand. The synthesized complex was characterized by elemental analysis, infrared (IR) spectroscopy, ultraviolet-visible (UV-vis) spectroscopy and differential thermal/thermogravimetric analysis (TG/DTA). The complex was further confirmed by single crystal X-ray diffraction (XRD) as triclinic with space group P-1. The desired complex, subjected to thermal decomposition at low temperature of 400 ºC in an open atmosphere, revealed a novel and facile synthesis of pure NiO nanoparticles with uniform spherical particle; the structure of the NiO nanoparticles product was elucidated on the basis of Fourier transform infrared (FT-IR), UV-vis spectroscopy, TG/DTA, XRD, scanning electron microscopy (SEM), energy-dispersive X-ray spectrometry (EDXS) and transmission electron microscopy (TEM). PMID:24351867

Synthesis, crystal growth, structural, thermal and optical properties of naphthalene picrate an organic NLO material.

PubMed

Chandramohan, A; Bharathikannan, R; Kandavelu, V; Chandrasekaran, J; Kandhaswamy, M A

2008-12-01

Crystalline substance of naphthalene picrate (NP) was synthesized and single crystals were grown using slow evaporation solution growth technique. The solubility of the naphthalene picrate complex was estimated using different solvents such as chloroform and benzene. The material was characterized by elemental analysis, powder X-ray diffraction (XRD), nuclear magnetic resonance (NMR) and fourier transform-infrared (FT-IR) techniques. The electronic absorption was studied through UV-vis spectrophotometer. Thermal behavior and stability of the crystal were studied using thermogravimetric (TG) and differential thermal analysis (DTA) techniques. The second harmonic generation (SHG) of the material was confirmed using Nd:YAG laser.

Copolymers of polyaniline and poly-o-toluidine: Electrochemical synthesis and characterization

NASA Astrophysics Data System (ADS)

Yadav, Pooja C.; Deshmukh, Megha A.; Patil, Harshada K.; Bodkhe, Gajanan A.; Sayyad, Pasha W.; Ingle, Nikesh N.; Shirsat, Mahendra D.

2018-05-01

In the present study we have reported Electrochemical polymerization of poly(Aniline) (PANI), Poly(O-Toluidine) (POT) and poly(Aniline-co-O-Toluidine) (PAOT) copolymers. Electrochemical Synthesis of PANI, POT and Poly(Aniline-co-O-Toluidine) was done by using Cyclic Voltammetry technique. The morphological study done by Atomic Force Microscopy (AFM) which shows that formation of uniform granular structure and topographic changes in each respective thin film. Spectroscopic characterization was done by FTIR spectroscopy. The FT-IR study revealed the formation of PANI/POT/Poly(Aniline co O-Toluidine) with a absorption band are reported. For structural information done by X-ray diffraction(XRD) Characterization.

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

Mascarenhas, N. P., E-mail: naveenmascarenhas@gmail.com; Crasta, V.; Gonsalves, R. A.

To enhance the physical and mechanical properties of Chitosan (CS) and to improve the functionality of CS towards some specific applications, we have blended CS with polystyrene (PS) to form blended films. The Fourier Transform Infrared Spectroscopy (FT-IR) has been performed on the prepared films to confirm functional groups and formation of the blends. Thermal analysis (TGA and DSC) is carried out to study thermal stability of the blended films. From X-ray diffraction (XRD) studies, the material reveals amorphous nature and hence it may be used for adsorption process. The versatility of the blends, such as film-forming ability, hydrophilicity, biodegradabilitymore » and biocompatibility are comparable with the existing blends.« less

New polyurethane nanocomposites based on soya oil.

PubMed

Mohammed, Issam Ahmed; Abd Khadir, Nurul Khizrien; Jaffar Al-Mulla, Emad Abbas

2014-01-01

New polyurethane (PU) nanocomposites were prepared from a dispersion of 0 - 5% montmorillonite (MMT) clay with isocyanate and soya oil polyol that was synthesized via transesterification of triglycerides to reduce petroleum dependence. FT-IR spectra indicate the presence of hydrogen bonding between nanoclay and the polymer matrix, whereas the exfoliated structure of clay layers was confirmed by X-ray diffraction (XRD) and transmission electron microscopy (TEM). Optical microscopy, mechanical and thermal analyses were done to investigate significant improvement of the nanocomposites. The results showed PU-3% nanoclay (NC) showed optimum results in mechanical properties such as tensile and flexural strength but the lowest in impact strength.

Sol-gel synthesis and characterizations of crystalline NaGd(WO4)2 powder for anisotropic transparent ceramic laser application

NASA Astrophysics Data System (ADS)

Durairajan, A.; Thangaraju, D.; Balaji, D.; Moorthy Babu, S.

2013-02-01

NaGd(WO4)2 powders were synthesized at different pH (3.5, 4.5, 5.5, 6.5 and 7.5) values by conventional Pechini method. Sodium and gadolinium nitrate salts and ammonium paratungstate are used as starting precursors. Metal cations were chelated by citric acid and individual citrates were bound together with ethylene glycol. Synthesized gel was analyzed using differential thermal analysis (DTA), thermo gravimetric (TG) and FT-IR spectroscopy to understand the degradation of gel and formation of metal citrates. Calcined powders (250, 600, 700 and 800 °C) were characterized by powder XRD, FT-IR, Raman and FE-SEM analysis. The temperature dependent phase formation was examined by powder XRD. The morphological changes at different pH derived powders were observed with FE-SEM micrographs. Stepwise organic liberation with respect to temperature and presence of carbon content in the pre-fired powder were analyzed using FT-IR analysis. Raman spectrum reveals disordered tungstate vibrations in the NGW matrix.

Frequency dependent dielectric properties of combustion synthesized Dy2Ti2O7 pyrochlore oxide

NASA Astrophysics Data System (ADS)

Jeyasingh, T.; Saji, S. K.; Kavitha, V. T.; Wariar, P. R. S.

2018-05-01

Nanocrystalline pyrochlore material Dysprosium Titanate (Dy2Ti2O7) has been synthesized through a single step optimized combustion route. The phase purity and phase formation of the combustion product has been characterized using X-Ray diffraction analysis (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR) analysis. X-Ray diffraction analysis (XRD) reveal that Dy2Ti2O7 is highly crystalline in nature with cubic structure in the Fd3m space group. The microstructures and average particle size of the prepared nanopowder were examined by High Resolution Transmission Electron Microscopy (HR-TEM). The optical band gap of the Dy2Ti2O7 nanoparticles is determined from the absorption spectrum, was attributed to direct allowed transitions through optical band gap of 3.98 eV. The frequency dependent dielectric measurements have been carried out on the sintered pellet in the frequency range 1 Hz-10 MHz. The measured value of dielectric constant (ℇ') was ˜ 43 and loss tangent (tan δ) was 4×10-3 at 1 MHz, at room temperature.

Facile green synthesis of fluorescent N-doped carbon dots from Actinidia deliciosa and their catalytic activity and cytotoxicity applications

NASA Astrophysics Data System (ADS)

Arul, Velusamy; Sethuraman, Mathur Gopalakrishnan

2018-04-01

Green synthesis of fluorescent nitrogen doped carbon dots (N-CDs) using Actinidia deliciosa (A. deliciosa) fruit extract as a carbon precursor and aqueous ammonia as a nitrogen dopant is reported here. The synthesized N-CDs were characterized by high resolution transmission electron microscopy (HR-TEM), energy dispersive spectroscopy (EDS), selected area electron diffraction (SAED), UV-Visible spectroscopy (UV-Vis), fluorescence spectroscopy, Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). The average size of the N-CDs was approximately 3.59 nm and the calculated inter layer distance was found to be 0.21 nm. Raman spectroscopy and SAED pattern revealed the graphitic nature of the synthesized N-CDs. The N-CDs were found to emit intense blue color at 405 nm under the excitation of 315 nm. The doping of nitrogen over the surface of the N-CDs was confirmed by EDS, FT-IR and XPS studies. The synthesized N-CDs were found to exhibit excellent catalytic activity in the reduction of Rhodamine-B using sodium borohydrate. The MTT assay was used to evaluate the cytotoxicity and biocompatibility of N-CDs towards L-929 and MCF-7 cells. From the results obtained, it was found that the N-CDs exhibit low cytotoxicity and superior biocompatibility on both L-929 and MCF-7 cells.

Crystallization of a non-steroidal anti-inflammatory drug from ethanol-water solution in presence of polymers: physicochemical characterization and release behaviour from suppositories.

PubMed

Mallick, Subrata; Dey, Pintu K; Sannigrahi, Santanu; Mitra, Avishek

2004-01-01

Altered crystallization condition has been designed and adopted to a model non-steroidal anti-inflammatory drug, while crystallizing from ethanol-water solution in absence and presence of polymers such as Eudragit RS and ethylcellulose. To minimize the gastro-intestinal side effects nimesulide was considered as a model drug candidate for the development of suppository formulation. Physicochemical characteristics of the crystals were evaluated by Scanning Electron Microscopy (SEM). X-ray diffraction (XRD) and Fourier Transformed Infrared Spectroscopy (FT-IR). Smoothness and sharpness of the crystal have been decreased with increased concentration of a polymer. A little change in crystal habit and geometry has also been observed. Crystals are discrete in nature and more than 90% were in the range of 20-90 micron. The X-ray diffractions of nimesulide crystallized in absence of polymer and physical mixture of drug-polymer revealed fewer high intensity reflections when compared with the drug crystallized in presence of Eudragit RS, which testified a slight decreased ordering of crystal lattice in the latter. In presence of ethylcellulose, slightly increased ordering of crystal lattice was observed. No strong interactions were noticed as revealed by FT-IR spectroscopy. Drug dissolution rate from suppository formulations containing nimesulide crystallized in presence of polymer was found to delay as compared with the suppository prepared by nimesulide crystallized in absence of polymer.

Synthesis and structural studies of Mg doped LiNi0.5Mn0.5O2 cathode materials for lithium-ion batteries

NASA Astrophysics Data System (ADS)

Murali, N.; Margarette, S. J.; Madhuri Sailaja, J.; Kondala Rao, V.; Himakar, P.; Kishore Babu, B.; Veeraiah, V.

2018-02-01

Layered Mg doped LiNi0.5Mn0.5O2 materials have been synthesized by sol-gel method. The physical properties of these materials were examined by XRD, FESEM and FT-IR studies. From XRD patterns, the phase formation of α-NaFeO2 layered structure with R\\bar 3m space group is confirmed. The surface morphology of the synthesized materials has been examined by FESEM analysis in which the average particle size is found to be about 2 - 2.5 µm. These materials show some changes in the local ion environment, as examined by FT-IR studies.

Synthesis, characterization, bioactivity and antibacterial studies of silver doped calcium borosilicate glass-ceramics

NASA Astrophysics Data System (ADS)

Kumar, Alesh; Mariappan, C. R.

2018-04-01

Bioactive glass-ceramics 45.8 mol% SiO- 45.8 CaO - 8.4 B2O3 doped with Ag2O were synthesized by sol-gel method. The glass-ceramic nature of samples was confirmed by X-ray diffraction (XRD) and transmission electron microscopy (TEM) analysis. Fourier transform infrared (FT-IR) spectra reveal the probable stretching and bending vibration modes of silicate and borate groups. UV-Visible spectra reveal the presence of Ag+ ions and metallic Ag in the glass matrix for Ag2O doped ceramic sample. Biocompatibility of the glass nature of samples was studied by soaking of samples in Dulbecco's Modified Eagle's Medium (DMEM) with subsequent XRD studies. It was found that bone-like apatite formation on the glasses after soaked in DMEM. Antibacterial studies of glass ceramics powder against gram positive and negative microorganisms were carried out.

The alterations in high density polyethylene properties with gamma irradiation

NASA Astrophysics Data System (ADS)

Zaki, M. F.; Elshaer, Y. H.; Taha, Doaa. H.

2017-10-01

In the present investigation, high density polyethylene (HDPE) polymer has been used to study the alterations in its properties under gamma-irradiation. Physico-chemical properties have been investigated with different spectroscopy techniques, Fourier Transform Infrared spectroscopy (FTIR), X-ray diffraction (XRD), biocompatibility properties, as well as, mechanical properties change. The FT-IR analysis shows the formation of new band at 1716 cm-1 that is attributed to the oxidation of irradiated polymer chains, which is due to the formation of carbonyl groups (C˭O). XRD patterns show that a decrease in the crystallite size and increase in the Full Width at Half Maximum (FWHM). This means that the crystallinity of irradiated samples is decreased with increase in gamma dose. The contact angle measurements show an increase in the surface free energy as the gamma irradiation increases. The measurements of mechanical properties of irradiated HDPE samples were discussed.

Mulberry leaf extract mediated synthesis of gold nanoparticles and its anti-bacterial activity against human pathogens

NASA Astrophysics Data System (ADS)

Adavallan, K.; Krishnakumar, N.

2014-06-01

Gold nanoparticles (Au-NPs) were synthesized at room temperature using Morus alba (mulberry) leaf extract as reducing and stabilizing agent. The development of plant mediated synthesis of nanoparticles is gaining importance due to its simplicity, low cost, non-toxicity, eco-friendliness, long term stability and reproducible aqueous synthesis method to obtain a self-assembly of nearly monodispersed Au-NPs. The formation and morphology of biosynthesized nanoparticles are investigated with the help of UV-Vis spectroscopy, dynamic light scattering (DLS), transmission electron microscopy (TEM), atomic force microscopy (AFM), x-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FT-IR) techniques. Au-NPs formation was screened by UV-Vis spectroscopy through color conversion due to surface plasmon resonance band at 538 nm for Au-NPs. DLS studies revealed that the average size of Au-NPs was 50 nm. TEM studies showed the particles to be nearly spherical with few irregular shapes and particle size ranges 15-53 nm. The AFM image clearly shows the surface morphology of the well-dispersed Au-NPs with less than 50 nm. The high crystallinity of nanoparticles is evident from bright circular spots in the selected area electron diffraction (SAED) pattern. X-ray diffraction pattern showed high purity and face-centered cubic structure of Au-NPs. The FT-IR results indicate the presence of different functional groups present in the biomolecule capping the nanoparticles. Further, biosynthesized Au-NPs show strong zone of inhibition against Vibrio cholera (gram-negative) and Staphylococcus aureus (gram-positive) whereas, chemically synthesized Au-NPs and mulberry leaf extract exhibit a fair zone of inhibition.

Structure analysis and spectroscopic characterization of 2-Fluoro-3-Methylpyridine-5-Boronic Acid with experimental (FT-IR, Raman, NMR and XRD) techniques and quantum chemical calculations

NASA Astrophysics Data System (ADS)

Alver, Özgür; Dikmen, Gökhan

2016-03-01

Possible stable conformers, geometrical molecular structures, vibrational properties as well as band assignments, nuclear magnetic shielding tensors of 2-Fluoro-3-Methylpyridine-5-Boronic Acid (2F3MP5BA) were studied experimentally and theoretically using FT-IR, Raman, (CP/MAS) NMR and XRD spectroscopic methods. FT-IR and Raman spectra were evaluated in the region of 3500-400 cm-1, and 3200-400 cm-1, respectively. The optimized geometric structures, vibrational wavenumbers and nuclear magnetic shielding tensors were examined using Becke-3-Lee-Yang-Parr (B3LYP) hybrid density functional theory method with 6-311++G(d, p) basis set. 1H, 13C NMR chemical shifts were calculated using the gauge invariant atomic orbital (GIAO) method. 1H, 13C, APT and HETCOR NMR experiments of title molecule were carried out in DMSO solution. 13C CP/MAS NMR measurement was done with 4 mm zirconium rotor and glycine was used as an external standard. Single crystal of 2F3MP5BA was also prepared for XRD measurements. Assignments of vibrational wavenumbers were also strengthened by calculating the total energy distribution (TED) values using scaled quantum mechanical (SQM) method.

Ft-Ir Spectroscopic Analysis of Potsherds Excavated from the First Settlement Layer of Kuriki Mound, Turkey

NASA Astrophysics Data System (ADS)

Bayazit, Murat; Isik, Iskender; Cereci, Sedat; Issi, Ali; Genc, Elif

The region covering Southeastern Anatolia takes place in upper Mesopotamia, so it has numerous cultural heritages due to its witness to various social movements of different civilizations in ancient times. Kuruki Mound is located on the junction point of Tigris River and Batman Creek, near Oymatas village which is almost 15 km to Batman, Turkey. The mound is dated back to Late Chalcolithic. Archaeological excavations are carried out on two hills named as “Kuriki Mound-1” and “Kuriki Mound-2” in which 4-layer and 2-layer settlements have been revealed, respectively. This region will be left under the water by the reservoir lake of Ilısu Dam when its construction is completed. Thus, characterization of ancient materials such as potsherds, metals and skeleton ruins should be rapidly done. In this study, 12 potsherds excavated from Layer-1 (the first settlement layer after the surface) in Kuriki Mound-2 were investigated by FT-IR spectrometry. Energy dispersive X-ray fluorescence (EDXRF) and X-ray diffraction (XRD) analyses were used as complementary techniques in order to expose chemical and mineralogical/phase contents, respectively. Obtained results showed that the potteries have been produced with calcareous clays and they include moderate amounts of MgO, K2O, Na2O and Fe2O3 in this context. Additionally, high temperature phases have also been detected with XRD analyses in some samples.

Synthesis and photocatalytic degradation study of methylene blue dye under visible light irradiation by Fe1-xBixVO4 solid solutions (0 ≤ x ≤ 1.0)

NASA Astrophysics Data System (ADS)

Bera, Ganesh; Reddy, V. R.; Mal, Priyanath; Das, Pradip; Turpu, G. R.

2018-05-01

The novel hetero-structures Fe1-xBixVO4 solid solutions (0 ≤ x ≤ 1.0) with the two dissimilar end member of FeVO4 - BiVO4, were successfully synthesized by the standard solid state reaction method. The structural and chemical properties of as prepared photo-catalyst samples were characterized by X-ray diffraction (XRD), Raman spectroscopy, Fourier transform infrared spectroscopy (FT-IR) and UV-visible absorption spectroscopy techniques. It is confirmed from the results of XRD, Raman and FT-IR that FeVO4 and BiVO4 are in triclinic (space group P-1 (2)) and monoclinic (space group I2/b (15)) phases respectively. The Bi incorporation into Fe site of FeVO4 emerges as hetero-structures of both the end members of the solid solutions. In addition, the photocatalytic activity in the degradation of methylene blue (MB) dye under visible light irradiation was carried out through UV-visible spectroscopy measurement of photo-catalysts FeVO4, BiVO4 and mixed phases of both photo-catalyst. The results indicate that under visible light irradiation the photocatalytic activity of mixed phases were very effective and higher than the both single phases of the solid solutions. The composition x= 0.25 exhibits an excellent photocatalytic property for the degradation of MB solution under visible light irradiation rather than other.

Green synthesis of silver nanoparticles using Cordia dichotoma fruit extract and its enhanced antibacterial, anti-biofilm and photo catalytic activity

NASA Astrophysics Data System (ADS)

Bharathi, Devaraj; Vasantharaj, Seerangaraj; Bhuvaneshwari, V.

2018-05-01

The present study describes the antibacterial, anti-biofilm and photo catalytic activity of silver nanoparticles synthesized using Cordia dichotoma fruits (Cd-AgNPs) for the first time. The phyto-synthesized Cd-AgNPs were characterized by UV-Visible spectroscopy, Field emission-scanning electron microscopy (FE-SEM), Transmission electron microscopy (TEM), Energy dispersive x-ray spectrometer (EDX), Fourier transform infrared spectroscopy (FT-IR), and x-ray diffraction (XRD). FE-SEM and TEM observation showed that the average size of 2–60 nm with spherical shape of Cd-AgNPs and the presence of phyto-compounds which are responsible for capping and reduction were studied by FT-IR. XRD studies revealed the face-centered cubic structure of Cd-AgNPs. The synthesized Cd-AgNPs showed significant antibacterial activity against Gram-positive Staphylococcus aureus and Gram-negative Escherichia coli, assayed using agar well diffusion method. Phyto-synthesized Cd-AgNPs exhibited more than 90% inhibition of biofilm activity formed by S. aureus and E. coli. Furthermore, photocatalytic degradation of crystal violet (CV) under UV light irradiation using Cd-AgNPs was performed. Synthesized Cd-AgNPs exhibited ∼85% degradation activity for CV. Collectively, our findings suggest that C.dichotoma is a green source for the eco-friendly synthesis of Cd-AgNPs, which further can be used as a novel biocidal agent against bacterial pathogens and a potent photo catalytic agent.

Evaluation of SLS: APG mixed surfactant systems as carrier for solid dispersion.

PubMed

Patel, Ashok R; Joshi, Vishal Y

2008-01-01

The present investigation aims at studying the effect of mixed surfactant system of sodium lauryl sulphate (SLS) and alkyl polyglucosides (C(10)APG, C(12)APG and C(12/14)APG) on dissolution rate enhancement of poorly water soluble drug. Aceclofenac--a non-steroidal anti-inflammatory agent was used as a model drug as it has limited water solubility. The influence of the surfactant concentration in various blends on dissolution rate of Solid Dispersion (SD), prepared using solution method with ethanol as the solvent was studied and the advantage of mixed surfactant systems over the individual surfactants was illustrated by differences in the in-vitro dissolution profiles of SD. Physico chemical evaluation (critical micellar concentration, zeta potential and beta-parameter calculations) was carried out to study the mixed surfactant systems. Solid mixtures were characterized by Infrared spectroscopy (FT-IR); X-ray diffraction studies (XRD) and scanning electron microscopy (SEM). It was seen that the dissolution rate of aceclofenac from SD increased with the increase in the APG proportion relative to SLS with the optimum ratio of 0.2 SLS:0.8 APG showing the best effect in all cases. Results obtained from physico-chemical evaluation (the decrease in the value of critical micelle concentration and higher negative value of beta-parameters) suggested the existence of synergism between surfactants blends. The observed results in the dissolution rate enhancement could be attributed to the drug--surfactant interactions as evident from FT-IR, SEM and XRD results.

Structural and electrical characterization of annealed Si1-xCx/SiC thin film prepared by magnetron sputtering

NASA Astrophysics Data System (ADS)

Huang, Shi-Hua; Liu, Jian

2014-05-01

Si-rich Si1—xCx /SiC multilayer thin films are prepared using magnetron sputtering, subsequently followed by thermal annealing in the range of 800-1200 °C. The influences of annealing temperature (Ta) on the formation of Si and/or SiC nanocrystals (NCs) and on the electrical characteristics of the multilayer film are investigated by using a variety of analytical techniques, including X-ray diffraction (XRD), Raman spectroscopy and Fourier transform infrared spectrometry (FT-IR), current—voltage (I—V) technique, and capacitance-voltage (C—V) technique. XRD and Raman analyses indicate that Si NCs begin to form in samples for Ta >= 800 °C. At annealing temperatures of 1000 °C or higher, the formation of Si NCs is accompanied by the formation of SiC NCs. With the increase in the annealing temperature, the shift of FT-IR Si—C bond absorption spectra toward a higher wave number along with the change of band shape can be explained by a Si—C transitional phase between the loss of substitutional carbon and the formation of SiC precipitates and a precursor for the growth of SiC crystalline. The C—V and I—V results indicate that the interface quality of Si1—xCx/SiC multilayer film is improved significantly and the leakage current is reduced rapidly for Ta >= 1000 °C, which can be ascribed to the formation of Si and SiC NCs.

Selective determination of gold(III) ion using CuO microsheets as a solid phase adsorbent prior by ICP-OES measurement.

PubMed

Rahman, Mohammed M; Khan, Sher Bahadar; Marwani, Hadi M; Asiri, Abdullah M; Alamry, Khalid A; Al-Youbi, Abdulrahman O

2013-01-30

We have prepared calcined CuO microsheets (MSs) by a wet-chemical process using reducing agents in alkaline medium and characterized by UV/vis., fourier transform infrared (FT-IR) spectroscopy, powder X-ray diffraction (XRD), and field-emission scanning electron microscopy (FESEM) etc. The detailed structural, compositional, and optical characterizations of the MSs were evaluated by XRD pattern, FT-IR, X-ray photoelectron spectroscopy (XPS), and UV-vis spectroscopy, respectively which confirmed that the obtained MSs are well-crystalline CuO and possessed good optical properties. The CuO MSs morphology was investigated by FESEM, which confirmed that the calcined nanomaterials were sheet-shaped and grown in large-quantity. Here, the efficiency of the CuO MS was applied for a selective adsorption of gold(III) ion prior to its detection by inductively coupled plasma-optical emission spectrometry (ICP-OES). The selectivity of CuO MSs towards various metal ions, including Au(III), Cd(II), Co(II), Cr(III), Fe(III), Pd(II), and Zn(II) was analyzed. Based on the adsorption isotherm study, it was confirmed that the selectivity of MSs phase was mostly towards Au(III) ion. The static adsorption capacity for Au(III) was calculated to be 57.0 mg g(-1). From Langmuir adsorption isotherm, it was confirmed that the adsorption process was mainly monolayer-adsorption onto a surface containing a finite number of adsorption sites. Copyright © 2012 Elsevier B.V. All rights reserved.

Characterization of rice starch-ι-carrageenan biodegradable edible film. Effect of stearic acid on the film properties.

PubMed

Thakur, Rahul; Saberi, Bahareh; Pristijono, Penta; Golding, John; Stathopoulos, Costas; Scarlett, Christopher; Bowyer, Michael; Vuong, Quan

2016-12-01

The main aim of this study was to develop rice starch (RS), ι-carrageenan (ι-car) based film. Different formulations of RS (1-4%, w/w), ι-car (0.5-2%, w/w) was blended with stearic acid (SA; 0.3-0.9%, w/w) and glycerol (1%, w/w) as a plasticizer. The effect of film ingredients on the thickness, water vapour permeability (WVP), film solubility (FS), moisture content (MC), colour, film opacity (FO), tensile strength (TS), elongation-at-break (EAB) of film was examined. Interactions and miscibility of partaking components was studied by using Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD). Hydrocolloid suspension solution of mix polysaccharides imparted a significant impact (p<0.05) on the important attributes of resulting edible film. TS and EAB of film were improved significantly (p<0.05) when ι-car was increased in the film matrix. Formulation F1 comprising 2% ι-car, 2% RS, 0.3% SA, Gly 30% w/w and 0.2% surfactant (tween ® 20) provided film with good physical, mechanical and barrier properties. FT-IR and XRD results reveal that molecular interactions between RS-ι-car have a great impact on the film properties confining the compatibility and miscibility of mixed polysaccharide. Results of the study offers new biodegradable formulation for application on fruit and vegetables. Copyright © 2016 Elsevier B.V. All rights reserved.

Purification, characterization and antioxidant properties of a novel polysaccharide extracted from Sorghum bicolor (L.) seeds in sausage.

PubMed

Ben Slima, Sirine; Ktari, Naourez; Trabelsi, Imen; Moussa, Hafedh; Makni, Iskandar; Ben Salah, Riadh

2018-01-01

A novel polysaccharide named Sorghum Water-Soluble Polysaccharide (SWSP) was purified from Sorghum bicolor (L.) seeds. It was structurally characterized by high performance liquid chromatography (HPLC), thin layer chromatography (TLC), Fourier transform-infrared spectroscopy analysis (FT-IR), X-ray diffraction (XRD) and mass spectroscopy (MS). HPLC and TLC showed that SWSP is a glucose polymer. The FT-IR spectrum proved the polysaccharide characteristic band of SWSP. XRD and microscopy analyses revealed that SWSP is a semi-crystalline polymer. Functional properties of SWSP were determined based on Water Holding Capacity (WHC), Oil Holding Capacity (OHC) and emulsification properties. SWSP showed good WHC and OHC, recorded at 3.01±0.03 and 1.02±0.03g/g, respectively and exhibited excellent emulsion properties even after 168h (61.5±0.02%). The effect of SWSP on oxidative stability of sausage during storage up to 12days at 4°C was investigated. Results showed a high rate (P<0.05) of oxymyoglobin and low lipid oxidation. The antioxidant activities of SWSP were also studied in vitro. Results demonstrated that the polysaccharides exhibited interesting 1,1-diphenyl-2-picrylhydrazyl (DPPH), ABTS radical scavenging, and ß-carotene bleaching inhibition activities. Overall, this natural polysaccharide was proved to enhance the oxidation stability of sausages, since it can efficiently substitute synthetic antioxidants in meat industry. Copyright © 2017 Elsevier B.V. All rights reserved.

Sustained release effects of berberine-loaded chitosan microspheres on in vitro chondrocyte culture.

PubMed

Zhou, Yan; Liu, Shiqing; Ming, Jianghua; Li, Yaming; Deng, Ming; He, Bin

2017-10-01

The low bioavailability and short biological half-life of berberine chloride (BBR) negatively affect the protective role of this compound against osteoarthritis (OA). The present study was performed to evaluate the effectiveness of sustained BBR release system. Novel BBR-loaded chitosan microspheres (BBR-loaded CMs) were successfully synthesized using an ionic cross-linking method for sustained release. The basic characteristics of the prepared microspheres were subsequently evaluated by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD) techniques, encapsulation efficiency (EE), and in vitro release experiments. BBR-loaded CMs displayed spherical forms to encapsulate a considerable quantity of BBR (100.8 ± 2.7 mg/g); these microspheres also exhibited an ideal releasing profile. The FT-IR spectra and XRD results revealed that BBR-loaded CMs were successfully synthesized via electrostatic interaction. In vitro experiments further showed that BBR-loaded CMs significantly inhibited sodium nitroprusside (SNP)-stimulated chondrocyte apoptosis as well as cytoskeletal remodeling, and led to increasing mitochondrial membrane potential and maintaining the nuclear morphology. BBR-loaded CMs exerted markedly higher anti-apoptotic activity in the treatment of OA, and markedly inhibited the protein expression levels of caspase-3, a disintegrin, and metalloproteinase with thrombospondin motifs (ADAMTS)-5 and matrix metalloproteinase (MMP)-13 induced by SNP in rat articular chondrocytes, compared with free BBR at equivalent concentration. Therefore, novel BBR-loaded CMs may offer potential for application in the treatment of OA.

Eco-friendly preparation of zinc oxide nanoparticles using Tabernaemontana divaricata and its photocatalytic and antimicrobial activity.

PubMed

Raja, A; Ashokkumar, S; Pavithra Marthandam, R; Jayachandiran, J; Khatiwada, Chandra Prasad; Kaviyarasu, K; Ganapathi Raman, R; Swaminathan, M

2018-04-01

The present work reports the green synthesis of Zinc Oxide Nanoparticles (ZnO NPs) using aqueous Tabernaemontana divaricata green leaf extract. ZnO NPs have been characterized by X-ray diffraction (XRD), Ultra Violet-Visible (UV-Vis) studies, Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM) and Fourier Transform-Infra Red (FT-IR) analysis. XRD pattern analysis confirms the presence of pure hexagonal wurtzite crystalline structure of ZnO. The TEM images reveal the formation of spherical shape ZnO NPs with the sizes ranging from 20 to 50 nm. The FT-IR analysis suggests that the obtained ZnO NPs have been stabilized through the interactions of steroids, terpenoids, flavonoids, phenyl propanoids, phenolic acids and enzymes present in the leaf extract. Mechanism for the formation of ZnO NPs using Tabernaemontana divaricata as bioactive compound is proposed. As prepared ZnO NPs reveals antibacterial activity against three bacterial strains, Salmonella paratyphi, Escherichia coli and Staphylococcus aureus. The ZnO NPs shows higher antibacterial activity against S. aureus and E. coli and lesser antibacterial activity against S. paratyphi compared to the standard pharmaceutical formulation. Photocatalytic activity of synthesized ZnO NPs was analyzed for methylene blue (MB) dye degradation with sunlight. Almost complete degradation of dye occurred in 90 min. This nano-ZnO, prepared by eco-friendly method will be much useful for dye removal and bacterial decontamination. Copyright © 2018. Published by Elsevier B.V.

Preparation of long alumina fibers by sol-gel method using tartaric acid

NASA Astrophysics Data System (ADS)

Tan, Hong-Bin

2011-12-01

Long alumina fibers were prepared by sol-gel method. The spinning sol was obtained by mixing aluminum nitrate, tartaric acid, and polyvinylpyrrolidone with a mass ratio of 10:3:1.5. Thermogravimetry-differential scanning calorimetry (TG-DSC), Fourier transform infrared (FT-IR) spectra, X-ray diffraction (XRD), and scanning electron microscopy (SEM) were used to characterize the properties of the gel and ceramic fibers. A little of α-Al2O3 phase is observed in the alumina precursor gel fibers sintered at 1273 K. The fibers with a uniform diameter can be obtained when sintered at 1473 K, and its main phase is also indentified as α-Al2O3.

Synthesis, characterization and luminescent properties of mixed phase bismuth molybdate-doped with Eu3+ ions

NASA Astrophysics Data System (ADS)

Wang, Liyong; Guo, Xiaoqing; Cai, Xiaomeng; Song, Qingwei; Han, Yuanyuan; Jia, Guang

2018-02-01

Red phosphors of Eu3+-doped bismuth molybdate (BMO) are prepared by a low temperature hydrothermal method assisting with Phenol Formaldehyde resin (PFr), and characterized by X-ray diffraction (XRD) patterns, Fourier transform infrared-spectroscopy (FT-IR), thermogravimetric analyzer (TGA), differential thermal analyzer (DTA), and photoluminescence (PL) spectroscopy. PL properties influence factors including molar ratio of Bi3+ and Mo3+ ions, PFr dosage and dopants concentration are discussed in detail. The results show that BMO can act as a useful host for Eu3+ ions doping, and energy transferring from Bi3+ to Eu3+ achieved efficiently, the BMO phosphors displayed intense red color emission under ultraviolet light excitation.

Efficient mechanochemical bifunctional nanocatalysts for the conversion of isoeugenol to vanillin

NASA Astrophysics Data System (ADS)

Ostovar, Somayeh; Franco, Ana; Puente-Santiago, Alain R.; Pinilla-de Dios, María; Rodríguez-Padrón, Daily; Shaterian, Hamid R.; Luque, Rafael

2018-04-01

A novel highly functionalized nanocatalyst composed of iron containing SBA-15 material modified with sulfonic acid groups was synthesized by a mechanochemical approach. A full characterization of the obtained nanoreactor was performed by N2 physisorption isotherms analysis, transmission electron microscopy (TEM), X-ray powder diffraction (XRD) and Fourier-Infrared Spectroscopy (FT-IR). The mechanochemically synthesized nanocatalyst displays a high isoeugenol conversion to vanillin under mild conditions using H2O2 as oxidizing agent. Interestingly, this conversion resulted to be higher than that one obtained with the same material synthesized by an impregnation method. Additionally, the nanoreactor showed excellent reusability over four successive runs under the studied reaction conditions.

Enhanced corrosion resistance of strontium hydroxyapatite coating on electron beam treated surgical grade stainless steel

NASA Astrophysics Data System (ADS)

Gopi, D.; Rajeswari, D.; Ramya, S.; Sekar, M.; R, Pramod; Dwivedi, Jishnu; Kavitha, L.; Ramaseshan, R.

2013-12-01

The surface of 316L stainless steel (316L SS) is irradiated by high energy low current DC electron beam (HELCDEB) with energy of 500 keV and beam current of 1.5 mA followed by the electrodeposition of strontium hydroxyapatite (Sr-HAp) to enhance its corrosion resistance in physiological fluid. The coatings were characterised by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and High resolution scanning electron microscopy (HRSEM). The Sr-HAp coating on HELCDEB treated 316L SS exhibits micro-flower structure. Electrochemical results show that the Sr-HAp coating on HELCDEB treated 316L SS possesses maximum corrosion resistance in Ringer's solution.

Synthesis, characterization and properties of L-arginine-passivated silver nanocolloids

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

Sunatkari, A. L., E-mail: ashok.sunatkari@rediffmail.com; Talwatkar, S. S.; Tamgadge, Y. S.

2016-05-06

We investigate the effect of L-arginine-surface passivation on localised surface plasmon resonance (LSPR), size and stability of colloidal Silver Nanoparticles (AgNPs) synthesized by chemical reduction method. The surface Plasmon resonance absorption peak of AgNPs shows blue shift with the increase in L-arginine concentration. Transmission electron microscopy (TEM) analysis confirmed that the average size of AgNPs reduces from 10 nm to 6 nm as the concentration of L-Arginine increased from 1 to 5 mM. The X-ray diffraction study (XRD) confirmed the formation face-centred cubic (fcc) structured AgNPs. FT-IR studies revealed strong bonding between L-arginine functional groups and AgNPs.

Synthesis and properties of precipitated cobalt ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Ristic, Mira; Krehula, Stjepko; Reissner, Michael; Jean, Malick; Hannoyer, Beatrice; Musić, Svetozar

2017-07-01

The formation and properties of cobalt ferrite were investigated with XRD, FT-IR, FE-SEM, Mössbauer and magnetometry. Cobalt ferrite samples were prepared (a) by combining coprecipitation Co(OH)2/2Fe(OH)3, using NaOH between pH 5.2 and 11.4 and autoclaving, and (b) by autoclaving the Co(OH)2/2Fe(OH)3 coprecipitate in a very strong alkaline medium. XRD and FE SEM showed that both CoFe2O4 crystallites and particles were in the nanosize range. The FT-IR spectra were typical of spinel ferrites. Cobalt ferrite precipitated at pH 7.2 and at 11.4 contained a small fraction of α-Fe2O3, whereas in the sample precipitated at pH 11.4 a very small amount (traces) of α-FeOOH were detected by FT-IR, additionally. Parameters obtained by Mössbauer spectroscopy suggested a structural migration of cobalt and iron ions in prepared cobalt ferrite spinels with the prolonged time of autoclaving. Magnetic measurements showed the magnetic behaviour typical of spinel ferrite nanoparticles.

In search of the elusive IrB{sub 2}: Can mechanochemistry help?

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

Xie, Zhilin; Blair, Richard G.; Department of Physics, University of Central Florida, Orlando, FL 32816

The previously unknown hexagonal ReB{sub 2}-type IrB{sub 2} diboride and orthorhombic IrB monoboride phases were produced by mechanochemical syntheses. High energy ball milling of elemental Ir and B powder for 30 h, followed by annealing of the powder at 1050 °C for 48 h, resulted in the formation of the desired phases. Both traditional laboratory and high resolution synchrotron X-ray diffraction (XRD) analyses were used for phase identification of the synthesized powder. In addition to XRD, scanning electron microscopy and transmission electron microscopy were employed to further characterize the microstructure of the phases produced. - Graphical abstract: ReB{sub 2}-type IrB{submore » 2} and a new IrB have been successfully synthesized for the first time using mechanochemical method. Crystal structures of IrB{sub 2} and IrB were studied by synchrotron X-ray diffraction. Microstructures of the new phases were characterized by SEM and TEM. - Highlights: • ReB{sub 2}-type IrB{sub 2} and a new IrB have been synthesized by mechanochemical method. • Crystal structures of IrB{sub 2} and IrB were studied by synchrotron XRD. • Microstructures of the new phases were characterized by SEM and TEM.« less

Structural and magnetic properties of nanocrystalline NiFe2O4 thin film prepared by spray pyrolysis technique

NASA Astrophysics Data System (ADS)

Chavan, Apparao R.; Chilwar, R. R.; Shisode, M. V.; Hivrekar, Mahesh M.; Mande, V. K.; Jadhav, K. M.

2018-05-01

The nanocrystalline NiFe2O4 thin film has been prepared using a spray pyrolysis technique on glass substrate. The prepared thin film was characterized by using X-ray diffraction (XRD), Fourier transform Infrared spectroscopy (FTIR), and Field Emission-Scanning Electron Microscopy (FE-SEM) characterization techniques for the structural and microstructural analysis. The magnetic property was measured using vibrating sample magnetometer (VSM) at room temperature. X-ray diffraction studies show the formation of single phase spinel structure of the thin film. The octahedral and tetrahedral vibration in the sample was studied by Fourier transform infrared (FT-IR) spectra. Magnetic hysteresis loop was recorded for thin film at room temperature. At 15 kOe, saturation magnetization (Ms) was found to increase while coercivity (Hc) decreases with thickness of the NiFe2O4 thin film.

Visible-light-assisted SLCs template synthesis of sea anemone-like Pd/PANI nanocomposites with high electrocatalytic activity for methane oxidation in acidic medium

NASA Astrophysics Data System (ADS)

Tan, De-Xin; Wang, Yan-Li

2018-03-01

Sea anemone-like palladium (Pd)/polyaniline (PANI) nanocomposites were synthesized via visible-light-assisted swollen liquid crystals (SLCs) template method. The resulting samples were characterized by transmission electron microscopy (TEM), selected area electron diffraction (SAED), energy dispersive spectrometer (EDS), x-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), ultraviolet-visible (UV–vis) absorption spectroscopy and Fourier transform infrared (FT-IR) spectroscopy, respectively. The electrocatalytic properties of Pd/PANI nanocomposites modified glass carbon electrode (GCE) for methane oxidation were investigated by cycle voltammetry (CV) and chronoamperometry. Those dispersed sea anemone-like Pd/PANI nanocomposites had an average diameter of 320 nm. The obtained Pd nanoparticles with an average diameter of about 45 nm were uniformly distributed in PANI matrix. Sea anemone-like Pd/PANI nanocomposites exhibited excellent electrocatalytic activity and stability for oxidation of methane (CH4).

Synthesis, molecular structure, FT-IR, Raman, XRD and theoretical investigations of (2E)-1-(5-chlorothiophen-2-yl)-3-(naphthalen-2-yl)prop-2-en-1-one.

PubMed

Chidan Kumar, Chandraju Sadolalu; Fun, Hoong Kun; Parlak, Cemal; Rhyman, Lydia; Ramasami, Ponnadurai; Tursun, Mahir; Chandraju, Siddegowda; Quah, Ching Kheng

2014-11-11

A novel (2E)-1-(5-chlorothiophen-2-yl)-3-(naphthalen-2-yl)prop-2-en-1-one [C17H11ClOS] compound has been synthesized and its structure has been characterized by FT-IR, Raman and single-crystal X-ray diffraction techniques. The isomers, optimized geometrical parameters, normal mode frequencies and corresponding vibrational assignments of the compound have been examined by means of the density functional theory method, employing, the Becke-3-Lee-Yang-Parr functional and the 6-311+G(3df,p) basis set. Reliable vibrational assignments and molecular orbitals have been investigated by the potential energy distribution and natural bonding orbital analyses, respectively. The compound crystallizes in the monoclinic space group P2₁/c with the unit cell parameters a=5.7827(8)Å, b=14.590(2)Å, c=16.138(2)Å and β=89.987 (°). The CC bond of the central enone group adopts an E configuration. There is a good agreement between the theoretically predicted structural parameters and vibrational frequencies and those obtained experimentally. Copyright © 2014 Elsevier B.V. All rights reserved.

Green synthesis of nitrogen-doped graphitic carbon sheets with use of Prunus persica for supercapacitor applications

NASA Astrophysics Data System (ADS)

Atchudan, Raji; Edison, Thomas Nesakumar Jebakumar Immanuel; Perumal, Suguna; Lee, Yong Rok

2017-01-01

Nitrogen-doped graphitic carbon sheets (N-GCSs) were prepared from the extract of unripe Prunus persica fruit by a direct hydrothermal method. The synthesized N-GCSs were examined by high resolution transmission electron microscopy (HRTEM), nitrogen adsorption-desorption isotherms, X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and Fourier transform infrared (FT-IR) spectroscopy. HRTEM showed that the synthesized carbon sheets were graphitic with lattice fringes and an inter-layer distance of 0.36 nm. Doping with the nitrogen moiety present over the synthesized GCSs was confirmed by XPS, FT-IR spectroscopy, and energy dispersive X-ray spectroscopy elemental mapping. The fruit extract associated with hydrothermal-carbonization method is economical and eco-friendly with a single step process. The resulting carbon sheets could be modified and are promising candidates for nano-electronic applications, including supercapacitors. The synthesized N-GCSs-2 provided a high specific capacitance of 176 F g-1 at a current density of 0.1 A g-1. This electrode material has excellent cyclic stability, even after 2000 cycles of charge-discharge at a current density of 0.5 A g-1.

Synthesis, structural and vibrational investigation on 2-phenyl-N-(pyrazin-2-yl)acetamide combining XRD diffraction, FT-IR and NMR spectroscopies with DFT calculations.

PubMed

Lukose, Jilu; Yohannan Panicker, C; Nayak, Prakash S; Narayana, B; Sarojini, B K; Van Alsenoy, C; Al-Saadi, Abdulaziz A

2015-01-25

The optimized molecular structure, vibrational frequencies, corresponding vibrational assignments of 2-phenyl-N-(pyrazin-2-yl)acetamide have been investigated experimentally and theoretically using Gaussian09 software package. The title compound was optimized by using the HF/6-31G(6D,7F) and B3LYP/6-31G(6D,7F) calculations. The geometrical parameters are in agreement with the XRD data. The stability of the molecule arising from hyper-conjugative interaction and charge delocalization has been analyzed using NBO analysis. Gauge-including atomic orbital (1)H-NMR chemical shifts calculations were carried out and compared with experimental data. The HOMO and LUMO analysis is used to determine the charge transfer within the molecule. Molecular electrostatic potential was performed by the DFT method. First hyperpolarizability is calculated in order to find its role in non linear optics. From the XRD data, in the crystal, molecules are held together by strong C-H⋯O and N-H⋯O intermolecular interactions. Copyright © 2014 Elsevier B.V. All rights reserved.

Application of glucose as a green capping agent and reductant to fabricate CuI micro/nanostructures

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

Tavakoli, Farnosh; Salavati-Niasari, Masoud, E-mail: salavati@kashanu.ac.ir; Ghanbari, Davood

Graphical abstract: - Highlights: • CuI nanostructures were prepared via a simple precipitation method. • Glucose as a green capping agent and reductant was applied. • The effect of glucose concentration on the morphology of CuI was investigated. • According to XRD results, pure cubic phase CuI have been formed by using glucose. - Abstract: In this work, CuI micro/nanostructures have been successfully prepared via a simple precipitation route at room temperature. By using glucose as a clean reducing agent with different concentrations, CuI micro/nanostructures with various morphologies were obtained. Besides glucose, Na{sub 2}SO{sub 3}, KBH{sub 4} and N{sub 2}H{submore » 4}·H{sub 2}O have been applied as reductant. X-ray diffraction (XRD), scanning electron microscopy (SEM), photoluminescence spectroscopy, X-ray energy dispersive spectroscopy (EDS) and Fourier transformed infrared (FT-IR) spectroscopy were used to characterize the as-produced CuI micro/nanostructures. According to the XRD results, it was found that pure cubic phase CuI have been formed by using glucose.« less

Synthesis and Characterization of Titanium Dioxide Thin Film for Sensor Applications

NASA Astrophysics Data System (ADS)

Latha, H. K. E.; Lalithamba, H. S.

2018-03-01

Titanium oxide (TiO2) nanoparticles (metal oxide semiconductor) are successfully synthesized using hydrothermal method for sensor application. Titanium dioxide and Sodium hydroxide are used as precursors. These reactants are mixed and calcinated at 400 °C to produce TiO2 nanoparticles. The crystalline structure, morphology of synthesized TiO2 nanoparticles are studied using x-ray diffraction (XRD), Fourier Transform Infrared (FTIR) analysis and scanning electron microscopy (SEM). XRD results revealed that the prepared TiO2 sample is highly crystalline, having Anatase crystal structure. FT-IR spectra peak at 475 cm‑1 indicated characteristic absorption bands of TiO2 nanoparticles. The XRD and FTIR result confirmed the formation of high purity of TiO2 nanoparticles. The SEM image shows that TiO2 nanoparticles prepared in this study are spherical in shape. Synthesized TiO2 nanoparticles are deposited on glass substrate at room temperature using E beam evaporation method to determine gauge factor and found to be 4.7. The deposited TiO2 thin films offer tremendous potential in the applications of electronic and magneto–electric devices.

Synthesis, spectroscopic (UV-Vis, FT-IR and NMR), single crystal XRD of 3,5-diethyl -2,6-di(thiophen-2-yl)piperidin-4-on-1-ium picrate: A comprehensive experimental and computational study

NASA Astrophysics Data System (ADS)

Arockia doss, M.; Rajarajan, G.; Thanikachalam, V.; Selvanayagam, S.; Sridhar, B.

2017-01-01

A piperidin-4-one containing picrate 3,5-diethyl -2,6-di(thiophen-2-yl)piperidin-4-on-1-ium picrate [3,5-DPPP] was synthesized. The molecular structure of 3,5-DPPP was confirmed by FT-IR, NMR, Uv-Vis, single crystal XRD analysis and DFT and HF methods with 6-31G(d,p) basis set. The XRD data confirm the transfer of protons from picric acid (O2) to piperidin-4-one ring (N1). The 3,5-DPPP compound is stabilized by the presence of intermolecular and intramolecular hydrogen bonds (N-H⋯O, C-H⋯S and C-H⋯O). Density functional theory and HF calculations have been used widely for calculating a wide variety of molecular properties such as optimized structure, FT-IR and Uv-Vis spectra, and provided reliable results which are in agreement with experimental data. The charge density data have been used to understand the properties of molecular systems. Furthermore, several quantum chemical insights have been obtained in the form of the total and partial density of states, the HOMO-LUMO energy gap and electrostatic potential map etc. In addition, the polarizability and first hyperpolarizability were calculated to show the potential applications of 3,5-DPPP in nonlinear optics.

Synthesis, structural, thermal and Hirshfeld surface analysis of novel [1,2,4]triazolo[3,4-b][1,3,4] thiadiazine carrying 1,4-benzothiazine-3-one moiety

NASA Astrophysics Data System (ADS)

Shruthi, C.; Ravindrachary, V.; Guruswamy, B.; Lokanath, N. K.; Kumara, Karthik; Goveas, Janet

2018-05-01

Needle shaped single crystal of the title compound was grown by slow evaporation solution growth technique using ethanol as solvent. The grown single crystal was characterized using FT-IR, Single crystal XRD and Thermal analysis. The FT-IR spectrum confirms the molecular structure and identifies the different functional groups present in the compound. Single crystal XRD study reveals that the crystallized compound belongs to the monoclinic crystal system with P21/c space group and the corresponding cell parameters were identified. The thermal stability of the material was determined using both TGA and DTA analysis. The intermolecular interaction of each individual atom in the crystal lattice was estimated using Hirshfeld surface and finger print analysis.

Maltodextrin: A consummate carrier for spray-drying of xylooligosaccharides.

PubMed

Zhang, Liangqing; Zeng, Xianhai; Fu, Nan; Tang, Xing; Sun, Yong; Lin, Lu

2018-04-01

The aim of this study was to evaluate the influence of spray-drying on the powder qualities and microstructures of prebiotic xylooligosaccharides (XOS). The relationships between glass transition temperature (T g ) and XOS retention, moisture content, drying yield as well as specific surface area under different inlet air temperatures and maltodextrin concentrations were investigated. Antioxidant activity retention, hygroscopicity, color attributes, X-ray diffraction (XRD), scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FT-IR) of the spray-dried XOS product were also assessed. The results indicated that an increase in inlet air temperature decreased the moisture content, hence the T g value was increased. Higher maltodextrin concentration increased the T g value, and was attributed to the molecular weight increase. The wall deposition was a tendency to occur when the temperature beyond the T g , reduced the drying yield. Higher temperature and wall deposition promoted the decomposition of XOS into monosaccharide. The crust formation rate of droplets and stickiness of microparticles were affected by T g , and hence, influenced the specific surface area. The antioxidant activity retention of XOS exhibited a concentration-dependent behavior. The hygroscopicity of the microparticles could be reduced by both of the low inlet air temperature and high maltodextrin concentration. According to the results of color attributes, XRD and SEM, the particles were colorless and amorphous, and tended to become more spherical and scattered with the addition of maltodextrin. The FT-IR analysis confirmed that no chemical reaction occurred between XOS and agent, which indicated that maltodextrin is a promising carrier for producing bioactive XOS powder. Copyright © 2018 Elsevier Ltd. All rights reserved.

Obtaining titanium dioxide nanoparticles with spherical shape and antimicrobial properties using M. citrifolia leaves extract by hydrothermal method.

PubMed

M, Sundrarajan; K, Bama; M, Bhavani; S, Jegatheeswaran; S, Ambika; A, Sangili; P, Nithya; R, Sumathi

2017-06-01

In this work, we synthesized titanium dioxide (TiO 2 ) nanoparticles using leaf extract of Morinda citrifolia (M. citrifolia) by the advanced hydrothermal method. The synthesized TiO 2 nanoparticles were characterized by X-ray diffraction (XRD), Fourier transmission infrared (FT-IR), Ultraviolet-visible diffuse reflectance (UV-Vis DRS), Ultraviolet-visible spectroscopy (UV-Vis), Raman spectroscopy, and scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM with EDX) techniques. The XRD major peak at 27.3° corresponds to the (110) lattice plane of tetragonal rutile TiO 2 phase and average crystalline size of nanoparticles is 10nm. The FT-IR result confirmed that TiO 2 nanoparticles and the presences of very few amount of anthraquinone and phenolic compounds of the leaf extract. The obtained nanoparticles were also characterized by UV-Vis DRS absorption spectroscopy and an intense band at 423nm clearly reveals the formation of nanoparticles. SEM images with EDX spectra clearly reveal the size of the nanoparticles, between 15 and 19nm in excellent quasi-spherical shape, by virtue of stabilization (capping) agent. The presence of elements-titanium and oxygen was verified with EDX spectrum. Furthermore, the inhibitory activity of green synthesized TiO 2 nanoparticles was tested against human pathogens like Staphylococcus aureus, Escherichia coli, Bacillus subtilis, Pseudomonas aeruginosa, Candida albicans, and Aspergillus niger by the agar well-diffusion method. The TiO 2 nanoparticles exhibited superior antimicrobial activity against Gram-positive bacteria, demonstrating their antimicrobial value against pathogenic diseases. Copyright © 2017 Elsevier B.V. All rights reserved.

Synthesis of silver nanoparticles from stem bark of Cochlospermum religiosum (L.) Alston: an important medicinal plant and evaluation of their antimicrobial efficacy

NASA Astrophysics Data System (ADS)

Sasikala, A.; Linga Rao, M.; Savithramma, N.; Prasad, T. N. V. K. V.

2015-10-01

The use of different parts of plants for the synthesis of nanoparticles is considered as a green technology as it does not involve any harmful chemicals. Herein, we report on rapid biosynthesis of silver nanoparticles (SNPs) from aqueous stem bark extract of Cochlospermum religiosum a medicinal plant. The reduced silver nanoparticles were characterized by using UV-Visible spectroscopy (UV-Vis), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis, atomic force microscopy, and Fourier transform infrared (FT-IR). The UV-Visible spectrum of the aqueous medium containing silver nanoparticles showed an absorption peak at around 445 nm, XRD showed that the particles are crystalline in nature, with a face-centered cubic structure and the SEM images showed that the spherical-shaped silver nanoparticles were observed and the size range was found to be 20-35 nm. FT-IR spectroscopy analysis revealed that carbohydrate, polyphenols, and protein molecules were involved in the synthesis and capping of silver nanoparticles. These phytosynthesized SNPs were tested for their antimicrobial activity and it analyzed by measuring the inhibitory zone. Cochlospermum religiosum aqueous stem bark extract of SNPs showed highest toxicity to Staphylococcus followed by Pseudomonas, Escherichia coli and Bacillus and lowest toxicity towards Proteus. Whereas in fungal species highest inhibition zone against Aspergillus flavus followed by Rhizopus, Fusarium, and Curvularia, and minimum inhibition zone was observed against Aspergillus niger species. The outcome of this study could be useful for the development of value added products from indigenous medicinal plants of India for nanotechnology-based biomedical applications.

Synthesis, characterization, and controlled release anticorrosion behavior of benzoate intercalated Zn-Al layered double hydroxides

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

Wang, Yi; Zhang, Dun, E-mail: zhangdun@qdio.ac.cn

2011-11-15

Graphical abstract: The benzoate anion released from Zn-Al LDHs provides a more effective long-term protection against corrosion of Q235 carbon steel in 3.5% NaCl solution. Highlights: {yields} A benzoate anion corrosion inhibitor intercalated Zn-Al layered double hydroxides (LDHs) has been assembled by coprecipitation method. {yields} The kinetic simulation indicates that the ion-exchange one is responsible for the release process and the diffusion through particle is the rate limiting step. {yields} A significant reduction of the corrosion rate is observed when the LDH nanohybrid is present in the corrosive media. -- Abstract: Corrosion inhibitor-inorganic clay composite including benzoate anion intercalated Zn-Almore » layered double hydroxides (LDHs) are assembled by coprecipitation. Powder X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectrum analyses indicate that the benzoate anion is successfully intercalated into the LDH interlayer and the benzene planes are vertically bilayer-positioned as a quasi-guest ion-pair form in the gallery space. Kinetic simulation for the release data, XRD and FT-IR analyses of samples recovered from the release medium indicate that ion-exchange is responsible for the release process and diffusion through the particle is also indicated to be the rate-limiting step. The anticorrosion capabilities of LDHs loaded with corrosion inhibitor toward Q235 carbon steel are analyzed by polarization curve and electrochemical impedance spectroscopy methods. Significant reduction of corrosion rate is observed when the LDH nanohybrid is present in the corrosive medium. This hybrid material may potentially be applied as a nanocontainer in self-healing coatings.« less

Synthesis and characterization of oleic acid surface modified magnetic iron oxide nanoparticles by using biocompatible w/o microemulsion for heavy metal removal

NASA Astrophysics Data System (ADS)

Rose, Laili Che; Suhaimi, Hamdan; Mamat, Mazidah; Lik, Thang Zhe

2017-09-01

Oleic acid modified magnetic iron oxide nanoparticles (OA-MIONs) was prepared for removal of Cu2+ ion from aqueous solution. OA-MIONs was prepared by W/O microemulsion template which composed of mixed non-ionic surfactants and 1-hexanol as emulsifier. The effect of weight ratio of the constituent of microemulsion template on the physical and chemical properties of OA-MIONs was studied by characterization using Fourier transform infrared (FT-IR), scanning electron microscopy (SEM) and X-ray powder diffraction (XRD) analysis. FT-IR spectra showed that all templates shared similar chemical structure with slight difference in the peak intensity. Scanning electron micrograph illustrated that the OA-MIONs synthesized via template with the lowest weight ratio of emulsifier to heptane had a more regular spherical shape and was well-distributed. XRD had confirmed that the identity of synthesized OA-MIONs was Fe3O4. Based on the characterization result, the template with lowest weight ratio of emulsifier to heptane was chosen for the heavy metal adsorption study. The adsorption capacity OA-MIONs as a function of pH, contact time and adsorbent dosage were studied. The adsorption process reached equilibrium for 90 minutes and successfully adsorbed 43% of Cu2+ ion from aqueous solution. The adsorption behavior was well described by Langmuir isotherm. The maximum adsorption capacity was determined and found to be 555.56 mg/g. The value of Langmuir equilibrium parameter, RL was found between 0 and 1, suggested that a favorable monolayer adsorption process had taken out.

Antimicrobial and anticancer activities of porous chitosan-alginate biosynthesized silver nanoparticles.

PubMed

Venkatesan, Jayachandran; Lee, Jin-Young; Kang, Dong Seop; Anil, Sukumaran; Kim, Se-Kwon; Shim, Min Suk; Kim, Dong Gyu

2017-05-01

The main aim of this study was to obtain porous antimicrobial composites consisting of chitosan, alginate, and biosynthesized silver nanoparticles (AgNPs). Chitosan and alginate were used owing to their pore-forming capacity, while AgNPs were used for their antimicrobial property. The developed porous composites of chitosan-alginate-AgNPs were characterized using Fourier transform infrared spectroscopy (FT-IR), ultraviolet-visible spectroscopy, X-ray diffraction (XRD) analysis, and scanning electron microscopy (SEM). The FT-IR results revealed the presence of a strong chemical interaction between chitosan and alginate due to polyelectrolyte complex; whereas, the XRD results confirmed the presence of AgNPs in the composites. The dispersion of AgNPs in the porous membrane was uniform with a pore size of 50-500μm. Antimicrobial activity of the composites was checked with Escherichia coli and Staphylococcus aureus. The developed composites resulted in the formation of a zone of inhibition of 11±1mm for the Escherichia coli, and 10±1mm for Staphylococcus aureus. The bacterial filtration efficiency of chitosan-alginate-AgNPs was 1.5-times higher than that of the chitosan-alginate composite. The breast cancer cell line MDA-MB-231 was used to test the anticancer activity of the composites. The IC 50 value of chitosan-alginate-AgNPs on MDA-MB-231 was 4.6mg. The developed chitosan-alginate-AgNPs composite showed a huge potential for its applications in antimicrobial filtration and cancer treatment. Copyright © 2017 Elsevier B.V. All rights reserved.

Role of humic acid on oral drug delivery of an antiepileptic drug.

PubMed

Mirza, Mohd Aamir; Agarwal, Suraj Prakash; Rahman, Md Akhlaquer; Rauf, Abdur; Ahmad, Niyaz; Alam, Aftab; Iqbal, Zeenat

2011-03-01

Humic acid (HA) is omnipresent in natural organic matter that is a macromolecular, negatively charged polyelectrolyte that contains a hydrophobic core. It is also present in a significant amount in Shilajit (used frequently in traditional medicines), which is used in this study as a source of extraction. HA is evaluated for the oral drug delivery of carbamazepine (CBZ). HA is used in this study to increase the dissolution, intestinal permeation, and pharmacodynamic response of CBZ (bio pharmaceutics classification system (BCS) II) by the technique of complexation and other related mechanism reported with humic substances. Different complexation techniques were explored in this study for the entrapment of CBZ, which was authenticated by molecular modeling and conformational analysis. These were further characterized using differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FT-IR), and X-ray diffraction (XRD). Solubility analysis and dissolution release profile were carried out to access the in vitro parameters. For ex vivo studies, rat gut intestinal permeability was done. And finally pharmacodynamic evaluation (maximal electroshock method) was carried out for optimized complexes. Molecular modeling approach and instrumental analysis (DSC, XRD, and FT-IR) confirmed the entrapment of CBZ inside the complexing agent. Increased solubility (∼1742%), sustained release (∼78%), better permeability (∼3.5 times), and enhanced pharmacodynamic responses conferred the best to 1:2 freeze dried (FD) and then 1:2 kneading (KD) complexes compared with pure CBZ. Now it could be concluded that HA may be tried as a complexing agent for antiepileptic drug and other classes of low water-soluble drug.

Synthesis and Characterization of a New Co-Crystal Explosive with High Energy and Good Sensitivity

NASA Astrophysics Data System (ADS)

Gao, Han; Jiang, Wei; Liu, Jie; Hao, Gazi; Xiao, Lei; Ke, Xiang; Chen, Teng

2017-10-01

A new energetic co-crystal consisting of one of the most powerful explosive molecules 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane (CL-20) and the military explosive cyclotrimethylenetrinitramine (RDX) was prepared with a simple solvent evaporation method. Scanning electron microscopy (SEM) revealed the morphology of the bar-shaped product, which differed greatly from the morphology of the individual components. Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, X-ray diffraction spectrum (XRD), and differential scanning calorimetry (DSC) proved the formation of the co-crystal at the molecular level. The result of mechanical sensitivity test indicated the sensitivity was effectively reduced compared to raw CL-20. Finally, a possible crystallization mechanism was discussed.

Photodegradation of methyl red under visible light by mesoporous carbon nitride

NASA Astrophysics Data System (ADS)

Hu, Yueyue; Zhang, Min; Xiao, Zaozao; Jiang, Tao; Yan, Bing; Li, Jian

2018-02-01

Mesoporous carbon nitride (mpg-C3N4) with tunable microstructure has been successfully prepared through a simple polymerization reaction of cyanamide by a nano hard-templating approach. The obtained materials have been characterized using X-ray diffraction (XRD), N2 adsorption, and Fourier transform infrared (FT-IR) spectroscopy. The results show that the pore diameter of the mpg-C3N4 materials can be easily tuned from 3.8 to 10.5 nm. The mpg-C3N4 materials are demonstrated to exhibit much higher visible light photocatalytic activity than that of g-C3N4 for the degradation of aqueous methyl red (MR). The high surface areas and large pore volume contributed to the efficient visible light photocatalytic activity.

A novel ultrasonication method in the preparation of zirconium impregnated cellulose for effective fluoride adsorption.

PubMed

Barathi, M; Kumar, A Santhana Krishna; Rajesh, N

2014-05-01

In the present work, we propose for the first time a novel ultrasound assisted methodology involving the impregnation of zirconium in a cellulose matrix. Fluoride from aqueous solution interacts with the cellulose hydroxyl groups and the cationic zirconium hydroxide. Ultrasonication ensures a green and quick alternative to the conventional time intensive method of preparation. The effectiveness of this process was confirmed by comprehensive characterization of zirconium impregnated cellulose (ZrIC) adsorbent using Fourier transform infrared spectroscopy (FT-IR), energy dispersive X-ray spectrometry (EDX) and X-ray diffraction (XRD) studies. The study of various adsorption isotherm models, kinetics and thermodynamics of the interaction validated the method. Copyright © 2013 Elsevier B.V. All rights reserved.

Photo and Thermal Behavior of New Reinforced Polyamide-nanocomposite Montmorillonite on 2,3-Pyrazin Dicarboxylic Acid

NASA Astrophysics Data System (ADS)

Faghihi, Khalil; Samiei, Mojtaba; Hajibeygi, Mohsen

2012-06-01

Two new samples of reinforce polyamidemontmorillonite nanocomposites were synthesized by a convenient solution intercalation technique. Polyamide (PA) 3 as a source of polymer matrix was synthesized by the direct polycondensation reaction of pyrazine 2,3-dicarboxylic acid 1 with 4,4'-diamino diphenyl ether 2 in the presence of triphenyl phosphite (TPP), CaCl2, pyridine and N-methyl-2-pyrrolidone (NMP). The resulting nanocomposite films were characterized by Fourier transform infrared spectra (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM) and thermogravimetric analysis (TGA). The results showed that organo-modified clay was dispersed homogeneously in PA matrix. TGA indicated an enhancement of thermal stability of new nanocomposites compared with the pure polymer.

In situ surface treatment of nanocrystalline MFe2O4 (M = Co, Mg, Mn, Ni) spinel ferrites using linseed oil

NASA Astrophysics Data System (ADS)

Gherca, Daniel; Cornei, Nicoleta; Mentré, Olivier; Kabbour, Houria; Daviero-Minaud, Sylvie; Pui, Aurel

2013-12-01

This paper reports the synthesis by coprecipitation method of MFe2O4 nanoparticles using linseed oil as the in-situ surfactant. The decomposition process of the precursors and the formation process of MFe2O4 were investigated by thermogravimetric analysis and differential thermal analysis (TG-DTA). The crystal structure and surface morphology were examined by means of X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM) analysis. The results demonstrate that the surface of MFe2O4 with a diameter in the range 5-13 nm, is activated with hydrophilic groups of the surfactant which coat them and enhance the stability. Magnetic properties are discussed.

Plasma induced grafting carboxymethyl cellulose on multiwalled carbon nanotubes for the removal of UO(2)(2+) from aqueous solution.

PubMed

Shao, Dadong; Jiang, Zhongqing; Wang, Xiangke; Li, Jiaxing; Meng, Yuedong

2009-01-29

Carboxymethyl cellulose (CMC) is grafted on multiwalled carbon nanotubes (MWCNT) by using plasma techniques. The CMC grafted MWCNT (MWCNT-g-CMC) is characterized by using Fourier transform infrared spectra (FT-IR), Raman spectra, powder X-ray diffraction (XRD), thermogravimetric analysis (TGA)-differential thermal analysis (DTA), scanning electron microscopy (SEM), and N(2)-BET methods in detail. The application of MWCNT-g-CMC in the removal of UO(2)(2+) from aqueous solution is investigated. MWCNT-g-CMC has much higher sorption ability in the removal of UO(2)(2+) than raw MWCNT. The MWCNT-g-CMC is a suitable material in the preconcentration and solidification of heavy metal ions from large volume of aqueous solutions.

Study of the thermal treatment of SiO2 aggregate

NASA Astrophysics Data System (ADS)

Tahiri, N.; Khouchaf, L.; Elaatmani, M.; Louarn, G.; Zegzouti, A.; Daoud, M.

2014-08-01

Crystalline quality and the silanoles defects (Si-OH) present within the structure of natural SiO2 play an important role in its reactivity. In this work, the relationship between the loss of silanoles and the crystallinity improvement upon heating between 450 °C and 650 °C was shown using X-Ray Diffraction (XRD) and Fourier Transform mid Infrared Spectroscopy in Attenuated Total Reflection (ATR). A shift of the principal band Si-O-Si from 1078 cm-1 to 1082 cm-1 and the decrease of the intensity of the Si-OH bands at 555cm-1and at 950cm-1 upon heating between 450 °C and 650 °C were shown. The reduction of the band is correlated to the loss of silanoles. In agreement with FT-IR results, the decrease of the FWHM of the XRD peaks shows that the crystalline quality is improved upon heating. This result leads to a decrease of the reactivity of SiO2 aggregate under chemical attacks.

An electrochemical sensor based on nitrogen doped carbon material prepared from nitrogen-containing precursors

NASA Astrophysics Data System (ADS)

Cui, G. Y.; Wang, C. Y.; Xiang, G. Q.; Zhou, B.

2018-01-01

In this work, a nitrogen doped carbon material (NDC) was prepared by using a copper adenine complex as precursor and applied to electrochemical sensing of Vitamin B2 (VB2). The experimental results show that the nitrogen doped carbon material is obtained after calcination at 650 °C under argon atmosphere, afterwards, which were characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), fourier transform infrared (FT-IR), and electrochemical method. According to the XRD data, the product was a carbon material, and infrared data demonstrates that there are two kinds of carbonyl nitrogen combination, respectively, C-N and C = N combination of ways. Importantly, we used NDC to construct electrochemical biosensor to detect VB2 by differential pulse voltammetry (DPV). The linear range was 6 × 10-6 - 3.5 × 10-4 M (R=0.9962), the minimum detection limit was 5.4 × 10-6 M, and the sensitivity is better. Consequently, it has better sensing performance.

Synthesis, optical properties and efficient photocatalytic activity of CdO/ZnO hybrid nanocomposite

NASA Astrophysics Data System (ADS)

Reddy, Ch Venkata; Babu, B.; Shim, Jaesool

2018-01-01

Pure CdO, ZnO and CdO/ZnO hybrid nanocomposite photocatalyst were synthesized using simple co-precipitation technique and studied in detail. The synthesized photocatalysts were characterized using several measurements such as X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), surface analysis (BET), diffuse reflectance UV-vis spectroscopy, X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, FT-IR, TG-DTA and photoluminescence (PL). The XRD results revealed that the hexagonal and cubic crystal structure of CdO and ZnO nanoparticles. The optical response for the composite showed the presence of separate absorption signature for CdO and ZnO in the visible region at about 510 nm and 360 nm respectively. The CdO/ZnO hybrid nanocomposite photocatalyst exhibited enhanced photocatalytic degradation activity compared to pristine CdO and ZnO. The enhanced photocatalytic activity may be due to the higher specific surface area and significantly reduced the electron-hole recombination rate.

Intercalation of IR absorber into layered double hydroxides: Preparation, thermal stability and selective IR absorption

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

Zhu, Haifeng; Tang, Pinggui; Feng, Yongjun, E-mail: yjfeng@mail.buct.edu.cn

2012-03-15

Highlights: Black-Right-Pointing-Pointer PMIDA anions were intercalated into Mg{sub 2}Al-NO{sub 3} LDH by anion-exchange method. Black-Right-Pointing-Pointer The prepared material has highly selective IR absorption property in 9-11 {mu}m. Black-Right-Pointing-Pointer The obtained material has practical applications as heat-retaining additive. -- Abstract: N-phosphonomethyl aminodiacetic acid (PMIDA) was intercalated into the interlayer spacing of layered double hydroxides (LDH) by an anion-exchange method. The intercalated LDHs were characterized by various techniques such as powder X-ray diffraction (XRD), FT-IR spectroscopy, elemental analysis and simultaneous thermogravimetric and mass spectrometry (TG-MS) in details. The results show the formation of Mg{sub 2}Al-PMIDA LDH based on the expansion of d-spacingmore » from 0.89 nm to 1.22 nm and the disappearance of the characteristic IR absorption band at 1384 cm{sup -1} for NO{sub 3}{sup -} anions. The incorporation of Mg{sub 2}Al-PMIDA LDH into the low density polyethylene (LDPE) as an additive enhances the selectivity of IR absorption in the main wavelength region 9-11 {mu}m for radiant heat loss at night. Mg{sub 2}Al-PMIDA LDH as a heat-retaining additive has practical application in agricultural plastic films.« less

Experimental (13C NMR, 1H NMR, FT-IR, single-crystal X-ray diffraction) and DFT studies on 3,4-bis(isoproylamino)cyclobut-3-ene-1,2-dione.

PubMed

Süleymanoğlu, Nevin; Ustabaş, Reşat; Alpaslan, Yelda Bingöl; Eyduran, Fatih; Ozyürek, Cengiz; Iskeleli, Nazan Ocak

2011-12-01

In this work, 3,4-bis(isoproylamino)cyclobut-3-ene-1,2-dione C(10)H(16)N(2)O(2) (I), was synthesized and characterized by (13)C NMR, (1)H NMR, FT-IR, UV-vis spectroscopy and single-crystal X-ray diffraction. DFT method with 6-31G(d,p) basis set has been used to calculate the optimized geometrical parameters, atomic charges, vibrational frequencies and chemical shift values. The calculated vibrational frequencies and chemical shift values are compared with experimental FT-IR and NMR spectra. The results of the calculation shows good agreement between experimental and calculated values of the compound I. The existence of N-H⋯O type intermolecular ve C-H⋯O type intramolecular hydrogen bonds can be deduced from differences between experimental and calculated results of FT-IR and NMR. In addition, the molecular electrostatic potential map and frontier molecular orbitals and electronic absorption spectra were performed at B3LYP/6-31G(d,p) level of theory. HOMO-LUMO electronic transition of 4.90 eV are derived from the contribution of the bands π→π* and n→π* The spectral results obtained from FT-IR, NMR and X-ray of I revealed that the compound I is in predominantly enamine tautomeric form, which was supported by DFT calculations. Copyright © 2011 Elsevier B.V. All rights reserved.

Biofabrication of zinc oxide nanoparticles using fruit extract of Rosa canina and their toxic potential against bacteria: A mechanistic approach.

PubMed

Jafarirad, Saeed; Mehrabi, Meysam; Divband, Baharak; Kosari-Nasab, Morteza

2016-02-01

The use of plant extract in the biosynthesis of nanoparticles (NPs) can be an eco-friendly approach and have been suggested as a possible alternative to classic methods namely physical and chemical procedures. In this study, the biosynthesis of zinc oxide (ZnO) NPs by both "conventional heating" (CH) and "microwave irradiation" (MI) methods has been reported. Stable and spherical ZnONPs were produced using zinc nitrate and flesh extract of Rosa canina fruit (rosehip) which was used as a precursor. The flesh extract acts as a reducing and capping agent for generation of ZnONPs. The structural, morphological and colloidal properties of the as-synthesized NPs have been confirmed by X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Energy Dispersive X-ray (EDX), Fourier transform Infrared (FT-IR) and Dynamic Light Scattering (DLS). In comparison with the CH method, the MI method has some advantages such as significantly short reaction time (within 8min) owing to the high heating rate and thus the accelerated reaction rate. Both methods led to the synthesis of nearly identical NPs with respect to shape and size according to the results of DLS, XRD and SEM techniques. The possible mechanism for synthesis pathway has been proposed based on FT IR results, XRD patterns, potentiometric data and antioxidant activity. In addition, the antibacterial activity of as-prepared ZnONPs was investigated against several bacteria such as Listeria monocytogenes, Escherichia coli, Salmonella typhimurium. Moreover, the efficacy of ZnONPs to treat cancer cell lines were measured by means of cell viability test via MTT assay in which concentrations of 0.05 and 0.1mg/mL of ZnONPs induced a very low toxicity. Thus, the present investigation reveals that ZnONPs have the potential for various medical and industrial applications. Copyright © 2015 Elsevier B.V. All rights reserved.

Preparation and characterization of bee venom-loaded PLGA particles for sustained release.

PubMed

Park, Min-Ho; Jun, Hye-Suk; Jeon, Jong-Woon; Park, Jin-Kyu; Lee, Bong-Joo; Suh, Guk-Hyun; Park, Jeong-Sook; Cho, Cheong-Weon

2016-12-14

Bee venom-loaded poly(lactic-co-glycolic acid) (PLGA) particles were prepared by double emulsion-solvent evaporation, and characterized for a sustained-release system. Factors such as the type of organic solvent, the amount of bee venom and PLGA, the type of PLGA, the type of polyvinyl alcohol, and the emulsification method were considered. Physicochemical properties, including the encapsulation efficiency, drug loading, particle size, zeta-potential and surface morphology were examined by Fourier transform infrared (FT-IR) spectroscopy, differential scanning calorimetry (DSC), and X-ray diffraction (XRD). The size of the bee venom-loaded PLGA particles was 500 nm (measured using sonication). Zeta-potentials of the bee venom-loaded PLGA particles were negative owing to the PLGA. FT-IR results demonstrated that the bee venom was completely encapsulated in the PLGA particles, indicated by the disappearance of the amine and amide peaks. In addition, sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) analysis indicated that the bee venom in the bee venom-loaded PLGA particles was intact. In vitro release of the bee venom from the bee venom-loaded PLGA particles showed a sustained-release profile over 1 month. Bee venom-loaded PLGA particles can help improve patients' quality of life by reducing the number of injections required.

Preparation of PEO/Clay Nanocomposites Using Organoclay Produced via Micellar Adsorption of CTAB

PubMed Central

Gürses, Ahmet; Ejder-Korucu, Mehtap; Doğar, Çetin

2012-01-01

The aim of this study was the preparation of polyethylene oxide (PEO)/clay nanocomposites using organoclay produced via micellar adsorption of cethyltrimethyl ammonium bromide (CTAB) and their characterisation by X-ray diffraction (XRD), and Fourier transform infrared (FT-IR) spectra, and the investigation of certain mechanical properties of the composites. The results show that the basal distance between the layers increased with the increasing CTAB/clay ratio as parallel with the zeta potential values of particles. By considering the aggregation number of CTAB micelles and interlayer distances of organo-clay, it could be suggested that the predominant micelle geometry at lower CTAB/clay ratios is an ellipsoidal oblate, whereas, at higher CTAB/clay ratios, sphere-ellipsoid transition occurs. The increasing tendency of the exfoliation degree with an increase in clay content may be attributed to easier diffusion of PEO chains to interlayer regions. FT-IR spectra show that the intensity of Si-O stretching vibrations of the organoclays (1050 cm−1) increased, especially in the ratios of 1.0 g/g clay and 1.5 g/g clay with the increasing CTAB content. It was observed that the mechanical properties of the composites are dependent on both the CTAB/clay ratios and clay content of the composites. PMID:23365515

Facile and low temperature route to synthesis of CuS nanostructure in mesoporous material by solvothermal method.

PubMed

Sohrabnezhad, Sh; Zanjanchi, M A; Hosseingholizadeh, S; Rahnama, R

2014-04-05

The synthesis of CuS nanomaterial in MCM-41 matrix has been realized by chemical synthesis between MCM-41, copper sulfate pentahydrate and thiourea via a solvothermal method in ethylene glycol and water, separately. X-ray diffraction analysis (XRD), diffuse reflectance spectroscopy (DRS), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and fourier transform infrared (FT-IR) were used to characterize the products. At synthesized CuS/MCM-41 sample in ethylene glycol, X-ray diffraction and diffuse reflectance spectroscopy showed pure covellite phase of copper sulfide with high crystality. But prepared CuS/MCM-41 sample in water shows the covellite, chalcocite and the djurleite phase of copper sulfide nanostructures. The formation of CuS nanostructures was confirmed by FT-IR. Photocatalytic activity of CuS/MCM-41 nanocomposites was studied for degradation of Methylene Blue (MB) under visible light. The CuS/MCM-41 nanocomposite is more effective nanocatalyst than synthesized CuS/MCM-41 sample in water for degradation of methylene blue. Several parameters were examined, catalyst amount (0.1-1gL(-1)), pH (1-13) and initial concentration of MB (0.96-10ppm). The extent of degradation was estimated from the residual concentration by spectrophotometrically. The support size was obtained in the range 60-145nm by TEM. In the same way, the average size of copper sulfide in CuSMCM-41E and CuS/MCM-41W nanostructures were obtained about 10nm and 16nm, respectively. Copyright © 2013 Elsevier B.V. All rights reserved.

Structural and microstructural aspects of asbestos-cement waste vitrification

NASA Astrophysics Data System (ADS)

Iwaszko, Józef; Zawada, Anna; Przerada, Iwona; Lubas, Małgorzata

2018-04-01

The main goal of the work was to evaluate the vitrification process of asbestos-cement waste (ACW). A mixture of 50 wt% ACW and 50 wt% glass cullet was melted in an electric furnace at 1400 °C for 90 min and then cast into a steel mold. The vitrified product was subjected to annealing. Optical microscopy, scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD) were used to evaluate the effects of the vitrification. The chemical constitution of the material before and after the vitrification process was also analyzed. It was found that the vitrified product has an amorphous structure in which the components of asbestos-cement waste are incorporated. MIR spectroscopy showed that the absorption bands of chrysotile completely disappeared after the vitrification process. The results of the spectroscopic studies were confirmed by X-ray studies - no diffraction reflections from the chrysotile crystallographic planes were observed. As a result of the treatment, the fibrous asbestos construction, the main cause of its pathogenic properties, completely disappeared. The vitrified material was characterized by higher resistance to ion leaching in an aquatic environment than ACW and a smaller volume of nearly 72% in relation to the apparent volume of the substrates. The research has confirmed the high effectiveness of vitrification in neutralizing hazardous waste containing asbestos and the FT-IR spectroscopy was found to be useful to identify asbestos varieties and visualizing changes caused by the vitrification process. The work also presents the current situation regarding the utilization of asbestos-containing products.

Synthesis, spectroscopic, thermal and structural properties of [M(3-aminopyridine)2Ni(μ-CN)2(CN)2]n (M(II) = Co and Cu) heteropolynuclear cyano-bridged complexes

NASA Astrophysics Data System (ADS)

Kartal, Zeki

2016-01-01

Two novel cyano-bridged heteropolynuclear complexes, [Co(3-aminopyridine)2Ni(μ-CN)2(CN)2]n and [Cu(3-aminopyridine)2Ni(μ-CN)2(CN)2]n have been synthesized and characterized by elemental, thermal, FT-IR and FT-Raman spectroscopies. The structures of complexes have been determined by X-ray powder diffraction. The FT-IR and FT-Raman spectra of complexes have been recorded in the region of 3500-400 cm-1 and 3500-100 cm-1, respectively. General information was acquired about structural properties of these complexes from FT-IR and FT-Raman spectra by considering changes at characteristic peaks of the cyano group and 3AP. The splitting of the ν(Ctbnd N) stretching bands in the FT-IR spectra for complexes indicates the presence of terminal and bridging cyanides. The thermal behaviors of these complexes have been also investigated in the range of 25-950 °C using TG and DTG methods. Magnetic susceptibility measurements were made at room temperature using Gouy-balance.

Comparative study of hydroxyapatite from eggshells and synthetic hydroxyapatite for bone regeneration.

PubMed

Lee, Sang-Woon; Kim, Seong-Gon; Balázsi, Csaba; Chae, Weon-Sik; Lee, Hee-Ok

2012-03-01

The objective of this study was to evaluate the physical properties of synthetic hydroxyapatite (sHA) and hydroxyapatite from eggshells (eHA) by Fourier-transform infrared (FT-IR) and x-ray diffraction (XRD) and to compare the regenerative ability of the bone using sHA and eHA in a rabbit calvarial defect model. FT-IR and XRD were used to compare the physical properties of sHA and eHA. sHA was purchased from Sigma, and eHA was kindly donated from the Hungarian academy of science. Sixteen New Zealand white rabbits were used for the animal study. After the formation of a bilateral parietal bony defect (diameter 8.0 mm), either sHA or eHA was grafted into the defect. The defect in the control was left unfilled. Bone regeneration was evaluated by histomorphometry at 4 and 8 weeks after the operation. The peak broadening of the XRD experiments were in agreement with scanning electron microscope observation; the sHA had a smaller granule size than the eHA. The eHA had impurities phases of CaO (International Center for Diffraction Data (ICDD) 075-0264) and Ca(OH)(2) (ICDD 072-0156). Total new bone was 17.11 ± 10.24% in the control group, 28.81 ± 12.63% in sHA group, and 25.68 ± 10.89% in eHA group at 4 weeks after the operation. The difference was not statistically significant (P > .05). Total new bone at 8 weeks after the operation was 27.50 ± 10.89% in the control group, 38.62 ± 17.42% in sHA group, and 41.99 ± 8.44% in the eHA group. When comparing the sHA group to the control group, the difference was not statistically significant (P > .05). However, the eHA group was significantly different from the control group (P = .038). When comparing the eHA group to the sHA group, the difference was not statistically significant (P > .05). Both types of HA showed higher bone formation than the unfilled control. However, eHA had significantly higher bone formation than the unfilled control at 8 weeks after operation. Copyright © 2012 Elsevier Inc. All rights reserved.

Structure and magnetic properties of SiO{sub 2}/PCL novel sol–gel organic–inorganic hybrid materials

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

Catauro, Michelina, E-mail: michelina.catauro@unina2.it; Bollino, Flavia; Cristina Mozzati, Maria

2013-07-15

Organic–inorganic nanocomposite materials have been synthesized via sol–gel. They consist of an inorganic SiO{sub 2} matrix, in which different percentages of poly(ε-caprolactone) (PCL) have been incorporated. The formation of H-bonds among the carbonyl groups of the polymer chains and Si–OH group of the inorganic matrix has been proved by means of Fourier transform infrared spectroscopy (FT-IR) analysis and has been confirmed by solid-state nuclear magnetic resonance (NMR). X-Ray diffraction (XRD) analysis highlighted the amorphous nature of the synthesized materials. Scanning electron microscope (SEM) micrograph and atomic force microscope (AFM) topography showed their homogeneous morphology and nanostructure nature. Considering the opportunitymore » to synthesize these hybrid materials under microgravity conditions by means of magnetic levitation, superconducting quantum interference device (SQUID) magnetometry has been used to quantify their magnetic susceptibility. This measure has shown that the SiO{sub 2}/PCL hybrid materials are diamagnetic and that their diamagnetic susceptibility is independent of temperature and increases with the PCL amount. - Graphical abstract: Characterization and magnetic properties of SiO{sub 2}/PCL organic–inorganic hybrid materials synthesized via sol–gel. FT-IR, Fourier transform infrared spectroscopy; solid-state NMR: solid-state nuclear magnetic resonance; SQUID: superconducting quantum interference device. - Highlights: • Sol–gel synthesis of SiO{sub 2}/PCL amorphous class I organic–inorganic hybrid materials. • FT-IR and NMR analyses show the hydrogen bonds formation between SiO{sub 2} and PCL. • AFM and SEM analyses confirm that the SiO{sub 2}/PCL are homogenous hybrid materials. • The SQUID measures show that the simples are diamagnetic. • Diamagnetic susceptibility of SiO{sub 2}/PCL materials increases with the PCL amount.« less

Influence of nickel substitution on crystal structure and magnetic properties of strontium ferrite preparation via sol-gel auto-combustion route

NASA Astrophysics Data System (ADS)

Roohani, Ebrahim; Arabi, Hadi; Sarhaddi, Reza

2018-01-01

In this research, SrFe12-xNixO19 (x = 0 - 1) hexagonal ferrites were prepared by sol-gel auto-combustion method. Effect of Ni substitution on structural, morphological and magnetic properties of nanoparticles was investigated by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), Transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM), respectively. The XRD results confirmed that all samples with x ≤ 0.5 have single phase M-type strontium ferrite structure, whereas for the SrFe12-xNixO19 samples with x > 0.5, the spinel NiFe2O4 phase has also appeared. The lattice parameters and crystallite sizes of the powders were concluded from the XRD data and Williamson-Hall method. Magnetic analyses showed that the coercivity of powders decreased from 5672 Oe to 639 Oe while the saturation magnetization increased from 74 emu/g to 81 emu/g with nickel substitution. The results of this study suggest that the strontium hexaferrites doped with Ni are suitable for applications in high density magnetic recording media as well as microwave devices because of their promising magnetic properties.

Ultrasonic-assisted synthesis of nano lead(II) coordination polymer as precursors for preparation of lead(II) oxide nano-structures: Thermal, optical properties and XRD studies.

PubMed

Ghavidelaghdam, Elham; Shahverdizadeh, Gholam Hossein; Motameni Tabatabai, Javad; Mirtamizdoust, Babak

2018-04-01

Nano structure of a lead (II) coordination polymer [Pb 2 (C 2 Cl 3 O 2 ) 2 (NO 3 ) 2 (C l2 H 8 N 2 ) 2 ] n (1), has been synthesized by a sonochemical method in different concentrations. The nano particles were characterized by scanning electron microscopy (SEM) X-ray powder diffraction (XRD), FT-IR spectroscopy and elemental analyses. The thermal stability of nano structure is closely investigated via thermal gravimetric (TGA), and compared with crystalline structure. The compounds are then heated to 600 °C to produce PbO nano particles. The resulting PbO is characterized through XRD and SEM analyses. Concentration of initial reagents effects on size and morphology of nano-structured compound 1 have been studied and show that low concentrations of initial reagents decreased particles size and leaded to uniform nano particles morphology. The photoluminescence properties of the prepared compound, as crystalline and as nanoparticles, have been investigated. The result showed a good correlation between the size and emission wavelength. Copyright © 2017. Published by Elsevier B.V.

Characterization of sodium phenytoin co-gelled with titania for a controlled drug-release system

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

Lopez, T.; Instituto Nacional de Neurologia y Neurocirugia 'MVS', Av. Insurgentes Sur 3877. Col. La Fama. P.O. Box 14269 Mexico D. F.; Quintana, P.

2007-08-15

Sodium phenytoin, C{sub 15}H{sub 11}N{sub 2}NaO{sub 2}, in several concentrations was co-gelled with titania (TiO{sub 2}), by a sol-gel process. This technique is a promising method to encapsulate several drugs, in this case, phenytoin is an anticonvulsant used to control epileptic seizures. Samples were prepared by adding different concentrations (X = 50, 100, 200 and 250 mg per 20 g of titania matrix) of sodium phenytoin (Ph) to a solution of titanium n-butoxide. The resulting titania-Ph-X materials were characterized by transmission electron microscopy (TEM), Fourier transformed infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), and Brunauer-Emmet-Teller (BET) surface areas. The porous nanomaterialsmore » showed a wide range of particle size, from 10 to 210 nm, with a mean pore diameter of 5 nm. X-ray diffraction showed an amorphous structure of the prepared samples.« less

Spinel NixZn1-xFe2O4 (0.0 ≤ x ≤ 1.0) nano-photocatalysts: Synthesis, characterization and photocatalytic degradation of methylene blue dye

NASA Astrophysics Data System (ADS)

Padmapriya, G.; Manikandan, A.; Krishnasamy, V.; Jaganathan, Saravana Kumar; Antony, S. Arul

2016-09-01

Spinel NixZn1-xFe2O4 (x = 0.0 to 1.0) nanoparticles were successfully synthesized by a simple microwave combustion method (MCM) using metal nitrates as raw materials and glycine as the fuel. The structural, morphological and opto-magnetic properties of the spinel NixZn1-xFe2O4 ferrites were determined by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), high resolution scanning electron microscopy (HR-SEM), energy dispersive X-ray (EDX) spectroscopy, high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED) pattern, UV-Visible diffuse reflectance spectroscopy (DRS), photoluminescence (PL) spectroscopy and vibrating sample magnetometer (VSM). Powder XRD, and EDX analysis was confirmed the formation of pure phase of spinel ferrites. HR-SEM and HR-TEM analysis was confirmed the formation of sphere like-particle morphology of the samples with smaller agglomeration. VSM analysis clearly showed the superparamagnetic and ferromagnetic nature of the samples. The Ms value is 3.851 emu/g for undoped ZnFe2O4 sample and it increased with increase in Ni content. Photo-catalytic degradation (PCD) of methylene blue (MB) dye using the samples were carried out and observed good PCD results.

Preparation of Copper (II) Containing Phosphomolybdic Acid Salt as Catalyst for the Synthesis of Biodiesel by Esterification.

PubMed

Cai, Jie; Zhang, Qiu-Yun; Wei, Fang-Fang; Huang, Jin-Shu; Feng, Yun-Mei; Ma, Hai-Tao; Zhang, Yutao-

2018-04-01

Copper (II) containing phosphomolybdic acid (PMA) catalysts were synthesized by ion exchange method and characterization using various physico-chemical techniques such as X-ray diffraction (XRD), fourier transform infrared spectroscopy (FT-IR), thermogravimetric (TG) and scanning electron microscopy (SEM). The characterization results showed that the Keggin ions were retained in the catalysts and possessed well thermal stability. The catalytic esterification of lauric acid with methanol could be easily achieved about 78.7% conversion under optimum condition, the catalyst also contributed to the stability of the catalyst in which it can be reused for a certain time. This study demonstrated an alternative approach to biodiesel production with high efficiency by Cu (II) ion exchanged phosphomolybdic acid catalyst in the esterification catalytic.

Conductivity study of thermally stabilized RuO2/polythiophene nanocomposites

NASA Astrophysics Data System (ADS)

Hebbar, Vidyashree; Bhajantri, R. F.

2018-04-01

The polymer nanocomposites of Ruthenium oxide (RuO2) filled polythiophene (PT) were synthesized by polymerization using chemical method. The purity of the synthesized polymer composite is verified using X-Ray diffraction (XRD). The structural discrepancies of the RuO2 filled PT composites are studied by Fourier transform infrared (FT-IR) spectroscopy. The phase transition and thermal stability of the prepared composite is revised by thermal characterization such as differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). The DC conductivity of RuO2 filled PT composite in the form of pellets is calculated using current-voltage (I-V) characterization by two-probe method. The enhancement in conductivity with increased RuO2 content in PT matrix is examined, which is the required property for electrical and electronic applications in supercapacitors.

A facile mechanochemical approach to synthesize Zn-Al layered double hydroxide

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

Qu, Jun, E-mail: forsjun@whut.edu.cn; He, Xiaoman; Chen, Min

2017-06-15

In this study, a mechanochemical route to synthesize Zn-Al layered double hydroxide (LDH) was introduced, in which Zn basic carbonate and Al hydroxide were first dry milled into an activated state and then agitated in water to obtain the final products. The as-prepared samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Thermogravimetry (TG) and Scanning electron microscopy (SEM). The products possessed a high crystallinity of Zn–Al LDH phase without any other impurities, proving a facile and effective preparation of Zn–Al LDH by using non-heating mechanochemical approach. - Highlights: • A non-heating mechanochemical route to synthesize Zn-Almore » LDH. • The products possessed high crystalline Zn-Al LDH phase. • No emission of other impurities or wastewater.« less

Tetrapeptide-coumarin conjugate 3D networks based on hydrogen-bonded charge transfer complexes: gel formation and dye release.

PubMed

Guo, Zongxia; Gong, Ruiying; Jiang, Yi; Wan, Xiaobo

2015-08-14

Oligopeptide-based derivatives are important synthons for bio-based functional materials. In this article, a Gly-(L-Val)-Gly-(L-Val)-coumarin (GVGV-Cou) conjugate was synthesized, which forms 3D networks in ethanol. The gel nanostructures were characterized by UV-vis spectroscopy, FT-IR spectroscopy, X-ray diffraction (XRD), SEM and TEM. It is suggested that the formation of charge transfer (CT) complexes between the coumarin moieties is the main driving force for the gel formation. The capability of the gel to encapsulate and release dyes was explored. Both Congo Red (CR) and Methylene Blue (MB) can be trapped in the CT gel matrix and released over time. The present gel might be used as a functional soft material for guest encapsulation and release.

Rapid preparation process of antiparkinsonian drug Mucuna pruriens silver nanoparticle by bioreduction and their characterization

PubMed Central

Arulkumar, Subramanian; Sabesan, Muthukumaran

2010-01-01

Backgorund: Development of biologically inspired experimental processes for the synthesis of nanoparticles is evolving an important branch of nanotechnology. Methods: The bioreduction behavior of plant seed extract of Mucuna pruriens in the synthesis of silver nanoparticles was investigated employing UV/visible spectrophotometry, X-ray diffraction (XRD), and transmission electron microscopy (TEM), Fourier transform – infra red (FT- IR). Result: M. pruriens was found to exhibit strong potential for rapid reduction of silver ions. The formation of nanoparticles by this method is extremely rapid, requires no toxic chemicals, and the nanoparticles are stable for several months. Conclusion: The main conclusion is that the bioreduction method to produce nanoparticles is a good alternative to the electrochemical methods and it is expected to be biocompatible. PMID:21808573

Ag-doped CdO nanocatalysts: Preparation, characterization and catechol oxidase activity

NASA Astrophysics Data System (ADS)

El-Kemary, Maged; El-Mehasseb, Ibrahim; El-Shamy, Hany

2018-06-01

Silver doped cadmium oxide (Ag/CdO) nanoparticles with an average size of 41 nm have been successfully synthesized via thermal decomposition and liquid impregnation technique. The structural characterization has been performed by using several spectroscopic techniques, e.g., X-ray diffraction (XRD), scanning electron microscopy (SEM) and fourier-transform infrared (FT-IR). The catechol oxidase has been studied by UV-visible absorption spectroscopy and fourier-transform infrared as well as the mechanism has been assured by cyclic voltammetry and fluorescence spectroscopy. The results indicate that the oxidation does not occur in the presence of unsupported cadmium oxide particles by silver and in the same time, the catechol oxidase activity of silver doped CdO nanoparticles were improved by about three orders of magnitude than silver ions.

Production and characterization of hydrophobic zinc borate by using palm oil

NASA Astrophysics Data System (ADS)

Acarali, Nil Baran; Tugrul, Nurcan; Derun, Emek Moroydor; Piskin, Sabriye

2013-11-01

Zinc borate (ZB) was synthesized using zinc oxide, boric acid synthesized from colemanite, and reference ZB as seed. The effects of reaction parameters such as reaction time, reactant ratio, and seed ratio on its yield were examined. Then, the effects of palm oil with solvents (isopropyl alcohol (IPA), ethanol, and methanol) added to the reaction on its hydrophobicity were explored. Reactions were carried out under determined reaction conditions with magnetically and mechanically stirred systems. The produced ZB was characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), and measurements of contact angle identified hydrophobicity. The results showed that hydrophobic ZB was successfully produced under determined reaction conditions. The change of process parameters influenced its yield and the usage of palm oil provided hydrophobicity.

Hydroxyapatite nanocrystals: simple preparation, characterization and formation mechanism.

PubMed

Mohandes, Fatemeh; Salavati-Niasari, Masoud; Fathi, Mohammadhossein; Fereshteh, Zeinab

2014-12-01

Crystalline hydroxyapatite (HAP) nanoparticles and nanorods have been successfully synthesized via a simple precipitation method. To control the shape and particle size of HAP nanocrystals, coordination ligands derived from 2-hydroxy-1-naphthaldehyde were first prepared, characterized by Fourier transform infrared (FT-IR) and proton nuclear magnetic resonance ((1)H-NMR) spectroscopies, and finally applied in the synthesis process of HAP. On the other hand, the HAP nanocrystals were also characterized by several techniques including powder X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). According to the FE-SEM and TEM micrographs, it was found that the morphology and crystallinity of the HAP powders depended on the coordination mode of the ligands. Copyright © 2014 Elsevier B.V. All rights reserved.

Synthesis and characterization of ZnO incorporated magnetically recoverable KIT-6 as a novel and efficient catalyst in the preparation of symmetrical N, N‧-alkylidene bisamides

NASA Astrophysics Data System (ADS)

Saadati-Moshtaghin, Hamid Reza; Zonoz, Farrokhzad Mohammadi; Amini, Mostafa M.

2018-04-01

A novel magnetically recoverable nanocomposite consisting of the NiFe2O4 core and KIT-6 mesoporous silica shell incorporated with ZnO nanoparticles was constructed. This nanocomposite was characterized by Fourier transform infrared (FT-IR), powder X-ray diffraction (XRD), Brunauer Emmett Teller (BET), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) and vibrating sample magnetometry (VSM). This new nanocomposite demonstrated a catalytic performance in the synthesis of symmetrical N,N‧-alkylidene bisamides at the condensation reaction under solvent-free conditions. The nanocatalyst could simply be recovered from the reaction environment by using an exterior magnet and reused five times without a remarkable losing in the catalytic property.

Molecular structure, FT-IR, NBO, HOMO and LUMO, MEP and first order hyperpolarizability of (2E)-1-(2,4-Dichlorophenyl)-3-(3,4,5-trimethoxyphenyl)prop-2-en-1-one by HF and density functional methods.

PubMed

Sheena Mary, Y; Yohannan Panicker, C; Anto, P L; Sapnakumari, M; Narayana, B; Sarojini, B K

2015-01-25

(2E)-1-(2,4-Dichlorophenyl)-3-(3,4,5-trimethoxyphenyl)prop-2-en-1-one is synthesized by using 2,4-dichloroacetophenone and 3,4,5-trimethoxybenzaldehyde in ethanol. The structure of the compound was confirmed by IR and single crystal X-ray diffraction studies. FT-IR spectrum of (2E)-1-(2,4-dichloro-phenyl)-3-(3,4,5-trimethoxyphenyl)prop-2-en-1-one was recorded and analyzed. The crystal structure is also described. The vibrational wavenumbers were computed using HF and DFT methods and are assigned with the help of potential energy distribution method. The first hyperpolarizability and infrared intensities are also reported. The geometrical parameters of the title compound obtained from XRD studies are in agreement with the calculated (DFT) values. The stability of the molecule arising from hyper-conjugative interaction and charge delocalization has been analyzed using NBO analysis. The HOMO and LUMO analysis are used to determine the charge transfer within the molecule. MEP was performed by the DFT method. From the MEP map of the title molecule, negative region is mainly localized over the electronegative oxygen atoms, in the carbonyl group and the oxygen atom O4 of the methoxy group and the maximum positive region is localized on the phenyl rings. Copyright © 2014 Elsevier B.V. All rights reserved.

Synthesis, photoluminescence and Magnetic properties of iron oxide (α-Fe2O3) nanoparticles through precipitation or hydrothermal methods

NASA Astrophysics Data System (ADS)

Lassoued, Abdelmajid; Lassoued, Mohamed Saber; Dkhil, Brahim; Ammar, Salah; Gadri, Abdellatif

2018-07-01

In this work the iron oxide (α-Fe2O3) nanoparticles are synthesized using two different methods: precipitation and hydrothermal. Size, structural, optical and magnetic properties were determined and compared using X-ray diffraction (XRD), Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), Fourier Transform Infra-Red (FT-IR), Raman spectroscopy, Differential Thermal Analysis (DTA), Thermogravimetric Analysis (TGA), Ultraviolet-Visible (UV-Vis) analysis, Superconducting QUantum Interference Device (SQUID) magnetometer and Photoluminescence (PL). XRD data further revealed a rhombohedral (hexagonal) structure with the space group (R-3c) and showed an average size of 21 nm for hydrothermal samples and 33 nm for precipitation samples which concorded with TEM and SEM images. FT-IR confirms the phase purity of the nanoparticles synthesized. The Raman spectroscopy was used not only to prove that we have synthesized pure α-Fe2O3 but also to identify their phonon modes. The TGA showed three mass losses, whereas DTA resulted in three endothermic peaks. The decrease in the particle size of hematite of 33 nm for precipitation samples to 21 nm for hydrothermal samples is responsible for increasing the optical band gap of 1.94-2.10 eV where, the relation between them is inverse relationship. The products exhibited the attractive magnetic properties with good saturation magnetization, which were examined by a SQUID magnetometer. Photoluminescence measurements showed a strong emission band at 450 nm. Pure hematite prepared by hydrothermal method has smallest size, best crystallinity, highest band gap and best value of saturation magnetization compared to the hematite elaborated by the precipitation method.

Synthesis and structural characterization of magnetic cadmium sulfide-cobalt ferrite nanocomposite, and study of its activity for dyes degradation under ultrasound

NASA Astrophysics Data System (ADS)

Farhadi, Saeed; Siadatnasab, Firouzeh

2016-11-01

Cadmium sulfide-cobalt ferrite (CdS/CFO) nanocomposite was easily synthesized by one-step hydrothermal decomposition of cadmium diethyldithiocarbamate complex on the CoFe2O4 nanoparticles at 200 °C. Spectroscopic techniques of powder X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), UV-visible spectroscopy, field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDX), Brunauer-Emmett-Teller (BET), and magnetic measurements were applied for characterizing the structure and morphology of the product. The results of FT-IR, XRD and EDX indicated that the CdS/CFO was highly pure. SEM and TEM results revealed that the CdS/CFO nanocomposite was formed from nearly uniform and sphere-like nanoparticles with the size of approximately 20 nm. The UV-vis absorption spectrum of the CdS/CFO nanocomposite showed the band gap of 2.21 eV, which made it suitable for sono-/photo catalytic purposes. By using the obtained CdS/CFO nanocomposite, an ultrasound-assisted advanced oxidation process (AOP) has been developed for catalytic degradation of methylene blue (MB), Rhodamine B (RhB), and methyl orange (MO)) in the presence of H2O2 as a green oxidant. CdS/CFO nanocomposite exhibited excellent sonocatalytic activity, so that, dyes were completely degraded in less than 10 min. The influences of crucial factors such as the H2O2 amount and catalyst dosage on the degradation efficiency were evaluated. The as-prepared CdS/CFO nanocomposite exhibited higher catalytic activity than pure CdS nanoparticles. Moreover, the magnetic property of CoFe2O4 made the nanocomposite recyclable.

Solid state synthesis of starch-capped silver nanoparticles.

PubMed

Hebeish, A; Shaheen, Th I; El-Naggar, Mehrez E

2016-06-01

The present research addresses the establishment of a technique which is solely devoted to environmentally friendly one-pot green synthesis of dry highly stable powdered silver nanoparticles (AgNPs) using starch as both reductant and stabilizing agent in the presence of sodium hydroxide. It is believed that the sodium hydroxide can improve the reduction potential of starch. Thus when the alkali treated starch is submitted to addition of silver nitrate (AgNO3), the alkali treated starch induces the well-established dual role of starch; reduction of silver ions (Ag(+)) to AgNPs and capping the as-formed AgNPs to prevent them from further growth and agglomeration. Beside assessment of AgNPs formation, structural and morphological characteristics of AgNPs are investigated by making use of UV-vis spectroscopy, transmission electron microscopy (TEM), dynamic light scattering (DLS), zeta potential, FT-IR and X-ray diffraction (XRD) analysis. Research outputs signify (a) the absorbance around 410-420nm in the UV-vis spectra of AgNPs appears most, probably owing to the presence of nanosized silver particles and the intensity of this peak increases by increasing AgNO3 concentration; (b) that highly stable AgNPs with well-dispersed particle are successfully prepared using the present research-based innovation; (c) that the size of AgNPs does not exceed 30nm with sphere-like morphology even at the highest Ag(+) concentration employed during synthesis operation; (d) that the XRD and FT-IR confirm the successful preparation of pure AgNPs without noticeable impurities; (d) and that the one-pot synthesis of powdered AgNPs in large scale is clean and easily operated and easily transportation which may be applied as per demands of industries such as textile and painting industry. Copyright © 2016. Published by Elsevier B.V.

Fabrication and Characterization of Dense Zirconia and Zirconia-Silica Ceramic Nanofibers

PubMed Central

Guo, Guangqing; Fan, Yuwei

2011-01-01

The objective of this study was to prepare dense zirconia-yttria (ZY), zirconia-silica (ZS) and zirconia-yttria-silica (ZYS) nanofibers as reinforcing elements for dental composites. Zirconium (IV) propoxide, yttrium nitrate hexahydrate, and tetraethyl orthosilicate (TEOS) were used as precursors for the preparation of zirconia, yttria, and silica sols. A small amount (1–1.5 wt%) of polyethylene oxide (PEO) was used as a carry polymer. The sols were preheated at 70 °C before electrospinning and their viscosity was measured with a viscometer at different heating time. The gel point was determined by viscosity–time (η–t) curve. The ZY, ZS and ZYS gel nanofibers were prepared using a special reactive electrospinning device under the conditions near the gel point. The as-prepared gel nanofibers had diameters between 200 and 400 nm. Dense (nonporous) ceramic nanofibers of zirconia-yttria (96/4), zirconia-silica (80/20) and zirconia-yttria-silica (76.8/3.2/20) with diameter of 100–300 nm were obtained by subsequent calcinations at different temperatures. The gel and ceramic nanofibers obtained were characterized by scanning electron microscope (SEM), high-resolution field-emission scanning electron microscope (FE-SEM), thermogravimetric analyzer (TGA), differential scanning calorimeter (DSC), Fourier transform infrared spectrometer (FT-IR), and X-ray diffraction (XRD). SEM micrograph revealed that ceramic ZY nanofibers had grained structure, while ceramic ZS and ZYS nanofibers had smooth surfaces, both showing no visible porosity under FE-SEM. Complete removal of the polymer PEO was confirmed by TGA/DSC and FT-IR. The formation of tetragonal phase of zirconia and amorphous silica was proved by XRD. In conclusion, dense zirconia-based ceramic nanofibers can be fabricated using the new reactive sol–gel electrospinning technology with minimum organic polymer additives. PMID:21133090

Production of polyimide ceria nanocomposites by development of molecular hook technology in nano-sonochemistry.

PubMed

Hatami, Mehdi

2018-06-01

Poly(amic acid), the precursor of polyimide (PI), was used for the preparation of PI/CeO 2 nanocomposites (NC)s by ultrasonic assisted technique via insertion of the surface modified CeO 2 nanoparticles (NP)s into PI matrix. In the preparation stages, in the first, the modifications of CeO 2 NPs by using hexadecyltrimethoxysilane (HDTMS) as a binder were targeted using ultrasonic waves. In the second step, newly designed PI structure was formed from the sonochemical imidization process as a molecular hook. In this step two different reactions were occurred. The acetic acid elimination reaction in the main chain of macromolecule, and the acetylation reaction in the side chains of poly(amic acid) were accomplished. By acetylation process the hook structure was created for trapping of the modified nanoparticles. In the final step the preparation of PI NCs were achieved by sonochemical process. The structural and thermal properties of pure PI and PI/CeO 2 NCs were studied by several techniques such as fourier transform infrared spectroscopy (FT-IR), nuclear magnetic resonance spectroscopy (NMR), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), atomic force microscopy (AFM), X-ray diffraction (XRD), and thermal analyses. FT-IR and 1 H NMR spectra confirmed the success in preparation of PI matrix. The FE-SEM, TEM, and AFM analyses showed the uniform distribution of CeO 2 NPs in PI matrix. The XRD patterns of NCs show the presence of crystalline CeO 2 NPs in amorphous PI matrix. The thermal analysis results reveal that, with increases in the content of CeO 2 NPs in PI matrix, the thermally stability factors of samples were improved. Copyright © 2018 Elsevier B.V. All rights reserved.

Towards the development of a novel bioinspired functional material: synthesis and characterization of hybrid TiO2/DHICA-melanin nanoparticles.

PubMed

Pezzella, Alessandro; Capelli, Luigia; Costantini, Aniello; Luciani, Giuseppina; Tescione, Fabiana; Silvestri, Brigida; Vitiello, Giuseppe; Branda, Francesco

2013-01-01

A large number of recent literature data focus on modification/modulation of surface chemistry of inorganic materials in order to improve their functional properties. Melanins, a wide class of natural pigments, are recently emerging as a powerful organic component for developing bioinspired active material for a large number of applications from organoelectronics to bioactive compounds. Here we report the use of the approach referred as "chimie douce", involving in situ formation of the hybrids through reactions of precursors under mild conditions, to prepare novel hybrid functional architectures based on eumelanin like 5,6 dihydroxyindole-2-carboxylic acid (DHICA) polymer and TiO2. Two synthesis procedures were carried out to get DHICA-melanin coated TiO2 nanoparticles as well as mixed DHICA/TiO2 hybrid nanostructures. Such systems were characterized through EPR, FT-IR and fluorescence spectroscopy, thermogravimetric analysis (TGA), X-ray diffraction (XRD), and TEM microscopy in order to assess the effect of synthesis path as well as of DHICA content on structural, morphological and optical properties of TiO2 nanostructures. In particular, EPR, FT-IR spectra and TGA analysis confirmed the presence of DHICA-melanin in these samples. TEM measurements indicated the formation of the nanoparticles having relatively narrow size distribution with average particle size of about 10nm. DHICA-melanin does act as a morphological agent affecting morphology of hybrid nanostructures. XRD analysis proved that TiO2 hybrid nanoparticles kept anatase structures for DHICA-melanin contents within the range of investigated compositions, i.e. up to 50% wt/wt. Copyright © 2012 Elsevier B.V. All rights reserved.

Synthesis and characterization of silver doped hydroxyapatite nanocomposite coatings and evaluation of their antibacterial and corrosion resistance properties in simulated body fluid.

PubMed

Mirzaee, Majid; Vaezi, Mohammadreza; Palizdar, Yahya

2016-12-01

Silver-doped hydroxyapatite (Ca10-xAgx(PO4)6(OH)2-x) films were synthesized and deposited on anodized titanium (Ti) using electrophoretic. The influence of different silver-dopant contents (X=0, 0.02, 0.05, 0.08 and 0.1) on the phase formation and microstructure of the powders were characterized by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscope (XPS), and Fourier transform infrared spectrum analysis (FT-IR). XRD analysis confirmed the formation of Hexagonal structure of hydroxyapatite (HAp) annealed at 600°C with a small shift in the major peak position toward lower angles with adding silver. FT-IR spectroscopy disclosed the presence of the different vibrational modes matching to phosphates and hydroxyl groups and the absence of any band characteristics to silver. XPS analysis showed that 75% and 23% of silver was in the chemical states of Ag(2+) and Ag(+), respectively. However, only about 2% of silver was in the Ag(0) state, resulting in the high quality of nanocomposite films. The anodization treatment improves the bond strength between the Ag doped HAp deposited layers on TiO2. HAp and silver doped HAp (X=0.05) are regarded to be hydrophilic due to a large number of -OH groups on the surface. The sample with content of silver (x=0.05) also showed excellent antimicrobial efficacy (>99% reduction in viable cells). Electrochemical reveals the passive current densities of the HAp coated anodized Ti are lower than those of silver doped HAp coated anodized Ti, leading to a slightly lower corrosion resistance. Copyright © 2016 Elsevier B.V. All rights reserved.

Evaluation of structural and optical properties of Ce3+ ions doped (PVA/PVP) composite films for new organic semiconductors

NASA Astrophysics Data System (ADS)

Ali, F. M.; Kershi, R. M.; Sayed, M. A.; AbouDeif, Y. M.

2018-06-01

Polymer blend films based on Polyvinyl alcohol (PVA)/Poly(vinylpyrrolidone) (PVP) doped with different concentration of cerium ions [(PVA/PVP)-x wt.% Ce3+] (x = 3%, 5%, 10% and 15%) were prepared by the conventional solution casting technique. The characteristics of the prepared polymer composite films were studied using X-ray diffraction (XRD), FT-IR and UV-Vis. spectroscopy. The XRD patterns of the investigated samples revealed a clear reduction on the structural parameters such as crystallinity degree and cluster size D of the doped PVA/PVP blend films compared with the virgin one whereas there is no big difference in the d spacing of the product composite films. Significant changes in FT-IR spectra are observed which reveal an interactions between the cerium ions and PVA/PVP blends. The absorption spectra in the ultraviolet-visible region showed a wide red shift in the fundamental absorption edge of (PVA/PVP)-x wt. % Ce3+ composites. The optical gap Eg gradually decreased from 4.54 eV for the undoped PVA/PVP film to 3.10 eV by increasing Ce3+ ions content. The optical dispersion parameters have been analyzed according to Wemple-Didomenico single oscillator model. The dispersion energy Ed, the single oscillator energy Eo, the average inter-band oscillator wavelength λo and the static refractive index no are strongly affected by cerium ions doping. Cerium ions incorporation in PVA/PVP blend films leads to a significant increase in the refractive index and decrease in the optical gap. These results are likely of great important in varieties of applications including polymer waveguides, organic semiconductors, polymer solar cells and optoelectronics devices.

Control of the shape and size of iron oxide (α-Fe2O3) nanoparticles synthesized through the chemical precipitation method

NASA Astrophysics Data System (ADS)

Lassoued, Abdelmajid; Dkhil, Brahim; Gadri, Abdellatif; Ammar, Salah

Hematite (α-Fe2O3) nanoparticles were synthesized via a simple chemical precipitation method. The impact of varying the concentration of precursor on the crystalline phase, size and morphology of α-Fe2O3 products was explored. The characteristic of the synthesized hematite nanoparticles were evaluated by X-ray diffraction (XRD), Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), Fourier Transform Infra-Red (FT-IR) spectroscopy, Raman spectroscopy, Differential Thermal Analysis (DTA), Thermo Gravimetric Analysis (TGA), Ultraviolet-Visible (UV-Vis) analysis and Photoluminescence (PL). XRD data revealed a rhombohedral (hexagonal) structure with the space group R-3c in all samples. Uniform spherical like morphology was confirmed by TEM and SEM. The result revealed that the particle sizes were varied between 21 and 82 nm and that the increase in precursor concentration (FeCl3, 6H2O) is accompanied by an increase in the particle size of 21 nm for pure α-Fe2O3 synthesized with [Fe3+] = 0.05 M at 82 nm for pure α-Fe2O3 synthesized with [Fe3+] = 0.4 M. FT-IR confirms the phase purity of the nanoparticles synthesized. The Raman spectroscopy was used not only to prove that we have synthesized pure hematite but also to identify their phonon modes. The thermal behavior of compound was studied by using TGA/DTA results: The TGA showed three mass losses, whereas DTA resulted in three endothermic peaks. Besides, the optical investigation revealed that samples have an optical gap of about 2.1 eV and that this value varies as a function of the precursor concentration.

The use of novel biodegradable, optically active and nanostructured poly(amide-ester-imide) as a polymer matrix for preparation of modified ZnO based bionanocomposites

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

Abdolmaleki, Amir, E-mail: abdolmaleki@cc.iut.ac.ir; Nanotechnology and Advanced Materials Institute, Isfahan University of Technology, Isfahan 84156-83111, Islamic Republic of Iran; Mallakpour, Shadpour, E-mail: mallak@cc.iut.ac.ir

Highlights: Black-Right-Pointing-Pointer A novel biodegradable and nanostructured PAEI based on two amino acids, was synthesized. Black-Right-Pointing-Pointer ZnO nanoparticles were modified via two different silane coupling agents. Black-Right-Pointing-Pointer PAEI/modified ZnO BNCs were synthesized through ultrasound irradiation. Black-Right-Pointing-Pointer ZnO particles were dispersed homogeneously in PAEI matrix on nanoscale. Black-Right-Pointing-Pointer The effect of ZnO nanoparticles on the properties of synthesized polymer was examined. -- Abstract: A novel biodegradable and nanostructured poly(amide-ester-imide) (PAEI) based on two different amino acids, was synthesized via direct polycondensation of biodegradable N,N Prime -bis[2-(methyl-3-(4-hydroxyphenyl)propanoate)]isophthaldiamide and N,N Prime -(pyromellitoyl)-bis-L-phenylalanine diacid. The resulting polymer was characterized by FT-IR, {sup 1}H NMR,more » specific rotation, elemental analysis, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD) and field emission scanning electron microscopy (FE-SEM) analysis. The synthesized polymer showed good thermal stability with nano and sphere structure. Then PAEI/ZnO bionanocomposites (BNCs) were fabricated via interaction of pure PAEI and ZnO nanoparticles. The surface of ZnO was modified with two different silane coupling agents. PAEI/ZnO BNCs were studied and characterized by FT-IR, XRD, UV/vis, FE-SEM and TEM. The TEM and FE-SEM results indicated that the nanoparticles were dispersed homogeneously in PAEI matrix on nanoscale. Furthermore the effect of ZnO nanoparticle on the thermal stability of the polymer was investigated with TGA and DSC technique.« less

Sol-gel dip coating of yttria-stabilized tetragonal zirconia dental ceramic by aluminosilicate nanocomposite as a novel technique to improve the bonding of veneering porcelain.

PubMed

Madani, Azamsadat; Nakhaei, Mohammadreza; Karami, Parisa; Rajabzadeh, Ghadir; Salehi, Sahar; Bagheri, Hossein

2016-01-01

The aim of this in vitro study was to evaluate the effect of silica and aluminosilicate nanocomposite coating of zirconia-based dental ceramic by a sol-gel dip-coating technique on the bond strength of veneering porcelain to the yttria-stabilized tetragonal zirconia polycrystal (Y-TZP) in vitro. Thirty Y-TZP blocks (10 mm ×10 mm ×3 mm) were prepared and were assigned to four experimental groups (n=10/group): C, without any further surface treatment as the control group; S, sandblasted using 110 μm alumina powder; Si, silica sol dip coating + calcination; and Si/Al, aluminosilicate sol dip coating + calcination. After preparing Y-TZP samples, a 3 mm thick layer of the recommended porcelain was fired on the coated Y-TZP surface. Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive X-ray analysis were used to characterize the coating and the nature of the bonding between the coating and zirconia. To examine the zirconia-porcelain bond strength, a microtensile bond strength (μTBS) approach was chosen. FT-IR study showed the formation of silica and aluminosilicate materials. XRD pattern showed the formation of new phases consisting of Si, Al, and Zr in coated samples. SEM showed the formation of a uniform coating on Y-TZP samples. Maximum μTBS values were obtained in aluminosilicate samples, which were significantly increased compared to control and sandblasted groups (P=0.013 and P<0.001, respectively). This study showed that aluminosilicate sol-gel dip coating can be considered as a convenient, less expensive reliable method for improving the bond strength between dental Y-TZP ceramics and veneering porcelain.

Sol–gel dip coating of yttria-stabilized tetragonal zirconia dental ceramic by aluminosilicate nanocomposite as a novel technique to improve the bonding of veneering porcelain

PubMed Central

Madani, Azamsadat; Nakhaei, Mohammadreza; Karami, Parisa; Rajabzadeh, Ghadir; Salehi, Sahar; Bagheri, Hossein

2016-01-01

The aim of this in vitro study was to evaluate the effect of silica and aluminosilicate nanocomposite coating of zirconia-based dental ceramic by a sol–gel dip-coating technique on the bond strength of veneering porcelain to the yttria-stabilized tetragonal zirconia polycrystal (Y-TZP) in vitro. Thirty Y-TZP blocks (10 mm ×10 mm ×3 mm) were prepared and were assigned to four experimental groups (n=10/group): C, without any further surface treatment as the control group; S, sandblasted using 110 μm alumina powder; Si, silica sol dip coating + calcination; and Si/Al, aluminosilicate sol dip coating + calcination. After preparing Y-TZP samples, a 3 mm thick layer of the recommended porcelain was fired on the coated Y-TZP surface. Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive X-ray analysis were used to characterize the coating and the nature of the bonding between the coating and zirconia. To examine the zirconia–porcelain bond strength, a microtensile bond strength (μTBS) approach was chosen. FT-IR study showed the formation of silica and aluminosilicate materials. XRD pattern showed the formation of new phases consisting of Si, Al, and Zr in coated samples. SEM showed the formation of a uniform coating on Y-TZP samples. Maximum μTBS values were obtained in aluminosilicate samples, which were significantly increased compared to control and sandblasted groups (P=0.013 and P<0.001, respectively). This study showed that aluminosilicate sol–gel dip coating can be considered as a convenient, less expensive reliable method for improving the bond strength between dental Y-TZP ceramics and veneering porcelain. PMID:27478376

The role of extracellular DNA in uranium precipitation and biomineralisation.

PubMed

Hufton, Joseph; Harding, John H; Romero-González, Maria E

2016-10-26

Bacterial extra polymeric substances (EPS) have been associated with the extracellular precipitation of uranium. Here we report findings on the biomineralisation of uranium, with extracellular DNA (eDNA) used as a model biomolecule representative of EPS. The complexation and precipitation of eDNA with uranium were investigated as a function of pH, ionic strength and varying concentrations of reactants. The role of phosphate moieties in the biomineralisation mechanism was studied by enzymatically releasing phosphate (ePO 4 ) from eDNA compared to abiotic phosphate (aPO 4 ). The eDNA-uranium precipitates and uranium minerals obtained were characterised by Attenuated Total Reflectance-Fourier Transform Infrared (ATR-FT-IR) spectroscopy, Scanning Electron Microscopy-Energy Dispersive X-Ray analysis (SEM-EDX), X-Ray Powder Diffraction (XRD) and X-Ray Photoelectron Spectroscopy (XPS). ATR-FT-IR showed that at pH 5, the eDNA-uranium precipitation mechanism was predominantly mediated by interactions with phosphate moieties from eDNA. At pH 2, the uranium interactions with eDNA occur mainly through phosphate. The solubility equilibrium was dependent on pH with the formation of precipitate reduced as the pH increased. The XRD data confirmed the formation of a uranium phosphate precipitate when synthesised using ePO 4 . XPS and SEM-EDX studies showed the incorporation of carbon and nitrogen groups from the enzymatic orthophosphate hydrolysis on the obtained precipitated. These results suggested that the removal of uranium from solution occurs via two mechanisms: complexation by eDNA molecules and precipitation of a uranium phosphate mineral of the type (UO 2 HPO 4 )·xH 2 O by enzymatic orthophosphate hydrolysis. This demonstrated that eDNA from bacterial EPS is a key contributor to uranium biomineralisation.

Preparation and controlled release of mesoporous MCM-41/propranolol hydrochloride composite drug.

PubMed

Zhai, Qing-Zhou

2013-01-01

This article used MCM-41 as a carrier for the assembly of propranolol hydrochloride by the impregnation method. By means of chemical analysis, powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy and low-temperature N(2) adsorption-desorption at 77 K, the characterization was made for the prepared materials. The propranolol hydrochloride guest assembly capacity was 316.20 ± 0.31 mg/g (drug/MCM-41). Powder XRD test results indicated that during the process of incorporation, the frameworks of the MCM-41 were not destroyed and the crystalline degrees of the host-guest nanocomposite materials prepared still remained highly ordered. Characterization by SEM and TEM showed that the composite material presented spherical particle and the average particle size of composite material was 186 nm. FT-IR spectra showed that the MCM-41 framework existed well in the (MCM-41)-propranolol hydrochloride composite. Low-temperature nitrogen adsorption-desorption results at 77 K showed that the guest partially occupied the channels of the molecular sieves. Results of the release of the prepared composite drug in simulated body fluid indicated that the drug can release up to 32 h and its maximum released amount was 99.20 ± 0.11%. In the simulated gastric juice release pattern of drug, the maximum time for the drug release was discovered to be 6 h and the maximum cumulative released amount of propranolol hydrochloride was 45.13 ± 0.23%. The drug sustained-release time was 10 h in simulated intestinal fluid and the maximum cumulative released amount was 62.05 ± 0.13%. The prepared MCM-41 is a well-controlled drug delivery carrier.

Experimental and theoretical studies on the structure and spectroscopic properties of (E)-1-(2-aminophenyl)-3-(pyridine-4-yl) prop-2-en-1-one

NASA Astrophysics Data System (ADS)

Cruz Ortiz, Andrés Felipe; Sánchez López, Alberto; García Ríos, Alejandro; Cuenú Cabezas, Fernando; Rozo Correa, Ciro Eduardo

2015-10-01

(E)-1-(2-aminophenyl)-3-(pyridine-4-yl)prop-2-en-1-one (or simply 2-aminochalcone) was synthetized and characterized by elemental analysis, FT-IR, NMR, MS and XRD. Molecular geometry optimization, vibrational harmonic frequencies, 1H and 13C NMR chemical shifts were calculated by ab initio (HF and MP2) and density functional theory (DFT) methods, with B3LYP and B3PW91 functionals, using GAUSSIAN 09 program package without any constraint on the geometry. With VEDA software vibrational frequencies were assigned in terms of the potential energy distribution. A detailed interpretation of the FT-IR, NMR and XRD, experimental and calculated, is reported. The HOMO and LUMO energy gap that reflects the chemical activity of the molecule were also studied by DFT and above basis set. All theoretical results correspond to a great extent to experimental ones.

Synthesis, crystal structure, NLO and Hirshfeld surface analysis of 1,2,3-triazolyl chalcone single crystal

NASA Astrophysics Data System (ADS)

Shruthi, C.; Ravindrachary, V.; Guruswamy, B.; Lokanath, N. K.; Kumara, Karthik; Goveas, Janet

2018-05-01

Needle shaped brown coloured single crystal of the title compound was grown by slow evaporation technique using methanol as solvent. The grown crystal was characterized using FT-IR, Single crystal XRD, UV-visible and NLO studies. Crystal structure was confirmed by FT-IR study and the functional groups were identified. XRD study reveals that the crystal belongs to orthorhombic crystal system with pnaa space group and the corresponding cell parameters were calculated. UV-visible spectrum shows that the crystal is transparent in the entire visible region and absorption takes place in the UV-range. NLO efficiency of the crystal obtained 0.66 times that of urea was determined by SHG test. The intermolecular interaction and percentage contribution of each individual atom in the crystal lattice was quantized using Hirshfeld surface and 2D finger print analysis.

In search of the elusive IrB 2: Can mechanochemistry help?

DOE PAGES

Xie, Zhilin; Blair, Richard G.; Orlovskaya, Nina; ...

2015-10-20

We produced hexagonal ReB 2-type IrB 2 diboride and orthorhombic IrB monoboride phases, that were previously unknown and saw them produced by mechanochemical syntheses. High energy ball milling of elemental Ir and B powder for 30 h, followed by annealing of the powder at 1050 °C for 48 h, resulted in the formation of the desired phases. Both traditional laboratory and high resolution synchrotron X-ray diffraction (XRD) analyses were used for phase identification of the synthesized powder. Additionally, scanning electron microscopy and transmission electron microscopy were employed, along with XRD, to further characterize the microstructure of the phases produced.

In search of the elusive IrB 2: Can mechanochemistry help?

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

Xie, Zhilin; Blair, Richard G.; Orlovskaya, Nina

We produced hexagonal ReB 2-type IrB 2 diboride and orthorhombic IrB monoboride phases, that were previously unknown and saw them produced by mechanochemical syntheses. High energy ball milling of elemental Ir and B powder for 30 h, followed by annealing of the powder at 1050 °C for 48 h, resulted in the formation of the desired phases. Both traditional laboratory and high resolution synchrotron X-ray diffraction (XRD) analyses were used for phase identification of the synthesized powder. Additionally, scanning electron microscopy and transmission electron microscopy were employed, along with XRD, to further characterize the microstructure of the phases produced.

Spectroscopic investigation on the efficient organic nonlinear crystals of pure and diethanolamine added DAST.

PubMed

Karthikeyan, C; Haja Hameed, A S; Sagaya Agnes Nisha, J; Ravi, G

2013-11-01

4-N,N'-dimethylamino-N-methyl-4-stilbazolium toyslate (DAST) and diethanolamine (DEA) added DAST crystals are grown by slow cooling method. The corresponding powder samples are examined by characterization studies such as XRD, FT-IR, FT-Raman, UV-Vis-NIR and photoluminescence studies. From the powder X-ray diffraction, their lattice parameter values are found out. Since the vibrational spectra of the molecules are considerably contributed to their linear and nonlinear optical effects, Infrared and Raman spectroscopic studies are carried out for the samples. The UV-Vis-NIR absorption spectra of the samples are used to find the nature of transitions occurred in the samples. Using the density functional theory, highest occupied molecular orbital (HOMO) and lowest unoccupied molecular orbital (LUMO) analyses are done in order to explain the transition and density of states (DOS). The first order hyperpolarizability is calculated by HF and B3LYP/6-311 G(d,p) basis sets for the DAST molecule. From the photoluminescence (PL) spectral studies, the strong excitation emissions are observed. Copyright © 2013 Elsevier B.V. All rights reserved.

Synthesis of nanocrystalline Gd2Ti2O7 by combustion process and its structural, optical and dielectric properties

NASA Astrophysics Data System (ADS)

Jeyasingh, T.; Saji, S. K.; Wariar, P. R. S.

2017-07-01

Nanosized pyrochlore material Gadolinium Titanate (Gd2Ti2O7) powder was prepared by modified single step auto-ignition combustion process. The phase formation has been investigated using X-Ray diffraction analysis (XRD). The crystalline pyrochlore phase is further confirmed by the presence of metal-oxygen bonds in the FT-IR spectra. XRD analysis revealed that Gd2Ti2O7 has a cubic structure with Fd3m space group. The combustion powder was sintered to high density (97% of theoretical density) at ˜13000 C for 4h and the surface morphology was examined by Scanning Electron Microscopy (SEM). The optical band gap of Gd2Ti2O7 determined from the absorption spectrum is found to be 4.2 eV, which corresponds to direct allowed transitions. The dielectric measurements were carried out using LCR meter in the radio frequency region at room temperature. The sintered Gd2Ti2O7 has a dielectric constant (Ɛr) = 40 and dielectric loss (tan δ) = 0.01 at 1MHz.

Chitosan/graphene oxide biocomposite film from pencil rod

NASA Astrophysics Data System (ADS)

Gea, S.; Sari, J. N.; Bulan, R.; Piliang, A.; Amaturrahim, S. A.; Hutapea, Y. A.

2018-03-01

Graphene Oxide (GO) has been succesfully synthesized using Hummber method from graphite powder of pencil rod. The excellent solubility of graphene oxide (GO)in water imparts its feasibilty as new filler for reinforcement hydrophilic biopolymers. In this research, the biocomposite film was fabricated from chitosan/graphene oxide. The characteristics of graphene oxide were investigated using Fourier Transform Infrared (FT-IR) and X-ray Diffraction (XRD). The results of the XRD showed graphene structur in 2θ, appeared at 9.0715°with interlayer spacing was about 9.74063Å. Preparation films with several variations of chitosan/graphene oxide was done by casting method and characterized by mechanical and morphological analysis. The mechanical properties of the tensile test in the film show that the film CS/GO (85: 15)% has the optimum Young’s modulus size of 2.9 GPa compared to other variations of CS / GO film. Morphological analysis film CS/GO (85:15)% by Scanning Electron Microscopy (SEM), the obtained biocomposites film showed fine dispersion of GO in the CS matrix and could mix each other homogeneously.

Effect of L-Cysteine doping on growth and some characteristics of potassium dihydrogen phosphate single crystals

NASA Astrophysics Data System (ADS)

Mahadik, Ashwini; Soni, P. H.; Desai, C. F.

2017-12-01

Among quite a number of technologically important NLO materials, Potassium Dihydrogen Phosphate (KDP) is one of the most favourable ones for second harmonic generation applications, such as in electro-optic modulators, parametric oscillators and harmonic generators. The authors report here their studies on KDP crystals doped with L-Cysteine (1 mol% and 2 mol%). The dopant inclusion in the crystals was confirmed using Fourier transform infrared (FT-IR) spectroscopy and Powder X-Ray Diffraction (XRD). The XRD results also confirm the tetragonal structure with lattice parameters a = b = 7.45 Å and c = 6.98 Å. The presence of functional groups of crystals was analyzed using the FTIR spectra. For band gap evaluation, UV-Vis spectra were used and it was found to be 3.41 eV, 4.40eVand 4.50 eV, respectively in the cases of pure KDP, 1 mol% and 2 mol% L-Cysteine dopings. The spectra quality indicates good transparency of the doped crystals in the visible region, a feature quite desirable for applications in optoelectronics.

Mesoporous CdS via Network of Self-Assembled Nanocrystals: Synthesis, Characterization and Enhanced Photoconducting Property.

PubMed

Patra, Astam K; Banerjee, Biplab; Bhaumik, Asim

2018-01-01

Semiconduction nanoparticles are intensively studied due to their huge potential in optoelctronic applications. Here we report an efficient chemical route for hydrothermal synthesis of aggregated mesoporous cadmium sulfide (CdS) nanoparticles using supramolecular-assembly of ionic and water soluble sodium salicylate as the capping agent. The nanostructure, mesophase, optical property and photoconductivity of these mesoporous CdS materials have been characterized by using small and wide angle powder X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), N2-sorption, Raman analysis, Fourier transformed infrared (FT-IR), UV-Visible DSR spectroscopy, and photoconductivity measurement. Wide angle XRD pattern and high resolution TEM image analysis suggested that the particle size of the materials is within 10 nm and the nanoparticles are in well-crystallized cubic phase. Mesoporous CdS nanoparticles showed drastically enhanced photoelectrochemical response under visible light irradiation on entrapping a photosensitizer (dye) molecule in the interparticle spaces. Efficient synthesis strategy and the enhanced photo response in the mesoporous CdS material could facilitate the designing of other porous semiconductor oxide/sulfide and their applications in photon-to-electron conversion processes.

In-situ Polymerization of Polyaniline/Polypyrrole Copolymer using Different Techniques

NASA Astrophysics Data System (ADS)

Hammad, A. S.; Noby, H.; Elkady, M. F.; El-Shazly, A. H.

2018-01-01

The morphology and surface area of the poly(aniline-co-pyrrole) copolymer (PANPY) are important properties which improve the efficiency of the copolymer in various applications. In this investigation, different techniques were employed to produce PANPY in different morphologies. Aniline and pyrrole were used as monomers, and ammonium peroxydisulfate (APS) was used as an oxidizer with uniform molar ratio. Rapid mixing, drop-wise mixing, and supercritical carbon dioxide (ScCO2) polymerization techniques were appointed. The chemical structure, crystallinity, porosity, and morphology of the composite were distinguished by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), Brunauer, Emmett and Teller (BET) analysis, and transmission electron microscopy (TEM) respectively. The characterization tests indicated that the polyaniline/polypyrrole copolymer was successfully prepared with different morphologies. Based on the obtained TEM, hollow nanospheres were formed using rapid mixing technique with acetic acid that have a diameter of 75 nm and thickness 26 nm approximately. Also, according to the XRD, the produced structures have a semi- crystalline structure. The synthesized copolymer with ScCO2-assisted polymerization technique showed improved surface area (38.1 m2/g) with HCl as dopant.

UV-visible spectroscopic estimation of photodegradation of rhodamine-B dye using tin(IV) oxide nanoparticles.

PubMed

Sangami, G; Dharmaraj, N

2012-11-01

Nanocrystalline, tin(IV) oxide (SnO(2)) particles has been prepared by thermal decomposition of tin oxalate precursor obtained from the reactions of tin(IV) chloride and sodium oxalate using eggshell membrane (ESM). The as-prepared SnO(2) nanoparticles were characterized by thermal studies, transmission electron microscopy (TEM), powder X-ray diffraction (XRD), Raman, FT-IR and UV-visible studies and used as a photocatalyst for the degradation of rhodamine-B (Rh-B) dye. The size of the prepared nanoparticles was in the range of 5-12nm as identified from the TEM images. Powder XRD data revealed the presence of a tetragonal, rutile crystalline phase of the tin(IV) oxide nanoparticles. Thermal analysis showed that the decomposition of tin oxalate precursor to yield the titled tin(IV) oxide nanoparticles was completed below 500°C. The extent of degradation of Rh-B in the presence of SnO(2) monitored by absorption spectral measurements demonstrated that 94.48% of the selected dye was degraded upon irradiation with UV light for 60 min. Copyright © 2012 Elsevier B.V. All rights reserved.

Role of triton X-100 and hydrothermal treatment on the morphological features of nanoporous hydroxyapatite nanorods.

PubMed

Iyyappan, E; Wilson, P; Sheela, K; Ramya, R

2016-06-01

Hydroxyapatite (HA) particles were synthesized using Ca(NO3)2·4H2O and (NH4)2HPO4 as precursors with varying contents of non-ionic surfactant viz., triton X-100 (organic modifier) via co-precipitation method followed by hydrothermal treatment. The prepared HA particles have been characterized by X-ray diffraction (XRD), Fourier Transform Infrared spectroscopy (FT-IR), Energy Dispersive X-ray Analysis (EDX), High Resolution Scanning Electron Microscopy (HRSEM), High Resolution Transmission Electron Microscopy (HRTEM) and Nitrogen adsorption-desorption experiments. The XRD and FTIR studies indicate the formation of HA phase in all the synthesized samples. The specific roles of triton X-100 and hydrothermal treatment in dispersing and in directing the crystal growth respectively have been discussed by comparing the observations from individual experiments using triton X-100 and hydrothermal treatment with that of combined protocol involving both. The plausible mechanism for the individual roles of both triton X-100 and hydrothermal treatment have been proposed. Copyright © 2016 Elsevier B.V. All rights reserved.

Molten salt synthesis and luminescent properties of YVO4:Ln (Ln = Eu3+, Dy3+) nanophosphors.

PubMed

Liu, Chenglu; Wang, Fang; Jia, Peiyun; Lin, Jun; Zhou, Zhiqiang

2012-01-01

Eu3+ and Dy(3+)-doped YVO4 nanocrystallites were successfully prepared at 400 degrees C in equal moles of NaNO3 and KNO3 molten salts. X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, transmission electronic microscopy (TEM), photoluminescence (PL) spectrum and lifetime were used to characterize the nanocrystallites. XRD results demonstrate that NaOH concentration and annealing temperature play important roles in phase purity and crystallinity of the nanocrystallites, the optimum NaOH concentration and annealing temperature being 6:40 and 400 degrees C respectively. TEM micrographs show the nanocrystallites are well crystallized with a cubic morphology in an average grain size of about 18 nm. Upon excitation of the vanadate group at 314 nm, YVO4:Eu3+ and YVO4:Dy3+ nanocrystallites exhibit the characteristic emission of Eu3+ and Dy3+, which indicates that there is an energy transfer from the vanadate group to the rare earth ions. Moreover, the structure and luminescent properties of the nanocrystallites were compared with their bulk counterparts with same composition in detail.

Comparison of In Situ Polymerization and Solution-Dispersion Techniques in the Preparation of Polyimide/Montmorillonite (MMT) Nanocomposites

PubMed Central

Ahmad, Mansor Bin; Gharayebi, Yadollah; Salit, Mohd. Sapuan; Hussein, Mohd. Zobir; Shameli, Kamyar

2011-01-01

In this paper, Polyimide/Montmorillonite Nanocomposites (PI/MMT NCs), based on aromatic diamine (4-Aminophenyl sulfone) (APS) and aromatic dianhydride (3,3′,4,4′-benzophenonetetracarboxylic dianhydride) (BTDA) were prepared using in situ polymerization and solution-dispersion techniques. The prepared PI/MMT NCs films were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). The XRD results showed that at the content of 1.0 wt % Organo Montmorillonite (OMMT) for two techniques and 3.0 wt % OMMT for the in situ polymerization technique, the OMMT was well-intercalated, exfoliated and dispersed into polyimide matrix. The OMMT agglomerated when its amount exceeded 10 wt % and 3.0 wt % for solution-dispersion and in situ polymerization techniques respectively. These results were confirmed by the TEM images of the prepared PI/MMT NCs. The TGA thermograms indicated that thermal stability of prepared PI/MMT NCs were increased with the increase of loading that, the effect is higher for the samples prepared by in situ polymerization technique. PMID:22016643

Comparison of in situ polymerization and solution-dispersion techniques in the preparation of Polyimide/Montmorillonite (MMT) Nanocomposites.

PubMed

Ahmad, Mansor Bin; Gharayebi, Yadollah; Salit, Mohd Sapuan; Hussein, Mohd Zobir; Shameli, Kamyar

2011-01-01

In this paper, Polyimide/Montmorillonite Nanocomposites (PI/MMT NCs), based on aromatic diamine (4-Aminophenyl sulfone) (APS) and aromatic dianhydride (3,3',4,4'-benzophenonetetracarboxylic dianhydride) (BTDA) were prepared using in situ polymerization and solution-dispersion techniques. The prepared PI/MMT NCs films were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). The XRD results showed that at the content of 1.0 wt % Organo Montmorillonite (OMMT) for two techniques and 3.0 wt % OMMT for the in situ polymerization technique, the OMMT was well-intercalated, exfoliated and dispersed into polyimide matrix. The OMMT agglomerated when its amount exceeded 10 wt % and 3.0 wt % for solution-dispersion and in situ polymerization techniques respectively. These results were confirmed by the TEM images of the prepared PI/MMT NCs. The TGA thermograms indicated that thermal stability of prepared PI/MMT NCs were increased with the increase of loading that, the effect is higher for the samples prepared by in situ polymerization technique.

Influence of the synthesis parameters on the properties of amidoxime grafted sepiolite nanocomposites

NASA Astrophysics Data System (ADS)

Taimur, Shaista; Yasin, Tariq

2017-11-01

Novel polyacrylonitrile (PAN) grafted sepiolite nanocomposites were synthesized via emulsion polymerization. The influence of synthesis parameters on the degree of grafting was studied by varying the concentrations of monomer, initiator and surfactant. The nitrile groups of PAN were chemically modified into amidoxime. Both the grafting and amidoxime percentages were determined gravimetrically and maximum grafting of 373% was achieved at 5% acrylonitrile, 1% surfactant and 0.1% initiator concentrations. The presence of vibration at 2242 cm-1 in Fourier transform infrared (FT-IR) spectrum and x-ray diffraction (XRD) reflection at 2θ = 16.9° (010) confirmed the grafting of PAN chains onto modified sepiolite. XRD patterns also indicated a decrease in crystallinity of sepiolite and appearance of new amorphous region in grafted nanocomposites. The morphological changes of sepiolite during silanization and grafting of PAN is also confirmed by field emission scanning electron microscope (FESEM). Transmission electron microscope (TEM) images clearly showed the shortening of fibers after silanization of sepiolite and the same were involved in heterogeneous nucleation in micelles. These developed amidoxime grafted sepiolite nanocomposites can be used as adsorbent for the metal recovery.

Chemically functionalized ZnS quantum dots as new optical nanosensor of herbicides

NASA Astrophysics Data System (ADS)

Masteri-Farahani, M.; Mahdavi, S.; Khanmohammadi, H.

2018-03-01

Surface chemical functionalization of ZnS quantum dots (ZnS-QDs) with cysteamine hydrochloride resulted in the preparation of an optical nanosensor for detection of herbicides. Characterization of the functionalized ZnS-QDs was performed with physicochemical methods such as x-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy, energy dispersive x-ray (EDX) analysis, ultraviolet-visible (UV–vis) and photoluminescence (PL) spectroscopies. The optical band gap of the functionalized ZnS-QDs was determined by using Tauc plot as 4.1 eV. Addition of various herbicides resulted in the linearly fluorescence quenching of the functionalized ZnS-QDs according to the Stern-Volmer equation. The functionalized ZnS-QDs can be used as simple, rapid, and inexpensive nanosensor for practical detection and measurement of various herbicides.

Magnetic cellulose/Ag as a novel eco-friendly nanobiocomposite to catalyze synthesis of chromene-linked nicotinonitriles.

PubMed

Maleki, Ali; Movahed, Hamed; Ravaghi, Parisa

2017-01-20

In this work, design, preparation and performance of magnetic cellulose/Ag nanobiocomposite as a recyclable and highly efficient heterogeneous nanocatalyst is described. Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD) pattern, vibrating sample magnetometer (VSM) curve, field-emission scanning electron microscopy (FE-SEM) image, energy dispersive X-ray (EDX) analysis and thermogravimetric analysis/differential thermal analysis (TGA/DTA) were used for the characterization. Then, its activity was investigated in the synthesis of 2-amino-6-(2-oxo-2H-chromen-3-yl)-4-phenylnicotinonitrile derivatives. The main advantages of the reaction are high yields and short reaction times. The remarkable magnetic property of the nanobiocomposite catalyst provides easy separation from the reaction mixture by an external magnet without considerable loss of its catalytic activity. Copyright © 2016 Elsevier Ltd. All rights reserved.

Green synthesis and spectral characterization of silver nanoparticles from Lakshmi tulasi (Ocimum sanctum) leaf extract

NASA Astrophysics Data System (ADS)

Subba Rao, Y.; Kotakadi, Venkata S.; Prasad, T. N. V. K. V.; Reddy, A. V.; Sai Gopal, D. V. R.

2013-02-01

A simple method for the green synthesis of silver nanoparticles (AgNPs) using aqueous extract of Lakshmi tulasi (Ocimum sanctum) leaf as a reducing and stabilizing agent. AgNPs were rapidly synthesized using aqueous extract of tulasi leaf with AgNO3 solution within 15 min. The green synthesized AgNPs were characterized using physic-chemical techniques viz., UV-Vis, X-ray diffraction (XRD), scanning electron microscope (SEM) coupled with X-ray energy dispersive spectroscopy (EDX) and Fourier transform-infrared spectroscopy (FT-IR). Characterization data reveals that the particles were crystalline in nature and triangle shaped with an average size of 42 nm. The zeta potential of AgNPs were found to be -55.0 mV. This large negative zeta potential value indicates repulsion among AgNPs and their dispersion stability.

Green synthesis of silver nanoparticles using Alternanthera dentata leaf extract at room temperature and their antimicrobial activity

NASA Astrophysics Data System (ADS)

Kumar, Deenadayalan Ashok; Palanichamy, V.; Roopan, Selvaraj Mohana

2014-06-01

A green rapid biogenic synthesis of silver nanoparticles AgNPs using Alternanthera dentata (A. dentata) aqueous extract was demonstrated in this present study. The formation of silver nanoparticles was confirmed by Surface Plasmon Resonance (SPR) at 430 nm using UV-visible spectrophotometer. The reduction of silver ions to silver nanoparticles by A. dentata extract was completed within 10 min. Synthesized nanoparticles were characterized using UV-visible spectroscopy; Fourier transformed infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy and transmission electron microscopy (TEM). The extracellular silver nanoparticles synthesis by aqueous leaf extract demonstrates rapid, simple and inexpensive method comparable to chemical and microbial methods. The colloidal solution of silver nanoparticles were found to exhibit antibacterial activity against Escherichia coli, Pseudomonas aeruginosa, Klebsiella pneumonia and, Enterococcus faecalis.

Synthesis and characterization of nanocomposite polymer blend electrolyte thin films by spin-coating method

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

Chapi, Sharanappa; Niranjana, M.; Devendrappa, H., E-mail: dehu2010@gmail.com

2016-05-23

Solid Polymer blend electrolytes based on Polyethylene oxide (PEO) and poly vinyl pyrrolidone (PVP) complexed with zinc oxide nanoparticles (ZnO NPs; Synthesized by Co-precipitation method) thin films have prepared at a different weight percent using the spin-coating method. The complexation of the NPs with the polymer blend was confirmed by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR). The variation in film morphology was examined by polarized optical micrographs (POMs). The thermal behavior of blends was investigated under non-isothermal conditions by differential thermal analyses (DTA). A single glass transition temperature for each blend was observed, which supports the existence ofmore » compatibility of such system. The obtained results represent that the ternary based thin films are prominent materials for battery and optoelectronic device applications.« less

A simple and facile synthesis of MPA capped CdSe and CdSe/CdS core/shell nanoparticles

NASA Astrophysics Data System (ADS)

Sukanya, D.; Sagayaraj, P.

2015-06-01

II-VI semiconductor nanostructures, in particular, CdSe quantum dots have drawn a lot of attention because of their promising potential applications in biological tagging, photovoltaic, display devices etc. due to their excellent optical properties, high emission quantum yield, size dependent emission wavelength and high photostability. In this paper, we describe the synthesis and properties of mercaptopropionic acid capped CdSe and CdSe/CdS nanoparticles through a simple and efficient co-precipitation method followed by hydrothermal treatment. The growth process, characterization and the optical absorption as a function of wavelength for the synthesized MPA capped CdSe and CdSe/CdS nanoparticles have been determined using X-ray diffraction study (XRD), Ultraviolet-Visible spectroscopy (UV-Vis), Fourier transform infrared spectroscopy (FT-IR) and High Resolution Transmission Electron Microscopy (HRTEM).

Defect-Induced Luminescence of a Self-Activated Borophosphate Phosphor

NASA Astrophysics Data System (ADS)

Han, Bing; Liu, Beibei; Dai, Yazhou; Zhang, Jie

2018-05-01

A self-activated borophosphate phosphor Ba3BPO7 was prepared via typical solid-state reaction in thermal-carbon reduction atmosphere. The structural and luminescence properties were investigated using x-ray powder diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, and photoluminescence spectroscopy. Upon excitation with ultraviolet (UV) light, the as-prepared phosphor shows bright greenish-yellow emission with a microsecond-level fluorescence lifetime, which could result from the oxygen vacancies produced in the process of solid-state synthesis. The possible luminescence mechanism is proposed. Through the introduction of defects in the host, this work realizes visible luminescence in a pure borophosphate compound that does not contain any rare earth or transition metal activators, so it is helpful to develop defect-related luminescent materials in view of energy conservation and environmental protection for sustainable development.

Synthesis, physicochemical and optical properties of bis-thiosemicarbazone functionalized graphene oxide

NASA Astrophysics Data System (ADS)

Kumar, Santosh; Wani, Mohmmad Y.; Arranja, Claudia T.; Castro, Ricardo A. E.; Paixão, José A.; Sobral, Abilio J. F. N.

2018-01-01

Fluorescent materials are important for low-cost opto-electronic and biomedical sensor devices. In this study we present the synthesis and characterization of graphene modified with bis-thiosemicarbazone (BTS). This new material was characterized using Fourier transform infrared spectroscopy (FT-IR), Ultraviolet-visible (UV-Vis) and Raman spectroscopy techniques. Further evaluation by X-ray diffraction (XRD), thermo-gravimetric analysis (TGA), differential scanning calorimetry (DSC), scanning electron microscopy (SEM) and atomic-force microscopy (AFM) allowed us to fully characterize the morphology of the fabricated material. The average height of the BTSGO sheet is around 10 nm. Optical properties of BTSGO evaluated by photoluminescence (PL) spectroscopy showed red shift at different excitation wavelength compared to graphene oxide or bisthiosemicarbazide alone. These results strongly suggest that BTSGO material could find potential applications in graphene based optoelectronic devices.

Sonochemical fabrication of fluorinated mesoporous titanium dioxide microspheres

NASA Astrophysics Data System (ADS)

Yu, Changlin; Yu, Jimmy C.; Chan, Mui

2009-05-01

A sonochemical-hydrothermal method for preparing fluorinated mesoporous TiO 2 microspheres was developed. Formation of mesoporous TiO 2 and doping of fluorine was achieved by sonication and then hydrothermal treatment of a solution containing titanium isopropoxide, template, and sodium fluoride. The as-synthesized TiO 2 microspheres were characterized by X-ray diffraction (XRD), Fourier translation infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray (EDX) spectroscopy, photoluminescence spectroscopy (PL), and BET surface areas. The P123 template was removed completely during the hydrothermal and washing steps, which was different from the conventional calcination treatment. The as- synthesized TiO 2 microspheres had good crystallinity and high stability. Results from the photocatalytic degradation of methylene blue (MB) showed that fluorination could remarkably improve the photocatalytic activity of titanium dioxide.

Adsorption of dodecylamine hydrochloride on graphene oxide in water

NASA Astrophysics Data System (ADS)

Chen, Peng; Li, Hongqiang; Song, Shaoxian; Weng, Xiaoqing; He, Dongsheng; Zhao, Yunliang

Cationic surfactants in water are difficult to be degraded, leading to serious water pollution. In this work, graphene oxide (GO) was used as an adsorbent for removing Dodecylamine Hydrochloride (DACl), a representative cationic surfactant. X-ray diffraction (XRD), FT-IR spectroscopy and atomic force microscope (AFM) were used to characterize the prepared GO. The adsorption of DACl on GO have been investigated through measurements of adsorption capacity, zeta potential, FTIR, and X-ray photoelectron spectroscopy (XPS). The experimental results have shown that the adsorption kinetics could be described as a rate-limiting pseudo second-order process, and the adsorption isotherm agreed well with the Freundlich model. GO was a good adsorbent for DACl removal, compared with coal fly ash and powdered activated carbon. The adsorption process was endothermic, and could be attributed to electrostatic interaction and hydrogen bonding between DACl and GO.

Hybrid magnetic materials formed by ferritin intercalated into a layered double hydroxide

NASA Astrophysics Data System (ADS)

Clemente-León, Miguel; Coronado, Eugenio; Primo, Vicent; Ribera, Antonio; Soriano-Portillo, Alejandra

2008-12-01

A hybrid magnetic material formed by ferritin intercalated into a layered double hydroxide (LDH) of Mg and Al (Mg/Al molar ratio 2) is prepared and characterized through powder X-ray diffraction (XRD), thermogravimetric analysis (TGA), Fourier transform infrared (FT-IR) spectroscopy, electron probe microanalysis (EPMA) and high resolution transmission electron microscopy (HRTEM). One observes an enhancement in the thermal stability of the ferritin molecules when they are inserted in the layered material. Magnetic measurements of the hybrid material exhibit the typical superparamagnetic behaviour of the ferritin molecule. On the other hand, the intercalation of ferritin into the LDH guarantees a homogeneous dispersion of the ferritin molecules, which do not aggregate even after calcination of the sample. This feature allows obtaining well-dispersed magnetic metal oxide nanoparticles upon calcination of the hybrid material.

Elaboration of the hydroxyapatite with different precursors and application for the retention of the lead.

PubMed

Meski, S; Ziani, S; Khireddine, H; Yataghane, F; Ferguene, N

2011-01-01

Carbonate hydroxyapatite (CHAP) was synthesized from different precursors; synthetic (CaCO3 and Ca(OH)2) and natural (egg shell before and after calcinations at 900 degrees C) under different conditions and characterized by using TG/DTG analysis, X-ray powder diffraction (XRD) method and Fourier transform infrared (FT-IR) spectroscopy techniques. The results of these analyses indicate that the four powders present the same structure of hydroxyapatite. Furthermore the four powders obtained were used for the retention of lead. The results obtained indicated that all powders present high adsorption capacity for lead, but from environmental and economic views, the hydroxyapatite synthesized from eggshell no calcined (HA2) is most advantageous. The influence of different sorption parameters, such as: initial metal concentration, equilibration time, solution pH and sorbent dosage was studied and discussed.

Synthesis, characterization, biocompatibility of hydroxyapatite-natural polymers nanocomposites for dentistry applications.

PubMed

Chung, Jin-Hwan; Kim, Young Kyung; Kim, Kyo-Han; Kwon, Tae-Yub; Vaezmomeni, Seyede Ziba; Samiei, Mohammad; Aghazadeh, Marzyeh; Davaran, Soodabeh; Mahkam, Mehrdad; Asadi, Ghale; Akbarzadeh, Abolfazl

2016-01-01

Hydroxyapatite (HA), the main mineral component of bones and teeth, was synthesized by using the reaction between calcium nitrate tetrahydrate Ca(NO3)2∙4H2O and diammonium hydrogen phosphate (NH4)2HPO4 (DAHP) with a chemical precipitation method. The objective of this study is to utilize novel inorganic-organic nanocomposites for biomedical applications. HA is an inorganic component (75% w) and chitosan, alginate and albumin (Egg white) are organic components of nanocomposites (25% w). Nanocomposites were prepared in deionized water solutions, at room temperature, using a mechanical and magnetic stirrer for 48 h. The microstructure and morphology of sintered n-HAP were tested at different preheating temperature and laser sintering speed with scanning electron microscopy (SEM), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR).

Synthesis and characterization of polyethylene glycol mediated silver nanoparticles by the green method.

PubMed

Shameli, Kamyar; Ahmad, Mansor Bin; Jazayeri, Seyed Davoud; Sedaghat, Sajjad; Shabanzadeh, Parvaneh; Jahangirian, Hossein; Mahdavi, Mahnaz; Abdollahi, Yadollah

2012-01-01

The roles of green chemistry in nanotechnology and nanoscience fields are very significant in the synthesis of diverse nanomaterials. Herein, we report a green chemistry method for synthesized colloidal silver nanoparticles (Ag NPs) in polymeric media. The colloidal Ag NPs were synthesized in an aqueous solution using silver nitrate, polyethylene glycol (PEG), and β-D-glucose as a silver precursor, stabilizer, and reducing agent, respectively. The properties of synthesized colloidal Ag NPs were studied at different reaction times. The ultraviolet-visible spectra were in excellent agreement with the obtained nanostructure studies performed by transmission electron microscopy (TEM) and their size distributions. The Ag NPs were characterized by utilizing X-ray diffraction (XRD), zeta potential measurements and Fourier transform infrared (FT-IR). The use of green chemistry reagents, such as glucose, provides green and economic features to this work.

Surfaces wettability and morphology modulation in a fluorene derivative self-assembly system

NASA Astrophysics Data System (ADS)

Cao, Xinhua; Gao, Aiping; Zhao, Na; Yuan, Fangyuan; Liu, Chenxi; Li, Ruru

2016-04-01

A new organogelator based on fluorene derivative (gelator 1) was designed and synthesized. Organogels could be obtained via the self-assembly of the derivative in acetone, toluene, ethyl acetate, hexane, DMSO and petroleum ether. The self-assembly process was thoroughly characterized using field-emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), UV-vis, FT-IR and the contact angle. Surfaces with different morphologies and wetting properties were formed via the self-assembly of gelator 1 in the six different solvents. Interestingly, a superhydrophobic surface with a contact angle of 150° was obtained from organogel 1 in DMSO and exhibited the lotus-effect. The sliding angle necessary for a water droplet to move on the glass was only 15°. Hydrogen bonding and van der Waals forces were attributed as the main driving forces for gel formation.

Synthesis and characterization of a prominent NLO active MOF of lead with 1,5-naphthalenedisulfonic acid

NASA Astrophysics Data System (ADS)

Prasad, S. Shibu; Sudarsanakumar, M. R.; Dhanya, V. S.; Suma, S.; Kurup, M. R. Prathapachandra

2018-09-01

A new metal-organic framework of lead, [Pb(1,5-nds)(H2O)3]n (1,5-nds = 1,5-naphthalenedisulfonate) having prominent nonlinear optical property has been prepared by single gel diffusion technique at ambient condition using sodium metasilicate. The second harmonic generation efficiency was analyzed using Kurtz and Perry powder method and was found to be 30 times as large as potassium dihydrogen phosphate (KDP). Single crystal X-ray diffraction studies reveal the crystal structure. The grown crystals were further characterized by elemental analysis, powder XRD study, thermogravimetry, FT-IR and UV-visible spectral studies. The Pb2S2O4 rings in the crystal structure form a 1D channel. Hydrogen bonding and π-π interactions provide additional stability to the compound. Photoluminescence studies were also carried out.

Visible light driven photocatalytic degradation of methylene blue using novel camphor sulfonic acid doped polycarbazole/g-C3N4 nanocomposite

NASA Astrophysics Data System (ADS)

Praveena, P.; Dhanavel, S.; Sangamithirai, D.; Narayanan, V.; Stephen, A.

2018-04-01

A novel polycabazole(PCz)/graphitic carbon nitride(g-C3N4) nanocomposite was synthesized via chemical oxidative polymerization method. In the present work, camphor sulfonic acid (CSA) was used as a dopantand ammonium peroxydisulphate (APS) was used as an oxidizing agent. The PCz/g-C3N4 nanocompositewas characterizedusing X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and UV-Visible spectroscopy (UV-Vis). The obtained results confirm the successful formation of PCz/g-C3N4 nanocomposite. Visible light induced photocatalytic activity of the novel catalyst was demonstrated using methylene blue as a target pollutant. The results suggestthat PCz/g-C3N4 nanocomposite can be used as an effective catalyst for the degradation of organic pollutants from waste water.

Low frequency sonochemical synthesis of nanoporous amorphous manganese dioxide (MnO2) and adsorption of remazol reactive dye

NASA Astrophysics Data System (ADS)

Hasan, Siti Zubaidah; Yusop, Muhammad Rahimi; Othman, Mohamed Rozali

2015-09-01

Nanoporous amorphous-MnO2 was synthesized by sonochemical process (sonication) on the solid manganese (II) acetate tetrahydrate (Mn(CH3COO)2.4H2O) in 0.1 M KMnO4. The product was characterized by X-ray diffraction (XRD), morphology of the material was scanned by Field Emission Scanning Electron Microscopy (FE-SEM) and absorptions of MnO2 bonding was characterized by Fourier Transform Infra-Red Spectrometer (FT-IR). Remazol reactive dye or Red 3BS, was used in the adsorption study using nanoporous amorphous-MnO2. In batch experiment, 10 ppm of Remazol reactive dye was used and experiment was carried out at room temperature. Adsorption of Remazol dye on 0.2g synthesized nanoporous amorphous-MnO2 showed 99 - 100% decolorization.

New Poly(amide-imide)/Nanocomposites Reinforced Silicate Nanoparticles Based on N-pyromellitimido-L-phenyl Alanine Containing Ether Moieties

NASA Astrophysics Data System (ADS)

Faghihi, Khalil; Shabanian, Meisam; Dadfar, Ehsan

2012-02-01

A series of Poly(amide-imide)/montmorillonite nanocomposites containing N-pyromellitimido-L-phenyl alanine moiety in the main chain were synthesized by a convenient solution intercalation technique. Poly(amide-imide) (PAI) 5 as a source of polymer matrix was synthesized by the direct polycondensation reaction of N-pyromellitimido-L-phenyl alanine 3 with 4,4'-diamino diphenyl ether 4 in the presence of triphenyl phosphite (TPP), CaCl2, pyridine and N-methyl-2-pyrrolidone (NMP). The resulting nanocomposite films were characterized by Fourier transform infrared spectra (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM) and thermogravimetric analysis (TGA). The results showed that organo-modified clay was dispersed homogeneously in PAI matrix. TGA indicated an enhancement of thermal stability of new nanocomposites compared with the pure polymer.

Thermal and Optical Properties of New Poly(amide-imide)/Nanocomposite Reinforced by Layer Silicate Containing Diphenyl Ether Moieties

NASA Astrophysics Data System (ADS)

Faghihi, Khalil; Faramarzi, Ellahe; Shabanian, Meisam

2011-04-01

New poly(amide-imide)-montmorillonite reinforced nanocomposites containing Bis(4-N-trimellitylimido) diphenyl ether moiety in the main chain were synthesized by a convenient solution intercalation technique. Poly(amide-imide) (PAI) 4 was synthesized by the direct polycondensation reaction of Bis(4-N-trimellitylimido) diphenyl ether 3 with 4,4'-diamino diphenyl ether 2 in the presence of triphenyl phosphite (TPP), CaCl2, pyridine and N-methyl-2-pyrrolidone (NMP). Morphology and structure of the resulting PAI-nanocomposite films 4a and 4b with 10 and 20 mass% silicate particles respectively, were characterized by FT-IR spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM). The properties of nanocomposites films were investigated by using Uv-vis spectroscopy, thermogravimetric analysis (TGA) and water uptake measurements.

Studies on the chemical synthesis and characterization of lead oxide nanoparticles with different organic capping agents

NASA Astrophysics Data System (ADS)

Arulmozhi, K. T.; Mythili, N.

2013-12-01

Lead oxide (PbO) nanoparticles were chemically synthesized using Lead (II) acetate as precursor. The effects of organic capping agents such as Oleic acid, Ethylene Diamine Tetra Acetic acid (EDTA) and Cetryl Tri Methyl Butoxide (CTAB) on the size and morphology of the nanoparticles were studied. Characterization techniques such as X-ray diffraction (XRD), Fourier Transform-Infrared spectroscopy (FT-IR), Photoluminescence (PL) Field Emission Scanning Electron Microscopy (FE-SEM), Energy Dispersive Spectroscopy (EDS) and Transmission Electron Microscopy (TEM) were used to analyse the prepared nanoparticles for their physical, structural and optical properties. The characterization studies reveal that the synthesized PbO nanoparticles had well defined crystalline structure and sizes in the range of 25 nm to 36 nm for capping agents used and 40 nm for pure PbO nanoparticles.

Magnetic graphene oxide for adsorption of organic dyes from aqueous solution

NASA Astrophysics Data System (ADS)

Drashya, Lal, Shyam; Hooda, Sunita

2018-05-01

Graphene oxide (GO), a 2-D carbon nanomaterial, large surface area, oxygen-containing groups (like: hydroxyl, epoxy and carboxyl) and excellent water dispersibility due to it is good adsorbent dye removal from pollutant water1. But it's difficult to separate GO from water after adsorption. Therefore, Iron oxide was introduced in Graphene oxide by decorating method to make separation more efficient2. We present herein a one step process to prepare Magnetic Graphene oxide (MGO). The Fourier transform infrared spectrometer (FT-IR), X-ray diffraction (XRD) and Raman Spectroscopy characterized the chemical structure of the MGO composite. The adsorption of dyes onto MGO was studied in relation to initial concentration of Dyes, contact time, adsorbent dose, temperature and pH value of solution. We have studied adsorption capacity of different dyes (Methylene blue and crystal violet) by MGO.

Extraction and physicochemical characterization of chitin and chitosan from Zophobas morio larvae in varying sodium hydroxide concentration.

PubMed

Soon, Chu Yong; Tee, Yee Bond; Tan, Choon Hui; Rosnita, Abdul Talib; Khalina, Abdan

2018-03-01

Large amount of sodium hydroxide (NaOH) is consumed to remove the protein content in chitin biomass during deproteinization. However, excessive NaOH concentration used might lead to the reduction of cost effectiveness during chitin extraction. Hence, the present study aimed to extract and evaluate the physicochemical properties of chitin and chitosan isolated from superworm (Zophobas morio) larvae using 0.5M-2.0M of NaOH. The extracted chitin and chitosan were subjected to Fourier Transform Infrared Spectroscopy (FT-IR), elemental analysis, Scanning Electron Microscope (SEM), Thermogravimetric Analysis (TGA), Differential Scanning Calorimetry (DSC) and X-ray Diffraction (XRD). The 0.5M NaOH treatment resulted in the highest yield of chitin (5.43%), but produced the lowest yield (65.84%) of chitosan. The extracted chitin samples had relatively high degree of acetylation (DA) (82.39%-101.39%). Both chitin and chitosan showed smooth surface with tiny pores. The extracted chitin samples were confirmed as α-chitin based on the FT-IR and TGA. The chitin samples were amorphous with low degree of crystallinity. From TGA, the Chitosan 3 extracted was partially deacetylated. Both DPPH radical scavenging and ferric-chelating assay showed positive correlation with DD of chitosan isolates. However, the chitosan isolates were not fully dissolved, resulting in lower radical scavenging and ferric-chelating ability compared to commercial chitosan. Copyright © 2017. Published by Elsevier B.V.

Biocompatible interpolymer complex matrix tablets - an oral sustained release class-III antidiabetic drug

NASA Astrophysics Data System (ADS)

Ershadul Haque, S. K.; Sheela, A.

2017-11-01

Development of sustained release formulations of Metformin hydrochloride (Met) having low bioavailability and short half-life is one of the frontier areas of research towards achieving novel drug delivery systems. Towards the same, we have prepared interpolymer complexes (IPCs) of chitosan (CH) and two different viscosity grades of hydroxypropyl methylcellulose - HPMC (K4M and K100M) in various ratios, say, 4:6, 2:8, 1:9, respectively. The IPCs are characterized by Fourier transform infrared spectroscopy (FT-IR) and Thermo gravimetric analysis (TGA) techniques. Drug compatibility study is carried out by FT-IR and powder X-ray diffraction (XRD) techniques. The physical properties and drug content of formulated tablets are evaluated and found to be optimum. In addition, in vitro drug release kinetics is carried out at two different pH, say, 1.2 and 6.8. The release pattern from different polymeric matrices is shown in figure below: a) Chitosan, HPMC K4M and HPMC K100M b) IPCs of CH/HPMC K4M in [2:3, 1:4 and 1:9 ratios] c) IPCs of CH/HPMC K100M in [2:3, 1:4 and 1:9 ratios]. From the study, it has been observed that the drug release is sustained for a period of 12h in 1:9 ratio of CH: K100M IPC due to the formation of complex network matrix.

Immobilization of pectinase onto Fe3O4@SiO2-NH2 and its activity and stability.

PubMed

Fang, Gang; Chen, Honggao; Zhang, Yunpeng; Chen, Anqing

2016-07-01

Fe3O4 magnetic nanometer particles (MNPS) with a diameter of 30-40nm and coated by ammoniated silicon dioxides were developed by sol-gel method. The X-ray diffraction (XRD) pattern indicates that the Fe3O4 is wrapped in the amorphous SiO2, and the Fourier-transform infrared spectroscopy (FT-IR) analysis confirmed the NH2 group had been successfully introduced onto the surface of Fe3O4@SiO2 nanoparticles. The main factors related to the immobilization process of pectinase onto the magnetic support were optimized by multi-factor orthogonal experiments, and the recommended combination is that 3% glutaraldehyde (coupling agent), pH=8.0, 50°C, and cross-linking time 8h. Scanning electron microscope (SEM) and FT-IR analyses confirmed that the pectinase had been immobilized onto the surface of the amino modified nanoparticles. The storage stability and reusability of the pectinase were enhanced by the immobilization that 64.4% of the total starting activity was retrieved after 7 recycling batches and only about 21.1% of the total activity was lost after 30-day storage. For the application of the immobilized pectinase, the optimal pH and temperature were 8.5 and 55°C, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

Vibrational spectra, powder X-ray diffractions and physical properties of cyanide complexes with 1-ethylimidazole

NASA Astrophysics Data System (ADS)

Kürkçüoğlu, Güneş Süheyla; Kiraz, Fulya Çetinkaya; Sayın, Elvan

2015-10-01

The heteronuclear tetracyanonickelate(II) complexes of the type [M(etim)Ni(CN)4]n (hereafter, abbreviated as M-Ni-etim, M = Mn(II), Fe(II) or Co(II); etim = 1-ethylimidazole, C5H8N2) were prepared in powder form and characterized by FT-IR and Raman spectroscopy, powder X-ray diffraction (PXRD), thermal (TG; DTG and DTA), and elemental analysis techniques. The structures of these complexes were elucidated using vibrational spectra and powder X-ray diffraction patterns with the peak assignment to provide a better understanding of the structures. It is shown that the spectra are consistent with a proposed crystal structure for these compounds derived from powder X-ray diffraction measurements. Vibrational spectra of the complexes were presented and discussed with respect to the internal modes of both the etim and the cyanide ligands. The C, H and N analyses were carried out for all the complexes. Thermal behaviors of these complexes were followed using TG, DTG and DTA curves in the temperature range 30-700 °C in the static air atmosphere. The FT-IR, Raman spectra, thermal and powder X-ray analyses revealed no significant differences between the single crystal and powder forms. Additionally, electrical and magnetic properties of the complexes were investigated. The FT-IR and Raman spectroscopy, PXRD, thermal and elemental analyses results propose that these complexes are similar in structure to the Hofmann-type complexes.

Dissolution enhancement of tadalafil by liquisolid technique.

PubMed

Lu, Mei; Xing, Haonan; Yang, Tianzhi; Yu, Jiankun; Yang, Zhen; Sun, Yanping; Ding, Pingtian

2017-02-01

This study aimed to enhance the dissolution of tadalafil, a poorly water-soluble drug by applying liquisolid technique. The effects of two critical formulation variables, namely drug concentration (17.5% and 35%, w/w) and excipients ratio (10, 15 and 20) on dissolution rates were investigated. Pre-compression tests, including particle size distribution, flowability determination, Fourier transform infrared (FT-IR), differential scanning calorimetry (DSC), X-ray diffractometry (XRD) and scanning electron microscopy (SEM), were carried out to investigate the mechanism of dissolution enhancement. Tadalafil liquisolid tablets were prepared and their quality control tests, dissolution study, contact angle measurement, Raman mapping, and storage stability test were performed. The results suggested that all the liquisolid tablets exhibited significantly higher dissolution rates than the conventional tablets and pure tadalafil. FT-IR spectrum reflected no drug-excipient interactions. DSC and XRD studies indicated reduction in crystallinity of tadalafil, which was further confirmed by SEM and Raman mapping outcomes. The contact angle measurement demonstrated obvious increase in wetting property. Taken together, the reduction of particle size and crystallinity, and the improvement of wettability were the main mechanisms for the enhanced dissolution rate. No significant changes were observed in drug crystallinity and dissolution behavior after storage based on XRD, SEM and dissolution results.

Structural, magnetic and dielectric properties of polyaniline/MnCoFe2O4 nanocomposites

NASA Astrophysics Data System (ADS)

Chitra, Palanisamy; Muthusamy, Athianna; Jayaprakash, Rajan

2015-12-01

Ferromagnetic PANI containing MnCoFe2O4 nanocomposites were synthesized by in-situ chemical polymerization of aniline incorporated MnCoFe2O4 nanoparticles (20%, 10% w/w of fine powders) with and without ultrasonic treatment. The MnCoFe2O4 nanoparticles were synthesized by auto combustion method. The PANI/MnCoFe2O4 nanocomposites were characterized with Fourier transform infrared (FTIR), X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). The average particle size of the resulting PANI/MnCoFe2O4 nanocomposites was confirmed from the TEM and XRD analysis. The structure and morphology of the composites were confirmed by FT-IR spectroscopy, XRD and SEM. In addition, the electrical and magnetic properties of the nanocomposites were investigated. The PANI/MnCoFe2O4 nanocomposites under applied magnetic field exhibited the hysteresis loops of ferromagnetic nature at room temperature. The variation of Dielectric constant, Dielectric loss, and AC conductivity of PANI/MnCoFe2O4 nanocomposites at room temperature as a function of frequency in the range 50 Hz-5 MHz has been studied. Effect of ultrasonication on the PANI/MnCoFe2O4 nanocomposites was also investigated.

Effect of annealing temperature on optical properties of binary zinc tin oxide nano-composite prepared by sol-gel route using simple precursors: structural and optical studies by DRS, FT-IR, XRD, FESEM investigations.

PubMed

Habibi, Mohammad Hossein; Mardani, Maryam

2015-02-25

Binary zinc tin oxide nano-composite was synthesized by a facile sol-gel method using simple precursors from the solutions consisting of zinc acetate, tin(IV) chloride and ethanol. Effect of annealing temperature on optical and structural properties was investigated using X-ray diffraction (XRD), diffuse reflectance spectra (DRS), field emission scanning electron microscopy (FESEM) and Fourier transform infrared spectroscopy (FTIR). XRD results revealed the existence of the ZnO and SnO2 phases. FESEM results showed that binary zinc tin oxide nano-composites ranges from 56 to 60 nm in diameter at 400°C and 500°C annealing temperatures respectively. The optical band gap was increased from 2.72 eV to 3.11 eV with the increasing of the annealing temperature. FTIR results confirmed the presence of zinc oxide and tin oxide and the broad absorption peaks at 3426 and 1602 cm(-1) can be ascribed to the vibration of absorptive water, and the absorption peaks at 546, 1038 and 1410 cm(-1) are due to the vibration of Zn-O or Sn-O groups in binary zinc tin oxide. Copyright © 2014 Elsevier B.V. All rights reserved.

4-Methyl-1H-Indazole-5-Boronic acid: Crystal structure, vibrational spectra and DFT simulations

NASA Astrophysics Data System (ADS)

Dikmen, Gökhan

2017-12-01

Molecular structure, conformer forms, geometric parameters and vibrational assignments and properties of 4-Methyl-1H-Indazole-5-Boronic Acid (4M1HI5BA) were theoretically and experimentally studied using Raman, FT-IR, XRD spectroscopic methods and quantum chemical calculations. Raman and FT-IR spectra were examined range from 4000 to 400 cm-1. Moreover, single crystals of 4M1HI5BA were prepared in order to use in XRD experiments. Vibrational assignments were carried out using total energy distribution (TED) values. Furthermore, HOMO and LUMO were calculated for 4M1HI5BA. Four different conformations of 4M1HI5BA were calculated in only gas phase. The theoretical and experimental results show that in order to predict vibrational wavenumbers B3LYP/6-311++G(d,p) may provide acceptable results and the most stable conformer of 4M1HI5BA is predicted to be envelope conformer.

Photoluminescence studies on holmium (III) and praseodymium (III) doped calcium borophosphate (CBP) phosphors

NASA Astrophysics Data System (ADS)

Reddy Prasad, V.; Damodaraiah, S.; Devara, S. N.; Ratnakaram, Y. C.

2018-05-01

Using solid state reaction method, Ho3+ and Pr3+ doped calcium borophosphate (CBP) phosphors were prepared. These phosphors were characterized using XRD, SEM, FT-IR, 31P solid state NMR, photoluminescence (PL) and decay profiles. Structural details were discussed from XRD and FT-IR spectra. From 31P NMR spectra of these phosphors, mono-phosphate complexes Q0-(PO43-) were observed. Photoluminescence spectra were measured for both Ho3+ and Pr3+ doped calcium borophosphate phosphors and the spectra were studied for different concentrations. Decay curves were obtained for the excited level, 5F4+5S2 of Ho3+ and 1D2 level of Pr3+ in these calcium borophosphate phosphors and lifetimes were measured. CIE color chromaticity diagrams are drawn for these two rare earth ions in calcium borophosphate phosphors. Results show that Ho3+ and Pr3+ doped CBP phosphors might be served as green and red luminescence materials.

Spectroscopic studies on sidewall carboxylic acid functionalization of multi-walled carbon nanotubes with valine

NASA Astrophysics Data System (ADS)

Deborah, M.; Jawahar, A.; Mathavan, T.; Dhas, M. Kumara; Benial, A. Milton Franklin

2015-03-01

The valine functionalized multi-walled carbon nanotubes (MWCNTS) were prepared and characterized by using XRD, UV-Vis, FT-IR, EPR, SEM, and EDX, spectroscopic techniques. The enhanced XRD peak (0 0 2) intensity was observed for valine functionalized MWCNTs compared with oxidized MWCNTs, which is likely due to sample purification by acid washing. UV-Vis study shows the formation of valine functionalized MWCNTs. FT-IR study confirms the presence of functional groups of oxidized MWCNTs and valine functionalized MWCNTs. The ESR line shape analysis indicates that the observed EPR line shape is a Gaussian line shape. The g-values indicate that the systems are isotropic in nature. The morphology study was carried out for oxidized MWCNTs and valine functionalized MWCNTs by using SEM. The EDX spectra revealed that the high purity of oxidized MWCNTs and valine functionalized MWCNTs. The functionalization has been chosen because, functionalization of CNTs with amino acids makes them soluble and biocompatible. Thus, they have potential applications in the field of biosensors and targeted drug delivery.

Deposition of GdVO4:Eu3+ nanoparticles on silica nanospheres by a simple sol gel method

NASA Astrophysics Data System (ADS)

Liu, Guixia; Hong, Guangyan; Wang, Jinxian; Dong, Xiangting

2006-07-01

The deposition and coating of GdVO4:Eu3+ nanoparticles on spherical silica was carried out using a simple sol-gel method at low temperature. The GdVO4:Eu3+-coated silica composites obtained were characterized by differential thermal analysis (DTA), thermogravimetric (TG) analysis, x-ray diffraction (XRD), Fourier-transform IR spectroscopy (FT-IR), transmission electron microscopy (TEM), x-ray photoelectron spectroscopy (XPS), photoluminescence spectra, and kinetic decay. It is found that the ~5 nm GdVO4:Eu3+ nanoparticles coating the silica spheres are crystal in the as-prepared samples and the crystallinity increases with increasing annealing temperature. The composites obtained are spherical in shape with an average size of 100 nm. The GdVO4:Eu3+ nanoparticles are linked with silica cores by a chemical bond. The photoluminescence spectra of the obtained GdVO4:Eu3+-coated silica composites are similar to those of the bulk GdVO4:Eu3+ phosphors. The strongest peak is near 617 nm, which indicates that Eu3+ is located in the low symmetry site with non-inversion centre.

Surface segregation of additives on SnO 2 based powders and their relationship with macroscopic properties

NASA Astrophysics Data System (ADS)

Pereira, Gilberto J.; Castro, Ricardo H. R.; Hidalgo, Pilar; Gouvêa, Douglas

2002-07-01

Surface properties of ceramic powders frequently play an important role in producing high-quality, high-performance, and reliable ceramic products. These properties are related to the surface bond types and interactions with the surroundings. Oxide surfaces generally contain adsorbed hydroxyl groups and modifications in the chemical composition of the surface may be studied by infrared spectroscopy. In this work, we prepared SnO 2 containing Fe or Mg ions by organic chemical route derived from Pechini's method. The prepared powders were characterized by infrared spectroscopy (FT-IR), X-ray diffraction (XRD), dynamic electrophoretic mobility and surface area determination. Results demonstrated that the studied additives segregate onto the oxide surface and modify the hydroxyl IR bands of the adsorbed hydroxyl groups. These surface modifications change some macroscopic properties of the powder such as the isoelectric point (IEP) in aqueous suspensions and the final specific surface area. The increase of the surface area with additive concentration is supposedly due to the reduction of surface energy of the powders when additives segregate on the powder surface.

Spectroscopic characterization of zinc oxide nanorods synthesized by solid-state reaction

NASA Astrophysics Data System (ADS)

Prasad, Virendra; D'Souza, Charlene; Yadav, Deepti; Shaikh, A. J.; Vigneshwaran, Nadanathangam

2006-09-01

Well-crystallized zinc oxide nanorods have been fabricated by single step solid-state reaction using zinc acetate and sodium hydroxide, at room temperature. The sodium lauryl sulfate (SLS) stabilized zinc oxide nanorods were characterized by using X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy and photoluminescence spectroscopy. The X-ray diffraction revealed the wurtzite structure of zinc oxide. The size estimation by XRD and TEM confirmed that the ZnO nanorods are made of single crystals. The growth of zinc oxide crystals into rod shape was found to be closely related to its hexagonal nature. The mass ratio of SLS:ZnO in the nanorods was found to be 1:10 based on the thermogravimetric analysis. Blue shift of photoluminescence emission was noticed in the ZnO nanorods when compared to that of ZnO bulk. FT-IR analysis confirmed the binding of SLS with ZnO nanorods. Apart from ease of preparation, this method has the advantage of eco-friendliness since the solvent and other harmful chemicals were eliminated in the synthesis protocol.

Hydrothermal synthesis, crystal structures, and enantioselective adsorption property of bis(L-histidinato)nickel(II) monohydrate

NASA Astrophysics Data System (ADS)

Ramos, Christian Paul L.; Conato, Marlon T.

2018-05-01

Despite the numerous researches in metal-organic frameworks (MOFs), there are only few reports on biologically important amino acids, histidine in particular, on its use as bridging ligand in the construction of open-framework architectures. In this work, hydrothermal synthesis was used to prepare a compound based on Ni2+ and histidine. The coordination assembly of imidazole side chain of histidine with divalent nickel ions in aqueous condition yielded purple prismatic solids. Single crystal X-ray diffraction (XRD) analysis of the product revealed structure for Ni(C6H8N3O2)2 • H2O that has a monoclinic (C2) structure with lattice parameters, a = 29.41, b = 8.27, c = 6.31 Å, β = 90.01 ˚. Circular dichroism - optical rotatory dispersion (CD-ORD), Powder X-ray diffraction (PXRD) and Fourier transform - infrared spectroscopy (FT-IR) analyses are conducted to further characterize the crystals. Enantioselective adsorption analysis using racemic mixture of 2-butanol confirmed bis(L-histidinato)nickel(II) monohydrate MOF crystal's enantioselective property preferentially favoring the adsorption of (S)-2-butanol isomer.

Green synthesis of soya bean sprouts-mediated superparamagnetic Fe 3O 4 nanoparticles

NASA Astrophysics Data System (ADS)

Cai, Yan; Shen, Yuhua; Xie, Anjian; Li, Shikuo; Wang, Xiufang

2010-10-01

Superparamagnetic Fe 3O 4 nanoparticles were first synthesized via soya bean sprouts (SBS) templates under ambient temperature and normal atmosphere. The reaction process was simple, eco-friendly, and convenient to handle. The morphology and crystalline phase of the nanoparticles were determined from scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and X-ray diffraction (XRD) spectra. The effect of SBS template on the formation of Fe 3O 4 nanoparticles was investigated using X-ray photoemission spectroscopy (XPS) and Fourier-transform infrared spectroscopy (FT-IR). The results indicate that spherical Fe 3O 4 nanoparticles with an average diameter of 8 nm simultaneously formed on the epidermal surface and the interior stem wall of SBS. The SBS are responsible for size and morphology control during the whole formation of Fe 3O 4 nanoparticles. In addition, the superconducting quantum interference device (SQUID) results indicate the products are superparamagnetic at room temperature, with blocking temperature ( TB) of 150 K and saturation magnetization of 37.1 emu/g.

Synthesis and luminescence properties of cinnamide based nanohybrid materials containing Eu (II) ions

NASA Astrophysics Data System (ADS)

Kiran Kumar, A. B. V.; Jayasimhadri, M.; Cha, Hyeongrae; Chen, Kuangcai; Lim, Jae-Min; Lee, Yong-Ill

2011-07-01

In the present work, the cinnamide based organic-inorganic hybrid luminescent materials were prepared by using sol-gel technique, in which both the components are covalently linked via Si-C bonds. The organic precursor N-(3-(triethoxysilyl)propyl)cinnamide (Cn-Si) was synthesized by (3-aminopropyl) triethoxysilane being reacted with cinnamoyal chloride. Finally, novel hybrid materials were prepared successfully through hydrolysis and polycondensation processes between the alkoxide groups of precursors Cn-Si and tetraethylorthosilane (TEOS) in the presence of europium nitrate. We have characterized thoroughly the prepared samples using FT-IR, thermal analysis (TGA/DTA), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), energy-dispersive spectroscopy (EDS) and photoluminescence (PL) spectroscopy. The results indicate that these materials exhibit the excellent thermal stability up to 350 °C. The X-ray diffraction patterns confirmed the amorphous nature of the developed materials. The rare-earth doped hybrid materials have exhibited an intense green emission at 530 nm with CIE chromaticity coordinates (0.4801, 0.4669). Whereas, the un-doped one gives some remarkable blue emission properties under UV excitation.

Synthesis and structural characterization of CdS nanoparticles

NASA Astrophysics Data System (ADS)

Kotkata, M. F.; Masoud, A. E.; Mohamed, M. B.; Mahmoud, E. A.

2009-08-01

Amorphous CdS nanoparticles capped with cetyltrimethyl ammonium bromide (CTAB) were synthesised under various conditions using a coprecipitation method. A blue shift in the band gap was observed in the UV-visible absorption spectra indicating the formation of nanoparticles of an approximate size of 8 nm. The recorded transmission electron micrographs confirmed this result. The phase-nature, phase transformation as well as the structure of the synthesised CdS nanoparticles have been extensively characterized using X-ray diffraction (XRD), radial distribution function (RDF), differential scanning calorimetry (DSC), Fourier transform infrared (FT-IR), Raman scattering (RS) and/or heat stage X-ray diffraction (HSXRD). Analysis of the obtained results revealed that the synthesised amorphous CdS nanoparticles could be transformed into CdS nanocrystals having a zinc blende or a wurtzite structure, relying on the applied heat treatment scheme. The rate of nanocrystal growth depends on the aging period, prior filtering the reacted materials, and its relation to the quality of the capping process. Five days aging period tends to enhance the stability of the grown phase with a remarkable surface stability.

Novel preparation of highly photocatalytically active copper chromite nanostructured material via a simple hydrothermal route

PubMed Central

Beshkar, Farshad; Zinatloo-Ajabshir, Sahar; Bagheri, Samira; Salavati-Niasari, Masoud

2017-01-01

Highly photocatalytically active copper chromite nanostructured material were prepared via a novel simple hydrothermal reaction between [Cu(en)2(H2O)2]Cl2 and [Cr(en)3]Cl3.3H2O at low temperature, without adding any pH regulator or external capping agent. The as-synthesized nanostructured copper chromite was analyzed by transmission electron microscopy (TEM), UV–vis diffuse reflectance spectroscopy, energy dispersive X-ray microanalysis (EDX), scanning electron microscopy (SEM), X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy. Results of the morphological investigation of the as-synthesized products illustrate that the shape and size of the copper chromite depended on the surfactant sort, reaction duration and temperature. Moreover, the photocatalytic behavior of as-obtained copper chromite was evaluated by photodegradation of acid blue 92 (anionic dye) as water pollutant. PMID:28582420

Polyaniline nanofiber/large mesoporous carbon composites as electrode materials for supercapacitors

NASA Astrophysics Data System (ADS)

Liu, Huan; Xu, Bin; Jia, Mengqiu; Zhang, Mei; Cao, Bin; Zhao, Xiaonan; Wang, Yu

2015-03-01

A composite of polyaniline nanofiber/large mesoporous carbon (PANI-F/LMC) hybrid was prepared by an in situ chemical oxidative polymerization of aniline monomer with nano-CaCO3 templated LMC as host matrix for supercapacitors. The morphology, composition and electronic structure of the composites (PANI-F/LMC) together with pure PANI nanofibers and the LMC were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), FT-IR, X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). It is found that the PANI nanofibers were incorporated into the large mesochannels of LMC with interpenetrating framework formed. Such unique structure endows the PANI-F/LMC composite with a high capacitance of 473 F g-1 at a current load of 0.1 A g-1 with good rate performance and cycling stability, suggesting its potential application in the electrode material for supercapacitors.

Rapid and solvent-free solid-state synthesis and characterization of Zn3V2O8 nanostructures and their phenol red aqueous solution photodegradation

NASA Astrophysics Data System (ADS)

Mazloom, Fatemeh; Masjedi-Arani, Maryam; Salavati-Niasari, Masoud

2017-08-01

Zinc vanadate (Zn3V2O8) nanostructures have been successfully synthesized via simple, rapid and solvent-free solid-state method by using different complex precursors of Zn and NH4VO3 as novel starting materials. Effects of various zinc (II) Schiff base complex precursors and calcination temperatures were investigated to reach optimum condition. It was found that particle size and optical property of the as-prepared products could be greatly influenced via these parameters. The products were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectra, energy dispersive X-ray microanalysis (EDX), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Photoluminescence and ultraviolet-visible (UV-Vis) spectroscopy. The photocatalytic activity of zinc vanadate nano and bulk structures were compared by degradation of phenol red aqueous solution.

Polyethyleneimine-modified superparamagnetic Fe3O4 nanoparticles: An efficient, reusable and water tolerance nanocatalyst

NASA Astrophysics Data System (ADS)

Khoobi, Mehdi; Delshad, Tayebeh Modiri; Vosooghi, Mohsen; Alipour, Masoumeh; Hamadi, Hosein; Alipour, Eskandar; Hamedani, Majid Pirali; Sadat ebrahimi, Seyed Esmaeil; Safaei, Zahra; Foroumadi, Alireza; Shafiee, Abbas

2015-02-01

A novel magnetically separable catalyst was prepared based on surface modification of Fe3O4 magnetic nanoparticle (MNPs) with polyethyleneimine (PEI) via covalent bonding. [3-(2,3-Epoxypropoxy)propyl]trimethoxysilane (EPO) was used as cross linker to bond PEI on the surface of MNPs with permanent stability in contrast to PEI coating via electrostatic interactions. The synthesized catalyst was characterized by Fourier transform infrared (FT-IR), thermogravimetric analysis (TGA), X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and vibrating sample magnetometry (VSM). The catalyst show high efficiency for one-pot synthesis of 2-amino-3-cyano-4H-pyran derivatives via multi-component reaction (MCR). This procedure offers the advantages of green reaction media, high yield, short reaction time, easy purification of the products and simple recovery and reuse of the catalyst by simple magnetic decantation without significant loss of catalytic activity.

Sonochemically synthesized MnO2 nanoparticles as electrode material for supercapacitors.

PubMed

Gnana Sundara Raj, Balasubramaniam; Asiri, Abdullah M; Qusti, Abdullah H; Wu, Jerry J; Anandan, Sambandam

2014-11-01

In this study, manganese oxide (MnO2) nanoparticles were synthesized by sonochemical reduction of KMnO4 using polyethylene glycol (PEG) as a reducing agent as well as structure directing agent under room temperature in short duration of time and characterized by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Scanning electron microscope (SEM), Transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET) analysis. A supercapacitor device constructed using the ultrasonically-synthesized MnO2 nanoparticles showed maximum specific capacitance (SC) of 282Fg(-1) in the presence of 1M Ca(NO3)2 as an electrolyte at a current density of 0.5mAcm(-2) in the potential range from 0.0 to 1.0V and about 78% of specific capacitance was retained even after 1000 cycles indicating its high electrochemical stability. Copyright © 2013 Elsevier B.V. All rights reserved.

The fabrication of visible light responsive Ag-SiO2 co-doped TiO2 thin films by the sol-gel method

NASA Astrophysics Data System (ADS)

Dam Le, Duy; Dung Dang, Thi My; Thang Chau, Vinh; Chien Dang, Mau

2010-03-01

In this study we have successfully deposited Ag-SiO2 co-doped TiO2 thin films on glass substrates by the sol-gel method. After being coated by a dip coating method, the film was transparent, smooth and had strong adhesion on the glass surface. The deposited film was characterized by x-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), ultraviolet-visible spectroscopy (UV-Vis), a scanning electron microscope (SEM) and atomic force microscope (AFM) to investigate its crystallization, transmittance and surface structure. The antifogging ability is explained by the contact angle of water on the surface of the glass substrates under visible-light. The obtained results show that Ag-SiO2 co-doped TiO2 film has potential applications for self cleaning and anti-bacterial ceramic tiles.

A nanocomplex of Cu(II) with theophylline drug; synthesis, characterization, and anticancer activity against K562 cell line

NASA Astrophysics Data System (ADS)

Sahlabadi, Maryam; Daryanavard, Marzieh; Hadadzadeh, Hassan; Amirghofran, Zahra

2018-03-01

A new mononuclear of copper (II), [Cu(theophylline)2(H2O)3]·2H2O, has been synthesized by reaction of theophylline (1,3-dimethyl-7H-purine-2,6-dione) with copper (II) nitrate in water. Further, its nanocomplex has been prepared through the three different methods including sonication, grinding, and a combination thereof, sonication-grinding. The prepared nanocomplex was characterized using different techniques including FT-IR, UV-Vis, X-ray diffraction (XRD) analysis, and field-emission scanning electron microscopy (FE-SEM). Moreover, the anticancer activity of the precursor complex, nanocomplex, free theophylline ligand, and the starting copper salt (Cu(NO3)2·3H2O) was investigated against the K562 cell line. The results show that the nanocomplex is an effective nano metal-based anticancer agent with IC50 = 11.7 μM.

Characterization of konjac glucomannan-gelatin IPN physical hydrogel scaffold

NASA Astrophysics Data System (ADS)

Chen, Xiliang; Chen, Qinghua; Yan, Tingting; Liu, Jinkun

2017-06-01

A novel IPN hydrogel scaffold is prepared by freeze-drying method, in which konjac galactomannan (KGM) and gelatin are physically crosslinked respectively. This scaffold is thermostable, and the structure of this scaffold is analysed by scanning electron microscope, Fourier transform infrared spectrum, and X-ray diffraction method. The FT-IR results show that hydrogen bonds are formed between KGM and gelatin molecules, which hinder the formation of their respective crosslinking. This is consistent with the XRD results that the crystallinity gets lower in the IPN gels compared with pure gelatin and KGM gels. The morphologies of freeze-dried hydrogels are observed by SEM and the mechanical properties of the scaffolds are tested to analyse the relationship between the structures and properties. Although this novel IPN hydrogel is physical gel, it shows rubber-like performance as chemical gels. And it is nontoxic, so it can be used as the scaffold for cartilage tissue engineering that embedded in human bodies.

Anchoring of Cu(II) onto surface of porous metal-organic framework through post-synthesis modification for the synthesis of benzimidazoles and benzothiazoles

NASA Astrophysics Data System (ADS)

Kardanpour, Reihaneh; Tangestaninejad, Shahram; Mirkhani, Valiollah; Moghadam, Majid; Mohammadpoor-Baltork, Iraj; Zadehahmadi, Farnaz

2016-03-01

Efficient synthesis of various benzimidazoles and benzothiazoles under mild conditions catalyzed by Cu(II) anchored onto UiO-66-NH2 metal organic framework is reported. In this manner, first, the aminated UiO-66 was modified with thiophene-2-carbaldehyde and then the prepared Schiff base was reacted with CuCl2. The prepared catalyst was characterized by FT-IR, UV-vis, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), N2 adsorption, inductively coupled plasma atomic emission spectroscopy (ICP-AES) and field emission scanning electron microscopy (FE-SEM). The UiO-66-NH2-TC-Cu was applied as a highly efficient catalyst for synthesis of benzimidazole and benzothiazole derivatives by the reaction of aldehydes with 1,2-diaminobenzene or 2-aminothiophenol. The Cu(II)-containing MOF was reused several times without any appreciable loss of its efficiency.

Bioactivity of gelatin coated magnetic iron oxide nanoparticles: in vitro evaluation.

PubMed

Gaihre, Babita; Khil, Myung Seob; Kang, Hyo Kyoung; Kim, Hak Yong

2009-02-01

Current research explores formation of bone like apatite on gelatin coated magnetic iron oxide nanoparticles (GIOPs) to evaluate the bioactivity of the material. The GIOPs were soaked in simulated body fluid (SBF) and the apatite formation on the surface was investigated in regular interval of time. Fourier transform-infrared (FT-IR) and x-ray diffraction spectroscopic (XRD) analyses were done to investigate the chemical changes and field emission-scanning electron microscopic (FE-SEM) analysis was done to investigate the morphological changes occurring on the surface of the GIOPs after soaking in different time intervals. The kinetic studies of the apatite growth in SBF suggest that initially calcium and phosphorous ions were deposited to the surface of the GIOPs from the SBF leading to formation of amorphous Ca/P particles. Later, after 9 days of the incubation the amorphous particles were fused to form needle and blade like crystalline structures of bone like apatite.

Synthesis, characterization and catalytic activity of silver nanoparticles using Tribulus terrestris leaf extract.

PubMed

Ashokkumar, S; Ravi, S; Kathiravan, V; Velmurugan, S

2014-01-01

Biomediated silver nanoparticles were synthesized with the aid of an eco-friendly biomaterial, namely, aqueous Tribulus terrestris extract. Silver nanoparticles were synthesized using a rapid, single step, and completely green biosynthetic method employing aqueous T. terrestris leaf extracts as both the reducing and capping agent. Silver ions were rapidly reduced by aqueous T. terrestris leaf extracts, leading to the formation of highly crystalline silver nanoparticles. An attempt has been made and formation of the silver nanoparticles was verified by surface plasmon spectra using an UV-vis (Ultra violet), spectrophotometer. Morphology and crystalline structure of the prepared silver nanoparticles were characterized by TEM (Transmission Electron Microscope) and XRD (X-ray Diffraction), techniques, respectively. FT-IR (Fourier Transform Infrared), analysis suggests that the obtained silver nanoparticles might be stabilized through the interactions of carboxylic groups, carbonyl groups and the flavonoids present in the T. terrestris extract. Copyright © 2013 Elsevier B.V. All rights reserved.

PET-modified red mud as catalysts for oxidative desulfurization reactions.

PubMed

do Prado, Nayara T; Heitmann, Ana P; Mansur, Herman S; Mansur, Alexandra A; Oliveira, Luiz C A; de Castro, Cinthia S

2017-07-01

This work describes the synthesis of catalysts based on red mud/polyethylene terephthalate (PET) composites and their subsequent heat treatment under N 2 atmosphere. The materials were characterized by scanning electron microscopy (SEM), temperature programmed reduction (TPR), Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), thermogravimetric (TG) analysis and N 2 adsorption/desorption. The catalysts were evaluated in the oxidative desulfurization reaction of dibenzothiophene (DBT) in a biphasic system. The results indicated that the PET impregnation on red mud increased the affinity of the catalyst with the nonpolar phase (fuel), in which the contaminant was dissolved, allowing a higher conversion (up to 80%) and selectivity to the corresponding dibenzothiophene sulfone. The sulfone compound is more polar than DBT and diffused into the polar solvent as indicated by the data obtained via gas chromatography-mass spectrometry (GC-MS). Copyright © 2017. Published by Elsevier B.V.

Green synthesis of silver nanoparticles using Alternanthera dentata leaf extract at room temperature and their antimicrobial activity.

PubMed

Kumar, Deenadayalan Ashok; Palanichamy, V; Roopan, Selvaraj Mohana

2014-06-05

A green rapid biogenic synthesis of silver nanoparticles AgNPs using Alternanthera dentata (A. dentata) aqueous extract was demonstrated in this present study. The formation of silver nanoparticles was confirmed by Surface Plasmon Resonance (SPR) at 430nm using UV-visible spectrophotometer. The reduction of silver ions to silver nanoparticles by A. dentata extract was completed within 10min. Synthesized nanoparticles were characterized using UV-visible spectroscopy; Fourier transformed infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy and transmission electron microscopy (TEM). The extracellular silver nanoparticles synthesis by aqueous leaf extract demonstrates rapid, simple and inexpensive method comparable to chemical and microbial methods. The colloidal solution of silver nanoparticles were found to exhibit antibacterial activity against Escherichia coli, Pseudomonas aeruginosa, Klebsiella pneumonia and, Enterococcus faecalis. Copyright © 2014 Elsevier B.V. All rights reserved.

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

Li, Dongdong, E-mail: lidongchem@sina.cn; Zhu, Yuntao; Liang, Zhiqiang

Highlights: ► The synthesized mesoporous hydroxyapatite has nanostructure and bioactivity. ► The materials have high surface area and amino group. ► The materials show higher drug loading and slower release rate than pure HAP. - Abstract: Mesoporous nanosized hydroxyapatite (HAP) functionalized by alendronate (ALN) was synthesized using cationic surfactant CTAB as template. The structural, morphological and textural properties were fully characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and N{sub 2} adsorption/desorption. Then the obtained materials were performed as drug delivery carriers using ibuprofen (IBU) as a model drug to investigate their drug storage/releasemore » properties in simulated body fluid (SBF). The materials showed relatively slower release rate compared with HAP due to the ionic interaction between -NH{sub 3}{sup +} on the matrix and -COO{sup −}belongs to IBU. The system provides a new concept for improving the drug loading or slowing down the release rate.« less

Low frequency sonochemical synthesis of nanoporous amorphous manganese dioxide (MnO{sub 2}) and adsorption of remazol reactive dye

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

Hasan, Siti Zubaidah; Yusop, Muhammad Rahimi; Othman, Mohamed Rozali, E-mail: rozali@ukm.edu.my

2015-09-25

Nanoporous amorphous-MnO{sub 2} was synthesized by sonochemical process (sonication) on the solid manganese (II) acetate tetrahydrate (Mn(CH{sub 3}COO){sub 2}.4H{sub 2}O) in 0.1 M KMnO{sub 4}. The product was characterized by X-ray diffraction (XRD), morphology of the material was scanned by Field Emission Scanning Electron Microscopy (FE-SEM) and absorptions of MnO{sub 2} bonding was characterized by Fourier Transform Infra-Red Spectrometer (FT-IR). Remazol reactive dye or Red 3BS, was used in the adsorption study using nanoporous amorphous-MnO{sub 2}. In batch experiment, 10 ppm of Remazol reactive dye was used and experiment was carried out at room temperature. Adsorption of Remazol dye onmore » 0.2g synthesized nanoporous amorphous-MnO{sub 2} showed 99 – 100% decolorization.« less

Fast Extraction and Detection of 4-Methylimidazole in Soy Sauce Using Magnetic Molecularly Imprinted Polymer by HPLC.

PubMed

Feng, Zufei; Lu, Yan; Zhao, Yingjuan; Ye, Helin

2017-11-02

On the basis of magnetic molecularly imprinted polymer (MMIP) solid-phase extraction coupled with high performance liquid chromatography, we established a new method for the determination of the 4-methylimidazole (4-MEI) in soy sauce. Scanning electron microscopy (SEM), Fourier transform infrared (FT-IR), X-ray diffraction (XRD) and vibrating sample magnetometer (VSM) were used to characterize the synthesized MMIPs. To evaluate the polymers, batch rebinding experiments were carried out. The binding strength and capacity were determined from the derived Freundlich isotherm (FI) equation. The selective recognition capability of MMIPs was investigated with a reference compound and a structurally similar compound. As a selective pre-concentration sorbents for 4-methylimidazole in soy sauce, the MMIPs showed a satisfied recoveries rate of spiked samples, ranged from 97% to 105%. As a result, the prepared MMIPs could be applied to selectively pre-concentrate and determine 4-methylimidazole in soy sauce samples.

Rapid detection of HSO4- in water: Novel immobilized azo-azomethine colorimetric anion receptors on solid supports

NASA Astrophysics Data System (ADS)

Hezaveh, Saba Mahdavi; Khanmohammadi, Hamid; Zendehdel, Mojgan

2018-06-01

The immobilized azo-azomethine receptors on amorphous SiO2, S-B, SiO2 nanoparticles, S-NPs, and NaY zeolite, S-ZY, have been prepared and applied as solid phase sensors for detection of HSO4-, over other interfering anions, in 100% aqueous media. Remarkably, S-B and S-ZY show unique and rapid sensitivity towards HSO4-, which could it easily visualized through naked eye detection even at 5 × 10-4 mol L-1 and 4 × 10-4 mol L-1, respectively. The fabricated solid phase sensors were characterized using powder XRD diffraction, TGA-DTA, FE-SEM and also FT-IR techniques. Moreover, the related molecular anion receptor, HL, has been prepared and used for naked eye detection of F- and AcO-, in dry DMSO. The anions recognition ability of HL was also evaluated using UV-Vis and 1H NMR spectroscopic methods.

Sulfonated reduced graphene oxide as a highly efficient catalyst for direct amidation of carboxylic acids with amines using ultrasonic irradiation.

PubMed

Mirza-Aghayan, Maryam; Tavana, Mahdieh Molaee; Boukherroub, Rabah

2016-03-01

Sulfonated reduced graphene oxide nanosheets (rGO-SO3H) were prepared by grafting sulfonic acid-containing aryl radicals onto chemically reduced graphene oxide (rGO) under sonochemical conditions. rGO-SO3H catalyst was characterized by Fourier-transform infrared (FT-IR) spectroscopy, Raman spectroscopy, scanning electron microscopy (SEM), X-ray diffraction (XRD), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and X-ray photoelectron spectroscopy (XPS). rGO-SO3H catalyst was successfully applied as a reusable solid acid catalyst for the direct amidation of carboxylic acids with amines into the corresponding amides under ultrasonic irradiation. The direct sonochemical amidation of carboxylic acid takes place under mild conditions affording in good to high yields (56-95%) the corresponding amides in short reaction times. Copyright © 2015 Elsevier B.V. All rights reserved.

Cellulose synthesized by Enterobacter sp. FY-07 under aerobic and anaerobic conditions.

PubMed

Ma, Ting; Ji, Kaihua; Wang, Wei; Wang, Jinghong; Li, Zhaoyu; Ran, Haitao; Liu, Bin; Li, Guoqiang

2012-12-01

Enterobacter sp. FY-07 can produce bacterial cellulose (BC) under aerobic and anaerobic conditions. In static cultivation at 30 °C for 72 h under anoxic, oxygen-limited and aerated conditions, cellulose production exceeded 5 g/l, which indicated that oxygen was not essential for production of BC by Enterobacter sp. FY-07. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM) analysis showed that the microstructure of the BC was similar to that produced by aerobic bacteria such as Gluconacetobacter xylinum BCRC12335 and Acetobacter sp. V6. The crystallinity index of the BC was 63.3%. Water-holding capacity (approximately 11000%) and rehydration ratio (24.4%) were superior to those reported for BC produced by the aerobic bacteria G. xylinum BCRC12335 and Acetobacter sp. V6. These results will facilitate static submerged fermentation for the production of BC. Copyright © 2012 Elsevier Ltd. All rights reserved.

Synthesis of modified sepiolite-g-polystyrene sulfonic acid nanohybrids by radiation induced graft polymerization

NASA Astrophysics Data System (ADS)

Taimur, Shaista; Hassan, Muhammad Inaam ul; Yasin, Tariq; Ali, Syed Wasim

2018-07-01

In this study, polystyrene (PS) grafted sepiolite nanohybrid (MS-g-PS) was synthesized by using simultaneous radiation grafting technique in the presence of dichloromethane (DCM) as solvent. The radiation grafting process was carried out under inert atmosphere at room temperature using gamma rays from a Co-60 irradiator. The degree of grafting was affected by absorbed dose and monomer concentration in the mixture. Sulfonation of synthesized nanohybrid was carried out with sulfuric acid. Both the grafting of styrene and its sulfonate derivative were verified by Fourier transform infrared spectroscopy (FT-IR). The structural and morphological investigations of these nanohybrids have been investigated by X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM). The gravimetric investigations showed that grafting yield increases with the absorbed dose. Results showed that the system allows the controlled grafting of styrene onto sepiolite (Sep) in DCM.

Novel preparation and characterization of human hair-based nanofibers using electrospinning process.

PubMed

Park, Mira; Shin, Hye Kyoung; Panthi, Gopal; Rabbani, Mohammad Mahbub; Alam, Al-Mahmnur; Choi, Jawun; Chung, Hea-Jong; Hong, Seong-Tshool; Kim, Hak-Yong

2015-05-01

Human hair-based biocomposite nanofibers (NFs) have been fabricated by an electrospinning technique. Aqueous keratin extracted from human hair was successfully blended with poly(vinyl alcohol) (PVA). The focus here is on transforming into keratin/PVA nanofibrous membranes and insoluble property of electrospun NFs. The resulting hair-based NFs were characterized using Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM), X-ray diffraction (XRD), differential scanning colorimetry (DSC), and thermogravimetric analysis (TGA). Toward the potential use of these NFs after cross-linking with various weight fractions of glyoxal, its physicochemical properties, such as morphology, mechanical strength, crystallinity, and chemical structure were investigated. Keratin/PVA ratio of 2/1 NFs with 6 wt%-glyoxal showed good uniformity in fiber morphology and suitable mechanical properties, and excellent antibacterial activity providing a potential application of hair-based NFs in biomedical field. Copyright © 2015 Elsevier B.V. All rights reserved.

Preparation and characterization of graphene/CdS nanocomposites

NASA Astrophysics Data System (ADS)

Wu, Jili; Bai, Song; Shen, Xiaoping; Jiang, Lei

2010-11-01

Graphene-based nanocomposites are emerging as a new class of materials that hold promise for many applications. In this paper, we present a facile approach for the preparation of graphene/CdS nanocomposites through simple reflux processes, in which thiourea (CS(NH 2) 2) and thioacetamide (C 2H 5NS) act as a sulphide source, respectively. The samples were characterized by the X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectrum (FT-IR), ultraviolet-visible (UV-vis) spectroscopy and thermogravimetry analysis. It was shown that in the nanocomposites, the CdS nanoparticles were densely and uniformly deposited on the graphene sheets, and the sulphide source used has a great influence on the morphology, structure and property of the graphene/CdS nanocomposites. The good distribution of CdS nanoparticles on graphene sheets guarantees the efficient optoelectronic properties of graphene/CdS and would be promising for practical applications in future nanotechnology.

Characterization nano crystalline cellulose from sugarcane baggase for reinforcement in polymer composites: Effect of formic acid concentrations

NASA Astrophysics Data System (ADS)

Aprilia, N. A. S.; Mulyati, S.; Alam, P. N.; Karmila; Ambarita, A. C.

2018-04-01

Nanocellulose from sugarcane bagasse for reinforcement in polymer composites has isolated from formic acid (FA) with different concentration. This research was conducted with three level concentration of FA ei. 15, 30 and 50%. The nanocellulose were successfully prepared with variations of total yields of 66.66, 67.33 and 69.33% respectively with increase of FA concentrations at 6 hours of hidrolysis time. The obtained nanocellulose were characterized by fourier transform infrared (FT-IR) spectroscopy confirmed the introduction of carboxyl goups on the surface of cellulose. The X-ray diffraction (XRD) spectra proved the existence of cellulose, with a highly crystalline of 62.466, 71.033, and 76.296% with increase of FA concentrations. The size of crystallinity of nanocellulose were decreased with increased of FA concentration. The result investigated that size of crystallinity of nano cellulose reduced from 4.37, 4.15 and 3.94 nm.

Sodium alginate/graphene oxide composite films with enhanced thermal and mechanical properties.

PubMed

Ionita, Mariana; Pandele, Madalina Andreea; Iovu, Horia

2013-04-15

Sodium alginate/graphene oxide (Al/GO) nanocomposite films with different loading levels of graphene oxide were prepared by casting from a suspension of the two components. The structure, morphologies and properties of Al/GO films were characterized by Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), scanning (SEM) and transmission electron microscopy (TEM), thermal gravimetric (TG) analysis, and tensile tests. The results revealed that hydrogen bonding and high interfacial adhesion between GO filler and Al matrix significantly changed thermal stability and mechanical properties of the nanocomposite films. The tensile strength (σ) and Young's modulus (E) of Al films containing 6 wt% GO increased from 71 MPa and 0.85 GPa to 113 MPa and 4.18 GPa, respectively. In addition, TG analysis showed that the thermal stability of Al/GO composite films was better than that of neat Al film. Copyright © 2013 Elsevier Ltd. All rights reserved.

All-photonic drying and sintering process via flash white light combined with deep-UV and near-infrared irradiation for highly conductive copper nano-ink

PubMed Central

Hwang, Hyun-Jun; Oh, Kyung-Hwan; Kim, Hak-Sung

2016-01-01

We developed an ultra-high speed photonic sintering method involving flash white light (FWL) combined with near infrared (NIR) and deep UV light irradiation to produce highly conductive copper nano-ink film. Flash white light irradiation energy and the power of NIR/deep UV were optimized to obtain high conductivity Cu films. Several microscopic and spectroscopic characterization techniques such as scanning electron microscopy (SEM), a x-ray diffraction (XRD), and Fourier-transform infrared (FT-IR) spectroscopy were employed to characterize the Cu nano-films. Optimally sintered Cu nano-ink films produced using a deep UV-assisted flash white light sintering technique had the lowest resistivity (7.62 μΩ·cm), which was only 4.5-fold higher than that of bulk Cu film (1.68 μΩ•cm). PMID:26806215

Amine-functionalized magnetic mesoporous silica nanoparticles for DNA separation

NASA Astrophysics Data System (ADS)

Sheng, Wei; Wei, Wei; Li, Junjian; Qi, Xiaoliang; Zuo, Gancheng; Chen, Qi; Pan, Xihao; Dong, Wei

2016-11-01

We report a modified approach for the functionalized magnetic mesoporous silica nanoparticles (MMSN) using polymer microspheres incorporated with magnetic nanoparticles in the presence of cetyltrimethylammonium bromide (CTAB) and the core-shell magnetic silica nanoparticles (MSN). These particles were functionalized with amino groups via the addition of aminosilane directly to the particle sol. We then evaluate their DNA separation abilities and find the capacity of DNA binding significantly increased (210.22 μg/mg) compared with normal magnetic silica spheres (138.44 μg/mg) by using an ultraviolet and visible spectrophotometer (UV). The morphologies, magnetic properties, particle size, pore size, core-shell structure and Zeta potential are characterized by Fourier transform infrared spectroscopy (FT-IR), vibrating sample magnetometer (VSM), Transmission electron microscopy (TEM), Powder X-ray diffraction (XRD), and dynamic light scattering (DLS). This work demonstrates that our MMSN own an excellent potential application in bioseparation and drug delivery.

Synthesis of nanosize MCM-41 loaded with TiO 2 and study of its photocatalytic activity

NASA Astrophysics Data System (ADS)

Sadjadi, M. S.; Farhadyar, N.; Zare, K.

2009-07-01

In recent years, nanosized mesoporous materials have received significant attention due to their impact in different processes. Several diverse applications of these materials, e.g. high density magnetic recording, magnetic fluids, magnetic refrigeration as well as in photocatalysis, solar cells, photosensors, have triggered considerable research activities in the area of nanotechnology. In this work, nanosize MCM-41 was synthesized and loaded then with TiO 2 using tetra butoxy titanium (TBT). As prepared TiO 2 loaded materials was investigated by using X-ray diffraction (XRD), Transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR). The photocatalytic activity of the prepared TiO 2 loaded MCM-41 was finally evaluated by the degradation of methyl orange under irradiation of UV light. The result showed that TiO 2 loaded on nanosize MCM-41 has higher photocatalytic activity than that of TiO 2.

Efficient alkene epoxidation catalyzed by molybdenyl acetylacetonate supported on aminated UiO-66 metal-organic framework

NASA Astrophysics Data System (ADS)

Kardanpour, Reihaneh; Tangestaninejad, Shahram; Mirkhani, Valiollah; Moghadam, Majid; Mohammadpoor-Baltork, Iraj; Zadehahmadi, Farnaz

2015-03-01

Metal-organic frameworks (MOFs) containing Mo Schiff base complexes were prepared by post-synthesis method and applied as efficient catalysts in the epoxidation of alkenes with tert-BuOOH. In this manner, UiO-66-NH2 (UiO=University of Oslo) MOF was reacted with salicylaldehyde and thiophene-2-carbaldehyde to produce bidentate Schiff bases. Then, the Schiff base ligands were used for immobilization of molybdenyl acetylacetonate. These new catalysts were characterized by FT-IR, UV-vis spectroscopic techniques, X-ray diffraction (XRD), BET, inductively coupled plasma atomic emission spectroscopy (ICP-AES) and field emission scanning electron microscopy (FE-SEM). These catalytic systems showed excellent activity in the epoxidation of alkenes such as cyclic and linear ones with tert-butyl hydroperoxide (TBHP) in 1,2-dichloroethane, and reused several times without any appreciable loss of their activity.

Biodiesel production from palm oil using calcined waste animal bone as catalyst.

PubMed

Obadiah, Asir; Swaroopa, Gnanadurai Ajji; Kumar, Samuel Vasanth; Jeganathan, Kenthorai Raman; Ramasubbu, Alagunambi

2012-07-01

Waste animal bones was employed as a cost effective catalyst for the transesterification of palm oil. The catalyst was calcined at different temperatures to transform the calcium phosphate in the bones to hydroxyapatite and 800 °C was found to give the best yield of biodiesel. The catalyst was characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), energy dispersive spectrometry (EDS) and Fourier transform infrared spectrometry (FT-IR). Under the optimal reaction conditions of 20 wt.% of catalyst, 1:18 oil to methanol molar ratio, 200 rpm of stirring of reactants and at a temperature of 65 °C, the methyl ester conversion was 96.78% and it was achieved in 4h. The catalyst performed equally well as the laboratory-grade CaO. Animal bone is therefore a useful raw material for the production of a cheap catalyst for transesterification. Copyright © 2012 Elsevier Ltd. All rights reserved.

All-photonic drying and sintering process via flash white light combined with deep-UV and near-infrared irradiation for highly conductive copper nano-ink.

PubMed

Hwang, Hyun-Jun; Oh, Kyung-Hwan; Kim, Hak-Sung

2016-01-25

We developed an ultra-high speed photonic sintering method involving flash white light (FWL) combined with near infrared (NIR) and deep UV light irradiation to produce highly conductive copper nano-ink film. Flash white light irradiation energy and the power of NIR/deep UV were optimized to obtain high conductivity Cu films. Several microscopic and spectroscopic characterization techniques such as scanning electron microscopy (SEM), a x-ray diffraction (XRD), and Fourier-transform infrared (FT-IR) spectroscopy were employed to characterize the Cu nano-films. Optimally sintered Cu nano-ink films produced using a deep UV-assisted flash white light sintering technique had the lowest resistivity (7.62 μΩ·cm), which was only 4.5-fold higher than that of bulk Cu film (1.68 μΩ•cm).

In vitro and in vivo anti-inflammatory properties of green synthesized silver nanoparticles using Viburnum opulus L. fruits extract.

PubMed

Moldovan, Bianca; David, Luminita; Vulcu, Adriana; Olenic, Liliana; Perde-Schrepler, Maria; Fischer-Fodor, Eva; Baldea, Ioana; Clichici, Simona; Filip, Gabriela Adriana

2017-10-01

A green, rapid and cost effective method for the bio-synthesis of silver nanoparticles (AgNPs), using polyphenols present in European cranberry bush fruit extracts was developed. The obtained AgNPs were characterized by ultra-violet visible spectroscopy (UV-VIS), Fourier transform - infrared spectroscopy (FT-IR), transmission electron microscopy (TEM) and X-ray diffraction patterns (XRD). The average size of the spherical AgNPs was found to be 25nm. The anti-inflammatory effect of the biomaterials was investigated, both in vitro (on HaCaT cell line, exposed to UVB radiation) and in vivo (on acute inflammation model in Wistar rats). Our results support the conclusion that the photosynthesized silver nanoparticles present a potent anti-inflammatory activity and could be successfully used as therapeutic tools for treatment of inflammation. Copyright © 2017 Elsevier B.V. All rights reserved.

Facile synthesis, single crystal analysis, and computational studies of sulfanilamide derivatives

NASA Astrophysics Data System (ADS)

Tahir, Muhammad Nawaz; Khalid, Muhammad; Islam, Ayesha; Ali Mashhadi, Syed Muddassir; Braga, Ataualpa A. C.

2017-01-01

Antibacterial resistance is a worldwide problem. Sulfanilamide is widely used antibacterial. For the first time, we report here a simple method for the derivative synthesis of the title drugs, single crystal XRD and density functional theory (DFT) studies. The optimized molecular structure, natural bond orbital (NBO), frontier molecular orbitals (FMOs) molecular electrostatic potential studies (MEP) and Mulliken population analysis (MPA) have been performed using M06-2X/6-31G(d, p). The FT-IR spectra and thermodynamic parameters were calculated at M06-2X/6-311 + G(2d,p) and B3LYP/6-31G(d, p) levels respectively, while, the UV-Vis analysis was performed using TD-DFT/B3LYP/6-31G(d, p) method. The experimental FT-IR spectra of both compounds were also carried out to reconfirm sbnd H⋯Osbnd hydrogen bonds. The DFT optimized parameters exhibiting good agreement with the experimental data. NBO analysis explored the hyper conjugative interaction and stability of title crystals, especially, reconfirmed the existence of sbnd H⋯Osbnd hydrogen bonds between the dimers. The FT-IR, thermodynamic parameters, MEP and MPA also revealed the hydrogen bonding detail is harmonious to XRD data. As a matter of the fact, the hydrogen bonding is a significant parameter for the understanding and design of molecular crystals, subsequently; it can also play a vital role in the supramolecular chemistry. Moreover, the global reactivity descriptors suggest that title compounds might be bioactive.

Formulation and in vitro characterization of novel sildenafil citrate-loaded polyvinyl alcohol-polyethylene glycol graft copolymer-based orally dissolving films.

PubMed

Xu, Li-Li; Shi, Li-Li; Cao, Qing-Ri; Xu, Wei-Juan; Cao, Yue; Zhu, Xiao-Yin; Cui, Jing-Hao

2014-10-01

This work was aimed to develop novel sildenafil citrate (SC)-loaded polyvinyl alcohol (PVA)-polyethylene glycol (PEG) graft copolymer (Kollicoat(®) IR)-based orally dissolving films (ODFs) using a solvent casting method. Formulation factors such as plasticizers and disintegrants were optimized on the basis of characteristics of blank ODFs. The SC-loaded ODF with a loading capacity up to 6.25mg in an area of 6 cm(2) was prepared and evaluated in terms of mechanical properties, disintegration time and dissolution rate. The physicochemical properties of drug-loaded ODF were also investigated using the scanning electron microscope (SEM), X-ray diffraction (XRD), differential scanning calorimetry (DSC) and Fourier transform infrared spectroscopy (FT-IR). The blank ODF composed of Kollicoat(®) IR, sodium alginate (ALG-Na) and glycerol (10:2:1.5, w/w) had a remarkably short disintegration time of about 20s. The SC-loaded ODF showed a delayed disintegration time (about 25s), but exhibited improved mechanical properties when compared to the blank ODF. SC was homogeneously dispersed throughout the ODF and the crystalline form of drug had been partly changed, existing strong hydrogen bonding between the drug and carriers. The Kollicoat(®) IR/ALG-Na based ODFs containing SC might be an alternative to conventional tablet for the treatment of male erectile dysfunction. Copyright © 2014 Elsevier B.V. All rights reserved.

XRD and FTIR analysis heat treated lithium bismo-borate glasses doped with 1.0 mol% copper ferrite

NASA Astrophysics Data System (ADS)

Yadav, Arti; Narwal, P.; Dahiya, Manjeet S.; Dahiya, T.; Agarwal, A.; Khasa, S.

2018-05-01

Glasses of compositions of 20Li20 • xBi2O3• (79-x)B2O3 + (1.0 mol%) CuFe2O4, with 0 ≤ x ≤ 40 were prepared by melt-quench technique. To obtain the glass-ceramics the controlled heat treatment were given to the prepared glasses. Two nano crystalline phases, i.e., Li2B4O7 and LiB3O5 were observed from X-ray diffraction patterns of the prepared glass- ceramic samples. We investigated the change in coordination number of network formers B2O3 and Bi2O3 and network modifiers Bi2O3, Li2O and CuFe2O4. Crystallites size (lies in range ˜47-50nm) and lattice strain (ɛ) were calculated for major phases for all prepared samples. FT-IR study revealed the de-polymerization of borate groups that change with heat treatment and Bi2O3 content. Deconvolution of IR absorption spectra resolves the overlapped and hidden peaks in IR spectra. Sharp and more intense FTIR peaks confirm the vibrations due to crystallites Li2B4O7 and LiB3O5 and change in coordination of network forming borate units.

Synthesis and Characterization of Polyol-Assisted Nano Cu0.2Ni0.2Sn0.2Ba0.4 Fe2O4 by a Wet Hydroxyl Route

NASA Astrophysics Data System (ADS)

Pavithradevi, S.; Suriyanarayanan, N.; Boobalan, T.; Velumani, S.; Chandramohan, M.; Manivel Raja, M.

2017-08-01

Nanocrystalline spinel ferrite of composition Cu0.2Ni0.2Sn0.2Ba0.4 Fe2O4 has been synthesized by a wet hydroxyl chemical route in ethylene glycol as chelating agent and sodium hydroxide as precipitator at pH 8. Ethylene glycol has been used as the medium which serves as the solvent as well as a complexing agent. The synthesized particles are annealed at temperatures of 350°C, 700°C, and 1050°C. Thermogravimetric (TG) analysis confirms that at 240°C, ethylene glycol has evaporated completely, and a stable phase is formed above 670°C. Fourier transform infrared (FT-IR) spectroscopy of mixed Cu0.2Ni0.2Sn0.2Ba0.4 ferrite nanoparticles like as synthesized and annealed at 1050°C are recorded between 400 cm-1 and 4000 cm-1. FT-IR appraises the structural formation of Cu0.2Ni0.2Sn0.2Ba0.4 Fe2O4 between the as-synthesized sample and the sample annealed at 1050°C. Structural characterizations of all the samples are carried out by x-ray diffraction (XRD) technique. XRD reveals that the particle size increases with the increase in annealing temperatures. Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) confirms that the particles are flaky and spherical with the crystallite size in the range of 11-27 nm. The decrement of dielectric properties, like dielectric constant and dielectric loss, with the increment of frequency as seen in all the samples is an usual dielectric behavior of spinel ferrites. The lack of net magnetization is noticed immediately when the applied magnetic field is removed which prompts superparamagnetic behavior, as seen in all the samples.

Water absorption characteristics of novel Cu/LDPE nanocomposite for use in intrauterine devices.

PubMed

Xia, Xianping; Cai, Shuizhou; Hu, Junhui; Xie, Changsheng

2006-11-01

Intrauterine devices (IUDs), especially the copper-containing IUDs (Cu-IUDs), are one of the worldwide used forms for birth control, owing to their advantages of long-lasting and high efficacy, economy, safety, and reversibility. However, it is not perfect for the existing Cu-IUDs; some shortcomings related to its side effects have not been overcome yet. For this reason, a new Cu-IUDs material, the copper/low-density polyethylene (Cu/LDPE) nanocomposite, has been developed in our research team. The structure and water uptake characteristics of this new Cu-IUDs material have been investigated by using X-ray diffraction (XRD), Scanning electron microscopy (SEM), X-ray energy dispersive spectroscopy (EDS), Fourier transform infrared spectroscopy (FT-IR), and gravimetric analysis in this paper. The results of XRD, SEM, EDS, and FT-IR show three important outcomes associated with the structure of the nanocomposite. First, the nanocomposite is hybrid of the polymer and the copper nanoparticles (nano-Cu). Second, porosities, nano-Cu aggregates, and primary alcohol (R--CH(2)--OH) are existed in the nanocomposite. Third, the nano-Cu aggregates are distributed uniformly in the polymer matrix in general. The results of Gravimetric analysis, which associated with the water uptake characteristics of the nanocomposite, exhibit that the water absorption behavior of the nanocomposite obeys the classical diffusion theory very well, the water uptake of the nanocomposite increases with the increasing of the nano-Cu loading, and that the water uptake ability of the nanocomposite with 15.0 wt % nano-Cu (50 nm in diameter) is about 150 times larger than that of the base resin and about 45 times higher than that of the Cu/LDPE microcomposite with 15.0 wt % copper microparticles (5 microm in diameter). These water uptake characteristics are mainly attributed to the structure of the Cu/LDPE composites and the size effect of the nano-Cu. (c) 2006 Wiley Periodicals, Inc.

A Multi-Analytical Approach for the Evaluation of the Efficiency of the Conservation-Restoration Treatment of Moroccan Historical Manuscripts Dating to the 16th, 17th, and 18th Centuries.

PubMed

Hajji, Latifa; Boukir, Abdellatif; Assouik, Jamal; Kerbal, Abdelali; Kajjout, Mohamed; Doumenq, Pierre; De Carvalho, Maria Luisa

2015-08-01

The most critical steps during the conservation-restoration treatment applied in Moroccan libraries are the deacidification using immersion in a saturated aqueous calcium hydroxide (Ca(OH)2) solution and the consolidation of degraded manuscripts using Japanese paper. The present study aims to assess the efficiency of this restoration method using a multi-analytical approach. For this purpose, three ancient Arabic Moroccan manuscript papers dating back to the 16th, 17th, and 18th centuries were investigated to characterize the paper support and make a comparative study between pre-restoration and post-restoration states. Three structural and molecular characterization techniques including solid-state nuclear magnetic resonance spectroscopy on (13)C with cross-polarization and magic-angle spinning nuclear magnetic resonance ((13)C CP-MAS NMR), attenuated total reflectance Fourier transform infrared spectroscopy (ATR FT-IR), and X-ray diffraction (XRD) were used to elucidate the cellulose main features, to identify the inorganic composition of the papers, and to study the crystallinity of the samples. Inductively coupled plasma atomic emission spectrometry (ICP-AES) allowed us to obtain a qualitative and quantitative characterization of the mineral fillers used in the manufacturing of the papers. Scanning electron microscopy coupled to energy dispersive spectrometry (SEM-EDS) ascertained the state of conservation of the different papers and helped us to study the elemental composition of the samples. After restoration, it was shown that the deacidification improved the stability of papers by providing an important alkaline buffer, as demonstrated using FT-IR and energy dispersive spectrometry (EDS) results. However, XRD and ICP-AES did not confirm the pertinence of the treatment for all samples because of the unequal distribution of Ca on the paper surface during the restoration. The consolidation process was studied using SEM analysis; its effectiveness in restoring torn areas was found to be significant.

Synthesis, structural, DFT studies, docking and antibacterial activity of a xanthene based hydrazone ligand

NASA Astrophysics Data System (ADS)

Naseem, Saira; Khalid, Muhammad; Tahir, Muhammad Nawaz; Halim, Mohammad A.; Braga, Ataualpa A. C.; Naseer, Muhammad Moazzam; Shafiq, Zahid

2017-09-01

Herein, we present the synthesis of novel xanthene-based hydrazone (1). The chemical structure of 1 was resolved using spectroscopic techniques such as NMR, FT-IR, UV-VIS and X-ray crystallographic approaches. X-ray diffraction analysis shows that the compound (1) crystallizes in triclinic crystal lattice with the Pbar1 space group and diffused to form multi-layered structure due to non-covalent interactions such as intramolecular hydrogen bonding (H.B). In addition to experimental investigation, density functional theory (DFT) calculation with M06-2X/6-31G(d,p) and B3LYP/6-31G(d,p) level of theories was performed on compound (1) to obtain optimized geometry, spectroscopic and electronic properties. DFT optimized geometry shows good agreement with the experimental XRD structure. The hyper conjugative interactions and hydrogen bonding network are responsible for the stability of compound (1) as revealed by natural bond orbital (NBO) calculation. Moreover, hydrogen bonding network in the dimer is confirmed by FT-IR and thermodynamic studies showing excellent agreement with XRD and NBO findings. TD-DFT/UV-VIS analysis provides insight that maximum excitation is found in 1 which shows good agreement with experimental UV-VIS result. The global reactivity parameters are calculated using the energies of frontier molecular orbitals also disclosed that the compound is more stable might be due to hydrogen bonding network. Experimental and molecular docking studies indicated that this compound has anti-bacterial and anti-diabetic properties. The binding affinity of this compound against the multidrug efflux pump subunit AcrB OS=Escherichia coli (strain K12) and Human Pancreatic Alpha-Amylase is -9.2 and -10.00 kcal/mol which are higher than the control drugs. Pi-Pi, Pi-anaion, amide-pi and pi-alkyl bonds play key role in drug-protein complexes.

Selective Iron(III) ion uptake using CuO-TiO2 nanostructure by inductively coupled plasma-optical emission spectrometry

PubMed Central

2012-01-01

Background CuO-TiO2 nanosheets (NSs), a kind of nanomaterials is one of the most attracting class of transition doped semiconductor materials due to its interesting and important optical, electrical, and structural properties and has many technical applications, such as in metal ions detection, photocatalysis, Chemi-sensors, bio-sensors, solar cells and so on. In this paper the synthesis of CuO-TiO2 nanosheets by the wet-chemically technique is reported. Methods CuO-TiO2 NSs were prepared by a wet-chemical process using reducing agents in alkaline medium and characterized by UV/vis., FT-IR spectroscopy, X-ray photoelectron spectroscopy (XPS), powder X-ray diffraction (XRD), and field-emission scanning electron microscopy (FE-SEM) etc. Results The structural and optical evaluation of synthesized NSs were measured by XRD pattern, Fourier transform infrared (FT-IR) and UV–vis spectroscopy, respectively which confirmed that the obtained NSs are well-crystalline CuO-TiO2 and possessing good optical properties. The morphological analysis of CuO-TiO2 NSs was executed by FE-SEM, which confirmed that the doped products were sheet-shaped and growth in large quantity. Here, the analytical efficiency of the NSs was applied for a selective adsorption of iron(III) ion prior to detection by inductively coupled plasma-optical emission spectrometry (ICP-OES). The selectivity of NSs towards various metal ions, including Au(III), Cd(II), Co(II), Cr(III), Fe(III), Pd(II), and Zn(II) was analyzed. Conclusions Based on the selectivity study, it was confirmed that the selectivity of doped NSs phase was the most towards Fe(III) ion. The static adsorption capacity for Fe(III) was calculated to be 110.06 mgg−1. Results from adsorption isotherm also verified that the adsorption process was mainly monolayer-adsorption onto a surface containing a finite number of CuO-TiO2 NSs adsorption sites. PMID:23244218

Investigation of polypyrrole/polyvinyl alcohol-titanium dioxide composite films for photo-catalytic applications

NASA Astrophysics Data System (ADS)

Cao, Shaoqiang; Zhang, Hongyang; Song, Yuanqing; Zhang, Jianling; Yang, Haigang; Jiang, Long; Dan, Yi

2015-07-01

Polypyrrole/polyvinyl alcohol-titanium dioxide (PPy/PVA-TiO2) composite films used as photo-catalysts were fabricated by combining TiO2 sol with PPy/PVA solution in which PPy was synthesized by in situ polymerization of pyrrole (Py) in polyvinyl alcohol (PVA) matrix and loaded on glass. The prepared photo-catalysts were investigated by X-ray diffraction (XRD), ultraviolet-visible diffuse reflection spectroscopy (UV-vis DRS), scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectra and photoluminescence (PL). The results indicate that the composites have same crystal structure as the TiO2 and extend the optic absorption from UV region to visible light region. By detecting the variation ratio, detected by ultraviolet-vis spectroscopy, of model pollutant rhodamine B (RhB) solution in the presence of the composite films under both UV and visible light irradiation, the photo-catalytic performance of the composite films was investigated. The results show that the PPy/PVA-TiO2 composite films show better photo-catalytic properties than TiO2 film both under UV and visible light irradiation, and the photo-catalytic degradation of RhB follows the first-order kinetics. The effects of the composition of composite films and the concentration of RhB on the photo-catalytic performance, as well as the possible photo-catalytic mechanism, were also discussed. By photo-catalytic recycle experiments, the structure stability of the PPy/PVA-TiO2 composite film was investigated and the results show that the photo-catalytic activity under both UV and visible light irradiation have no significant decrease after four times of recycle experiments, suggesting that the photo-catalyst film is stable during the photo-catalytic process, which was also confirmed by the XRD pattern and FT-IR spectra of the composite film before and after photo-catalytic.

Analysis of Roman age wall paintings found in Pordenone, Trieste and Montegrotto.

PubMed

Mazzocchin, G A; Agnoli, F; Salvadori, M

2004-10-20

The aim of the present work is the study of many fragments of wall painting from archaeological excavations in three different Roman age sites dating back to the I Century before Common Era: Pordenone (località Torre); Trieste (Crosada) and Padova (Montegrotto). The techniques used were optical microscopy, scanning electron microscopy (SEM), equipped with a EDS microanalysis detector, X-rays powder diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Fourier transform Raman spectroscopy (FT-Raman) and electron paramagnetic resonance (EPR) spectroscopy. The identified pigments were: cinnabar, hematite, celadonite, glauconite, cuprorivaite (Egyptian blue), yellow and red ochre, calcite, limonite, coal black. In general, the mortar preparation did not correspond to the complex procedure suggested by Vitruvius (De Architectura), but generally showed a porous layer, with crushed grains under the pigment layer. In some cases, two superimposed pigment layers were found: yellow superimposed on both red and pink, black on pink, green on black. The slight differences we found in the use of the pigments in the three studied sites might show that the same technology, culture and taste spread all over the Roman Empire in North Eastern Italy (X(a) Regio Venetia et Histria).

Novel synergistic transparent k-Carrageenan/Xanthan gum/Gellan gum hydrogel film: Mechanical, thermal and water barrier properties.

PubMed

Balasubramanian, R; Kim, Sam Soo; Lee, Jaewoong

2018-06-24

The aim is to develop novel synergistic transparent k-Carrageenan/Xanthan gum/Gellan gum (k-C/X/G) hydrogel films with different weight ratio composition and to study the effect of these compositions on the physical properties of the films. The structure and morphological properties of the films were investigated by Fourier-transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), X-ray diffraction (XRD) and differential scanning calorimeter (DSC). Results for FT-IR, DSC and SEM analysis showed a clear interaction between k-C, X, and G to form a new material. The mechanical, thermal and water barrier properties such as water vapor permeability (WVP), water contact angle (WCA) and moisture content were determined. The temperature at 5% weight loss (T 5% ) are in the range of 64.2-121.9 °C. The WVP exhibits are in the range of 1.8-2.4, contact angle are in the range of 32-65.8° and moisture content 16.5-21.51. The hydrogel film had good tensile strength of 19.1-31.0 MPa and elongation at break of 13-19% and tensile modulus of 1.6-2.4 GPa. The UV results indicate that the films were very transparent. The range of properties of the ternary k-C/X/G hydrogel films suggest that the presence molecular interaction and cross linking within the blends. Copyright © 2018. Published by Elsevier B.V.

Preparation and characterization of chitosan-natural nano hydroxyapatite-fucoidan nanocomposites for bone tissue engineering.

PubMed

Lowe, Baboucarr; Venkatesan, Jayachandran; Anil, Sukumaran; Shim, Min Suk; Kim, Se-Kwon

2016-12-01

Solid three dimensional (3D) composite scaffolds for bone tissue engineering were prepared using the freeze-drying method. The scaffolds were composed of chitosan, natural nano-hydroxyapatite (nHA) and fucoidan in the following combinations: chitosan, chitosan-fucoidan, chitosan-nHA, and chitosan-nHA-fucoidan. Fourier transform infrared spectroscopy (FT-IR), thermal gravimetric analysis (TGA), X-ray diffraction analysis (XRD), scanning electron microscopy (SEM), and optical microscopy (OM) were used to determine the physiochemical constituents and the morphology of the scaffolds. The addition of nHA into the chitosan-fucoidan composite scaffold reduced the water uptake and water retention. FT-IR analysis confirmed the presence of a phosphate group in the chitosan-nHA-fucoidan scaffold. This group is present because of the presence of nHA (isolated via alkaline hydrolysis from salmon fish bones). Microscopic results indicated that the dispersion of nHA and fucoidan in the chitosan matrix was uniform with a pore size of 10-400μm. The composite demonstrated a suitable micro architecture for cell growth and nutrient supplementation. This compatibility was further elucidated in vitro using periosteum-derived mesenchymal stem cells (PMSCs). The cells demonstrated high biocompatibility and excellent mineralization for the chitosan-nHA-fucoidan scaffold. We believe that a chitosan-nHA-fucoidan composite is a promising biomaterial for the scaffold that can be used for bone tissue regeneration. Copyright © 2016 Elsevier B.V. All rights reserved.

Green synthesis of Pd nanoparticles at Apricot kernel shell substrate using Salvia hydrangea extract: Catalytic activity for reduction of organic dyes.

PubMed

Khodadadi, Bahar; Bordbar, Maryam; Nasrollahzadeh, Mahmoud

2017-03-15

For the first time the extract of the plant of Salvia hydrangea was used to green synthesis of Pd nanoparticles (NPs) supported on Apricot kernel shell as an environmentally benign support. The Pd NPs/Apricot kernel shell as an effective catalyst was prepared through reduction of Pd 2+ ions using Salvia hydrangea extract as the reducing and capping agent and Pd NPs immobilization on Apricot kernel shell surface in the absence of any stabilizer or surfactant. According to FT-IR analysis, the hydroxyl groups of phenolics in Salvia hydrangea extract as bioreductant agents are directly responsible for the reduction of Pd 2+ ions and formation of Pd NPs. The as-prepared catalyst was characterized by Fourier transform infrared (FT-IR) and UV-Vis spectroscopy, field emission scanning electron microscopy (FESEM) equipped with an energy dispersive X-ray spectroscopy (EDS), Elemental mapping, X-ray diffraction analysis (XRD) and transmittance electron microscopy (TEM). The synthesized catalyst was used in the reduction of 4-nitrophenol (4-NP), Methyl Orange (MO), Methylene Blue (MB), Rhodamine B (RhB), and Congo Red (CR) at room temperature. The Pd NPs/Apricot kernel shell showed excellent catalytic activity in the reduction of these organic dyes. In addition, it was found that Pd NPs/Apricot kernel shell can be recovered and reused several times without significant loss of catalytic activity. Copyright © 2016 Elsevier Inc. All rights reserved.

Ultrasonically assisted solvothermal synthesis of novel Ni/Al layered double hydroxide for capturing of Cd(II) from contaminated water

NASA Astrophysics Data System (ADS)

Rahmanian, Omid; Maleki, Mohammad Hassan; Dinari, Mohammad

2017-11-01

A novel adsorbent of nickel aluminum layered double hydroxide (Ni/Al-LDH) was prepared through the precipitation of metal nitrates by ultrasonically assisted solvothermal method. The surface morphology, chemical structure and thermal properties of this compound were examined by X-ray diffraction (XRD), Fourier Transform Infrared (FT-IR), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and thermogravimetric analysis (TGA) techniques. The XRD, TEM and FE-SEM results established that the synthesized LDH have a well-ordered layer structure with good crystalline nature. Then it was applied to remove excessive Cd(II) ions from water and the effects of contact time, pH and adsorbent dose were examined at initial Cd(II) concentration of 10 mg/L. Results show that the time required to reach equilibrium was fast (40 min) and working pH solution was neutral (pH 7). Langmuir and Freundlich model of adsorption isotherms were explored; the results show that the Freundlich model was better fitted than that Langmuir model. This results predicting a multilayer adsorption of Cd(II) on LDH. The equilibrium kinetic adsorption data were fixed to the pseudo-second order kinetic equation.

Fabrication of chloroform sensor based on hydrothermally prepared low-dimensional β-Fe 2O 3 nanoparticles

NASA Astrophysics Data System (ADS)

Rahman, Mohammed M.; Jamal, A.; Khan, Sher Bahadar; Faisal, M.

2011-10-01

Hydrothermally prepared as-grown low-dimensional nano-particles (NPs) have been characterized using UV-vis spectroscopy, Fourier transform infrared (FT-IR) spectroscopy, powder X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), Raman spectroscopy, and electron dispersion spectroscopy (EDS). The uniformity of the nano-material was executed by the scanning electron microscopy, where the single phase of the nano-crystalline β-Fe 2O 3 was characterized using XRD techniques. β-Fe 2O 3 nanoparticles fabricated glassy carbon electrode (GCE) have improved chloroform-sensing performances in terms of electrical response ( I- V technique) for detecting analyte in liquid phase. The analytical performances were investigated, which showed that the better sensitivity, stability, and reproducibility of the sensor improved significantly by using Fe 2O 3 NPs thin-film on GCE. The calibration plot was linear ( R = 0.9785) over the large range of 12.0 μM to 12.0 mM. The sensitivity was calculated as 2.1792 μA cm -2 mM -1 with a detection limit of 4.4 ± 0.10 μM in short response time (10.0 s).

Fabrication of multicolor fluorescent polyvinyl alcohol through surface modification with conjugated polymers by oxidative polymerization

NASA Astrophysics Data System (ADS)

Hai, Thien An Phung; Sugimoto, Ryuichi

2018-06-01

A simple method for the preparation of multicolor polyvinyl alcohol (PVA) by chemical oxidative polymerization is introduced. The PVA surface was successfully modified with conjugated polymers composed of 3-hexylthiophene (3HT) and fluorene (F). The incorporation of the 3HT/F copolymer onto the PVA surface was confirmed by Fourier-transform infrared (FT-IR), ultraviolet-visible (UV-vis), and fluorescence spectroscopies, X-ray diffraction (XRD), as well as thermogravimetric analysis (TGA), contact angle, and field-emission scanning electron microscopy (FE-SEM) coupled with energy dispersive X-ray (EDX) analysis. Different 3HT/F ratios on the PVA surface result in optical properties that include multicolor-emission and absorption behavior. The color of the resultant (3HT/F)-g-PVA shifted from red to blue, and the quantum yield increased with increasing F content. The surface hydrophobicity of the modified PVA increased significantly through grafting with the conjugated polymers, with the water contact angle increasing by 30° compared to pristine PVA. The PVA XRD peaks were less intense following surface modification. Thermogravimetric analyses reveal that the thermal stability of the PVA decreases as a result of grafting with the 3HT/F copolymers.

Fabrication method and microstructural characteristics of coal-tar-pitch-based 2D carbon/carbon composites

NASA Astrophysics Data System (ADS)

Esmaeeli, Mohammad; Khosravi, Hamed; Mirhabibi, Alireza

2015-02-01

The lignin-cellulosic texture of wood was used to produce two-dimensional (2D) carbon/carbon (C/C) composites using coal tar pitch. Ash content tests were conducted to select two samples among the different kinds of woods present in Iran, including walnut, white poplar, cherry, willow, buttonwood, apricots, berry, and blue wood. Walnut and white poplar with ash contents of 1.994wt% and 0.351wt%, respectively, were selected. The behavior of these woods during pyrolysis was investigated by differential thermal analysis (DTA) and thermo gravimetric (TG) analysis. The bulk density and open porosity were measured after carbonization and densification. The microstructural characteristics of samples were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD), and Fourier-transform infrared (FT-IR) spectroscopy. The results indicate that the density of both the walnut and white poplar is increased, and the open porosity is decreased with the increasing number of carbonization cycles. The XRD patterns of the wood charcoal change gradually with increasing pyrolysis temperature, possibly as a result of the ultra-structural changes in the charcoal or the presence of carbonized coal tar pitch in the composite's body.

Synthesis, crystal structure analysis, spectral (NMR, FT-IR, FT-Raman and UV-Vis) investigations, molecular docking studies, antimicrobial studies and quantum chemical calculations of a novel 4-chloro-8-methoxyquinoline-2(1H)-one: An effective antimicrobial agent and an inhibition of DNA gyrase and lanosterol-14α-demethylase enzymes

NASA Astrophysics Data System (ADS)

Murugavel, S.; Sundramoorthy, S.; Lakshmanan, D.; Subashini, R.; Pavan Kumar, P.

2017-03-01

The novel title compound 4-chloro-8-methoxyquinoline-2(1H)-one (4CMOQ) has been synthesized by slow evaporation solution growth technique at room temperature. The synthesized 4CMOQ molecule was characterized experimentally by FT-IR, FT-Raman, UV-Vis, NMR and single crystal diffraction (XRD) and theoretically by quantum chemical calculations. The molecular geometry was also optimized using density functional theory (DFT/B3LYP) method with the 6-311++G (d,p) basis set in ground state and compared with the experimental data. The entire vibrational assignments of wave numbers were made on the basis of potential energy distribution (PED) by VEDA 4 programme. The nuclear magnetic resonance spectra (1H and 13C NMR) are obtained by using the gauge-invariant atomic orbital (GIAO) method. The change in electron density (ED) in the antibonding orbital's and stabilization energies E(2) of the molecule have been evaluated by natural bond orbital (NBO) analysis to give clear evidence of stabilization. Moreover, electronic characteristics such as HOMO and LUMO energies, Mulliken atomic charges and molecular electrostatic potential surface are investigated. Absorption spectrum analysis, nonlinear optical properties, chemical reactivity descriptors and thermodynamic features are also outlined theoretically. Molecular docking studies were executed to understand the inhibitory activity of 4CMOQ against DNA gyrase and Lanosterol 14 α-demethylase. The antimicrobial activity of 4CMOQ was determined against bacterial strains such as Escherichia coli, Staphylococcus aureus and Pseudomonas aeruginosa and fungal strains such as Aspergillus niger, Monascus purpureus and Penicillium citrinum. The obtained results show that the compound exhibited good to moderate antimicrobial activity.

Curcumin-β-cyclodextrin inclusion complex: stability, solubility, characterisation by FT-IR, FT-Raman, X-ray diffraction and photoacoustic spectroscopy, and food application.

PubMed

Mangolim, Camila Sampaio; Moriwaki, Cristiane; Nogueira, Ana Claudia; Sato, Francielle; Baesso, Mauro Luciano; Neto, Antônio Medina; Matioli, Graciette

2014-06-15

Curcumin was complexed with β-CD using co-precipitation, freeze-drying and solvent evaporation methods. Co-precipitation enabled complex formation, as indicated by the FT-IR and FT-Raman techniques via the shifts in the peaks that were assigned to the aromatic rings of curcumin. In addition, photoacoustic spectroscopy and X-ray diffraction, with the disappearance of the band related to aromatic rings, by Gaussian fitting, and modifications in the spectral lines, respectively, also suggested complex formation. The possible complexation had an efficiency of 74% and increased the solubility of the pure colourant 31-fold. Curcumin-β-CD complex exhibited a sunlight stability 18% higher than the pure colourant. This material was stable to pH variations and storage at -15 and 4°C. With an isothermal heating at 100 and 150°C for 2h, the material exhibited a colour retention of approximately 99%. The application of curcumin-β-CD complex in vanilla ice creams intensified the colour of the products and produced a great sensorial acceptance. Copyright © 2013 Elsevier Ltd. All rights reserved.

Evaluation of antibacterial and Antibiofilm activity of Synthesized Zinc-Hydroxyapatite Biocomposites from Labeo rohita fish scale waste

NASA Astrophysics Data System (ADS)

Sathiskumar, Swamiappan; Vanaraj, Sekar; Sabarinathan, Devaraj; Preethi, Kathirvel

2018-02-01

Materials based on hydroxyapatite (HAp) Synthesized from bio-wastes have been regarded as useful, novel, eco-friendly medical applications that are targeted primarily for their antibacterial nature. In the present study, HAp was Synthesized from the fish scales of Labeo rohita using alkaline heat treatment and subsequently mixed with 1, 2 and 3 wt% of zinc (Zn) at 800 °C using calcination method to yield Zn-HAp composites. A detailed characterization of the generated composites was analysed by XRD, FT-IR, SEM, EDX and DLS methods. Further, antibacterial and biofilm inhibitory activity of the generated composites was determined using strains of Staphylococcus aureus and Escherichia coli. The confirmation of the presence of zinc, confirmed by EDAX spectra, XRD, FT-IR, SEM and DLS observations, established that HAp and Zn-HAp composites were without impurities, irregular in shape and were 848 nm sized particles. Although 1-3 wt% Zn-HAp composites showed antibacterial activity, the 3 wt% Zn-HAp composite was found suitable to kill the surrounding bacterial growth and showed potent inhibitory activity against biofilm formation.

Spectroscopic studies on sidewall carboxylic acid functionalization of multi-walled carbon nanotubes with valine.

PubMed

Deborah, M; Jawahar, A; Mathavan, T; Dhas, M Kumara; Benial, A Milton Franklin

2015-03-15

The valine functionalized multi-walled carbon nanotubes (MWCNTS) were prepared and characterized by using XRD, UV-Vis, FT-IR, EPR, SEM, and EDX, spectroscopic techniques. The enhanced XRD peak (002) intensity was observed for valine functionalized MWCNTs compared with oxidized MWCNTs, which is likely due to sample purification by acid washing. UV-Vis study shows the formation of valine functionalized MWCNTs. FT-IR study confirms the presence of functional groups of oxidized MWCNTs and valine functionalized MWCNTs. The ESR line shape analysis indicates that the observed EPR line shape is a Gaussian line shape. The g-values indicate that the systems are isotropic in nature. The morphology study was carried out for oxidized MWCNTs and valine functionalized MWCNTs by using SEM. The EDX spectra revealed that the high purity of oxidized MWCNTs and valine functionalized MWCNTs. The functionalization has been chosen because, functionalization of CNTs with amino acids makes them soluble and biocompatible. Thus, they have potential applications in the field of biosensors and targeted drug delivery. Copyright © 2014 Elsevier B.V. All rights reserved.

Green synthesis, characterization and catalytic degradation studies of gold nanoparticles against congo red and methyl orange.

PubMed

Umamaheswari, C; Lakshmanan, A; Nagarajan, N S

2018-01-01

The present study reports, novel and greener method for synthesis of gold nanoparticles (AuNPs) using 5,7-dihydroxy-6-metoxy-3 ' ,4 ' methylenedioxyisoflavone (Dalspinin), isolated from the roots of Dalbergia coromandeliana was carried out for the first time. The synthesized gold nanoparticles were characterized by UV-Vis spectroscopy, high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED), Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD). The observed surface plasmon resonance (SPR) at 532nm in the UV-Vis absorption spectrum indicates the formation of gold nanoparticles. The powder XRD and SAED pattern for synthesized gold nanoparticles confirms crystalline nature. The HR-TEM images showed that the AuNPs formed were small in size, highly monodispersed and spherical in shape. The average particle sizes of the AuNPs are found to be ~10.5nm. The prepared AuNPs were found to be stable for more than 5months without any aggregation. The catalytic degradation studies of the synthesized AuNPs towards degradation of congo red and methyl orange, showed good catalytic in the complete degradation of both the dyes. The reduction catalyzed by gold nanoparticles followed the pseudo-first order kinetics, with a rate constant of 4.5×10 -3 s -1 (R 2 =0.9959) and 1.7×10 -3 s -1 (R 2 =0.9918) for congo red (CR) and methyl orange (MO), respectively. Copyright © 2017. Published by Elsevier B.V.

Crystal growth, characterization and theoretical studies of 4-aminopyridinium picrate

NASA Astrophysics Data System (ADS)

Aditya Prasad, A.; Muthu, K.; Rajasekar, M.; Meenatchi, V.; Meenakshisundaram, S. P.

2015-01-01

Single crystals of 4-aminopyridinium picrate (APP) were grown by slow evaporation of a mixed solvent system methanol-acetone (1:1, v/v) containing equimolar quantities of 4-aminopyridine and picric acid. Structure is elucidated by single crystal XRD analysis and the crystal belongs to monoclinic system with four molecules in the unit cell (space group P21/c) and the cell parameter values are, a = 8.513 Å (±0.015), b = 11.33 Å (±0.02), c = 14.33 Å (±0.03) and β = 104.15° (±0.019), V = 1340 A3 (±6) with refined R factors R1 = 0.0053 and wR2 = 0.0126. The electron density mapping is interpreted to find coordinates for each atom in the crystallized molecules. The various functional groups present in the molecule are confirmed by FT-IR analysis. UV-visible spectral analysis was used to determine the band gap energy of 4-aminopyridinium picrate. Powder X-ray diffraction pattern reveals the crystallinity of the as-grown crystal and it closely resembles the simulated XRD from the single crystal XRD analysis. Scanning electron microscopy reveals the surface morphology of the grown crystal. Optimized geometry is derived by Hartree-Fock theory calculations and the first-order molecular hyperpolarizability (β), theoretically calculated bond length, bond angles and excited state energy from theoretical UV-vis spectrum were estimated.

Facile preparation and characterization of pH sensitive Mt/CMC nanocomposite hydrogel beads for propranolol controlled release.

PubMed

Farhadnejad, Hassan; Mortazavi, Seyed Alireza; Erfan, Mohammad; Darbasizadeh, Behzad; Motasadizadeh, Hamidreza; Fatahi, Yousef

2018-05-01

The main aim of the present study was to design pH-sensitive nanocomposite hydrogel beads, based on carboxymethyl cellulose (CMC) and montmorillonite (Mt)-propranolol (PPN) nanohybrid, and evaluate whether the prepared nanocomposite beads could potentially be used as oral drug delivery systems. PPN-as a model drug-was intercalated into the interlayer space of Mt clay mineral via the ion exchange procedure. The resultant nanohybrid (Mt-PPN) was applied to fabricate nanocomposite hydrogel beads by association with carboxymethyl cellulose. The characterization of test samples was performed using different techniques: X-Ray Diffraction (XRD), IR spectroscopy (FT-IR), thermal gravity analysis (TGA), and scanning electron microscopy (SEM). The drug encapsulation efficiency was evaluated by UV-vis spectroscopy, and was found to be high for Mt/CMC beads. In vitro drug release test was performed in the simulated gastrointestinal conditions to evaluate the efficiency of Mt-PPN/CMC nanocomposite beads as a controlled-release drug carrier. The drug release profiles indicated that the Mt-PPN/CMC nanocomposite beads had high stability against stomach acid and a sustained- and controlled-release profile for PPN under the simulated intestinal conditions. Copyright © 2018 Elsevier B.V. All rights reserved.

Polyethyleneglycol/silver functionalized reduced graphene oxide aerogel for environmental application

NASA Astrophysics Data System (ADS)

Kumari, G. Vanitha; Asha, S.; Ananth, A. Nimrodh; Rajan, M. A. Jothi; Mathavan, T.

2018-04-01

Polyethylene glycol (PEG)/Silver (Ag) functionalized reduced graphene oxide aerogel (RGOA) was synthesized. PEG/Ag decorated reduced graphene oxide aerogel was characterized using XRD, Raman spectroscopy, Fourier transform infrared spectroscopy (FT-IR). The surface morphology of PEG/Ag/RGOA was analyzed using scanning electron microscope. The non-covalent interaction between reduced graphene oxide layers and the interaction between PEG and Ag on RGOA were studied by FT-IR spectra. It was observed that the interaction between Ag and PEG could enhance the properties of RGOA. Methyl Orange (MO) dye degradation was observed from UV-Vis Spectra. The process was studied by monitoring the simultaneous decrease in the height of UV-Vis absorption peak of dye solution. The results show that PEG/RGOA and PEG/Ag/RGOA are an efficient catalyst for dye degradation.

Synthesis, X-ray crystallography characterization, vibrational spectroscopic, molecular electrostatic potential maps, thermodynamic properties studies of N,N'-di(p-thiazole)formamidine.

PubMed

Rofouei, M K; Fereyduni, E; Sohrabi, N; Shamsipur, M; Attar Gharamaleki, J; Sundaraganesan, N

2011-01-01

In this work, we will report a combined experimental and theoretical study on molecular and vibrational structure of N,N'-di(p-thiazole)formamidine (DpTF). DpTF has been synthesized and characterized by elemental analysis, FT-IR, FT-Raman, 1H NMR, 13C NMR spectroscopy and X-ray single crystal diffraction. The FT-IR and FT-Raman spectra of DpTF were recorded in the solid phase. The optimized geometry was calculated by HF and B3LYP methods using 6-31G(d) basis set. The FT-IR and FT-Raman spectra of DpTF was calculated at the HF/B3LYP/6-31G(d) level and were interpreted in terms of potential energy distribution (PED) analysis. The scaled theoretical wavenumber showed very good agreement with the experimental values. A detailed interpretation of the infrared and Raman spectra of DpTF was reported. On the basis of vibrational analyses, the thermodynamic properties of the title compound at different temperatures have been calculated, revealing the correlations between Cp,m°, Sm°, Hm° and temperatures. Furthermore, molecular electrostatic potential maps (MESP) and total dipole moment properties of the compound have been calculated. Copyright © 2010 Elsevier B.V. All rights reserved.

Synthesis of metal complexes involving Schiff base ligand with methylenedioxy moiety: spectral, thermal, XRD and antimicrobial studies.

PubMed

Sundararajan, M L; Jeyakumar, T; Anandakumaran, J; Karpanai Selvan, B

2014-10-15

Metal complexes of Zn(II), Cd(II), Ni(II), Cu(II), Fe(III), Co(II), Mn(II) Hg(II), and Ag(I) have been synthesized from Schiff base ligand, prepared by the condensation of 3,4-(methylenedioxy)aniline and 5-bromo salicylaldehyde. All the compounds have been characterized by using elemental analysis, molar conductance, FT-IR, UV-Vis, (1)H NMR, (13)C NMR, mass spectra, powder XRD and thermal analysis (TG/DTA) technique. The elemental analysis suggests the stoichiometry to be 1:1 (metal:ligand). The FT-IR, (1)H NMR, (13)C NMR and UV-Vis spectral data suggest that the ligand coordinate to the metal atom by imino nitrogen and phenolic oxygen as bidentate manner. Mass spectral data further support the molecular mass of the compounds and their structure. Powder XRD indicates the crystalline state and morphology of the ligand and its metal complexes. The thermal behaviors of the complexes prove the presence of lattice as well as coordinated water molecules in the complexes. Melting point supports the thermal stability of all the compounds. The in vitro antimicrobial effects of the synthesized compounds were tested against five bacterial and three fungal species by well diffusion method. Antioxidant activities have also been performed for all the compounds. Metal complexes show more biological activity than the Schiff base. Copyright © 2014 Elsevier B.V. All rights reserved.

Correlations of Apparent Cellulose Crystallinity Determined by XRD, NMR, IR, Raman, and SFG Methods

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

Johnson, David K; Lee, Christopher; Dazen, Kevin

2015-07-04

Although the cellulose crystallinity index (CI) is used widely, its limitations have not been adequately described. In this study, the CI values of a set of reference samples were determined from X-ray diffraction (XRD), nuclear magnetic resonance (NMR), and infrared (IR), Raman, and vibrational sum frequency generation (SFG) spectroscopies. The intensities of certain crystalline peaks in IR, Raman, and SFG spectra positively correlated with the amount of crystalline cellulose in the sample, but the correlation with XRD was nonlinear as a result of fundamental differences in detection sensitivity to crystalline cellulose and improper baseline corrections for amorphous contributions. It ismore » demonstrated that the intensity and shape of the XRD signal is affected by both the amount of crystalline cellulose and crystal size, which makes XRD analysis complicated. It is clear that the methods investigated show the same qualitative trends for samples, but the absolute CI values differ depending on the determination method. This clearly indicates that the CI, as estimated by different methods, is not an absolute value and that for a given set of samples the CI values can be compared only as a qualitative measure.« less

Correlations of Apparent Cellulose Crystallinity Determined by XRD, NMR, IR, Raman, and SFG Methods

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

Lee, Christopher M; Dazen, Kevin; Kafle, Kabindra

2015-01-01

Although the cellulose crystallinity index (CI) is used widely, its limitations have not been adequately described. In this study, the CI values of a set of reference samples were determined from X-ray diffraction (XRD), nuclear magnetic resonance (NMR), and infrared (IR), Raman, and vibrational sum frequency generation (SFG) spectroscopies. The intensities of certain crystalline peaks in IR, Raman, and SFG spectra positively correlated with the amount of crystalline cellulose in the sample, but the correlation with XRD was nonlinear as a result of fundamental differences in detection sensitivity to crystalline cellulose and improper baseline corrections for amorphous contributions. It ismore » demonstrated that the intensity and shape of the XRD signal is affected by both the amount of crystalline cellulose and crystal size, which makes XRD analysis complicated. It is clear that the methods investigated show the same qualitative trends for samples, but the absolute CI values differ depending on the determination method. This clearly indicates that the CI, as estimated by different methods, is not an absolute value and that for a given set of samples the CI values can be compared only as a qualitative measure.« less

Comparison between infrared and Raman spectroscopic analysis of maturing rabbit cortical bone.

PubMed

Turunen, Mikael J; Saarakkala, Simo; Rieppo, Lassi; Helminen, Heikki J; Jurvelin, Jukka S; Isaksson, Hanna

2011-06-01

The molecular composition of the organic and inorganic matrices of bone undergoes alterations during maturation. The aim of this study was to compare Fourier transform infrared (FT-IR) and near-infrared (NIR) Raman microspectroscopy techniques for characterization of the composition of growing and developing bone from young to skeletally mature rabbits. Moreover, the specificity and differences of the techniques for determining bone composition were clarified. The humeri of female New Zealand White rabbits, with age range from young to skeletally mature animals (four age groups, n = 7 per group), were studied. Spectral peak areas, intensities, and ratios related to organic and inorganic matrices of bone were analyzed and compared between the age groups and between FT-IR and Raman microspectroscopic techniques. Specifically, the degree of mineralization, type-B carbonate substitution, crystallinity of hydroxyapatite (HA), mineral content, and collagen maturity were examined. Significant changes during maturation were observed in various compositional parameters with one or both techniques. Overall, the compositional parameters calculated from the Raman spectra correlated with analogous parameters calculated from the IR spectra. Collagen cross-linking (XLR), as determined through peak fitting and directly from the IR spectra, were highly correlated. The mineral/matrix ratio in the Raman spectra was evaluated with multiple different peaks representing the organic matrix. The results showed high correlation with each other. After comparison with the bone mineral density (BMD) values from micro-computed tomography (micro-CT) imaging measurements and crystal size from XRD measurements, it is suggested that Raman microspectroscopy is more sensitive than FT-IR microspectroscopy for the inorganic matrix of the bone. In the literature, similar spectroscopic parameters obtained with FT-IR and NIR Raman microspectroscopic techniques are often compared. According to the present results, however, caution is required when performing this kind of comparison.

Generation of drugs coated iron nanoparticles through high energy ball milling

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

Radhika Devi, A.; Murty, B. S.; Chelvane, J. A.

The iron nanoparticles coated with oleic acid and drugs such as folic acid/Amoxicillin were synthesized by high energy ball milling and characterized by X-ray diffraction, Transmission electron microscope, zeta potential, dynamic light scattering, Fourier Transform Infra red (FT-IR) measurements, and thermo gravimetric analysis (TGA). FT-IR and TGA measurements show good adsorption of drugs on oleic acid coated nanoparticles. Magnetic measurements indicate that saturation magnetization is larger for amoxicillin coated particles compared to folic acid coated particles. The biocompatibility of the magnetic nanoparticles prepared was evaluated by in vitro cytotoxicity assay using L929 cells as model cells.

Molecular and crystal structure of 2-{( E)-[(4-Methylphenyl)imino]methyl}-4-nitrophenol: A redetermination

NASA Astrophysics Data System (ADS)

Kaynar, Nihal Kan; Tanak, Hasan; Şahin, Songul; Dege, Necmi; Ağar, Erbil; Yavuz, Metin

2016-03-01

The crystal structure of the title compound, C14H12N2O3, was recently determined as a mixture of its neutral (OH containing) and zwitterionic (NH containing) forms, in a 0.60 (4): 0.40 (4) ratio using the X-ray determination. In this study, the title compound has been characterized by FT-IR and X-ray diffraction. The redetermination showed that the title compound has only enol (OH) form because of lack of the NH stretching vibration in FT-IR spectrum. In addition, the molecular structure and tautomerism of the title compound have been discussed.

Molecular and crystal structure of 2-((E)-[(4-Methylphenyl)imino]methyl)-4-nitrophenol: A redetermination

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

Kaynar, Nihal Kan, E-mail: nihal-kan84@windowslive.com; Tanak, Hasan; Şahin, Songul

The crystal structure of the title compound, C{sub 14}H{sub 12}N{sub 2}O{sub 3}, was recently determined as a mixture of its neutral (OH containing) and zwitterionic (NH containing) forms, in a 0.60 (4): 0.40 (4) ratio using the X-ray determination. In this study, the title compound has been characterized by FT-IR and X-ray diffraction. The redetermination showed that the title compound has only enol (OH) form because of lack of the NH stretching vibration in FT-IR spectrum. In addition, the molecular structure and tautomerism of the title compound have been discussed.

Synthesis and optical properties of polycrystalline Li2Al2B2O7 (LABO)

NASA Astrophysics Data System (ADS)

Dagdale, S. R.; Muley, G. G.

2016-05-01

A polycrystalline lithium aluminum borate (Li2Al2B2O7, LABO) has been synthesized by using simple solid-state technique. The obtained LABO polycrystalline was characterized by powder X-ray diffraction; Fourier transform infrared (FT-IR) spectroscopy and second harmonic generation (SHG) efficiency measurement. The functional groups were identified using the FT-IR spectroscopic data. The SHG efficiency of the polycrystalline material was obtained by the classic Kurtz powder technique using a fundamental wavelength 1064 nm of Nd:YAG laser and it is found to be 1.4 times that of potassium dihydrogen phosphate (KDP).

Effect of pulsed and continuous ultrasound on structural and magnetic properties of nano-sized Ni0.4Cu0.2Zn0.4Fe2O4 ferrite

NASA Astrophysics Data System (ADS)

Hassen, Harzali; Adel, Megriche; Arbi, Mgaidi

2018-03-01

Ultrasound-assisted co-precipitation has been used to prepare nano-sized Ni0.4Cu0.2Zn0.4Fe2O4 ferrite. Continuous (C-US) and pulsed (P-US) ultrasound modes are used at constant frequency = 20 kHz, reaction time = 2 h and pulse durations of 10 s on and 10 s off. All experiments were conducted at two temperatures 90 and 100°C. Samples were characterized by X-ray diffraction (XRD), Fourier transform spectroscopy (FT-IR), N2 adsorption isotherms at 77 k analysis (BET), transmission electron microscopy (TEM) and vibrating sample magnetometry (VSM) techniques. A nanocrystalline single-phase with particle size in the range 12-18 nm is obtained in both modes: continuous and pulsed ultrasound mode. FT-IR measurements show two absorption bands assigned to the tetrahedral and octahedral vibrations (ν1 and ν2) characteristics of cubic spinel ferrite. The specific surface area (S BET) is in the range of 110-140 m2 g-1 and an average pore size between 5.5 and 6.5 nm. The lowest values are obtained in pulsed mode. Finally, this work shows that the magnetic properties are affected by the ultrasound conditions, without affecting the particle shape. The saturation magnetization (Ms) values obtained for all samples are comparable. In P-US mode, the saturation magnetization (Ms) increases as temperature increases. Moreover, P-US mode opens a new avenue for synthesis of NiCuZn ferrites.

Thermal decomposition of ammonium perchlorate in the presence of Al(OH)(3)·Cr(OH)(3) nanoparticles.

PubMed

Zhang, WenJing; Li, Ping; Xu, HongBin; Sun, Randi; Qing, Penghui; Zhang, Yi

2014-03-15

An Al(OH)(3)·Cr(OH)(3) nanoparticle preparation procedure and its catalytic effect and mechanism on thermal decomposition of ammonium perchlorate (AP) were investigated using transmission electron microscopy (TEM), X-ray diffraction (XRD), thermogravimetric analysis and differential scanning calorimetry (TG-DSC), X-ray photoelectron spectroscopy (XPS), and thermogravimetric analysis and mass spectroscopy (TG-MS). In the preparation procedure, TEM, SAED, and FT-IR showed that the Al(OH)(3)·Cr(OH)(3) particles were amorphous particles with dimensions in the nanometer size regime containing a large amount of surface hydroxyl under the controllable preparation conditions. When the Al(OH)(3)·Cr(OH)(3) nanoparticles were used as additives for the thermal decomposition of AP, the TG-DSC results showed that the addition of Al(OH)(3)·Cr(OH)(3) nanoparticles to AP remarkably decreased the onset temperature of AP decomposition from approximately 450°C to 245°C. The FT-IR, RS and XPS results confirmed that the surface hydroxyl content of the Al(OH)(3)·Cr(OH)(3) nanoparticles decreased from 67.94% to 63.65%, and Al(OH)3·Cr(OH)3 nanoparticles were limitedly transformed from amorphous to crystalline after used as additives for the thermal decomposition of AP. Such behavior of Al(OH)(3)·Cr(OH)(3) nanoparticles promoted the oxidation of NH3 of AP to decompose to N2O first, as indicated by the TG-MS results, accelerating the AP thermal decomposition. Copyright © 2014 Elsevier B.V. All rights reserved.

Kinetics and thermodynamics studies on the BMP-2 adsorption onto hydroxyapatite surface with different multi-morphological features.

PubMed

Lu, Zhiwei; Huangfu, Changxin; Wang, Yanying; Ge, Hongwei; Yao, Yao; Zou, Ping; Wang, Guangtu; He, Hua; Rao, Hanbing

2015-01-01

The effect of the surface topography on protein adsorption process is of great significance for designing hydroxyapatite (HA) ceramic material surfaces. In this work, three different topographies of HA materials HA-sheet, HA-rod, and HA-whisker were synthesized and testified by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), Brunauer-Emmett-Teller (BET) and a field emission scanning electron microscopy (FE-SEM). We have systematically investigated the adsorption kinetics and thermodynamics of bone morphogenetic proteins (BMP-2) on the three different topography surfaces of HA, respectively. The results showed that the maximum adsorption capacities of HA-sheet, HA-rod and HA-whisker were (219.96 ± 10.18), (247.13 ± 12.35), and (354.67 ± 17.73) μg · g(-1), respectively. Kinetic parameters, rate constants, equilibrium adsorption capacities and related correlation coefficients, for each kinetic model were calculated as well as discussed. It demonstrated that the adsorption of BMP-2 onto HA could be described by the pseudo second-order equation. Adsorption of BMP-2 onto HA followed the Langmuir isotherm. It confirmed that compared with other samples HA-whisker had more adsorption sites for its high specific surface area which could provide more opportunities for protein molecules. The adsorption processes were endothermic (ΔH > 0), spontaneous (ΔG < 0) and entropy increasing (ΔS > 0). A possible adsorption mechanism has been proposed. In addition, the BMP-2 could be adsorbed to the surface which existed slight conformational changes by FT-IR. Copyright © 2015 Elsevier B.V. All rights reserved.

Kramers-Kronig method for determination of optical properties of PZT nanotubes fabricated by sol-gel method and porous anodic alumina with high aspect ratio

NASA Astrophysics Data System (ADS)

Pakizeh, Esmaeil; Moradi, Mahmood

2018-03-01

Ferroelectric Pb(ZrTi)O3 (PZT) nanotubes were prepared by sol-gel method and porous anodic alumina (PAA) membrane using spin-coating technique. This method is based on filling-pyrolysis-filling process and the use of one-stage alumina membranes. One of the advantages of this method is its rapidity, which takes only 1 h time before the calcination step. The effect of repeated pores filling was investigated to get the required size of nanotubes. The field emission scanning electron microscope (FE-SEM) images were shown that the PZT nanotubes have inner diameters in the range of 65-90 nm and length of about 50-60 μm. This means that the samples have a significant aspect ratio (700-800). Also the FE-SEM image confirmed that the highly ordered, hexagonally distributed PAA membranes with the pore diameter about 140-150 nm were formed. The X-ray diffraction (XRD) results showed that the PZT nanotubes have a tetragonal structure. The metal oxide bands like ZrO6 and TiO6 of the final PZT nanotubes were detected by Fourier transform infrared (FT-IR) analysis and confirmed the formation of perovskite structure. By using FT-IR spectroscopy and Kramers-Kronig transformation method, the optical constants like real 𝜀1(ω) and imaginary 𝜀2(ω) parts of dielectric function, extinction coefficient k(ω) and refractive index n(ω) were determined. It was shown that the optical constants of PZT nanotubes are different from PZT nanoparticles.

Highly efficient removal of chlorotetracycline from aqueous solution using graphene oxide/TiO2 composite: Properties and mechanism

NASA Astrophysics Data System (ADS)

Li, Zhaoqian; Qi, Mengyu; Tu, Chunyan; Wang, Weiping; Chen, Jianrong; Wang, Ai-Jun

2017-12-01

The extensive usage of chlorotetracycline (CTC) has caused the persistence of antibiotic residues in aquatic environments, resulting in serious threat to human health and ecosystems. In this study, graphene oxide/titanium dioxide (GO/TiO2) nanocomposite was successfully synthesized via in situ hydrolysis of tetra-n-butyl titanate (Ti(BuO)4) to TiO2 particles on GO sheets and used as adsorbent for efficient adsorptive removal of CTC from aqueous solution. The prepared GO/TiO2 was characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transformed infrared (FT-IR), Raman spectroscopy and X-ray photoelectron (XPS). Adsorption kinetics, isotherms and thermodynamics were systematically investigated to evaluate the adsorption properties of GO/TiO2. Adsorption mechanism was further analyzed by FT-IR, UV-vis and XPS. The results indicated that adsorption kinetics closely followed the pseudo-second order model; the maximum adsorption capacity determined by Langmuir model was 261.10 mg g-1 at 298 K and the thermodynamic studies revealed that the adsorption of CTC onto the GO/TiO2 was a spontaneous and endothermic process. Moreover, the interactions between CTC and GO/TiO2 were presumed to be ligand exchange between CTC and TiO2, while the π-π electron donor-acceptor interaction, hydrogen bond and cation-π bonding were constructed between CTC and GO. Finally, the prepared GO/TiO2 was successfully applied for the efficient removal of CTC from Wu River water.

Preparation and characterization of reinforced papers using nano bacterial cellulose.

PubMed

Tabarsa, Taghi; Sheykhnazari, Somayeh; Ashori, Alireza; Mashkour, Mahdi; Khazaeian, Abolghasem

2017-08-01

The main goal of this work was to reinforce softwood pulp (SP) with bacterial cellulose (BC) to generate a sustainable biocomposite. BC is a nanocellulose, which was anticipated to increase interfacial adhesion between the cellulosic fibers and BC. The organism used was Gluconacetobacter xylinus, which was incubated in a static Hestrin-Schramm culture at 28°C for 14days. The specimens of BC, SP and the reinforced SP with BC were characterized using X-ray diffraction (XRD), FT-IR, FESEM, and physico-mechanical testing. The crystallinity index was found to be 83 and 54% for BC and SP, respectively. FT-IR spectra showed that the composition of BC was fully different from that of SP fibers. Based on FESEM images, one can conclude that BC and softwood fibers do form a good combination with a nonporous structure. BC fibers fill in among the softwood fibers in the sheet. The physical and mechanical properties showed that as the dosage of BC increased, the properties of tensile index, tear index, and burst index greatly improved, while the porosity and the elongation decreased. The reason for the improved mechanical properties can be attributed to the increase of interfibrillar bonding which reduced porosity. This would be due to the high aspect ratio of BC that is capable of connecting between the cellulosic fibers and BC nanofibers, enhancing a large contact surface and therefore producing excellent coherence. This study suggests that BC could be a promising material for reinforcing composites at low loading. Copyright © 2017 Elsevier B.V. All rights reserved.

Preparation and characterization of highly water-soluble magnetic Fe3O4 nanoparticles via surface double-layered self-assembly method of sodium alpha-olefin sulfonate

NASA Astrophysics Data System (ADS)

Li, Honghong; Qin, Li; Feng, Ying; Hu, Lihua; Zhou, Chunhua

2015-06-01

A kind of double-layered self-assembly sodium alpha-olefin sulfonate (AOS) capped Fe3O4 magnetic nanoparticles (Fe3O4-AOS-MN) with highly water-solubility was prepared by a wet co-precipitation method with a pH of 4.8. The resulting Fe3O4-AOS-MN could be dispersed into water to form stable magnetic fluid without other treatments. The result of X-ray diffraction (XRD) indicated that the Fe3O4-AOS-MN maintained original crystalline structure and exhibited a diameter of about 7.5 nm. The iron oxide phase of nanoparticles determined by Raman spectroscopy is Fe3O4. Transmission electron microscopy (TEM) analysis confirmed that the Fe3O4-AOS-MN with spherical morphology were uniformly dispersed in water. FT-IR spectroscopy (FT-IR) and thermo-gravimetric analysis (TGA) verified the successful preparation of Fe3O4-AOS-MN capped with double-layered self-assembled AOS. The corresponding capacities of monolayer chemical absorption and the second-layer self-assembly absorption were respectively 4.07 and 14.71 wt% of Fe3O4-MN, which were much lower than those of other surfactants. Vibrating sample magnetometer (VSM) test result showed Fe3O4-AOS-MN possessed superparamagnetic behavior with the saturation magnetization value of about 44.45 emu/g. The blocking temperature TB of Fe3O4-AOS-MN capped with double-layered AOS is 170 K.

Synthesis, dielectric, conductivity and magnetic studies of LiNi1/3Co1/3Mn(1/3)-xAlxO2 (x = 0.0, 0.02, 0.04 and 0.06) for cathode materials of lithium-ion batteries

NASA Astrophysics Data System (ADS)

Murali, N.; Margarette, S. J.; Veeraiah, V.

Layered structure cathode materials LiNi1/3Co1/3Mn(1/3)-xAlxO2 (x = 0.0, 0.02, 0.04 and 0.06) are prepared by the sol-gel method by adding citric acid as chelating agent. The physical, electrical and magnetic properties of the synthesized materials are systematically discussed using the structural (XRD, FESEM with EDS and FT-IR), impedance (LCR) and electron spin resonance (ESR) measurements. The X-ray diffraction pattern of the synthesized samples possessed the α-NaFeO2 structure of the space group, R 3 bar m , with no evidence of any impurities. The peak intensity ratio I(104)/I(003) increased with Al concentration, which indicated the cation mixing between transition metal layer and lithium layer. The field effect scanning electron microscopy showed the particle size distribution in the range of 230-250 nm and EDS has been analysed for elemental mapping. The local structure is investigated by vibrational spectroscopy in FT-IR study. The impedance studies are characterized by complex impedance spectroscopy (CIS) in the frequency range from 42 Hz to 1 MHz at room temperature (30 °C). The dielectric properties are analyzed in the framework of complex dielectric permittivity and formalism of the complex electric modulus. For these samples, the ESR analysis of magnetic measurements, the degree of cation mixing, is estimated to be Ni2+(3b) = 2.75%.

Antibacterial efficacy of silver nanoparticles and ethyl acetate's metabolites of the potent halophilic (marine) bacterium, Bacillus cereus A30 on multidrug resistant bacteria.

PubMed

Arul, Dhayalan; Balasubramani, Govindasamy; Balasubramanian, Velramar; Natarajan, Thillainathan; Perumal, Pachiappan

2017-10-01

Bacteria are generally responsible for the prevalence of several diseases and pathogenic bacteria are showing increasing resistance to different antibacterials. During the present study an extremophilic bacterium-A30 isolated from the marine waters was characterized and evaluated against four multi-drug resistant (MDR) pathogens, viz; Methicillin-resistant Staphylococcus aureus (MRSA), Escherichia coli, Klebsiella pneumoniae, and Pseudomonas aeruginosa. The sensitivity pattern of the selected pathogens was tested with 31 antibiotics. Among the 47 marine microbial extracts tested on 4-MDR pathogens viz: Methicillin-resistant Staphylococcus aureus (MRSA), E. coli, K. pneumoniae and P. aeruginosa, only our strain A30 strain exhibited highest efficacy. This strain was subsequently subjected to 16S rDNA sequencing which confirmed its allocation as Bacillus cereus. Silver nanoparticle (AgNPs) synthesis and ethyl acetate extraction were performed using the supernatant of B. cereus. The synthesized AgNPs were characterized by UV-Visible, Fourier-transform infra-red (FT-IR), X-ray diffraction (XRD), Field emission-scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDX), and Zeta potential analyses. The presence of functional groups and 13 bioactive components in the ethyl acetate extract were analyzed using FT-IR and gas chromatography-mass spectrometry (GC-MS). The synthesized of AgNPs and the ethyl acetate extract showed preponderant activity against P. aeruginosa and MRSA, respectively. The effects of AgNPs were significant when compared to ethyl acetate extract. Therefore, the halophilic bacterium, B. cereus mediated AgNPs could provide antibacterial applications in the biomedical industries.

Effect of H{sub 3}PW{sub 12}O{sub 40} impregnation on Sn-MCM-41 mesoporous molecular sieves and their physico-chemical properties

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

Nedumaran, D.; Department of Chemistry, RMK Engineering College, Chennai; Pandurangan, A., E-mail: pandurangan_a@yahoo.com

2015-01-15

Graphical abstract: The wide angle XRD shows the well dispersion of HPWA in Sn-MCM-41. It enhances the total acidity of the material. The acidity of the material is correlated with sulfone selectivity. The FT-IR of dibenzothiophene and product shows the formation of sulfone (DBTO{sub 2}). - Highlights: • To enhance the total acidity of Sn-MCM-41 TPA is impregnated. • FT-IR and {sup 31}P MAS NMR confirms the HPWA intact on Sn-MCM-41. • EDAX shows the presence of W and P on Sn-MCM-41. • In ODS formation of sulfone was confirmed by FT-IR and {sup 1}H NMR. • The order ofmore » the catalytic activity of the catalysts are 18HSnM > 28HSnM > 8HSnM. - Abstract: Si-Sn-MCM-41 (Si/Sn = 110) mesoporous molecular sieve was synthesized by hydrothermal sol–gel method using cetyltrimethylammonium bromide (CTAB) as surfactant and SnCl{sub 4}·5H{sub 2}O as a metal source. To generate surface acidity of Si-Sn-MCM-41, 12-tungstophosphoric acid (HPWA) is impregnated on it. The acidity of HPWA loading on Sn-MCM-41 was investigated by temperature programmed desorption of NH{sub 3}. The diffused reflectance spectra of ultraviolet radiation, Raman spectra, FT-IR, {sup 29}Si-MAS NMR and {sup 31}P-MAS NMR techniques revealed the intact of α-Keggin anions on Sn-MCM-41. The wide angle XRD results showed that the HPWA is well dispersed on the support. The total acidity was enhanced with increase in loading of H{sub 3}PW{sub 12}O{sub 40}. The catalytic activity was examined in desulfurization of dibenzothiophene in vapor phase system. Among the catalysts 18% HPWA loaded Sn-MCM-41 showed good catalytic activity in desulfurization at 325 °C. The HPWA/Sn-MCM-41 are a suitable solid acid catalyst for converting organic sulfur into insoluble sulfone.« less

Ethanol electrooxidation in alkaline medium on electrochemically synthesized Co(OH)2/Au composite

NASA Astrophysics Data System (ADS)

Babu, Sreejith P.; Elumalai, Perumal

2017-01-01

Gold (Au), cobalt hydroxide (Co(OH)2) and different Co(OH)2/Au compositions were electro-deposited onto stainless steel by a potentiodynamic method from the respective metal-ion solutions. The deposits were characterized by x-ray diffraction (XRD), scanning electron microscope (SEM) and Fourier transformed infra-red spectroscopy (FT-IR). The XRD and IR data confirmed that the deposits were Au, α-Co(OH)2 or Co(OH)2/Au composites. The SEM observations confirmed that the morphology of the Au was spherical, while the α-Co(OH)2 was flakey with pores. The morphology of the Co(OH)2/Au composites consisted of highly agglomerated Au grains distributed on the Co(OH)2 matrix. The electrocatalytic activity of each of the Au, Co(OH)2 and Co(OH)2/Au-composite electrodes towards ethanol electrooxidation in an alkaline medium was investigated by cyclic voltammetry and chronoamperometry. It turned out that the Co(OH)2/Au-composite electrodes exhibited superior catalytic activity for ethanol electrooxidation compared with the pristine Au or Co(OH)2 electrodes. A peak current density as high as 25 mA cm-2 was exhibited by the Co(OH)2/ Au composite while the Au and Co(OH)2 showed only 0.9 and 13 mA cm-2, respectively. The enhanced conductivity of the Co(OH)2/Au matrix due to the presence of Au, as well as the combined catalytic activity, seemed to be responsible for the superior performance of the Co(OH)2/Au-composite electrodes.

Synthesis and characterization of struvite nano particles

NASA Astrophysics Data System (ADS)

Rathod, K. R.; Jogiya, B. V.; Chauhan, C. K.; Joshi, M. J.

2015-06-01

Struvite, Ammonium Magnesium Phosphate Hexahydrate [(AMPH) - (NH4)MgPO4.6(H2O)], is one of the fascinating inorganic phosphate minerals. Struvite is one of the components of the urinary stones. Struvite occurs as crystallites in urine and grows as a type of kidney stone. In this study, struvite nano particles were synthesized by wet chemical technique. The aqueous solutions containing dissolved Mg(CH3COO)2.4H2O and (NH4)H2PO4 mixed at the Mg/P molar ratio of 1.00. The synthesized struvite nano particles were characterized by XRD, FT-IR, Thermal Analysis and TEM. From XRD, crystal structure of the nano particle was found to be orthorhombic and crystalline size was found to be within 11 to 26 nm. The FT-IR spectrum for the struvite nano particles confirmed the presence of a water molecule and metal-oxygen stretching vibration, O-H stretching and bending, N-H bending and stretching, P-O bending and stretching vibrations. The Thermal Analysis was carried out from room temperature to 900°C. From TEM analysis, particle size was 23 to 30 nm. All the results were compared with bulk struvite.

Copper(II) complex with 6-methylpyridine-2-carboxyclic acid: Experimental and computational study on the XRD, FT-IR and UV-Vis spectra, refractive index, band gap and NLO parameters

NASA Astrophysics Data System (ADS)

Altürk, Sümeyye; Avcı, Davut; Başoğlu, Adil; Tamer, Ömer; Atalay, Yusuf; Dege, Necmi

2018-02-01

Crystal structure of the synthesized copper(II) complex with 6-methylpyridine-2-carboxylic acid, [Cu(6-Mepic)2·H2O]·H2O, was determined by XRD, FT-IR and UV-Vis spectroscopic techniques. Furthermore, the geometry optimization, harmonic vibration frequencies for the Cu(II) complex were carried out by using Density Functional Theory calculations with HSEh1PBE/6-311G(d,p)/LanL2DZ level. Electronic absorption wavelengths were obtained by using TD-DFT/HSEh1PBE/6-311G(d,p)/LanL2DZ level with CPCM model and major contributions were determined via Swizard/Chemissian program. Additionally, the refractive index, linear optical (LO) and non-nonlinear optical (NLO) parameters of the Cu(II) complex were calculated at HSEh1PBE/6-311G(d,p) level. The experimental and computed small energy gap shows the charge transfer in the Cu(II) complex. Finally, the hyperconjugative interactions and intramolecular charge transfer (ICT) were studied by performing of natural bond orbital (NBO) analysis.

Copper(II) complex with 6-methylpyridine-2-carboxyclic acid: Experimental and computational study on the XRD, FT-IR and UV-Vis spectra, refractive index, band gap and NLO parameters.

PubMed

Altürk, Sümeyye; Avcı, Davut; Başoğlu, Adil; Tamer, Ömer; Atalay, Yusuf; Dege, Necmi

2018-02-05

Crystal structure of the synthesized copper(II) complex with 6-methylpyridine-2-carboxylic acid, [Cu(6-Mepic) 2 ·H 2 O]·H 2 O, was determined by XRD, FT-IR and UV-Vis spectroscopic techniques. Furthermore, the geometry optimization, harmonic vibration frequencies for the Cu(II) complex were carried out by using Density Functional Theory calculations with HSEh1PBE/6-311G(d,p)/LanL2DZ level. Electronic absorption wavelengths were obtained by using TD-DFT/HSEh1PBE/6-311G(d,p)/LanL2DZ level with CPCM model and major contributions were determined via Swizard/Chemissian program. Additionally, the refractive index, linear optical (LO) and non-nonlinear optical (NLO) parameters of the Cu(II) complex were calculated at HSEh1PBE/6-311G(d,p) level. The experimental and computed small energy gap shows the charge transfer in the Cu(II) complex. Finally, the hyperconjugative interactions and intramolecular charge transfer (ICT) were studied by performing of natural bond orbital (NBO) analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

Assimilation of NH₄Br in Polyvinyl Alcohol/Poly(N-vinyl pyrrolidone) Polymer Blend-Based Electrolyte and Its Effect on Ionic Conductivity.

PubMed

Parameswaran, V; Nallamuthu, N; Devendran, P; Manikandan, A; Nagarajan, E R

2018-06-01

Biodegradable polymer blend electrolyte based on ammonium based salt in variation composition consisting of PVA:PVP were prepared by using solution casting technique. The obtained films have been analyzed by various technical methods like as XRD, FT-IR, TG-DSC, SEM analysis and impedance spectroscopy. The XRD and FT-IR analysis exposed the amorphous nature and structural properties of the complex formation between PVA/PVP/NH4Br. Impedance spectroscopy analysis revealed the ionic conductivity and the dielectric properties of PVA/PVP/NH4Br polymer blend electrolyte films. The maximum ionic conductivity was determined to be 6.14 × 10-5 Scm-1 for the composition of 50%PVA: 50%PVP: 10% NH4Br with low activation energy 0.3457 eV at room temperature. Solid state battery is fabricated using highest ionic conducting polymer blend as electrolyte with the configuration Zn/ZnSO4 · 7H2O (anode) ∥ 50%PVA: 50%PVP: 10% NH4Br ∥ Mn2O3 (cathode). The observed open circuit voltage is 1.2 V and its performance has been studied.

Synthesis, X-ray diffraction method, spectroscopic characterization (FT-IR, 1H and 13C NMR), antimicrobial activity, Hirshfeld surface analysis and DFT computations of novel sulfonamide derivatives

NASA Astrophysics Data System (ADS)

Demircioğlu, Zeynep; Özdemir, Fethi Ahmet; Dayan, Osman; Şerbetçi, Zafer; Özdemir, Namık

2018-06-01

Synthesized compounds of N-(2-aminophenyl)benzenesulfonamide 1 and (Z)-N-(2-((2-nitrobenzylidene)amino)phenyl)benzenesulfonamide 2 were characterized by antimicrobial activity, FT-IR, 1H and 13C NMR. Two new Schiff base ligands containing aromatic sulfonamide fragment of (Z)-N-(2-((3-nitrobenzylidene)amino)phenyl)benzenesulfonamide 3 and (Z)-N-(2-((4-nitrobenzylidene)amino)phenyl)benzenesulfonamide 4 were synthesized and investigated by spectroscopic techniques including 1H and 13C NMR, FT-IR, single crystal X-ray diffraction, Hirshfeld surface, theoretical method analyses and by antimicrobial activity. The molecular geometry obtained from the X-ray structure determination was optimized Density Functional Theory (DFT/B3LYP) method with the 6-311++G(d,p) basis set in ground state. From the optimized geometry of the molecules of 3 and 4, the geometric parameters, vibrational wavenumbers and chemical shifts were computed. The optimized geometry results, which were well represented the X-ray data, were shown that the chosen of DFT/B3LYP 6-311G++(d,p) was a successful choice. After a successful optimization, frontier molecular orbitals, chemical activity, non-linear optical properties (NLO), molecular electrostatic mep (MEP), Mulliken population method, natural population analysis (NPA) and natural bond orbital analysis (NBO), which cannot be obtained experimentally, were calculated and investigated.

Evaluation of photostability of solid-state nicardipine hydrochloride polymorphs by using Fourier-transformed reflection-absorption infrared spectroscopy - effect of grinding on the photostability of crystal form.

PubMed

Teraoka, Reiko; Otsuka, Makoto; Matsuda, Yoshihisa

2004-11-22

Photostability and physicochemical properties of nicardipine hydrochloride polymorphs (alpha- and beta-form) were studied by using Fourier-transformed reflection-absorption infrared spectroscopy (FT-IR-RAS) of the tablets, X-ray powder diffraction analysis, differential scanning calorimetry (DSC), and color difference measurement. It was clear from the results of FT-IR-RAS spectra after irradiation that nicardipine hydrochloride in the solid state decomposed to its pyridine derivative when exposed to light. The photostability of the ground samples of two forms was also measured in the same manner. The two crystalline forms of the drug changed to nearly amorphous form after 150 min grinding in a mixer mill. X-ray powder diffraction patterns of those ground samples showed almost halo patterns. The nicardipine hydrochloride content on the surface of the tablet was determined based on the absorbance at 1700 cm(-1) attributable to the C=O stretch vibration in FT-IR-RAS spectra before and after irradiation by fluorescent lamp (3500 lx). The photodegradation followed apparently the first-order kinetics for any sample. The apparent photodegradation rate constant of beta-form was greater than that of alpha-form. The ground samples decomposed rapidly under the same light irradiation as compared with the intact crystalline forms. The photodegradation rate constant decreased with increase of the heat of fusion. copyright 2004 Elsevier B.V.

Synthesis of ZnO Photocatalysts Using Various Surfactants

NASA Astrophysics Data System (ADS)

Yao, Chengli; Zhu, Jinmiao; Li, Hongying; Zheng, Bin; Wei, Yanxin

2017-12-01

Zinc oxide (ZnO) nanostructured materials have received significant attention because of their unique physicochemical and electronic properties. In particular, the functional properties of ZnO are owed to its morphology and defect structure. ZnO particles were successfully synthesized by chemical precipitation. CTAB (cetyltrimethylammonium bromide), BS-12 (dodecyl dimethyl betaine) and graphene oxide (GO) were selected as templates to induce the formation of ZnO, respectively. By varying the amount of surfactant added during the synthesis process, the structural properties and the crystalline phase of the synthesized nanospheres were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), ultraviolet and visible spectrophotometry (UV‒Vis). Simultaneously, photo catalytic degradation of Rhodamine B (RhB) was carried out under natural sunlight irradiation while ZnO or ZnO/GO particles were used as catalyst. GO is prone to induce formation of wurtzite hexagonal phase of ZnO. Compared with CTAB and BS-12, ZnO/GO composites had a remarkably photocatalytic degradation.

Hydrocracking of Jatropha Oil over non-sulfided PTA-NiMo/ZSM-5 Catalyst

PubMed Central

Yang, Xiaosong; Liu, Jing; Fan, Kai; Rong, Long

2017-01-01

The PTA-NiMo/ZSM-5 catalyst impregnated with phosphotungstic acid (PTA) was designed for the transformation of Jatropha oil into benzene, toluene, and xylenes (BTX) aromatics. The produced catalyst was characterized by N2 adsorption-desorption, powder X-ray diffraction (XRD), Fourier transform infrared (FT-IR), X-ray photoelectron spectroscopy (XPS), and the temperature-programmed desorption of ammonia (NH3-TPD). The catalytic performance was evaluated by gas chromatography (GC). The liquid products were 70 wt% of the feed oil, and the majority of the liquid products were BTX. The aromatization activity of the catalyst was improved by the addition of PTA and the hierarchical process. The favorable PTA amount was 20 wt% and the yield of BTX was 59 wt% at 380 °C, 3 MPa, H2/oil (v/v) = 1000 and LHSV = 1 h−1 over the PTA20-NiMo/HZ0.5 catalyst (PTA 20 wt%) without sulfurization. PMID:28134313

Synthesis of kenaf cellulose carbamate using microwave irradiation for preparation of cellulose membrane.

PubMed

Gan, Sinyee; Zakaria, Sarani; Chia, Chin Hua; Kaco, Hatika; Padzil, Farah Nadia Mohammad

2014-06-15

Cellulose carbamate (CCs) was produced from kenaf core pulp (KCP) using microwave reactor-assisted method. The effects of urea concentration and reaction time on the formation of nitrogen content in CCs were investigated. The CCs' solubility in LiOH/urea system was determined and its membranes were characterized. As the urea content and reaction time increased, the nitrogen content form in CCs increased which enhanced the CCs' solubility. The formation of CCs was confirmed by Fourier transform infrared spectroscopy (FT-IR) and nitrogen content analysis. The CCs' morphology was examined using Scanning electron microscopy (SEM). The cellulose II and crystallinity index of the membranes were confirmed by X-ray diffraction (XRD). The pore size of the membrane displayed upward trend with respect to the urea content observed under Field emission scanning electron microscope (FESEM). This investigation provides a simple and efficient procedure of CCs determination which is useful in producing environmental friendly regenerated CCs. Copyright © 2014 Elsevier Ltd. All rights reserved.

Antimicrobial cellulosic hydrogel from olive oil industrial residue.

PubMed

Dacrory, Sawsan; Abou-Yousef, Hussein; Abouzeid, Ragab E; Kamel, Samir; Abdel-Aziz, Mohamed S; El-Badry, Mohamed

2018-05-25

The cellulose-based antimicrobial hydrogel was prepared from seed and husk cellulosic fibers of olive industry residues by load silver nanoparticles (AgNPs) onto grafted acrylamide monomer (Am) cellulosic fibers. The grafting approach was the free radical mechanism by utilizing ceric ammonium nitrate (CAN) as initiator in aqueous medium and N,N methylene bisacrylamide (MBAm) as a cross linker. The effect of different grafting conditions on the properties of produced hydrogels has been studied by determining the grafting parameters, i.e. concentration of Am, MBAm, grafting time and temperature to optimize grafting yield (G %), grafting efficiency (GE %), and swelling %. Characterizations of the obtained hydrogels were performed through monitoring swelling behavior, FTIR spectroscopy, SEM, and EDX. AgNPs were grown into the prepared hydrogel. Hydrogel/AgNPs were characterized by FT-IR spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM). The hydrogel loaded AgNPs exhibit high efficient antimicrobial activity against Staphylococcus aureus, Pseudomonas aeruginosa, and Candida albicans. Copyright © 2018. Published by Elsevier B.V.

Functionalized mesoporous silica supported copper(II) and nickel(II) catalysts for liquid phase oxidation of olefins.

PubMed

Nandi, Mahasweta; Roy, Partha; Uyama, Hiroshi; Bhaumik, Asim

2011-12-14

Highly ordered 2D-hexagonal mesoporous silica has been functionalized with 3-aminopropyltriethoxysilane (3-APTES). This is followed by its condensation with a dialdehyde, 4-methyl-2,6-diformylphenol to produce an immobilized Schiff-base ligand (I). This material is separately treated with methanolic solution of copper(II) chloride and nickel(II) chloride to obtain copper and nickel anchored mesoporous materials, designated as Cu-AMM and Ni-AMM, respectively. The materials have been characterized by Fourier transform infrared (FT-IR) and UV-vis diffuse reflectance (DRS) spectroscopy, powder X-ray diffraction (XRD), transmission electron microscopy (TEM), N(2) adsorption-desorption studies and (13)C CP MAS NMR spectroscopy. The metal-grafted mesoporous materials have been used as catalysts for the efficient and selective epoxidation of alkenes, viz. cyclohexene, trans-stilbene, styrene, α-methyl styrene, cyclooctene and norbornene to their corresponding epoxides in the presence of tert-butyl hydroperoxide (TBHP) as the oxidant under mild liquid phase conditions.

Reactivity of Heteropolytungstate and Heteropolymolybdate Metal Transition Salts in the Synthesis of Dimethyl Carbonate from Methanol and CO2

PubMed Central

Aouissi, Ahmed; Al-Deyab, Salem S.; Al-Owais, Ahmad; Al-Amro, Amro

2010-01-01

A series of Keggin-type heteropoly compounds (HPC) having different countercations (Co, Fe) and different addenda atoms (W, Mo) were synthesized and characterized by means of Fourier-Transform Infrared Spectrometer (FT-IR) and X-ray powder diffraction (XRD). The catalytic properties of the prepared catalysts for the dimethyl carbonate (DMC) synthesis from CO2 and CH3OH were investigated. The experimental results showed that the catalytic activity is significantly influenced by the type of the countercation and addenda atoms transition metal. Among the catalysts examined, Co1.5PW12O40 is the most active for the DMC synthesis, owing to the synergetic effect between Co and W. Investigating the effect of the support showed that the least acidic one (Al2O3) enhanced the conversion but decreased the DMC selectivity in favor of that of methyl formate (MF), while that of dimethoxy methane remained stable. PMID:20717536

Hydrothermal preparation of silver telluride nanostructures and photo-catalytic investigation in degradation of toxic dyes

NASA Astrophysics Data System (ADS)

Gholamrezaei, Sousan; Salavati-Niasari, Masoud; Ghanbari, Davood; Bagheri, Samira

2016-01-01

Different morphologies of Ag2Te nanostructures were synthesized using TeCl4 as a new precursor and hydrazine hydrate as reducing agent by a hydrothermal method. Various parameters that affect on morphology and purity of nanostructures were optimized. According to our experiments the best time and temperature for preparation of this nanostructure are 12 h and 120 °C. The photo-catalytic behaviour of nanostructures in presence of UV- visible light for degradation of methyl orange was investigated. Results show that the presence of UV light is necessary for an efficient degradation of dye in aqueous solution. On the other hand, as observations propose the Ag2Te reveal a strong photoluminescence peak at room temperature that could be attributed to high level transition in the semiconductor. Nanostructures were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) techniques and UV-visible scanning spectrometer (UV-Vis).

Visible light assisted photodecolorization of eosin-Y in aqueous solution using hesperidin modified TiO2 nanoparticles

NASA Astrophysics Data System (ADS)

Vignesh, K.; Suganthi, A.; Rajarajan, M.; Sakthivadivel, R.

2012-03-01

Hesperidin a flavanoid, modified TiO2 nanoparticles (Hes-TiO2) was synthesized to improve the visible light driven photocatalytic performance of TiO2. The synthesized nanoparticles were characterized by UV-visible diffuse reflectance spectroscopy (UV-vis-DRS), FT-IR, powder X-ray diffraction (XRD) and scanning electron microscopy (SEM). The photocatalytic activity of Hes-TiO2 was investigated based on the decolorization of eosin-Y under visible light irradiation. Hes-TiO2 showed high efficiency for the decolorization of eosin-Y. The influences of various reaction parameters like effect of pH, catalyst dosage and initial dye concentration on the photocatalytic efficiency were investigated. The adsorption of eosin-Y on Hes-TiO2 was found favorable by the Langmuir approach. The removal percentage of chemical oxygen demand (COD) was determined to evaluate the mineralization of eosin-Y during photodecolorization. Based on the intermediates obtained in the GC-MS spectroscopic technique, a probable degradation mechanism has been proposed.

Self-assembled highly ordered ethane-bridged periodic mesoporous organosilica and its application in HPLC.

PubMed

Huang, Lili; Lu, Juan; Di, Bin; Feng, Fang; Su, Mengxiang; Yan, Fang

2011-09-01

Monodisperse spherical periodic mesoporous organosilicas (PMOs) with ethane integrated in the framework were synthesized and their application as stationary phase for chromatographic separation is demonstrated. The ethane-PMOs were prepared by condensation of 1,2-bis(triethoxysilyl)ethane (BTSE) in basic condition using octadecyltrimethylammonium chloride (C(18)TMACl) as template and ethanol as co-solvent. The morphology and mesoporous structure of ethane-PMOs were controlled under different concentrations of sodium hydroxide (NaOH) and EtOH. The results of scanning electron microscopy (SEM), transmission electron microscopy (TEM), powder X-ray diffraction (XRD), nitrogen sorption measurement, Fourier transform infrared spectroscopy (FT-IR) and elemental analysis showed that ethane-PMOs have spherical morphology, uniform particle distribution, highly ordered pore structure, high surface area and narrow pore-size distribution. The column packed with these materials exhibits good permeability, high chemical stability and good selectivity of mixtures of aromatic hydrocarbons in normal phase high-performance liquid chromatography (HPLC). Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Aminopropyl-functionalized ethane-bridged periodic mesoporous organosilica spheres: preparation and application in liquid chromatography.

PubMed

Li, Chun; Di, Bin; Hao, Weiqiang; Yan, Fang; Su, Mengxiang

2011-01-21

A synthetic approach for synthesizing spherical aminopropyl-functionalized ethane-bridged periodic mesoporous organosilicas (APEPMOs) is reported. The mesoporous material was prepared by a one-step co-condensation of 1,2-bis(triethoxysilyl)ethane (BTSE) and 3-aminopropyltriethoxysilane (APTES) using cetyltrimethylammonium chlorine (C(18)TACl) as a template with the aid of a co-solvent (methanol) in basic medium. The APEPMOs were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), powder X-ray diffraction (XRD), nitrogen sorption measurement, Fourier transform infrared spectroscopy (FT-IR) and elemental analysis. It was shown that this material exhibited spherical morphology, ordered cubic mesostructure and good mechanical strength. The APEPMOs were tested as a potential stationary phase for liquid chromatography (LC) because the column exhibited reduced back pressure. Moreover, they exhibited good chemical stability in basic mobile phase, which can be ascribed to the ethane groups in the mesoporous framework. Copyright © 2010 Elsevier B.V. All rights reserved.

Green synthesis of silver nanoparticles using Terminalia chebula extract at room temperature and their antimicrobial studies

NASA Astrophysics Data System (ADS)

Mohan Kumar, Kesarla; Sinha, Madhulika; Mandal, Badal Kumar; Ghosh, Asit Ranjan; Siva Kumar, Koppala; Sreedhara Reddy, Pamanji

2012-06-01

A green rapid biogenic synthesis of silver nanoparticles (Ag NPs) using Terminalia chebula (T. chebula) aqueous extract was demonstrated in this present study. The formation of silver nanoparticles was confirmed by Surface Plasmon Resonance (SPR) at 452 nm using UV-visible spectrophotometer. The reduction of silver ions to silver nanoparticles by T. chebula extract was completed within 20 min which was evidenced potentiometrically. Synthesised nanoparticles were characterised using UV-vis spectroscopy, Fourier transformed infrared spectroscopy (FT-IR), powder X-ray diffraction (XRD), transmission electron microscopy (TEM) and atomic force microscopy (AFM). The hydrolysable tannins such as di/tri-galloyl-glucose present in the extract were hydrolyzed to gallic acid and glucose that served as reductant while oxidised polyphenols acted as stabilizers. In addition, it showed good antimicrobial activity towards both Gram-positive bacteria (S. aureus ATCC 25923) and Gram-negative bacteria (E. coli ATCC 25922). Industrially it may be a smart option for the preparation of silver nanoparticles.

Sonochemical synthesis of terbium tungstate for developing high power supercapacitors with enhanced energy densities.

PubMed

Sobhani-Nasab, Ali; Rahimi-Nasrabadi, Mehdi; Naderi, Hamid Reza; Pourmohamadian, Vafa; Ahmadi, Farhad; Ganjali, Mohammad Reza; Ehrlich, Hermann

2018-07-01

Sonochemically prepared nanoparticles of terbium tungstate (TWNPs) were evaluated through scanning electron microscopy (SEM), thermogravimetric analysis (TGA), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR), UV-Vis spectroscopy, and the optimal products were further characterized in terms of their electrochemical properties using conventional and continuous cyclic voltammetry (CV, and CCV), galvanostatic charge/discharge technique, and electrochemical impedance spectroscopy (EIS). The CV studies indicated the TWNPs to have specific capacitance (SC) values of 336 and 205 F g -1 at 1 and 200 mV s -1 , and galvanostatic charge-discharge tests revealed the SC of the TWNP-based electrodes to be 300 F g -1 at 1 Ag -1 . Also continuous cyclic voltammetry evaluations proved the sample as having a capacitance retention value of 95.3% after applying 4000 potential cycles. In the light of the results TWNPs were concluded as favorable electrode materials for use in hybrid vehicle systems. Copyright © 2018 Elsevier B.V. All rights reserved.

Mechanochemical synthesis of dodecyl sulfate anion (DS-) intercalated Cu-Al layered double hydroxide

NASA Astrophysics Data System (ADS)

Qu, Jun; He, Xiaoman; Lei, Zhiwu; Zhang, Qiwu; Liu, Xinzhong

2017-12-01

Dodecyl sulfate anion (DS-) was successfully intercalated into the gallery space of Cu-Al layered double hydroxides (LDH) by a non-heating mechanochemical route, in which basic cupric carbonate (Cu2(OH)2CO3) and aluminum hydroxide (Al(OH)3) were first dry ground and then agitated in SDS solution under ambient environment. The organics modified Cu-Al LDH showed good adsorption ability toward 2,4-dichlorophenoxyacetic acid (2, 4-D). The prepared samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), CHS elemental analysis and Scanning electron microscopy (SEM). The LDH precursor prepared by ball-milling could directly react with SDS molecules forming a pure phase of DS- pillared Cu-Al LDH, which was not observed with the LDH product through the ion-exchange of DS- at room temperature. The process introduced here may be applied to manufacture other types of organic modified composites for pollutants removal and other applications.

Size- and morphology-controllable synthesis of MIL-96 (Al) by hydrolysis and coordination modulation of dual aluminium source and ligand systems.

PubMed

Liu, Dandan; Liu, Yunqi; Dai, Fangna; Zhao, Jinchong; Yang, Kang; Liu, Chenguang

2015-10-07

In this paper, an efficient method to fabricate Al-based metal organic framework (Al-MOF) MIL-96 crystals with controllable size and morphology, by mixing other forms of reactants to replace the coordination modulators or capping agents, is presented. The size and morphology of the MIL-96 crystals can be selectively varied by simply altering the ratio of dual reactants via their hydrolysis reaction. All the samples were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), Fourier Transform Infrared (FT-IR) spectroscopy, thermogravimetric analysis (TGA) and nitrogen sorption. Then based on the BFDH theory, a mechanism for the impact of hydrolysis of reactants on the crystal size and morphology is presented and discussed. We also evaluated the performance of these MOFs as sorbents for capturing CO2, and they all show enhanced adsorption properties compared with the bulk material, displaying high adsorption capacities on CO2 at atmospheric pressure and ambient temperature.

Friction behavior of Mg-Al-CO3 layered double hydroxide prepared by magnesite

NASA Astrophysics Data System (ADS)

Wang, Xiaobo; Bai, Zhimin; Zhao, Dong; Zhao, Fuyan

2013-07-01

In this paper, Mg-Al-CO3 LDH was prepared by magnesite under chemical precipitation and hydrothermal methods. In order to improve the dispersion of LDH in base oil, the as-prepared sample was modified with sodium laurate. The obtained material (GMAC-LDH) was characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), differential scanning calorimetry and thermo gravimetric analyzer (DSC-TGA) and scanning electron microscope (SEM). The results show that the modified LDH has platelet morphology with a near hexagon shape. In addition, the tribological properties of GMAC-LDH were evaluated by four-ball friction tester and gear tester. As a lubricant, GMAC-LDH possesses an excellent property on reducing friction and wear of friction pair. The results of friction tests indicated that the friction coefficient, diameter of wear scar and power consumption of the oil with GMAC-LDH was reduced by 11.0%, 8.5% and 2.1% as compared with that of base oil.

Biogenic copper oxide nanoparticles synthesis using Tabernaemontana divaricate leaf extract and its antibacterial activity against urinary tract pathogen

NASA Astrophysics Data System (ADS)

Sivaraj, Rajeshwari; Rahman, Pattanathu K. S. M.; Rajiv, P.; Salam, Hasna Abdul; Venckatesh, R.

2014-12-01

This investigation explains the biosynthesis and characterization of copper oxide nanoparticles from an Indian medicinal plant by an eco-friendly method. The main objective of this study is to synthesize copper oxide nanoparticles from Tabernaemontana divaricate leaves through a green chemistry approach. Highly stable, spherical copper oxide nanoparticles were synthesized by using 50% concentration of Tabernaemontana leaf extract. Formation of copper oxide nanoparticles have been characterized by UV-Vis absorption spectroscopy, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) with energy dispersive X-ray analysis (EDX) and transmission electron microscopy (TEM) analysis. All the analyses revealed that copper oxide nanoparticles were 48 ± 4 nm in size. Functional groups and chemical composition of copper oxide were also confirmed. Antimicrobial activity of biogenic copper oxide nanoparticles were investigated and maximum zone of inhibition was found in 50 μg/ml copper oxide nanoparticles against urinary tract pathogen (Escherichia coli).

A novel orange-red emitting NaCaVO{sub 4}:Sm{sup 3+} phosphor for solid state lighting

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

Biswas, Pankaj, E-mail: pankaj79biswas@gmail.com; Kumar, Vinay, E-mail: vinaykdhiman@yahoo.com; Ntwaeaborwa, O. M.

2016-05-06

The samarium doped NaCaVO{sub 4} phosphor was synthesized by the combustion method. The X-ray powder diffraction (XRD) analysis confirmed that the phosphor powder crystallized as orthorhombic structure belonging to space group Cmcm. From Williamson-Hall analysis the grain size and microstrain in the powder was estimated. The Fourier- transform infrared (FT-IR) studies further validated the formation of vanadate phase of the phosphor. Photoluminescence (PL) study revealed that the phosphor could be efficiently excited by UV-VIS from 200 nm to 500 nm. The 565 nm, 602 nm, 648 nm and 713 nm emissions were ascribed to {sup 4}G{sub 5/2} to {sup 6}H{submore » J} (J = 5/2, 7/2, 9/2 and 11/2) transitions of the Sm{sup 3+} ion. The present material may be explored as a novel phosphor to be excited by UV light emitting diodes (LEDs) chips for solid-state lighting and display applications.« less

Investigation of electrical studies of spinel FeCo2O4 synthesized by sol-gel method

NASA Astrophysics Data System (ADS)

Lobo, Laurel Simon; Kalainathan, S.; Kumar, A. Ruban

2015-12-01

In this work, spinel FeCo2O4 is synthesized by sol-gel method using succinic acid as a chelating agent at 900 °C. The structural, spectroscopic and morphological characterization was carried out by using X-ray diffraction (XRD), Fourier Transform Infrared Spectroscopy (FT-IR) and Scanning Electron Microscopy equipped with Energy Dispersive X-ray spectrometer (SEM-EDX). The M-H loop at room temperature confirms the ferromagnetic property of the sample. The frequency and temperature dependence of dielectric constant (εʹ) and dielectric loss (tan δ) shows the presence of Maxwell-Wagner relaxation in the sample due to the presence of oxygen vacancy. Nyquist plot for frequency and temperature domain signifies the presence of grain effect, grain boundary effect and electrode interface in the conduction process. Electric modulus under suppression of electrode polarization shows the grain and grain boundary effects. The electrode polarization is observed in the lower frequency range of the conductivity graph.

Preparation and Characterization of Self-Reinforced Antibacterial and Oil-Resistant Paper Using a NaOH/Urea/ZnO Solution.

PubMed

Jiao, Li; Ma, Jinxia; Dai, Hongqi

2015-01-01

This paper describes self-reinforced antibacterial and oil-resistant properties that were successfully prepared by surface selective dissolution of filter paper in a NaOH/Urea/ZnO (weight ratio of 8:12:0.25) aqueous solution. The effect of the processing time on the mechanical properties of this paper was evaluated at -12°C. The paper morphologies were characterized using Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS). The oil-resistance and antibacterial properties of the produced paper were also investigated. Excellent mechanical properties were observed for an optimized handling time. The tensile and burst strengths of the modified paper were in excess of 100% of the original. Meanwhile, the treated paper was completely oil-resistant within 24 h and demonstrated good antibacterial properties when exposed to Staphylococcus aureus. The traces of residual zinc oxide were found to be safe for food.

Improvement of the stability and activity of immobilized glucose oxidase on modified iron oxide magnetic nanoparticles

NASA Astrophysics Data System (ADS)

Abbasi, Mahboube; Amiri, Razieh; Bordbar, Abdol-Kalegh; Ranjbakhsh, Elnaz; Khosropour, Ahmad-Reza

2016-02-01

Immobilized proteins and enzymes are widely investigated in the medical field as well as the food and environmental fields. In this study, glucose oxidase (GOX) was covalently immobilized on the surface of modified iron oxide magnetic nanoparticles (MIMNs) to produce a bioconjugate complex. Transmission electron microscopy (TEM) and X-ray diffraction (XRD) were used to the size, shape and structure characterization of the MIMNs. Binding of GOX to these MIMNs was confirmed by using FT-IR spectroscopy. The stability of the immobilized and free enzyme at different temperature and pH values was investigated by measuring the enzymatic activity. These studies reveal that the enzyme's stability is enhanced by immobilization. Further experiments showed that the storage stability of the enzyme is improved upon binding to the MIMNs. The results of kinetic measurements suggest that the effect of the immobilization process on substrate and product diffusion is small. Such bioconjugates can be considered as a catalytic nanodevice for accelerating the glucose oxidation reaction for biotechnological purposes.

Synthesis of graphene oxide and reduced graphene oxide using volumetric method by a novel approach without NaNO2 or NaNO3

NASA Astrophysics Data System (ADS)

Gunda, Rajitha; Madireddy, Buchi Suresh; Dash, Raj Kishora

2018-02-01

In the present work, graphite was processed to graphene oxide (GO) using modified Hummer's method by volumetric titration approach, without attaining zero temperature and the addition of toxic chemicals (NaNO2/NaNO3). The complete oxidation of graphite to graphene oxide was obtained by controlled addition (volumetric titration) of KMnO4. The addition of higher KMnO4 resulted in partial oxidation and 2-3 mono-layers with less defects/disordered structure of reduced graphene oxide (RGO) sheets were achieved. Samples were analyzed by XRD, FT-IR, Raman analysis, and TEM analysis. X-ray diffraction displayed the oxidized peak of graphene oxide at 11.9° and reduced graphene oxide at 23.8°. The prolonged stability of the synthesized GO with lower mole ratios of oxidizing agent was confirmed from UV-visible spectroscopy. Based on the results, processed graphene oxide is found to be a candidate material for thermally stable capacitor application.

Preparation and Characterization of Self-Reinforced Antibacterial and Oil-Resistant Paper Using a NaOH/Urea/ZnO Solution

PubMed Central

Jiao, Li; Ma, Jinxia; Dai, Hongqi

2015-01-01

This paper describes self-reinforced antibacterial and oil-resistant properties that were successfully prepared by surface selective dissolution of filter paper in a NaOH/Urea/ZnO (weight ratio of 8:12:0.25) aqueous solution. The effect of the processing time on the mechanical properties of this paper was evaluated at -12°C. The paper morphologies were characterized using Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS). The oil-resistance and antibacterial properties of the produced paper were also investigated. Excellent mechanical properties were observed for an optimized handling time. The tensile and burst strengths of the modified paper were in excess of 100% of the original. Meanwhile, the treated paper was completely oil-resistant within 24 h and demonstrated good antibacterial properties when exposed to Staphylococcus aureus. The traces of residual zinc oxide were found to be safe for food. PMID:26465917

Investigation of optical properties and the photocatalytic activity of synthesized YbYO4 nanoparticles and YbVO4/NiWO4 nanocomposites by polymeric capping agents

NASA Astrophysics Data System (ADS)

Pourmasoud, Saeid; Sobhani-Nasab, Ali; Behpour, Mohsen; Rahimi-Nasrabadi, Mehdi; Ahmadi, Farhad

2018-04-01

YbVO4 nanoparticles YbVO4/NiWO4 nanocomposites were synthesized by simple and new method. The effect of various polymeric capping agents such as Tween 80, Tween 20 and PEG on the shape and size of YbVO4/NiWO4 nanocomposites were investigated. YbVO4/NiWO4 nanocomposites were analyzed through some techniques including, X-ray diffraction (XRD), Fourier-transform infrared (FT-IR) spectroscopy, vibrating sample magnetometer (VSM), thermogravimetry differential thermal analysis (TG-DTA), transmission electron microscopy (TEM), field emission electron microscopy (FESEM), ultraviolet-visible spectroscopy (UV-Vis), and energy-dispersive X-ray spectroscopy (EDX). This attempt is the first study on the photocatalytic performance of the YbVO4/NiWO4 nanocomposites in various conditions such as size of particles and kind of dyes (rhodamine B (Rh B), methylene blue (MB), methyl orange (MO), and phenol red (Ph R)), under visible light.

Biogenic Silver Nanoparticles by Gelidiella acerosa Extract and their Antifungal Effects

PubMed Central

Vivek, Marimuthu; Kumar, Palanisamy Senthil; Steffi, Sesurajan; Sudha, Sellappa

2011-01-01

The synthesis, characterization and application of biologically synthesized nanomaterials are an important aspect in nanotechnology. The present study deals with the synthesis of silver nanoparticles (Ag-NPs) using the aqueous extract of red seaweed Gelidiella acerosa as the reducing agent to study the antifungal activity. The formation of Ag-NPs was confirmed by UV-Visible Spectroscopy, X-Ray Diffraction (XRD) pattern, Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). The synthesized Ag-NPs was predominately spherical in shape and polydispersed. Fourier Transform Infra-Red (FT-IR) spectroscopy analysis showed that the synthesized nano-Ag was capped with bimolecular compounds which are responsible for reduction of silver ions. The antifungal effects of these nanoparticles were studied against Humicola insolens (MTCC 4520), Fusarium dimerum (MTCC 6583), Mucor indicus (MTCC 3318) and Trichoderma reesei (MTCC 3929). The present study indicates that Ag-NPs have considerable antifungal activity in comparison with standard antifungal drug, and hence further investigation for clinical applications is necessary. PMID:23408653

Influence of the ultrasound-assisted synthesis of Cu-BTC metal-organic frameworks nanoparticles on uptake and release properties of rifampicin.

PubMed

Abbasi, Amir Reza; Rizvandi, Maryam

2018-01-01

In this work, we study uptake and release properties of rifampicin (denoted henceforth as Rif) from ultrasound-assisted synthesis Cu-BTC nanoparticles in comparison with bulk Cu-BTC and activated carbon. To explore the absorption ability of the Cu-BTC to Rif, fresh sample of Cu-BTC was immersed in an aqueous solution of Rif and were monitored in real time with UV/vis spectroscopy. Results show that the adsorbed quantity of Rif over nano Cu-BTC (denoted henceforth as I) is much higher than those over a bulk Cu-BTC (denoted henceforth as II) and activated carbon. In compound I and all of the nano-MOFs the channel length is decreased so that the amount of adsorption is increased a little. The samples were characterized with X-ray powder diffraction (XRD), Scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), and UV/vis spectroscopy. Copyright © 2017 Elsevier B.V. All rights reserved.

Evaluation of calcination temperature and phase composition ratio for new hyroxyapatite

NASA Astrophysics Data System (ADS)

Salimi, M. N. Ahmad; Chin, H. S.

2017-10-01

The demand of production of hydroxyapatite (HA) has been increasing for the purpose of medical and dental application. HA possesses the excellent properties leads to the priority choice for ceramic bone replacement. Synthesis route by wet chemical precipitation is commonly practised in industrial scale. Calcium hydroxide and Orthophosphoric acid are the precursors for production scale. The synthesis of HA is conducted by varying the synthetic condition: stirring rate, calcium-phosphate and calcination temperature. This paper is focused on the properties of HA produced by regulating the synthetic condition so that the qualities of HA can be well performed. Characterization studies were also carried out by Fourier Transform Infrared Spectroscopy (FT-IR) for functional group identification, Scanning Electron Microscope (SEM) for surface morphology analysis and X-Ray Diffraction (XRD) for phase composition and crystallinity respectively. Narrow particle size distribution contributed to better quality of hydroxyapatite for bone replacement. Both calcium-phosphate ratio and calcination temperature would affect the phase composition of calcium phosphate.

Synthesis and characterization of curcumin loaded PLA-Hyperbranched polyglycerol electrospun blend for wound dressing applications.

PubMed

Perumal, Govindaraj; Pappuru, Sreenath; Chakraborty, Debashis; Maya Nandkumar, A; Chand, Dillip Kumar; Doble, Mukesh

2017-07-01

This study is aimed to develop curcumin (Cur) incorporated electrospun nanofibers of a blend of poly (lactic acid) (PLA) and hyperbranched polyglycerol (HPG) for wound healing applications. Both the polymers are synthesized and fabricated by electrospinning technique. The produced nanofibers were characterized by Scanning Electron Microscopy (SEM), X-Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FT-IR), Differential Scanning Colorimetry (DSC) and Thermogravimetric Analysis (TGA). Electrospun scaffolds (PLA/HPG/Cur) exhibits very high hydrophilicity, high swelling and drug uptake and promotes better cell viability, adhesion and proliferation when compared to PLA/Cur electrospun nanofibers. Biodegradation study revealed that the morphology of the nanofibers were unaffected even after 14days immersion in Phosphate Buffered Saline. In vitro scratch assay indicates that migration of the cells in the scratch treated with PLA/HPG/Cur is complete within 36h. These results suggest that PLA/HPG/Cur nanofibers can be a potential wound patch dressing for acute and chronic wound applications. Copyright © 2017 Elsevier B.V. All rights reserved.

Gelator-polysaccharide hybrid hydrogel for selective and controllable dye release.

PubMed

Li, Ping; Dou, Xiao-Qiu; Tang, Yi-Tian; Zhu, Shenmin; Gu, Jiajun; Feng, Chuan-Liang; Zhang, Di

2012-12-01

In this paper, 1,4-bi(phenylalanine-diglycol)-benzene (PDB) based Low-Molecular-Weight-Gelator (LMWG) hydrogels are modified using hydrophilic polysaccharide (sodium alginate). A set of techniques including Fourier transform infrared (FT-IR) spectroscopy, (1)H Nuclear Magnetic Resonance ((1)H NMR), X-ray powder diffraction (XRD), Ultraviolet-Visible (UV-Vis), and circular dichroism (CD) had confirmed a β-turn arrangement of PDB gelators and a semi-interpenetrating network (semi-IPN), which was formed through hydrogen bonds between LMWG fibers and polysaccharide chains. The evaluation of physicochemical properties of hydrogels indicates that gelator-polysaccharide hybrid hydrogels possess better mechanical and water retention properties than LMWG hydrogels. The release study of dyes (model drug) from both LMWG and hybrid hydrogels was carried out. Compared with PDB based hydrogels, hybrid hydrogels show a selective and controllable release property for certain dyes. The results suggest LMWG-polysaccharide hybrid gels may find potential applications as promising drug delivery vehicles for drug molecules. Copyright © 2012 Elsevier Inc. All rights reserved.

Self-healing Li-Al layered double hydroxide conversion coating modified with aspartic acid for 6N01 Al alloy

NASA Astrophysics Data System (ADS)

Zhang, Caixia; Luo, Xiaohu; Pan, Xinyu; Liao, Liying; Wu, Xiaosong; Liu, Yali

2017-02-01

A self-healing Li-Al layered double hydroxide conversion coating (LCC) modified with aspartic acid (ALCC) was prepared on 6N01 Al alloy for corrosion protection. Scanning electron microscopy (SEM) showed that a compact thin film has been successfully formed on the alloy. X-ray diffraction (XRD) and FT-IR spectra proved that species of aspartic acid anions were successfully intercalated into LCC. Potentiodynamic polarization, electrochemical impedance spectroscopy (EIS) and neutral salt spray (NSS) testing showed that the resultant ALCC could provide effective corrosion protection for the Al alloy. During immersion of the ALCC-coated alloy in 3.5% NaCl solution, new film was formed in the area of artificially introduced scratch, indicating its self-healing capability. XPS results demonstrated that Cl- anions exchange partial Asp anions according to the change content of element on conversion coating. From the above results, the possible mechanism via exchange/self-assembly was proposed to illustrate the phenomenon of self-healing.

Preparation and characterization of dialdehyde starch by one-step acid hydrolysis and oxidation.

PubMed

Zuo, Yingfeng; Liu, Wenjie; Xiao, Junhua; Zhao, Xing; Zhu, Ying; Wu, Yiqiang

2017-10-01

Dialdehyde starch was prepared by one-step synthesis of acid hydrolysis and oxidation, using corn starch as the raw material, sodium periodate (NaIO 4 ) as the oxidant, and hydrochloric acid (HCl) as the acid solution. The prepared dialdehyde starch was characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), and gel permeation chromatography (GPC). The results confirmed that oxidation occurred between the starch and NaIO 4 . The acid hydrolysis reaction reduced the molecular weight of starch and effectively improved the aldehyde group contents (92.7%). Scanning electron microscope (SEM) analysis indicated that the average particle size decreased after acid hydrolysis and oxidation reaction. X-ray diffraction (XRD) and thermal gravimetric analyzer (TGA) analysis demonstrated that the crystallinity of the obtained dialdehyde starch showed a downward trend and a decelerated thermal decomposition rate. The starch after acid hydrolysis and oxidation exhibited lower hot paste viscosity and higher reactivity. Copyright © 2017. Published by Elsevier B.V.

Synthesis and Characterization of Highly Intercalated Graphite Bisulfate

NASA Astrophysics Data System (ADS)

Salvatore, Marcella; Carotenuto, Gianfranco; De Nicola, Sergio; Camerlingo, Carlo; Ambrogi, Veronica; Carfagna, Cosimo

2017-03-01

Different chemical formulations for the synthesis of highly intercalated graphite bisulfate have been tested. In particular, nitric acid, potassium nitrate, potassium dichromate, potassium permanganate, sodium periodate, sodium chlorate, and hydrogen peroxide have been used in this synthesis scheme as the auxiliary reagent (oxidizing agent). In order to evaluate the presence of delamination, and pre-expansion phenomena, and the achieved intercalation degree in the prepared samples, the obtained graphite intercalation compounds have been characterized by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), X-ray powder diffraction (XRD), infrared spectroscopy (FT-IR), micro-Raman spectroscopy ( μ-RS), and thermal analysis (TGA). Delamination and pre-expansion phenomena were observed only for nitric acid, sodium chlorate, and hydrogen peroxide, while the presence of strong oxidizers (KMnO4, K2Cr2O7) led to stable graphite intercalation compounds. The largest content of intercalated bisulfate is achieved in the intercalated compounds obtained from NaIO4 and NaClO3.

Photocatalytic activity of Fe-doped CaTiO₃ under UV-visible light.

PubMed

Yang, He; Han, Chong; Xue, Xiangxin

2014-07-01

The photocatalytic degradation of methylene blue (MB) over Fe-doped CaTiO₃ under UV-visible light was investigated. The as-prepared samples were characterized using X-ray diffraction (XRD), scanning electron microscope (SEM) equipped with an energy dispersive spectrometer (EDS) system, Fourier transform infrared spectra (FT-IR), and UV-visible diffuse reflectance spectroscopy (DRS). The results show that the doping with Fe significantly promoted the light absorption ability of CaTiO₃ in the visible light region. The Fe-doped CaTiO₃ exhibited higher photocatalytic activity than CaTiO₃ for the degradation of MB. However, the photocatalytic activity of the Fe-doped CaTiO₃ was greatly influenced by the calcination temperature during the preparation process. The Fe-doped CaTiO₃ prepared at 500°C exhibited the best photocatalytic activity, with degradation of almost 100% MB (10ppm) under UV-visible light for 180 min. Copyright © 2014. Published by Elsevier B.V.

Green synthesis of the Pd nanoparticles supported on reduced graphene oxide using barberry fruit extract and its application as a recyclable and heterogeneous catalyst for the reduction of nitroarenes.

PubMed

Nasrollahzadeh, Mahmoud; Sajadi, S Mohammad; Rostami-Vartooni, Akbar; Alizadeh, Mohammad; Bagherzadeh, Mojtaba

2016-03-15

Through this manuscript the green synthesis of palladium nanoparticles supported on reduced graphene oxide (Pd NPs/RGO) under the mild conditions through reduction of the graphene oxide and Pd(2+) ions using barberry fruit extract as reducing and stabilizing agent is reported. The as-prepared Pd NPs/RGO was characterized by UV-vis spectroscopy, X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and energy dispersive X-ray spectroscopy (EDS). The Pd NPs/RGO could be used as an efficient and heterogeneous catalyst for reduction of nitroarenes using sodium borohydride in an environmental friendly medium. Excellent yields of products were obtained with a wide range of substrates and the catalyst was recycled multiple times without any significant loss of its catalytic activity. Copyright © 2015 Elsevier Inc. All rights reserved.

Green synthesis of size controllable gold nanoparticles

NASA Astrophysics Data System (ADS)

Mohan Kumar, Kesarla; Mandal, Badal Kumar; Kiran Kumar, Hoskote A.; Maddinedi, Sireesh Babu

2013-12-01

A facile rapid green eco-friendly method to synthesize gold nanoparticles (Au NPs) of tunable size using aqueous Terminalia arjuna fruit extracts has been demonstrated herein. Formation of Au NPs was confirmed by Surface Plasmon Resonance (SPR) study at 528 nm using UV-visible spectrophotometer. The time of reduction, size and morphological variations of Au NPs were studied with varying quantities of T. arjuna fruit aqueous extracts. Synthesized Au NPs were characterized using UV-visible spectroscopy, Fourier transformed infrared spectroscopy (FT-IR), powder X-ray diffraction (XRD), transmission electron microscopy (TEM) and Energy dispersive X-ray spectroscopy (EDAX). Polyphenols responsible for reduction of Au3+ to Au0 were identified using High Performance Liquid Chromatography (HPLC) as ascorbic acid, gallic acid and pyrogallol. The oxidized forms of polyphenols formed coordination with surface of Au NPs which protected their further growth and aggregation. We also propose a plausible mechanism how to tune size and shape of Au NPs by varying the quantity of extracts. Thus obtained Au NPs were stable for more than four months.

Photo-, sono- and sonophotocatalytic degradation of methylene blue using Fe3O4/ZrO2 composites catalysts

NASA Astrophysics Data System (ADS)

Kristianto, Y.; Taufik, A.; Saleh, R.

2017-07-01

In the present work, magnetite material Fe3O4/ZrO2 with various molar ratios was prepared by the two-step method (sol-gel followed by the ultrasonic-assisted method). The as-prepared samples were fairly characterized by various characterization methods, such as X-ray Diffraction (XRD), Vibrating Sample Magnetometer (VSM), Fourier Transform Infrared (FT-IR) and Thermal Gravimetric Analysis (TGA). The catalytic performance of the as-prepared samples was evaluated based on the degradation of methylene blue under UV light, ultrasound and combination of UV and ultrasound irradiation. The results revealed that the sample with Fe3O4:ZrO2 molar ratio of 0.5:1 showed the best catalytic performance under UV, ultrasound and UV + ultrasound irradiation. The degradation of methylene blue follows the order: sonophotocatalytic > sonocatalytic > photocatalytic. In addition, the effect of various scavengers has also been studied. Furthermore, all prepared samples could be used as a convenient recyclable catalyst.

Preparation of silver nano-particles immobilized onto chitin nano-crystals and their application to cellulose paper for imparting antimicrobial activity.

PubMed

Li, Zhihan; Zhang, Ming; Cheng, Dong; Yang, Rendang

2016-10-20

Immobilized silver nano-particles (Ag NPs) possess excellent antimicrobial properties due to their unique surface characteristics. In this paper, immobilized silver nano-particles were synthesized in the presence of chitin nano-crystals (CNC) based on the Tollens mechanism (reduction of silver ion by aldehydes in the chitosan oligosaccharides (COS)) under microwave-assisted conditions. The prepared Ag NPs-loaded CNC nano-composites were then applied onto the paper surface via coating for the preparation of antibacterial paper. Fourier transform infrared (FT-IR) and X-ray diffraction (XRD) results confirmed that the Ag NPs were immobilized onto the CNC. The transmission electron microscope (TEM) and scanning electron microscopy (SEM) results further revealed that the spherical Ag NPs (5-12nm) were well dispersed on the surface of CNC. The coated paper made from the Ag NPs-loaded CNC nano-composites exhibited a high effectiveness of the antibacterial activity against E. coli or S. aureus. Copyright © 2016 Elsevier Ltd. All rights reserved.

A novel flexible room temperature ethanol gas sensor based on SnO2 doped poly-diallyldimethylammonium chloride.

PubMed

Zhan, Shuang; Li, Dongmei; Liang, Shengfa; Chen, Xin; Li, Xia

2013-04-02

A novel flexible room temperature ethanol gas sensor was fabricated and demonstrated in this paper. The polyimide (PI) substrate-based sensor was formed by depositing a mixture of SnO2 nanopowder and poly-diallyldimethylammonium chloride (PDDAC) on as-patterned interdigitated electrodes. PDDAC acted both as the binder, promoting the adhesion between SnO2 and the flexible PI substrate, and the dopant. We found that the response of SnO2-PDDAC sensor is significantly higher than that of SnO2 alone, indicating that the doping with PDDAC effectively improved the sensor performance. The SnO2-PDDAC sensor has a detection limit of 10 ppm at room temperature and shows good selectivity to ethanol, making it very suitable for monitoring drunken driving. The microstructures of the samples were examined by scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscope (TEM) and Fourier transform infrared spectra (FT-IR), and the sensing mechanism is also discussed in detail.

Montmorillonite/graphene oxide/chitosan composite: Synthesis, characterization and properties.

PubMed

Yadav, Mithilesh; Ahmad, Sharif

2015-08-01

The present work reports the successful preparation, thermal and mechanical characterization of high performance films of Na(+) montmorillonite (MMT)/graphene oxide (GO)/chitosan (CS) composite using simple solution mixing evaporation method. The formations of films were verified by Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM), X-ray diffraction (XRD) and Raman spectroscopy. The thermal stability and mechanical properties of these films were investigated by thermogravimetric analysis (TGA) and mechanical testing (Instron 8871). The results obtained from these studies revealed that the composites of chitosan, MMT, and graphene oxide were homogeneous in nature. A synergistic effect of MMT and GO reinforcing on chitosan matrix was observed for the first time, in case of 5 wt.% MMT and 1 wt.% GO. The tensile strength of (5 wt.%) MMT/(1 wt.%) GO/CS composite was formed 9±0.23% and 27±0.25% higher than that of the (1 wt.%) GO/CS composite and chitosan, respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

Novel Blend for Producing Porous Chitosan-Based Films Suitable for Biomedical Applications

PubMed Central

Nady, Norhan; Kandil, Sherif H.

2018-01-01

In this work, a chitosan–gelatin–ferulic acid blend was used in different ratios for preparing novel films that can be used in biomedical applications. Both acetic and formic acid were tested as solvents for the chitosan–gelatin–ferulic acid blend. Glycerol was tested as a plasticizer. The thickness, mechanical strength, static water contact angle and water uptake of the prepared films were determined. Also, the prepared films were characterized using different analysis techniques such as Fourier transform infrared spectroscopy (FT-IR) analysis, X-ray diffraction (XRD), thermal gravimetric analysis (TGA), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM). Acetic acid produced continuous compact surfaces that are not recommended for testing in biomedical applications. The plasticized chitosan–gelatin–ferulic acid blend, using formic acid solvent, produced novel hexagonal porous films with a pore size of around 10–14 µm. This blend is recommended for preparing films (scaffolds) for testing in biomedical applications as it has the advantage of a decreased thickness. PMID:29301357

One-step synthesis of solid state luminescent carbon-based silica nanohybrids for imaging of latent fingerprints

NASA Astrophysics Data System (ADS)

Li, Feng; Li, Hongren; Cui, Tianfang

2017-11-01

Fluorescent carbon-based nanomaterials(CNs) with tunable visible emission are biocompatible, environment friendly and most suitable for various biomedical applications. Despite the successes in preparing strongly fluorescent CNs, preserving the luminescence in solid materials is still challenging because of the serious emission quenching of CNs in solid state materials. In this work, fluorescent carbon and silica nanohybrids (SiCNHs) were synthesized via a simple one-step hydrothermal approach by carbonizing sodium citrate and (3-aminopropyl)triethoxysilane(APTES), and hydrolysis of tetraethyl orthosilicate(TEOS). The resultant SiCNs were characterized through X-ray diffraction (XRD), transmission electron microscopy (TEM), FT-IR, X-ray photoelectron spectroscopy (XPS), and photoluminescence (PL) spectroscopy. The SiCNs exhibited strong fluorescence in both aqueous and solid states. The luminescent solid state SiCNs power were successfully used as a fluorescent labeling material for enhanced imaging of latent fingerprints(LFPs) on single background colour and multi-coloured surfaces substrates in forensic science for individual identification.

Tamoxifen citrate loaded chitosan-gellan nanocapsules for breast cancer therapy: development, characterisation and in-vitro cell viability study.

PubMed

Kathle, Pankaj Kumar; Gautam, Nivedita; Kesavan, Karthikeyan

2018-06-08

The objective of this study was to evaluate the potential of chitosan-gellan nanocapsules (CGNCs) for encapsulation and sustained release of Tamoxifen citrate (TMC) for breast cancer therapy. Polyelectrolyte complex coacervation method was used for production of CGNCs. Interaction studies were conducted by Fourier-transform infra-red (FT-IR), differential scanning colorimetric (DSC), and X-ray diffraction (XRD) to investigate any interaction between drug and excipients. Physicochemical parameters, in vitro drug release and release kinetic were studied. In vitro cell viability study using Michigan Cancer Foundation-7 (MCF-7) breast cancer cells was also investigated. CGNCs had a smooth surface and nanosize range with a positive surface charge and exhibited sustained drug release. Further, TMC loaded CGNCs were found to be more cytotoxic than the free drug in MCF-7. Thus CGNCs may be suitable for breast cancer treatment due to delivering the drug at the site of action for a prolonged period of time.

Bioinspired double polysaccharides-based nanohybrid scaffold for bone tissue engineering.

PubMed

Fan, Tiantang; Chen, Jingdi; Pan, Panpan; Zhang, Yujue; Hu, Yimin; Liu, Xiaocui; Shi, Xuetao; Zhang, Qiqing

2016-11-01

The fabrication of bone scaffolds with interconnected porous structure, adequate mechanical properties and excellent biocompatibility presents a great challenge. Herein, a hybrid nanostructured chitosan/chondroitin sulfate/hydroxyapatite (ChS/CSA/HAP) in situ composite scaffold was prepared by in situ fabrication and freeze-drying technique. The composition and morphology of scaffold were characterized by Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM). It proved that the low crystallinity of HAP crystals were uniformly distributed in ChS/CSA organic matrix and the nanostructured hybrid scaffold exhibited good mechanical property. The biocompatibility and in vitro bioactivity were detected by MTT-assay, maturation (alkaline phosphatase (ALP) activity), Hoechst 33258 and PI fluorescence staining. In vitro tests indicated that the hybrid scaffold not only promoted the adhesion and proliferation of osteoblasts, but also improved the growth of the osteoblasts. Therefore, it is promising for bone repair application in bone tissue engineering. Copyright © 2016 Elsevier B.V. All rights reserved.

Physicochemical properties and micro-structural characteristics in starch from kudzu root as affected by cross-linking.

PubMed

Chen, Boru; Dang, Leping; Zhang, Xiao; Fang, Wenzhi; Hou, Mengna; Liu, Tiankuo; Wang, Zhanzhong

2017-03-15

Kudzu starch was cross-linked with sodium trimetaphosphate (STMP) at different temperatures, time and of STMP concentrations in this work. The cross-linked starches (CLSs) were fractionated further into cross-linked amylose and amylopectin in order to compare the effect of cross-linking on the microstructure. According to scanning electron microscope (SEM), CLSs displayed the resemble appearance of spherical and polygonal shapes like NS. X-ray diffraction (XRD) revealed that amylose of native starch (A), NS and CLS displayed a combination of A-type and B-type structure, while that was not found in amylose of cross-linked starch (CLA). The deconvoluted fourier transform infrared (FT-IR) indicated that crystal structure of kudzu starch was losing with the proceeding of cross-linking reaction. The CLSs exhibited a higher retrogradation and freeze-thaw stability than NS. This was accompanied by a significant decrease in sedimentation, transparency, swelling power and solubility. Copyright © 2016 Elsevier Ltd. All rights reserved.

Synthesis and Characterization of Highly Intercalated Graphite Bisulfate.

PubMed

Salvatore, Marcella; Carotenuto, Gianfranco; De Nicola, Sergio; Camerlingo, Carlo; Ambrogi, Veronica; Carfagna, Cosimo

2017-12-01

Different chemical formulations for the synthesis of highly intercalated graphite bisulfate have been tested. In particular, nitric acid, potassium nitrate, potassium dichromate, potassium permanganate, sodium periodate, sodium chlorate, and hydrogen peroxide have been used in this synthesis scheme as the auxiliary reagent (oxidizing agent). In order to evaluate the presence of delamination, and pre-expansion phenomena, and the achieved intercalation degree in the prepared samples, the obtained graphite intercalation compounds have been characterized by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), X-ray powder diffraction (XRD), infrared spectroscopy (FT-IR), micro-Raman spectroscopy (μ-RS), and thermal analysis (TGA). Delamination and pre-expansion phenomena were observed only for nitric acid, sodium chlorate, and hydrogen peroxide, while the presence of strong oxidizers (KMnO 4 , K 2 Cr 2 O 7 ) led to stable graphite intercalation compounds. The largest content of intercalated bisulfate is achieved in the intercalated compounds obtained from NaIO 4 and NaClO 3 .

Achillea millefolium L. extract mediated green synthesis of waste peach kernel shell supported silver nanoparticles: Application of the nanoparticles for catalytic reduction of a variety of dyes in water.

PubMed

Khodadadi, Bahar; Bordbar, Maryam; Nasrollahzadeh, Mahmoud

2017-05-01

In this paper, silver nanoparticles (Ag NPs) are synthesized using Achillea millefolium L. extract as reducing and stabilizing agents and peach kernel shell as an environmentally benign support. FT-IR spectroscopy, UV-Vis spectroscopy, X-ray Diffraction (XRD), Field emission scanning electron microscopy (FESEM), Energy Dispersive X-ray Spectroscopy (EDS), Thermo gravimetric-differential thermal analysis (TG-DTA) and Transmission Electron Microscopy (TEM) were used to characterize peach kernel shell, Ag NPs, and Ag NPs/peach kernel shell. The catalytic activity of the Ag NPs/peach kernel shell was investigated for the reduction of 4-nitrophenol (4-NP), Methyl Orange (MO), and Methylene Blue (MB) at room temperature. Ag NPs/peach kernel shell was found to be a highly active catalyst. In addition, Ag NPs/peach kernel shell can be recovered and reused several times with no significant loss of its catalytic activity. Copyright © 2017 Elsevier Inc. All rights reserved.

SiO2/ZnO Composite Hollow Sub-Micron Fibers: Fabrication from Facile Single Capillary Electrospinning and Their Photoluminescence Properties.

PubMed

Song, Guanying; Li, Zhenjiang; Li, Kaihua; Zhang, Lina; Meng, Alan

2017-02-24

In this work, SiO2/ZnO composite hollow sub-micron fibers were fabricated by a facile single capillary electrospinning technique followed by calcination, using tetraethyl orthosilicate (TEOS), polyvinylpyrrolidone (PVP) and ZnO nanoparticles as raw materials. The characterization results of the scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR) spectra indicated that the asprepared composite hollow fibers consisted of amorphous SiO2 and hexagonal wurtzite ZnO. The products revealed uniform tubular structure with outer diameters of 400-500 nm and wall thickness of 50-60 nm. The gases generated and the directional escaped mechanism was proposed to illustrate the formation of SiO2/ZnO composite hollow sub-micron fibers. Furthermore, a broad blue emission band was observed in the photoluminescence (PL) of SiO2/ZnO composite hollow sub-micron fibers, exhibiting great potential applications as blue light-emitting candidate materials.

Synthesis and characterization of mangenese(III) porphyrin supported on imidazole modified chloromethylated MIL-101(Cr): A heterogeneous and reusable catalyst for oxidation of hydrocarbons with sodium periodate

NASA Astrophysics Data System (ADS)

Zadehahmadi, Farnaz; Tangestaninejad, Shahram; Moghadam, Majid; Mirkhani, Valiollah; Mohammadpoor-Baltork, Iraj; Khosropour, Ahmad R.; Kardanpour, Reihaneh

2014-10-01

In the present work, chloromethylated MIL-101(Cr) modified with imidazole, Im-MIL-101, was applied as a support for immobilizing of tetraphenylporphyrinatomangenese(III) chloride. The imidazole-bound MIL-101, Im-MIL-101, not only used as support for immobilization of manganese porphyrin but also applied as a heterogeneous axial base. The Mn(TPP)Cl@Im-MIL-101 catalyst was characterized by UV-vis, FT-IR, X-ray diffraction (XRD), N2 adsorption, field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray (EDX), elemental analysis and inductively coupled plasma (ICP) methods. The catalytic activity of this new catalytic system was investigated in the alkene epoxidation and alkane hydroxylation using NaIO4 as an oxidant in CH3CN/H2O at room temperature. This heterogeneous catalyst is highly efficient, stable and reusable in the oxidation of hydrocarbons.

Preparation and oil absorption properties of magnetic melamine sponge

NASA Astrophysics Data System (ADS)

Lei, LUO; Jia-qi, HU; Na, LV

2017-12-01

The magnetic melamine sponge (MS-Fe3O4) with magnetic response and high hydrophobicity was fabricated by two-step method. First, the magnetic nano-particles were fixed on the skeleton of melamine sponge (MS) using 3-hydroxytyramine hydrochloride and 1-dodecanethiol, then hydrophobicity modified with octadecyltrichlorosilane (OTS). The structures and chemical compositions of MS and MS-Fe3O4 were characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The wettability of the sample was obtained by using contact angle analysis system. MS-Fe3O4 endowed with outstanding selectivity and excellent oil absorption capacities, which can be widely used in absorbing various sorts of oil. The oil absorption capacities for crude oil, diesel oil, lubricating oil, soybean oil and peanut oil were 71g/g, 51g/g, 62g/g, 54g/g, 57g/g. In addition, MS-Fe3O4 showed excellent recyclability which can be forecasted as an ideal candidate for oil-water separation.

Preparation and luminescent properties of the novel polymer-rare earth complexes composed of Poly(ethylene-co-acrylic acid) and Europium ions

NASA Astrophysics Data System (ADS)

Wu, Yuewen; Hao, Haixia; Wu, Qingyao; Gao, Zihan; Xie, Hongde

2018-06-01

A series of novel polymer-rare earth complexes with Eu3+ ions have been synthesized and investigated successfully, including the binary complexes containing the single ligand poly(ethylene-co-acrylic acid) (EAA) and the ternary complexes using 1,10-phenanthroline (phen), dibenzoylmethane (DBM) or thenoyltrifluoroacetone (TTA) as the second ligand. Their structures have been characterized by Fourier transform infrared spectroscopy (FT-IR), elemental analysis and X-ray diffraction (XRD), which confirm that both EAA and small molecules participate in the coordination reaction with rare earth ions, and they can disperse homogeneously in the polymer matrixes. Both ultraviolet-visible (UV-vis) absorption and photoluminescence tests for the complexes have been recorded. The relationship between fluorescence intensity of polymer-rare earth complexes and the quantity of ligand EAA has been studied and discussed. The films casted from the complexes solution can emit strong characteristic red light under UV light excitation. All these results suggest that the complexes possess potential application as luminescent materials.

Effects of drying processes on starch-related physicochemical properties, bioactive components and antioxidant properties of yam flours.

PubMed

Chen, Xuetao; Li, Xia; Mao, Xinhui; Huang, Hanhan; Wang, Tingting; Qu, Zhuo; Miao, Jing; Gao, Wenyuan

2017-06-01

The effects of five different drying processes, air drying (AD), sulphur fumigation drying (SFD), hot air drying (HAD), freeze drying (FD) and microwave drying (MWD) for yams in terms of starch-related properties and antioxidant activity were studied. From the results of scanning electron microscopy (SEM), polarized optical microscopy (POM), X-ray diffraction (XRD), and Fourier transform infrared (FT-IR), the MWD sample was found to contain gelatinized starch granules. The FD yam had more slow digestible (SDS) and resistant starches (RS) compared with those processed with other modern drying methods. The bioactive components and the reducing power of the dried yams, were lower than those of fresh yam. When five dried samples were compared by principal component analysis, the HAD and SFD samples were observed to have the highest comprehensive principal component values. Based on our results, HAD would be a better method for yam drying than the more traditional SFD. Copyright © 2016 Elsevier Ltd. All rights reserved.

Immobilization of bacterial S-layer proteins from Caulobacter crescentus on iron oxide-based nanocomposite: synthesis and spectroscopic characterization of zincite-coated Fe₂O₃ nanoparticles.

PubMed

Habibi, Neda

2014-05-05

Zinc oxide was coated on Fe2O3 nanoparticles using sol-gel spin-coating. Caulobacter crescentus have a crystalline surface layer (S-layer), which consist of one protein or glycoprotein species. The immobilization of bacterial S-layers obtained from C. crescentus on zincite-coated nanoparticles of iron oxide was investigated. The SDS PAGE results of S-layers isolated from C. crescentus showed the weight of 50 KDa. Nanoparticles of the Fe2O3 and zinc oxide were synthesized by a sol-gel technique. Fe2O3 nanoparticles with an average size of 50 nm were successfully prepared by the proper deposition of zinc oxide onto iron oxide nanoparticles surface annealed at 450 °C. The samples were characterized by field-emission scanning electron microscope (FESEM), atomic force microscopy (AFM), powder X-ray diffraction (XRD) and Fourier-transform infrared spectroscopy (FT-IR). Copyright © 2014 Elsevier B.V. All rights reserved.

Fabrication, characterization and application of pectin degrading Fe3O4-SiO2 nanobiocatalyst.

PubMed

Seenuvasan, Muthulingam; Malar, Carlin Geor; Preethi, Sridhar; Balaji, Nagarajan; Iyyappan, Jeyaraj; Kumar, Madhava Anil; Kumar, Kannaiyan Sathish

2013-05-01

The covalent binding of pectinase onto amino functionalized silica-coated magnetic nanoparticles (CSMNPs) through glutaraldehyde activation was investigated for nanobiocatalyst fabrication. The average particle size and morphology of the nanoparticles were characterized using transmission electron microscopy (TEM). The statistical analysis for TEM image suggests that the coating and binding process did not cause any significant change in size of MNPs. The morphological and phase change of the magnetic nanoparticles (MNPs) after various coatings and immobilization were characterized by X-ray diffraction (XRD) studies. The various surface modifications and pectinase binding onto nanoparticles were confirmed by Fourier transform infrared (FT-IR) spectroscopy. The maximum activity of immobilized pectinase was obtained at its weight ratio of 19.0×10(-3) mg bound pectinase/mg CSMNPs. The pH, temperature, reusability, storage ability and kinetic studies were established to monitor their improved stability and activity of the fabricated nanobiocatalyst. Furthermore, the application was extended in the clarification of Malus domestica juice. Copyright © 2013 Elsevier B.V. All rights reserved.

Syntheses, crystal structures and photoluminescence properties of five Cd/Zn-organic frameworks

NASA Astrophysics Data System (ADS)

Li, Qing; Xue, Dong-Xu; Zhang, Yu-Feng; Zhang, Zong-Hui; Gao, Ziwei

2018-07-01

Luminescent metal-organic frameworks (MOFs) have displayed extensively potential applications for photocatalysis, photoluminescence, electroluminescence, chemical sensors et al. Herein, five new Cd/Zn-organic frameworks of [Cd(HL)C2H5OH] (1), [Cd(HL)(2,2‧-Bpy)H2O] (2), [Cd2(HL)2(Phen)2] (3), [Zn(HL)BIMB] (4), [Cd3(HL)3(4,4‧-Bpy)DMF]·(H2O) (5) have been deliberately constructed via solvothermal reactions of d10 transition metal salts, i.e. Cd(NO3)2•4H2O or Zn(NO3)2·6H2O, and a V-shaped semi-rigid organic linker of 4,4'-(hydroxymethanediyl) dibenzoic acid (H3L) along with the auxiliary poly-nitrogen ligands of 2,2‧-Bpy(2,2‧-bipyridine), Phen(phenanthroline), BIMB(1,1‧-benzene-1,4-diyldimethanediyl-bis-1H-imidazole) and 4,4‧-Bpy(4,4‧-bipyridine). The crystal structures of compounds 1-5 were precisely determined by single-crystal X-ray diffraction (SC-XRD), Powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FT-IR) and Thermogravimetic analysis (TGA). As revealed by SC-XRD, the isolated 1 presents a 2-periodic framework encompassing side-by-side channel-typed helical tubes. Compounds 2-4 display Z-shaped 1-periodic single chains, concomitant with twin chains and tubular structure, respectively. Interestingly, compound 5 demonstrates a two-fold interpenetrated 3-periodic skeleton in the presence of a rigid pillar of 4,4‧-Bpy. Additionally, photoluminescence properties of 1-5 were lastly investigated.

Green way genesis of silver nanoparticles using multiple fruit peels waste and its antimicrobial, anti-oxidant and anti-tumor cell line studies

NASA Astrophysics Data System (ADS)

Naganathan, Kiruthika; Thirunavukkarasu, Somanathan

2017-04-01

Green synthesis of silver nanoparticles (SNP) opens a new path to kill and prevent various infectious diseases and also tumor. In this study, we have synthesized silver nanoparticles using multiple fruit peel waste (pomegranate, orange, banana and apple (POBA)). The primarily nanoparticles formation has been confirmed by the color change. The synthesized SNP were analyzed by various physicochemical techniques such as UV- Visible spectroscopy, x-ray diffraction (XRD), fourier transform infra red (FT-IR) spectroscopy and transmission electron microscope (TEM). The formation of SNP was confirmed by its absorbance peak observed at 430 nm in UV-Visible spectrum. Further, the obtained SNP were identified by XRD and TEM, respectively to know the crystalline nature and size and shape of the particles. The activities of SNP were checked with human pathogens (Salmonella, E.coli and Pseudomonas), plant pathogen (Fusarium) and marine pathogen (Aeromonas hydrophila) and also studied the scavenging effect and anticancer properties against MCF-7 cell lines. This studies proves that the SNP prepared from fruit waste peel extract approach appears extremely fast, cost efficient, eco-friendly and alternative for conventional methods of SNP synthesis to promote the usage of these nanoparticles in medicinal application.

Steam-assisted crystallization of TPA{sup +}-exchanged MCM-41 type mesoporous materials with thick pore walls

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

Chen, Hong Li; Zhang, Kun; Wang, Yi Meng, E-mail: ymwang@chem.ecnu.edu.cn

2012-07-15

Highlights: ► Mesoporous Ti-containing silica with thicker pore walls was synthesized. ► Ion-exchange and steam-assisted crystallization led to MCM-41/MFI composite. ► The introduction of Ti inhibited the formation of separated MFI particles. ► Lower temperature favored retaining mesoporous characteristics and morphology. -- Abstract: Hierarchical MCM-41/MFI composites were synthesized through ion-exchange of as-made MCM-41 type mesoporous materials with tetrapropylammonium bromide and subsequent steam-assisted recrystallization. The obtained samples were characterized by powder X-ray diffraction (XRD), UV–vis diffuse reflectance spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), thermogravimetric analysis, FT-IR, {sup 1}H–{sup 13}C CP/MAS and nitrogen adsorption–desorption. The XRD patterns show thatmore » the MCM-41/MFI composite possesses both ordered MCM-41 phase and zeolite MFI phase. SEM and TEM images indicate that the recrystallized materials retained the mesoporous characteristics and the morphology of as-made mesoporous materials without the formation of bulky zeolite, quite different from the mechanical mixture of MCM-41 and MFI structured zeolite. Among others, lower recrystallization temperature and the introduction of the titanium to the parent materials are beneficial to preserve the mesoporous structure during the recrystallization process.« less

Broadband near-field infrared spectromicroscopy using photothermal probes and synchrotron radiation.

PubMed

Donaldson, Paul M; Kelley, Chris S; Frogley, Mark D; Filik, Jacob; Wehbe, Katia; Cinque, Gianfelice

2016-02-08

In this paper, we experimentally demonstrate the use of infrared synchrotron radiation (IR-SR) as a broadband source for photothermal near-field infrared spectroscopy. We assess two methods of signal transduction; cantilever resonant thermal expansion and scanning thermal microscopy. By means of rapid mechanical chopping (50-150 kHz), we modulate the IR-SR at rates matching the contact resonance frequencies of atomic force microscope (AFM) cantilevers, allowing us to record interferograms yielding Fourier transform infrared (FT-IR) photothermal absorption spectra of polystyrene and cyanoacrylate films. Complementary offline measurements using a mechanically chopped CW IR laser confirmed that the resonant thermal expansion IR-SR measurements were below the diffraction limit, with a spatial resolution better than 500 nm achieved at a wavelength of 6 μm, i.e. λ/12 for the samples studied. Despite achieving the highest signal to noise so far for a scanning thermal microscopy measurement under conditions approaching near-field (dictated by thermal diffusion), the IR-SR resonant photothermal expansion FT-IR spectra measured were significantly higher in signal to noise in comparison with the scanning thermal data.

Structural and magnetic properties of turmeric functionalized CoFe2O4 nanocomposite powder

NASA Astrophysics Data System (ADS)

Mehran, E.; Farjami Shayesteh, S.; Sheykhan, M.

2016-10-01

The structural and magnetic properties of the synthesized pure and functionalized CoFe2O4 magnetic nanoparticles (NPs) are studied by analyzing the results from the x-ray diffraction (XRD), transmission electron microscopy (TEM), FT-IR spectroscopy, thermogravimetry (TG), and vibrating sample magnetometer (VSM). To extract the structure and lattice parameters from the XRD analysis results, we first apply the pseudo-Voigt model function to the experimental data obtained from XRD analysis and then the Rietveld algorithm is used in order to optimize the model function to estimate the true intensity values. Our simulated intensities are in good agreement with the experimental peaks, therefore, all structural parameters such as crystallite size and lattice constant are achieved through this simulation. Magnetic analysis reveals that the synthesized functionalized NPs have a saturation magnetization almost equal to that of pure nanoparticles (PNPs). It is also found that the presence of the turmeric causes a small reduction in coercivity of the functionalized NPs in comparison with PNP. Our TGA and FTIR results show that the turmeric is bonded very well to the surface of the NPs. So it can be inferred that a nancomposite (NC) powder of turmeric and nanoparticles is produced. As an application, the anti-arsenic characteristic of turmeric makes the synthesized functionalized NPs or NC powder a good candidate for arsenic removal from polluted industrial waste water. Project supported by the University of Guilan and the Iran Nanotechnology Initiative Council.

Molecular docking and spectroscopic investigations aided by density functional theory of Parkinson's drug 2-(3,4-dihydroxyphenyl)ethylamine

NASA Astrophysics Data System (ADS)

Sherlin, Y. Sheeba; Vijayakumar, T.; Roy, S. D. D.; Jayakumar, V. S.

2018-05-01

Molecular geometry of Parkinson's drug 2-(3,4-Dihydroxyphenyl)ethylamine hydrochloride (Dopamine, DA) has been evaluated and compared with experimental XRD data. Molecular docking and vibrational spectral analysis of DA have been carried out using FT-Raman and FT-IR spectra aided by Density Functional Theory at B3LYP/6-311++G(d,p). The present investigation deals with the analysis of structural and spectral features responsible for drug activities, nature of hydrogen bonding interactions of the molecule and the correlation of Parkinson's nature with its molecular structural features.

Evaluation of morphological and chemical aspects of different wood species by spectroscopy and thermal methods

NASA Astrophysics Data System (ADS)

Popescu, Maria-Cristina; Popescu, Carmen-Mihaela; Lisa, Gabriela; Sakata, Yusaku

2011-03-01

The aim of this study is to find the most convenient procedure to make an easy differentiation between various kinds of wood. The wood samples used were: fir (Acer alba), poplar (Populus tremula), lime (Tillia cordata), sycamore (Acer pseudoplatanus), sweet cherry (Prunus avium), hornbeam (Carpinus betulus), walnut (Juglans regia), beech (Fagus sylvatica), oak (Quercus robur). The methods of investigation used were FT-IR spectroscopy, X-ray diffraction and thermogravimetry. By FT-IR spectroscopy, was observed that the ratio values of lignin/carbohydrate IR bands for wood decreases with increasing the average wood density, showing a decrease in lignin content. Also, the calculated values of lignin percentage from the FT-IR spectra are in very good correlation with the values from literature. Following the deconvolution process of the X-ray diffraction patterns, it was found that the degree of crystallinity, the apparent lateral crystallite size, the proportion of crystallite interior chains and cellulose fraction tend to increase with increasing of the wood density. Thermal analysis is able to give information about degradation temperatures for the principal components of different wood samples. The shape of DTG curves depends on the wood species that cause the enlargement of the peaks or the maxima of the decomposition step varies at larger or smaller temperatures ranges. The temperatures and weight loss percentage are particular for each kind of wood. This study showed that analytical methods used have the potential to be important sources of information for a quick evaluation of the chemical composition of wood samples.

Preparation and magnetic properties of nano size nickel ferrite particles using hydrothermal method

PubMed Central

2012-01-01

Background Nickel ferrite, a kind of soft magnetic materials is one of the most attracting class of materials due to its interesting and important properties and has many technical applications, such as in catalysis, sensors and so on. In this paper the synthesis of NiFe2O4 nanoparticles by the hydrothermal method is reported and the inhibition of surfactant (Glycerol or Sodium dodecyl sulfate) on the particles growth is investigated. Methods For investigation of the inhibition effect of surfactant on NiFe2O4 particles growth, the samples were prepared in presence of Glycerol and Sodium dodecyl sulfate. The X-ray powder diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), vibrating sample magnetometer (VSM) and inductively coupled plasma atomic emission spectrometer (ICP-AES) techniques were used to characterize the samples. Results The results of XRD and ICP-AES show that the products were pure NiFe2O4 and also nanoparticles grow with increasing the temperature, while surfactant prevents the particle growth under the same condition. The average particle size was determined from the Scherrer's equation and TEM micrographs and found to be in the range of 50-60 nm that decreased up to 10-15 nm in presence of surfactant. The FT-IR results show two absorption bands near to 603 and 490 cm-1 for the tetrahedral and octahedral sites respectively. Furthermore, the saturated magnetization and coercivity of NiFe2O4 nanoparticles were in the range of 39.60 emu/g and 15.67 Qe that decreased for samples prepared in presence of surfactant. As well as, the nanoparticles exhibited a superparamagnetic behavior at room temperature. Conclusions Nanosized nickel ferrite particles were synthesized with and without surfactant assisted hydrothermal methods. The results show that with increasing of temperature, the crystallinity of nanoparticles is increased. In the presence of surfactants, the crystallinity of NiFe2O4 nanoparticles decreased in comparison with surfactant- free prepared samples. All of the nickel ferrite nanoparticles were superparamagnetic at room temperature. Graphical abstract PMID:22462726

Preparation and magnetic properties of nano size nickel ferrite particles using hydrothermal method.

PubMed

Nejati, Kamellia; Zabihi, Rezvanh

2012-03-30

Nickel ferrite, a kind of soft magnetic materials is one of the most attracting class of materials due to its interesting and important properties and has many technical applications, such as in catalysis, sensors and so on. In this paper the synthesis of NiFe2O4 nanoparticles by the hydrothermal method is reported and the inhibition of surfactant (Glycerol or Sodium dodecyl sulfate) on the particles growth is investigated. For investigation of the inhibition effect of surfactant on NiFe2O4 particles growth, the samples were prepared in presence of Glycerol and Sodium dodecyl sulfate. The X-ray powder diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), vibrating sample magnetometer (VSM) and inductively coupled plasma atomic emission spectrometer (ICP-AES) techniques were used to characterize the samples. The results of XRD and ICP-AES show that the products were pure NiFe2O4 and also nanoparticles grow with increasing the temperature, while surfactant prevents the particle growth under the same condition. The average particle size was determined from the Scherrer's equation and TEM micrographs and found to be in the range of 50-60 nm that decreased up to 10-15 nm in presence of surfactant. The FT-IR results show two absorption bands near to 603 and 490 cm-1 for the tetrahedral and octahedral sites respectively. Furthermore, the saturated magnetization and coercivity of NiFe2O4 nanoparticles were in the range of 39.60 emu/g and 15.67 Qe that decreased for samples prepared in presence of surfactant. As well as, the nanoparticles exhibited a superparamagnetic behavior at room temperature. Nanosized nickel ferrite particles were synthesized with and without surfactant assisted hydrothermal methods. The results show that with increasing of temperature, the crystallinity of nanoparticles is increased. In the presence of surfactants, the crystallinity of NiFe2O4 nanoparticles decreased in comparison with surfactant- free prepared samples. All of the nickel ferrite nanoparticles were superparamagnetic at room temperature. GRAPHICAL

Structural and magnetic characterization of La{sub 0.8}Sr{sub 0.2}MnO{sub 3} nanoparticles prepared via a facile microwave-assisted method

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

Moradi, J., E-mail: j_moradi@yahoo.com; Ghazi, M.E.; Ehsani, M.H., E-mail: mhe_ehsani@yahoo.com

2014-07-01

Nanoparticles of La{sub 0.8}Sr{sub 0.2}MnO{sub 3} (LSMO) with different particle sizes are synthesized by a very fast, inexpensive, reproducible, and environmentally friendly method: the microwave irradiation of the corresponding mixture of nitrates. The structural and magnetic properties of the samples are investigated by the X-Ray diffraction (XRD), Fourier transform infra-red (FT-IR) spectroscopy, field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and magnetic (DC magnetization and AC susceptibility) measurements. The XRD study coupled with the Rietveld refinement show that all samples crystallize in a rhombohedral structure with the space group of R−3C. The FT-IR spectroscopy and FE-SEM images indicate formationmore » of the perovskite structure of LSMO. The DC magnetization measurements confirm the decrease in the particle size effects on the magnetic properties, e.g. reduction in the ferromagnetic (FM) moment and increase in the surface spin disorder. Magnetic dynamics of the samples studied by AC magnetic susceptibility shows that the magnetic behavior of the nanometer-sized samples is well-described by the Vogel-Fulcher and critical slowing down laws. Strong interaction between magnetic nanoparticles of LSMO was detected by fitting the experimental data with the mentioned models. - Graphical abstract: Temperature dependence of the magnetization M(T) was measured in the zero-field-cooling (ZFC) and field-cooling (FC) modes at the applied magnetic field of 100 Oe for the La{sub 0.8}Sr{sub 0.2}MnO{sub 3} with different size prepared via a facile microwave-assisted method. - Highlights: • Nanoparticles of La{sub 0.8}Sr{sub 0.2}MnO{sub 3} were synthesized by the microwave irradiation process. • The structural studies show that all samples crystallize in a rhombohedral structure with space group of R−3C. • The DC magnetic studies confirm tuning of the magnetic properties due to the particle size effects. • Magnetic dynamic studied by AC magnetic susceptibility indicate strong interaction between magnetic nanoparticles.« less

Development of curcumin-loaded solid lipid nanoparticles utilizing glyceryl monostearate as single lipid using QbD approach: Characterization and Evaluation of anticancer activity against human breast cancer cell line.

PubMed

Bhatt, Himanshu; Rompicharla, Sri Vishnu Kiran; Komanduri, Neeraja; Shah, Aashma; Paradkar, Sateja; Ghosh, Balaram; Biswas, Swati

2018-05-03

Solid lipid nanoparticles (SLNs) represent an affordable, easily scalable, stable and biocompatible drug delivery system with a high drug to lipid ratio which also improves solubility of poorly soluble drugs. SLNs were developed by using glyceryl monostearate as the single lipid in presence of surfactant Poloxamer 188 and evaluated the efficiency of the SLNs to load the therapeutic cargo, curcumin (CUR). The nano-formulation was optimized by Quality by Design approach to understand the effect of various process parameters on various quality attributes, including drug loadability, particle size and polydispersity. The nanoparticles were characterized using Differential scanning calorimetry (DSC), Fourier Transform Infra-red Spectroscopy (FT-IR) and X-Ray Diffraction (XRD) analysis. These novel SLNs were evaluated for in-vitro anticancer activity using breast adenocarcinoma cells (MDA-MB-231). The optimized formulation had particle size of 226.802±3.92 nm with low polydispersity index of 0.244±0.018. The % encapsulation of CUR into SLNs was found to be 67.88±2.08 %. DSC, FT-IR and XRD confirmed that the CUR was encapsulated stably into the lipid matrix, thereby improving the solubility of the drug. CUR-SLN showed sustained drug release in comparison to the free CUR solution. CUR-SLNs exhibited higher cellular uptake in human breast adenocarcinoma cells compared to free CUR at both 1 and 4 h time points. CUR-SLNs demonstrated decreased cell viability (43.97±1.53%) compared to free CUR (59.33±0.95%) at a concentration of 50 μg/mL after 24 h treatment. Further, treatment of MDA-MB-231 cells with CUR-SLNs for 24 h induced significantly higher apoptosis (37.28±5.3%) in cells compared to the free CUR (21.06±0.97%). The results provide strong rationale for further exploration of the newly developed CUR-SLN to be utilized as a potent chemotherapeutic agent in cancer therapy. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

FT-IR, FT-Raman spectra and DFT calculations of melaminium perchlorate monohydrate

NASA Astrophysics Data System (ADS)

Kanagathara, N.; Marchewka, M. K.; Drozd, M.; Renganathan, N. G.; Gunasekaran, S.; Anbalagan, G.

2013-08-01

Melaminium perchlorate monohydrate (MPM), an organic material has been synthesized by slow solvent evaporation method at room temperature. Powder X-ray diffraction analysis confirms that MPM crystal belongs to triclinic system with space group P-1. FTIR and FT Raman spectra are recorded at room temperature. Functional group assignment has been made for the melaminium cations and perchlorate anions. Vibrational spectra have also been discussed on the basis of quantum chemical density functional theory (DFT) calculations using Firefly (PC GAMESS) version 7.1 G. Vibrational frequencies are calculated and scaled values are compared with experimental values. The assignment of the bands has been made on the basis of the calculated PED. The Mulliken charges, HOMO-LUMO orbital energies are analyzed directly from Firefly program log files and graphically illustrated. HOMO-LUMO energy gap and other related molecular properties are also calculated. The theoretically constructed FT-IR and FT-Raman spectra of MPM coincide with the experimental one. The chemical structure of the compound has been established by 1H and 13C NMR spectra. No detectable signal was observed during powder test for second harmonic generation.

Thiobarbiturate and barbiturate salts of pefloxacin drug: Growth, structure, thermal stability and IR-spectra

NASA Astrophysics Data System (ADS)

Golovnev, Nicolay N.; Molokeev, Maxim S.; Lesnikov, Maxim K.; Sterkhova, Irina V.; Atuchin, Victor V.

2017-12-01

Three new salts of pefloxacin (PefH) with thiobarbituric (H2tba) and barbituric (H2ba) acids, pefloxacinium 2-thiobarbiturate trihydrate, PefH2(Htba)·3H2O (1), pefloxacinium 2-thiobarbiturate, PefH2(Htba) (2) and bis(pefloxacinium barbiturate) hydrate, (PefH2)2(Hba)2·2.56H2O (3) are synthesized and structurally characterized by the X-ray single-crystal diffraction. The structures of 1-3 contain intramolecular hydrogen bonds Csbnd H⋯F, Osbnd H⋯O. Intermolecular hydrogen bonds Nsbnd H⋯O and Osbnd H⋯O form a 2D plane network in 1. In 2 and 3, intermolecular hydrogen bonds Nsbnd H⋯O form the infinite chains. In 1-3, the Htba- and Hba- ions are connected with PefH2+ only by one intermolecular hydrogen bond Nsbnd H⋯O. In 2 and 3, two Htba- and Hba- ions are connected by two hydrogen bonds Nsbnd H⋯O. These pairs form infinite chains. All three structures are stabilized by the π-π interactions of the head-to-tail type between PefH2+ ions. Compounds 2 and 3 are characterized by powder XRD, TG-DSC and FT-IR.

Characterization of prepared In2O3 thin films: The FT-IR, FT-Raman, UV-Visible investigation and optical analysis.

PubMed

Panneerdoss, I Joseph; Jeyakumar, S Johnson; Ramalingam, S; Jothibas, M

2015-08-05

In this original work, the Indium oxide (In2O3) thin film is deposited cleanly on microscope glass substrate at different temperatures by spray pyrolysis technique. The physical properties of the films are characterized by XRD, SEM, AFM and AFM measurements. The spectroscopic investigation has been carried out on the results of FT-IR, FT-Raman and UV-Visible. XRD analysis exposed that the structural transformation of films from stoichiometric to non-stoichiometric orientation of the plane vice versa and also found that, the film is polycrystalline in nature having cubic crystal structure with a preferred grain orientation along (222) plane. SEM and AFM studies revealed that, the film with 0.1M at 500°C has spherical grains with uniform dimension. The complete vibrational analysis has been carried out and the optimized parameters are calculated using HF and DFT (CAM-B3LYP, B3LYP and B3PW91) methods with 3-21G(d,p) basis set. Furthermore, NMR chemical shifts are calculated by using the gauge independent atomic orbital (GIAO) technique. The molecular electronic properties; absorption wavelengths, excitation energy, dipole moment and frontier molecular orbital energies, molecular electrostatic potential energy (MEP) analysis and Polarizability first order hyperpolarizability calculations are performed by time dependent DFT (TD-DFT) approach. The energy excitation on electronic structure is investigated and the assignment of the absorption bands in the electronic spectra of steady compound is discussed. The calculated HOMO and LUMO energies showed the enhancement of energy gap by the addition of substitutions with the base molecule. The thermodynamic properties (heat capacity, entropy, and enthalpy) at different temperatures are calculated and interpreted in gas phase. Crown Copyright © 2015. Published by Elsevier B.V. All rights reserved.

Surface sodium lignosulphonate-immobilized sawdust particle as an efficient adsorbent for capturing Hg2+ from aqueous solution.

PubMed

Gao, Shan; Luo, Tiantian; Zhou, Qi; Luo, Wenjun; Li, Haifeng; Jing, Luru

2018-05-01

In this work, the soluble sodium lignosulphonate (LS Na ) molecules were successfully grafted onto the surface of pine sawdust (PSD) particles to obtain an efficient adsorbent (PSD-LS) for removing Hg 2+ from wastewater. In advance, the surface of sawdust particles were carboxymethylated by chloroacetic acid, the LS Na would be anchored on the surface by a heterogeneous esterification reaction occurred between the hydroxyl of LS Na and carboxyl on PSD surface. The resultant product (PSD-LS) exhibited a good adsorption performance for Hg 2+ with adsorption capacity up to 164.77 mg/g and it was characterized by scanning electron microscope (SEM), energy dispersive X-ray diffraction (EDX), Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD). The effects of pH, contact time, adsorption temperature and initial concentration on the adsorption of Hg 2+ were investigated. Results showed that the pseudo-second-order kinetics and Langmuir isotherm model could describe the adsorption process better. In addition, the composite adsorbent has outstanding reusability with high and stable desorption rates under several continuous cycle. These findings suggested that PSD-LS was a potential adsorbent to remove hazardous metal ions from wastewater. Copyright © 2018 Elsevier Inc. All rights reserved.

A novel green synthesis of Fe3O4-Ag core shell recyclable nanoparticles using Vitis vinifera stem extract and its enhanced antibacterial performance

NASA Astrophysics Data System (ADS)

Venkateswarlu, Sada; Natesh Kumar, B.; Prathima, B.; Anitha, K.; Jyothi, N. V. V.

2015-01-01

We described a novel and eco-friendly method for preparing Fe3O4-Ag core shell nanoparticles (CSNPs) with high magnetism and potent antibacterial activity. The Fe3O4-Ag CSNPs were obtained using waste material of Vitis vinifera (grape) stem extract as the green solvent, reducing and capping agent. The result recorded from X-ray powder diffraction (XRD), UV-vis spectrum, energy dispersive spectroscopy (EDS), Fourier transform infrared spectroscopy (FT-IR) supports the biosynthesis and characterization of Fe3O4-Ag CSNPs. From transmission electron microscopy (TEM) the size of the Fe3O4-Ag nanoparticles was measured below 50 nm; high-resolution TEM (HRTEM) indicates the core shell structure; and selected area electron diffraction (SAED) has revealed polycrystalline nature. Vibrating sample magnetometer (VSM) shows the ferromagnetic nature of Fe3O4-Ag CSNPs at room temperature with saturation magnetization of 15.74 emu/g. Further, these biogenic nanoparticles were highly hazardous to microorganisms. The antibacterial activity of biogenic Fe3O4-Ag CSNPs showed potent inhibitory activity against both Gram-positive and Gram-negative pathogens. These nanoparticles may also be reusable because of its excellent ferromagnetic property.

Improving antiproliferative effect of the anticancer drug cytarabine on human promyelocytic leukemia cells by coating on Fe3O4@SiO2 nanoparticles.

PubMed

Shahabadi, Nahid; Falsafi, Monireh; Mansouri, Kamran

2016-05-01

In this study, Fe3O4@SiO2-cytarabine magnetic nanoparticles (MNPs) were prepared via chemical coprecipitation reaction and coating silica on the surface of Fe3O4 MNPs by Stöber method via sol-gel process. The surface of Fe3O4@SiO2 MNPs was modified by an anticancer drug, cytarabine. The structural properties of the samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Zetasizer analyzer, and transmission electron microscopy (TEM). The results indicated that the crystalline phase of iron oxide NPs was magnetite (Fe3O4) and the average sizes of Fe3O4@SiO2-cytarabine MNPs were about 23 nm. Also, the surface characterization of Fe3O4@SiO2-cytarabine MNPs by FT-IR showed that successful coating of Fe3O4 NPs with SiO2 and binding of cytarabine drug onto the surface of Fe3O4@SiO2 MNPs were through the hydroxyl groups of the drug. The in vitro cytotoxic activity of Fe3O4@SiO2-cytarabine MNPs was investigated against cancer cell line (HL60) in comparison with cytarabine using MTT colorimetric assay. The obtained results showed that the effect of Fe3O4@SiO2-cytarabine magnetic nanoparticles on the cell lines were about two orders of magnitude higher than that of cytarabine. Furthermore, in vitro DNA binding studies were investigated by UV-vis, circular dichroism, and fluorescence spectroscopy. The results for DNA binding illustrated that DNA aggregated on Fe3O4@SiO2-cytarabine MNPs via groove binding. Copyright © 2016 Elsevier B.V. All rights reserved.

Poorly crystalline hydroxyapatite: A novel adsorbent for enhanced fulvic acid removal from aqueous solution

NASA Astrophysics Data System (ADS)

Wei, Wei; Yang, Lei; Zhong, Wenhui; Cui, Jing; Wei, Zhenggui

2015-03-01

In this study, poorly crystalline hydroxyapatite (HAP) was developed as an efficient adsorbent for the removal of fulvic acid (FA) from aqueous solution. Surface functionality, crystallinity, and morphology of the synthetic adsorbent were studied by Fourier-transformation infrared (FT-IR) spectroscopy, powder X-ray diffraction (XRD) and transmission electron microscopy (TEM). The effects of various parameters such as crystallinity of adsorbent, contact time, adsorbent dosage, pH, initial adsorbate concentration, temperature, ionic strength and the presence of alkaline earth metal ions on FA adsorption were investigated. Results indicated that the nanosized HAP calcined at lower temperature was poorly crystalline (Xc = 0.23) and had better adsorption capacity for FA than those (Xc = 0.52, 0.86) calcined at higher temperature. FA removal was increased with increases of adsorbent dosage, temperature, ionic strength and the presence of alkali earth metal ions, but decreased as the pH increased. Kinetic studies showed that pseudo-second-order kinetic model better described the adsorption process. Equilibrium data were best described by Sips models, and the estimated maximum adsorption capacity of poorly crystalline HAP was 90.20 mg/g at 318 K, displaying higher efficiency for FA removal than previously reported adsorbents. FT-IR results revealed that FA adsorption over the adsorbent could be attributed to the surface complexation between the oxygen atom of functional groups of FA and calcium ions of HAP. Regeneration studies indicated that HAP could be recyclable for a long term. Findings of the present work highlight the potential for using poorly crystalline HAP nanoparticles as an effective and recyclable adsorbent for FA removal from aqueous solution.

Synthesis, crystal structure, vibrational spectroscopy, optical properties and theoretical studies of a new organic-inorganic hybrid material: [((CH3)2NH2)(+)]6·[(BiBr6)(3-)]2.

PubMed

Ben Ahmed, A; Feki, H; Abid, Y

2014-12-10

A new organic-inorganic hybrid material, [((CH3)2NH2)(+)]6·[(BiBr6)(3-)]2, has been synthesized and characterized by X-ray diffraction, FT-IR, Raman spectroscopy and UV-Visible absorption. The studied compound crystallizes in the triclinic system, space group P1¯ with the following parameters: a=8.4749(6)(Å), b=17.1392(12)(Å), c=17.1392(12)(Å), α=117.339(0)°, β=99.487(0)°, γ=99.487(0)° and Z=2. The crystal lattice is composed of a two discrete (BiBr6)(3-) anions surrounded by six ((CH3)2NH2)(+) cations. Complex hydrogen bonding interactions between (BiBr6)(3-) and organic cations from a three-dimensional network. Theoretical calculations were performed using density functional theory (DFT) for studying the molecular structure, vibrational spectra and optical properties of the investigated molecule in the ground state. The full geometry optimization of designed system is performed using DFT method at B3LYP/LanL2DZ level of theory using the Gaussian03. The optimized geometrical parameters obtained by DFT calculations are in good agreement with single crystal XRD data. The vibrational spectral data obtained from FT-IR and Raman spectra are assigned based on the results of the theoretical calculations. The energy and oscillator strength calculated by Time-Dependent Density Functional Theory (TD-DFT) results complements with the experimental findings. The simulated spectra satisfactorily coincide with the experimental UV-Visible spectrum. The results show good consistent with the experiment and confirm the contribution of metal orbital to the HOMO-LUMO boundary. Copyright © 2014 Elsevier B.V. All rights reserved.

Spectral analysis of Cu 2+: B 2O 3-ZnO-PbO glasses

NASA Astrophysics Data System (ADS)

Lakshminarayana, G.; Buddhudu, S.

2005-11-01

A new series of heavy metal oxide (PbO) based zinc borate glasses in the chemical composition of (95 - x)B 2O 3-5ZnO- xPbO ( x = 10, 15, 20, 25, 30, 35, 40, 45 and 50 mol%) have been prepared to verify their UV filtering performance. Both direct and indirect optical band gaps ( Eopt) have been evaluated for these glasses. For a reference glass of 45B 2O 3-5ZnO-50PbO, refractive indices at different wavelengths are measured and found the results satisfactorily correlated with the theoretical data upon the computation of Cauchy's constants of A = 1.766029949, B = 159531.024 nm 2 and C = -1.078 × 10 10 nm 4. Measurements concerning X-ray diffraction (XRD), FT-IR, differential scanning colorimeter (DSC) profiles have been carried out for this glass. The FT-IR profile has revealed that the glass has both BO 3 and BO 4 units. From DSC thermogram, glass transition temperature ( Tg), crystallization temperature ( Tc) and melting temperature ( Tm) have been located and from them, other related parameters of the glass have also been calculated. Visible absorption spectra of 45B 2O 3-5ZnO-(50 - x)PbO- xCuO ( x = 0. 1, 0.2, 0.5 and 1.0 mol%) have revealed two absorption bands at around 400 nm ( 2B 1g → 2E g) and 780 nm ( 2B 1g → 2B 2g) of Cu 2+ ions, respectively. Emission bands at 422 and 512 nm are found for the 1 mol% CuO doped glass with excitations at 306 and 332 nm.

Photocatalytic activity of undoped and Ag-doped TiO{sub 2}-supported zeolite for humic acid degradation and mineralization

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

Lazau, C.; Ratiu, C.; National Institute for Research and Development in Microtechnologies, Erou Iancu Nicolae Street, 077190 Bucharest

2011-11-15

Highlights: {yields} Hybrid materials based on natural zeolite and TiO{sub 2} obtained by solid-state reaction. {yields} XRD proved the presence of anatase form of undoped and Ag-doped TiO{sub 2} onto zeolite. {yields} FT-IR spectra evidenced the presence on TiO{sub 2} bounded at the zeolite network. {yields} Ag-doped TiO{sub 2} onto zeolitic matrix exhibited an enhanced photocatalytic activity. -- Abstract: The hybrid materials based on natural zeolite and undoped and Ag-doped TiO{sub 2}, i.e., Z-Na-TiO{sub 2} and Z-Na-TiO{sub 2}-Ag, were successfully synthesized by solid-state reaction in microwave-assisted hydrothermal conditions. Undoped TiO{sub 2} and Ag-doped TiO{sub 2} nanocrystals were previously synthesized bymore » sol-gel method. The surface characterization of undoped TiO{sub 2}/Ag-doped TiO{sub 2} and natural zeolite hybrid materials has been investigated by X-ray diffraction, DRUV-VIS spectroscopy, FT-IR spectroscopy, BET analysis, SEM microscopy and EDX analysis. The results indicated that anatase TiO{sub 2} is the dominant crystalline type as spherical form onto zeolitic matrix. The presence of Ag into Z-Na-TiO{sub 2}-Ag was confirmed by EDX analysis. The DRUV-VIS spectra showed that Z-Na-TiO{sub 2}-Ag exhibited absorption within the range of 400-500 nm in comparison with Z-Na-TiO{sub 2} catalyst. The enhanced photocatalytic activity of Z-Na-TiO{sub 2}-Ag catalyst is proved through the degradation and mineralization of humic acid under ultraviolet and visible irradiation.« less

Interpreting the results of chemical stone analysis in the era of modern stone analysis techniques

PubMed Central

Gilad, Ron; Williams, James C.; Usman, Kalba D.; Holland, Ronen; Golan, Shay; Ruth, Tor; Lifshitz, David

2017-01-01

Introduction and Objective Stone analysis should be performed in all first-time stone formers. The preferred analytical procedures are Fourier-transform infrared spectroscopy (FT-IR) or X-ray diffraction (XRD). However, due to limited resources, chemical analysis (CA) is still in use throughout the world. The aim of the study was to compare FT-IR and CA in well matched stone specimens and characterize the pros and cons of CA. Methods In a prospective bi-center study, urinary stones were retrieved from 60 consecutive endoscopic procedures. In order to assure that identical stone samples were sent for analyses, the samples were analyzed initially by micro-computed tomography to assess uniformity of each specimen before submitted for FTIR and CA. Results Overall, the results of CA did not match with the FTIR results in 56% of the cases. In 16% of the cases CA missed the major stone component and in 40% the minor stone component. 37 of the 60 specimens contained CaOx as major component by FTIR, and CA reported major CaOx in 47/60, resulting in high sensitivity, but very poor specificity. CA was relatively accurate for UA and cystine. CA missed struvite and calcium phosphate as a major component in all cases. In mixed stones the sensitivity of CA for the minor component was poor, generally less than 50%. Conclusions Urinary stone analysis using CA provides only limited data that should be interpreted carefully. Urinary stone analysis using CA is likely to result in clinically significant errors in its assessment of stone composition. Although the monetary costs of CA are relatively modest, this method does not provide the level of analytical specificity required for proper management of patients with metabolic stones. PMID:26956131

Synthesis and characterization of monosodium urate (MSU) nano particles

NASA Astrophysics Data System (ADS)

Tank, Nirali S.; Rathod, K. R.; Parekh, B. B.; Parikh, K. D.; Joshi, M. J.

2016-05-01

In Gout the deposition of crystals of Monosodium Urate (MSU) in various connective tissues and joints occurs, which is very painful with immflamation. The deposition likely to begin with nano particles form and expected to grow in to micro-paricles and hence it is important to synthesize and characrterize MSU nano-particles. The MSU nano particles were synthesized by wet chemical method using NaOH and uric acid (C5H4N4O3) and then characterized by powder XRD, TEM, FT-IR and thermal analysis. From the powder XRD the triclinic structure was found and 40 nm average particle size was estimated by using Scherrer's formula. From TEM the particle size was found to be in the range of 20 to 60 nm. The FT-IR spectrum for the MSU nano particles confirmed the presence of O-H stretching, N-H stretching, N-H rocking, C = O, C = C Enol or Keto and C = N vibrations. The thermal analysis was carried out from room temperature to 900°C. With comparison to the bulk MSU the thermal stability of MSU nano particles was slightly higher and 1.5 water molecules were found to be associated with MSU nano particles. Present results are compared with the bulk MSU.

Enzymatic modification of chitosan by cinnamic acids: Antibacterial activity against Ralstonia solanacearum.

PubMed

Yang, Caifeng; Zhou, Yu; Zheng, Yu; Li, Changlong; Sheng, Sheng; Wang, Jun; Wu, Fuan

2016-06-01

This study aimed to identify chitosan polymers that have antibacterial activity against the bacterial wilt pathogen. The chitosan polymers were enzymatically synthesized using chitosan and five cinnamic acids (CADs): caffeic acid (CA), ferulic acid (FA), cinnamic acid (CIA), p-coumaric acid (COA) and chlorogenic acid (CHA), using laccase from Pleurotus ostreatus as a catalyst. The reaction was performed in a phosphate buffered solution under heterogenous reaction conditions. The chitosan derivatives (CTS-g-CADs) were characterized by FT-IR, XRD, TGA and SEM. FT-IR demonstrated that the reaction products bound covalently to the free amino groups or hydroxyl groups of chitosan via band of amide I or ester band. XRD showed a reduced packing density for grafted chitosan comparing to original chitosan. TGA demonstrated that CTS-g-CADs have a higher thermostability than chitosan. Additionally, chitosan and its derivatives showed similar antibacterial activity. However, the IC50 value of the chitosan-caffeic acid derivative (CTS-g-CA) against the mulberry bacterial wilt pathogen RS-5 was 0.23mg/mL, which was two-fifths of the IC50 value of chitosan. Therefore, the enzymatically synthesized chitosan polymers can be used to control plant diseases in biotechnological domains. Copyright © 2016 Elsevier B.V. All rights reserved.

Modeling and measurements of XRD spectra of extended solids under high pressure

NASA Astrophysics Data System (ADS)

Batyrev, I. G.; Coleman, S. P.; Stavrou, E.; Zaug, J. M.; Ciezak-Jenkins, J. A.

2017-06-01

We present results of evolutionary simulations based on density functional calculations of various extended solids: N-Si and N-H using variable and fixed concentration methods of USPEX. Predicted from the evolutionary simulations structures were analyzed in terms of thermo-dynamical stability and agreement with experimental X-ray diffraction spectra. Stability of the predicted system was estimated from convex-hull plots. X-ray diffraction spectra were calculated using a virtual diffraction algorithm which computes kinematic diffraction intensity in three-dimensional reciprocal space before being reduced to a two-theta line profile. Calculations of thousands of XRD spectra were used to search for a structure of extended solids at certain pressures with best fits to experimental data according to experimental XRD peak position, peak intensity and theoretically calculated enthalpy. Comparison of Raman and IR spectra calculated for best fitted structures with available experimental data shows reasonable agreement for certain vibration modes. Part of this work was performed by LLNL, Contract DE-AC52-07NA27344. We thank the Joint DoD / DOE Munitions Technology Development Program, the HE C-II research program at LLNL and Advanced Light Source, supported by BES DOE, Contract No. DE-AC02-05CH112.

Structural, magnetic and electronic structure properties of Co doped ZnO nanoparticles

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

Kumar, Shalendra, E-mail: shailuphy@gmail.com; School of Materials Science and Engineering, Changwon National University, Changwon, Gyeongnam 641-773; Song, T.K., E-mail: tksong@changwon.ac.kr

Highlights: • XRD and HR-TEM results show the single phase nature of Co doped ZnO nanoparticles. • XMCD and dc magnetization results indicate the RT-FM in Co doped ZnO nanoparticles. • Co L{sub 3,2} NEXAFS spectra infer that Co ions are in 2+ valence state. • O K edge NEXAFS spectra show that O vacancy increases with Co doping in ZnO. - Abstract: We reported structural, magnetic and electronic structure studies of Co doped ZnO nanoparticles. Doping of Co ions in ZnO host matrix has been studied and confirmed using various methods; such as X-ray diffraction (XRD), field emission scanningmore » electron microscopy (FE-SEM), energy dispersed X-ray (EDX), high resolution transmission electron microscopy (HR-TEM), Fourier transform infrared spectroscopy (FT-IR), near edge X-ray absorption fine structure (NEXAFS) spectroscopy, magnetic hysteresis loop measurements and X-ray magnetic circular dichroism (XMCD). From the XRD and HR-TEM results, it is observed that Co doped ZnO nanoparticles have single phase nature with wurtzite structure and exclude the possibility of secondary phase formation. FE-SEM and TEM micrographs show that pure and Co doped nanoparticles are nearly spherical in shape. O K edge NEXAFS spectra indicate that O vacancies increase with Co doping. The Co L{sub 3,2} edge NEXAFS spectra revealed that Co ions are in 2+ valence state. DC magnetization hysteresis loops and XMCD results clearly showed the intrinsic origin of temperature ferromagnetism in Co doped ZnO nanoparticles.« less

Fast Infrared Chemical Imaging with a Quantum Cascade Laser

PubMed Central

2015-01-01

Infrared (IR) spectroscopic imaging systems are a powerful tool for visualizing molecular microstructure of a sample without the need for dyes or stains. Table-top Fourier transform infrared (FT-IR) imaging spectrometers, the current established technology, can record broadband spectral data efficiently but requires scanning the entire spectrum with a low throughput source. The advent of high-intensity, broadly tunable quantum cascade lasers (QCL) has now accelerated IR imaging but results in a fundamentally different type of instrument and approach, namely, discrete frequency IR (DF-IR) spectral imaging. While the higher intensity of the source provides a higher signal per channel, the absence of spectral multiplexing also provides new opportunities and challenges. Here, we couple a rapidly tunable QCL with a high performance microscope equipped with a cooled focal plane array (FPA) detector. Our optical system is conceptualized to provide optimal performance based on recent theory and design rules for high-definition (HD) IR imaging. Multiple QCL units are multiplexed together to provide spectral coverage across the fingerprint region (776.9 to 1904.4 cm–1) in our DF-IR microscope capable of broad spectral coverage, wide-field detection, and diffraction-limited spectral imaging. We demonstrate that the spectral and spatial fidelity of this system is at least as good as the best FT-IR imaging systems. Our configuration provides a speedup for equivalent spectral signal-to-noise ratio (SNR) compared to the best spectral quality from a high-performance linear array system that has 10-fold larger pixels. Compared to the fastest available HD FT-IR imaging system, we demonstrate scanning of large tissue microarrays (TMA) in 3-orders of magnitude smaller time per essential spectral frequency. These advances offer new opportunities for high throughput IR chemical imaging, especially for the measurement of cells and tissues. PMID:25474546

Fast infrared chemical imaging with a quantum cascade laser.

PubMed

Yeh, Kevin; Kenkel, Seth; Liu, Jui-Nung; Bhargava, Rohit

2015-01-06

Infrared (IR) spectroscopic imaging systems are a powerful tool for visualizing molecular microstructure of a sample without the need for dyes or stains. Table-top Fourier transform infrared (FT-IR) imaging spectrometers, the current established technology, can record broadband spectral data efficiently but requires scanning the entire spectrum with a low throughput source. The advent of high-intensity, broadly tunable quantum cascade lasers (QCL) has now accelerated IR imaging but results in a fundamentally different type of instrument and approach, namely, discrete frequency IR (DF-IR) spectral imaging. While the higher intensity of the source provides a higher signal per channel, the absence of spectral multiplexing also provides new opportunities and challenges. Here, we couple a rapidly tunable QCL with a high performance microscope equipped with a cooled focal plane array (FPA) detector. Our optical system is conceptualized to provide optimal performance based on recent theory and design rules for high-definition (HD) IR imaging. Multiple QCL units are multiplexed together to provide spectral coverage across the fingerprint region (776.9 to 1904.4 cm(-1)) in our DF-IR microscope capable of broad spectral coverage, wide-field detection, and diffraction-limited spectral imaging. We demonstrate that the spectral and spatial fidelity of this system is at least as good as the best FT-IR imaging systems. Our configuration provides a speedup for equivalent spectral signal-to-noise ratio (SNR) compared to the best spectral quality from a high-performance linear array system that has 10-fold larger pixels. Compared to the fastest available HD FT-IR imaging system, we demonstrate scanning of large tissue microarrays (TMA) in 3-orders of magnitude smaller time per essential spectral frequency. These advances offer new opportunities for high throughput IR chemical imaging, especially for the measurement of cells and tissues.

Preparation and physicochemical characterization of cellulose nanocrystals from industrial waste cotton

NASA Astrophysics Data System (ADS)

Thambiraj, S.; Ravi Shankaran, D.

2017-08-01

We aimed to develop a simple and low-cost method for the production of high-performance cellulose nanomaterials from renewable and sustainable resources. Here, cellulose microcrystals (CMCs) were prepared by controlled acidic and basic hydrolysis of cotton from textile industry wastes. The resulted CMCs were further converted into cellulose nanocrystals (CNCs) with high crystallinity by acidic hydrolysis. The physicochemical characteristics and morphological feature of CMCs and CNCs were studied by various analytical techniques such as UV-vis spectroscopy, Fourier-transform infrared spectroscopy (FT-IR), Scanning electron microscope (SEM), Fluorescence spectroscopy, Atomic force microscopy (AFM), High-resolution transmission electron microscopy (HR-TEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). The isolated CNCs possess a needle-like morphological structure with the longitudinal and lateral dimensions of 180 ± 60 nm, 10 ± 1 nm, respectively. The AFM result reveals that the CNCs have a high aspect ratio of 40 ± 14 nm and the average thickness of 6.5 nm. The XRD and TEM analysis indicate that the synthesized CNCs possess face-centered cubic crystal structure. Preliminary experiments were carried out to fabricate CNCs incorporated poly (vinyl alcohol) (PVA) film. The results suggest that the concept of waste to wealth could be well executed from the prepared CNCs, which have great potential for various applications including bio-sensors, food packaging and drug delivery applications.

Preparation of N-doped ZnO-loaded halloysite nanotubes catalysts with high solar-light photocatalytic activity.

PubMed

Cheng, Zhi-Lin; Sun, Wei

2015-01-01

N-doped ZnO nanoparticles were successfully assembled into hollow halloysite nanotubes (HNTs) by using the impregnation method. The catalysts based on N-doped ZnO-loaded HNTs nanocomposites (N-doped ZnO/HNTs) were characterized by X-ray diffraction (XRD), transmission electron microscopy-energy dispersive X-ray (TEM-EDX), scanning electron microscopy-energy dispersive X-ray (SEM-EDX), UV-vis and Fourier transform infrared spectroscopy (FT-IR) techniques. The XRD pattern showed ZnO nanoparticles with hexagonal structure loaded on HNTs. The TEM-EDX analysis indicated ZnO particles with the crystal size of ca.10 nm scattered in hollow structure of HNTs, and furthermore the concentration of N atom in nanocomposites was up to 2.31%. The SEM-EDX verified most of N-ZnO nanoparticles existing in hollow nanotubes of HNTs. Besides containing an obvious ultraviolet absorbance band, the UV-vis spectra of the N-doped ZnO/HNTs catalysts showed an available visible absorbance band by comparing to HNTs and non-doped ZnO/HNTs. The photocatalytic activity of the N-doped ZnO/HNTs catalysts was evaluated by the degradation of methyl orange (MO) solution with the concentration of 20 mg/L under the simulated solar-light irradiation. The result showed that the N-doped ZnO/HNTs catalyst exhibited a desirable solar-light photocatalytic activity.

A facile biomimetic preparation of highly stabilized silver nanoparticles derived from seed extract of Vigna radiata and evaluation of their antibacterial activity

NASA Astrophysics Data System (ADS)

Choudhary, Manoj Kumar; Kataria, Jyoti; Cameotra, Swaranjit Singh; Singh, Jagdish

2016-01-01

The significant antibacterial activity of silver nanoparticles draws the major attention toward the present nanobiotechnology. Also, the use of plant material for the synthesis of metal nanoparticles is considered as a green technology. In this context, a non-toxic, eco-friendly, and cost-effective method has been developed for the synthesis of silver nanoparticles using seed extract of mung beans ( Vigna radiata). The synthesized nanoparticles have been characterized by UV-visible spectroscopy (UV-Vis), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), atomic absorption spectroscopy (AAS), and X-ray diffraction (XRD). The UV-visible spectrum showed an absorption peak at around 440 nm. The different types of phytochemicals present in the seed extract synergistically reduce the Ag metal ions, as each phytochemical is unique in terms of its structure and antioxidant function. The colloidal silver nanoparticles were observed to be highly stable, even after 5 months. XRD analysis showed that the silver nanoparticles are crystalline in nature with face-centered cubic geometry and the TEM micrographs showed spherical particles with an average size of 18 nm. Further, the antibacterial activity of silver nanoparticles was evaluated by well-diffusion method and it was observed that the biogenic silver nanoparticles have an effective antibacterial activity against Escherichia coli and Staphylococcus aureus. The outcome of this study could be useful for nanotechnology-based biomedical applications.

Synthesis and Characterization of SiO2@Y2MoO6:Eu3+ Core-Shell Structured Spherical Phosphors by Sol-Gel Process.

PubMed

Li, G Z; Liu, F H; Chu, Z S; Wu, D M; Yang, L B; Li, J L; Wang, M N; Wang, Z L

2016-04-01

SiO2@Y2MoO6:Eu3+ core-shell phosphors were prepared by the sol-gel process. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectra (EDS), transmission electron microscopy (TEM), photoluminescence (PL) spectra as well as kinetic decays were used to characterize the resulting SiO2@Y2MoO6:Eu3+ core-shell phosphors. The XRD results demonstrated that the Y2MoO6:Eu3+ layers on the SiO2 spheres crystallized after being annealed at 700 °C and the crystallinity increased with raising the annealing temperature. The obtained core-shell phosphors have spherical shape with narrow size distribution (average size ca. 640 nm), non-agglomeration, and smooth surface. The thickness of the Y2MoO6:Eu3+ shells on the SiO2 cores could be easily tailored by varying the number of deposition cycles (70 nm for four deposition cycles). The Eul+ shows a strong PL emission (dominated by 5D0-7F2 red emission at 614 nm) under the excitation of 347 nm UV light. The PL intensity of Eu3+ increases with increasing the annealing temperature and the number of coating cycles.

Green synthesis, characterization and antibacterial efficacy of palladium nanoparticles synthesized using Filicium decipiens leaf extract

NASA Astrophysics Data System (ADS)

Sharmila, G.; Farzana Fathima, M.; Haries, S.; Geetha, S.; Manoj Kumar, N.; Muthukumaran, C.

2017-06-01

Synthesis of metal nanoparticles through green chemistry route is an emerging eco-friendly approach in the present days. An eco-friendly, biogenic synthesis of palladium nanoparticles (PdNPs) using Filicium decipiens leaf extract was reported in the present study. The synthesized PdNPs were characterized by UV-visible spectroscopy, Transmission electron microscopy (TEM), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). The PdNPs formation was confirmed by UV-visible spectrophotometer and spherical shaped PdNPs with size range of 2-22 nm was observed in TEM analysis. Energy dispersive X-ray spectroscopy (EDS) analysis confirmed the presence of palladium in the synthesized nanoparticles. The crystalline nature of PdNPs was confirmed by XRD pattern and compared with the standard. The phytochemicals and proteins were identified by their functional groups in FT-IR spectrum and revealed the amide, amine groups present in F. decipiens may have involved in the bio-reduction reaction for PdNPs synthesis. Prepared PdNPs showed potential antibacterial activity against both Gram-positive and Gram-negative bacteria. F. decipiens leaf extract based PdNPs showed high bactericidal activity against Escherichia coli, Pseudomonas aeruginosa as compared to Staphylococcus aureus and Bacillus subtilis Results showed that phytochemicals rich F. decipiens leaf extract may be utilized as an effective non-toxic reducing agent for PdNPs synthesis and prepared PdNPs may useful in biomedical applications.

Formation and characterization of high surface area thermally stabilized titania/silica composite materials via hydrolysis of titanium(IV) tetra-isopropoxide in sols of spherical silica particles.

PubMed

Khalil, Kamal M S; Elsamahy, Ahmed A; Elanany, Mohamed S

2002-05-15

A direct synthetic route leading to titania particles dispersed on nonporous spherical silica particles has been investigated; 5, 10, and 20% (w/w) titania/silica sols mixtures were achieved via hydrolyzation of titanium tetra-isopropxide solution in the mother liquor of a freshly prepared sol of spherical silica particles (Stöber particles). Titania/silica materials were produced by subsequent drying and calcination of the xerogels so obtained for 3 h at 400 and 600 degrees C. The materials were investigated by means of thermal analyses (TGA and DSC), FT-IR, N(2) gas adsorption-desorption, powder X-ray diffraction (XRD), and transmission electron microscopy (TEM). In spite of the low surface area (13.1 m(2)/g) of the pure spherical silica particles calcined at 400 degrees C, high surface area and mesoporous texture titania/silica materials were obtained (e.g., S(BET) ca. 293 m(2)/g for the 10% titania/silica calcined at 400 degrees C). Moreover, the materials were shown to be amorphous toward XRD up to 600 degrees C, while reasonable surface areas were preserved. It has been concluded that dispersion of titania particles onto the surface of the nonporous spherical silica particles increase their roughness, therefore leading to composite materials of less firm packing and mesoporosity.

Investigation on the path process of M doped ZnO (M = Gd, Mg) via the sol-gel method from dried gel to stable nanostructure powder

NASA Astrophysics Data System (ADS)

Suharno; Soegijono, B.; Budiawanti, S.; Fadillah, L.

2017-04-01

Doping is one of the effective methods to modify the physical properties of ZnO material in order to extend its applications. An investigation on Zn1-xMxO (M = Gd, Mg and x = 0.00, 0.03) nanopowders that have been synthesized by sol-gel method and sintered at 600 °C for 2 hours was reported. The decomposition process of the dried gel system was investigated by thermal gravimetric analysis (TGA) and the nanopowders with different heating temperature were studied using FT-IR spectroscopy. The crystal structure of the nanopowders after sintering at 600 °C was obtained using X-ray diffraction (XRD). The TGA curves of the samples showed the various weight loss regions corresponding to the removal of starting materials and no weight loss was observed in the temperature range of 300 to 800 °C which corresponded to the phase-crystallization step. The FTIR spectra showed that ZnO band was assigned to the stretching frequency at 669 cm-1 while Gd/Mg doped ZnO was at 668 cm-1 and 666 cm-1. From the XRD studies, the crystal structure of the samples indicated single phase ZnO crystalline and confirmed hexagonal wurtzite structure (space group of P63mc).

Role of manganese dioxide in the recovery of oxide-sulphide zinc ore.

PubMed

Yang, Kun; Zhang, Libo; Zhu, Xingcai; Peng, Jinhui; Li, Shiwei; Ma, Aiyuan; Li, Haoyu; Zhu, Fei

2018-02-05

In this article, the role of MnO 2 in the recovery of oxide-sulphide zinc ore discussed. Through adopting various modern analysis techniques (such as X-ray diffraction pattern, X-ray photoelectron spectroscopy, scanning electron microscope, energy dispersive X-ray analysis, and fourier transform infrared spectroscopy), the function and mechanism of MnO 2 during the phase transformation process is found out. Thermodynamic mechanisms involved in the phase transformation process with or without addition of manganese dioxide investigated by exploiting the Equilib module of FactSage. What's more, XRD patterns, XPS spectra and SEM-EDAX analyses of zinc calcines verify well the calculations of FactSage. Results reveal that the addition of MnO 2 will produce an aggregation of ZnMn 2 O 4 , a valuable energy material, while roasting on its own, results in generating undesirable Zn 2 SiO 4 , the oxidation degree being relatively low. Moreover, XRD pattern of zinc calcine and FT-IR spectrum of yellow product collected in the calcination process prove that the sulphur-fixing value of the additive MnO 2 , which can promote transforming to the elemental sulphur. The volatile S can be collected through a simple guiding device. In this process, the emission of SO 2 effectively avoids, thus MnO 2 deems as a potential additive in the recovery of oxide-sulphide zinc ore. Copyright © 2017. Published by Elsevier B.V.

Study of 2,4-dichlorophenoxyacetic acid (2,4-D) removal by Cu-Fe-layered double hydroxide from aqueous solution

NASA Astrophysics Data System (ADS)

Nejati, Kamellia; Davary, Soheila; Saati, Marziye

2013-09-01

The hydrotalcite-like compound of Cu-Fe-layered double hydroxide was studied as a potential adsorbent of herbicide 2,4-dichlorophenoxyacetic acid (2,4-D). The nanoparticles of Cu-Fe layered double hydroxide were prepared by Cu/Fe molar ratio of 2:1 using a coprecipitation method at pH 8.5 and characterized by the X-ray powder diffraction (XRD), the Fourier transform infrared spectroscopy (FT-IR), the thermal gravimetric analysis (TGA) and the elemental analysis. The size and morphology of nanoparticles were examined by the transmission electron microscopy (TEM). The adsorption experiments on LDH, on the other hand, were conducted in three different procedures, namely, time-dependent, pH-dependent and temperature-dependent. Characterization of the adsorption products by the XRD method indicates that the intercalation of 2,4-D between the LDH layers has not occurred and the surface adsorption had taken place. The adsorption kinetic was tested for pseudo-first-order, pseudo-second-order, Elovich and Intra-particle diffusion kinetic models and the rate constants were calculated. The equilibrium adsorption data were described by Langmuir and Freundlich equations. It was observed that, the Langmuir isotherm slightly better fitted to the experimental data rather than that of Freundlich. In the adsorption experiments, the Gibbs free energy values, ΔG°, the enthalpy, ΔH°, and the entropy, ΔS° were also determined.

Effect of Modified Nanoclay Composite on Blended PVDF/PEG Electrolyte Membranes for Fuel Cell Applications

NASA Astrophysics Data System (ADS)

Bahavan Palani, P.; Sainul Abidin, K.; Kannan, R.; Rajashabala, S.

This research work describes the fabrication of polymer blend nanocomposite membranes using the solution casting method. These membranes were fabricated with Poly (Vinylidene Fluoride) (PVdF) as host, Poly (Ethylene Glycol) (PEG) in steps of 2wt.% as blending polymer and Montmorillonite (MMT) nanoclay particles in steps of 3wt.% which were used as received. The protonated MMT was synthesized through an ion exchange process with column chromatographic technique. The prepared membrane’s performance was investigated using different characterization techniques of Thermo Gravimetric Analysis (TGA), Fourier Transform Infrared Spectroscopy (FT-IR), X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), water uptake, IEC and electrochemical impedance spectroscopy. Thermal stability was decreased while adding PEG into PVDF but it is controlled with the addition of MMT on PVDF/PEG blend matrix. Moreover, It is noticed that, the increase of water uptake, IEC by the increasing additive concentration of PEG and MMT. XRD studies reveal the increased amorphous phase with uniform exfoliation of nanoclay particles. The highest proton conductivity value of 0.127S cm‑1 is obtained with 9wt.% of MMT in the PVdF/PEG/MMT composite membranes at room temperature with 100% Relative Humid (RH) condition and 10 V.% of sulfonation. The blended nanocomposite membranes fulfill the requirements of proton exchange membrane for fuel cell application.

Green synthesis of novel zinc iron oxide (ZnFe2O4) nanocomposite via Moringa Oleifera natural extract for electrochemical applications

NASA Astrophysics Data System (ADS)

Matinise, N.; Kaviyarasu, K.; Mongwaketsi, N.; Khamlich, S.; Kotsedi, L.; Mayedwa, N.; Maaza, M.

2018-07-01

The main motivation of the research study involves development of reliable, accurate, inexpensive and environmental friendly method for the synthesis of zinc ferrite (ZnFe2O4) nanocomposites. It was thought of interest to synthesized zinc ferrite via green synthetic method using Moringa Oleifera extract. For the first time, we used green synthetic route via Moringa Oleifera extract acted as both chelating and reducing agents to synthesis spinel ZnFe2O4 nanocomposites. The physical and electrochemical properties were characterized using different techniques such as High Resolve Transmission Electron Microscope (HRTEM) Energy Dispersive X-ray Spectroscopy (EDS) X-ray diffraction (XRD) Fourier transform-infrared (FT-IR) Cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The XRD pattern thus clearly illustrated that the ZnFe2O4 nanocmposites synthesized by the green method were good crystalline in nature. The time constant and exchange current of ZnFe2O4 nanocomposites from EIS analysis were calculated and found to be 5.2001 × 10-4 s/rad and 6.59432 × 10-4 A, respectively. Based on the electrochemical results, GCE/ZnFe2O4 electrode exhibited a good voltametric response, high electro-activity, and excellent electrochemical performance making it a highly suitable/promising electrode for electrochemical applications.

Synthesis and characterization of sulfate and dodecylbenzenesulfonate intercalated zinc iron layered double hydroxides by one-step coprecipitation route

NASA Astrophysics Data System (ADS)

Zhang, Hui; Wen, Xing; Wang, Yingxia

2007-05-01

Inorganic sulfate- and organic dodecylbenzenesulfonate (DBS)-intercalated zinc-iron layered double hydroxides (LDHs) materials were prepared by one-step coprecipitation method from a mixed salt solutions containing Zn(II), Fe(II) and Fe(III) salts. The as-prepared samples have been characterized by X-ray powder diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), low-temperature nitrogen adsorption, scanning electron microscopy (SEM), inductively coupled plasma emission spectroscopy (ICP), and Mössbauer spectroscopy (MS). The XRD analyses demonstrate the typical LDH-like layered structural characteristics of both products. The room temperature MS results reveal the characteristics of both the Fe(II) and Fe(III) species for SO 42--containing product, while only the Fe(III) characteristic for DBS-containing one. The combination characterization results and Rietveld analysis illustrate that the SO 42--containing product possesses the Green Rust two (GR2)-like crystal structure with an approximate chemical composition of [Zn 0.435·Fe II0.094·Fe III0.470·(OH) 2]·(SO 42-) 0.235·1.0H 2O, while the DBS-containing one exhibits the common LDH compound-like structure. The contact angle measurement indicates the evident hydrophobic properties of DBS-containing nanocomposite, compared with SO 42--containing product, due to the modification of the internal and external surface of LDHs by the organic hydrophobic chain of DBS.

The synthesis and the spectroscopic, thermal, and structural properties of the M2[(fumarate)Ni(CN)4]·2(1,4-Dioxane) clathrate (M = Co, Ni, Cd and Hg)

NASA Astrophysics Data System (ADS)

Kartal, Zeki; Yavuz, Abdülkerim

2018-03-01

In this study, the clathrates of fumarate-tetracyanonickel-dioxane, given by the formula M2[(fumarate)Ni(CN)4]·2(1,4-Dioxane) (M = Co, Ni, Cd and Hg), have been obtained for the first time through chemical methods. These clathrates have been characterized by elemental, thermal, FT-IR, and FT-Raman spectroscopies. The parameters of structures of clathrates have been determined by X-ray powder diffraction. The thermal behaviors of these clathrates have been also investigated by thermo-gravimetric analysis (TGA), differential thermal analysis (DTA), and derivative thermal gravimetric analysis (DTG) in the range of 20-900 °C. X-ray powder diffraction data have been recorded at ambient temperature in the 2θ range 5-50°. The FT-IR and FT-Raman spectra of clathrates have been recorded in the region of 4000-400 cm-1 and 4000-100 cm-1, respectively. The results of the spectral and thermal analyses of the newly synthesized clathrates of fumarate-tetracyanonickel-dioxane suggest that these clathrates are new examples of the Hofmann-type dioxane clathrates. In our study, the Hofmann-type dioxane clathrates, which are formed by bounding electrons of oxygen-donor atoms of fumarate ion ligand molecule to transition metal atoms, consist of the corrugated |M-Ni(CN)4|∞ polymeric layers, which are held in parallel through the chain of (-M-fumarate-M-).

FT-IR, FT-Raman spectra and DFT calculations of melaminium perchlorate monohydrate.

PubMed

Kanagathara, N; Marchewka, M K; Drozd, M; Renganathan, N G; Gunasekaran, S; Anbalagan, G

2013-08-01

Melaminium perchlorate monohydrate (MPM), an organic material has been synthesized by slow solvent evaporation method at room temperature. Powder X-ray diffraction analysis confirms that MPM crystal belongs to triclinic system with space group P-1. FTIR and FT Raman spectra are recorded at room temperature. Functional group assignment has been made for the melaminium cations and perchlorate anions. Vibrational spectra have also been discussed on the basis of quantum chemical density functional theory (DFT) calculations using Firefly (PC GAMESS) version 7.1 G. Vibrational frequencies are calculated and scaled values are compared with experimental values. The assignment of the bands has been made on the basis of the calculated PED. The Mulliken charges, HOMO-LUMO orbital energies are analyzed directly from Firefly program log files and graphically illustrated. HOMO-LUMO energy gap and other related molecular properties are also calculated. The theoretically constructed FT-IR and FT-Raman spectra of MPM coincide with the experimental one. The chemical structure of the compound has been established by (1)H and (13)C NMR spectra. No detectable signal was observed during powder test for second harmonic generation. Copyright © 2013 Elsevier B.V. All rights reserved.

FT-Raman, FT-IR spectra and total energy distribution of 3-pentyl-2,6-diphenylpiperidin-4-one: DFT method.

PubMed

Subashchandrabose, S; Saleem, H; Erdogdu, Y; Rajarajan, G; Thanikachalam, V

2011-11-01

FT-Raman and FT-IR spectra were recorded for 3-pentyl-2,6-diphenylpiperidin-4-one (PDPO) sample in solid state. The equilibrium geometries, harmonic vibrational frequencies, infrared and the Raman scattering intensities were computed using DFT/6-31G(d,p) level. Results obtained at this level of theory were used for a detailed interpretation of the infrared and Raman spectra, based on the total energy distribution (TED) of the normal modes. Molecular parameters such as bond lengths, bond angles and dihedral angles were calculated and compared with X-ray diffraction data. This comparison was good agreement. The intra-molecular charge transfer was calculated by means of natural bond orbital analysis (NBO). Hyperconjugative interaction energy was more during the π-π* transition. Energy gap of the molecule was found using HOMO and LUMO calculation, hence the less band gap, which seems to be more stable. Atomic charges of the carbon, nitrogen and oxygen were calculated using same level of calculation. Copyright © 2011 Elsevier B.V. All rights reserved.

Spectroscopic characterization of natural calcite minerals.

PubMed

Gunasekaran, S; Anbalagan, G

2007-11-01

The FT-IR, FT-Raman, NMR spectral data of ten different limestone samples have been compared. FT-IR and FT-Raman spectral data show that calcium carbonate in limestone, principally in the form of calcite, as identified by its main absorption bands at 1426, 1092, 876 and 712 cm(-1). The sharp diffractions at the d-spacings, 3.0348, 1.9166 and 1.8796 confirm the presence of calcite structure and the calculated lattice parameters are: a=4.9781 A, c=17.1188 A. The range of 13C chemical shifts for different limestone samples is very small, varying from 198.38 to 198.42 ppm. The observed chemical shifts are consistent with the identical C-O bonding in different limestone samples. 27Al MAS NMR spectra of the samples exhibit a central line at 1 ppm and another line at 60 ppm corresponding to octahedral and tetrahedral Al ions, respectively. The five component resonances were observed in 29Si MAS NMR spectrum of limestone and these resonances were assigned to Si (4 Al), Si (3 Al), Si (2 Al), Si (1 Al) and Si (0 Al) from low field to high field.

Molecular structure, spectroscopic studies and first-order molecular hyperpolarizabilities of ferulic acid by density functional study

NASA Astrophysics Data System (ADS)

Sebastian, S.; Sundaraganesan, N.; Manoharan, S.

2009-10-01

Quantum chemical calculations of energies, geometrical structure and vibrational wavenumbers of ferulic acid (FA) (4-hydroxy-3-methoxycinnamic acid) were carried out by using density functional (DFT/B3LYP/BLYP) method with 6-31G(d,p) as basis set. The optimized geometrical parameters obtained by DFT calculations are in good agreement with single crystal XRD data. The vibrational spectral data obtained from solid phase FT-IR and FT-Raman spectra are assigned based on the results of the theoretical calculations. The observed spectra are found to be in good agreement with calculated values. The electric dipole moment ( μ) and the first hyperpolarizability ( β) values of the investigated molecule have been computed using ab initio quantum mechanical calculations. The calculation results also show that the FA molecule might have microscopic nonlinear optical (NLO) behavior with non-zero values. A detailed interpretation of the infrared and Raman spectra of FA was also reported. The energy and oscillator strength calculated by time-dependent density functional theory (TD-DFT) results complements with the experimental findings. The calculated HOMO and LUMO energies shows that charge transfer occur within the molecule. The theoretical FT-IR and FT-Raman spectra for the title molecule have been constructed.

Synthesis and characterization of nano TiO2-SiO2: PVA composite - a novel route

NASA Astrophysics Data System (ADS)

Venckatesh, Rajendran; Balachandaran, Kartha; Sivaraj, Rajeshwari

2012-07-01

A novel, simple, less time consuming and cost-effective sol-gel method has been developed to synthesize nano titania-silica with polyvinyl alcohol (PVA) composite relatively at low temperature in acidic pH. Titania sol is prepared by hydrolysis of titanium tetrachloride and was mixed with silicic acid and tetrahydrofuran mixture. The reaction was carried out under vigorous stirring for 6 h and dried at room temperature with the addition of PVA solution. The resulting powders were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared (FT-IR), UV-visible spectroscopy and thermal techniques. The grain size of the particles was calculated by X-ray diffraction; surface morphology and chemical composition were determined from scanning electron microscopy-energy dispersive spectroscopy; metal oxide stretching was confirmed from FT-IR spectroscopy; bandgap was calculated using UV-visible spectroscopy, and thermal stability of the prepared composite was determined by thermogravimetric/differential thermal analysis. Since TiO2 got agglomerated on the surface of SiO2, effective absorptive sites increase which in turn increase the photocatalytic efficiency of the resulting composite.

A new photoluminescence emission peak of ZnO SiO2 nanocomposites and its energy transfer to Eu3+ ions

NASA Astrophysics Data System (ADS)

Hong, Jian-He; Cong, Chang-Jie; Zhang, Zhi-Guo; Zhang, Ke-Li

2007-07-01

This work reports a new photoluminescence (PL) emission peak at about 402 nm from amorphous ZnO nanoparticles in a silica matrix, and the energy transfer from it to Eu3+ ions. The amorphous ZnO SiO2 nanocomposites were prepared by the sol gel method, which is verified by X-ray diffraction (XRD) profiles and FT IR spectra. The luminescence emission spectra are fitted by four Gauss profiles, two of which at longer wavelength are due to the defects of the material and the others to amorphous ZnO nanoparticles and the Zn O Si interface state. With the reduction of Zn/Si ratio and diethanolamine, the relative intensities of visible emission decrease. The weak visible emission is due to the reduction of defects after calcined at high temperature. The new energy state at the Zn O Si interface results in strong emission at about 402 nm. When Eu3+ ions are co-doped, weak energy transfer from ZnO SiO2 nanocomposites to Eu3+ emission are observed in the excitation spectra.

Morphology and formation mechanism in precipitation of calcite induced by Curvibacter lanceolatus strain HJ-1

NASA Astrophysics Data System (ADS)

Zhang, Chonghong; Li, Fuchun; Lv, Jiejie

2017-11-01

Precipitation of calcium carbobate induced by microbial activities is common occurrence in controlled solution, but the formation mechanism and morphology in precipitation of calcite in solution systems is unclear, and the role of microbes is disputed. Here, culture experiment was performed for 50 days using the Curvibacter lanceolatus strain HJ-1 in a M2 culture medium, and the phase composition and morphology of the precipitates were characterized by the X-ray diffraction (XRD), Fourier transform infrared (FT-IR), and scanning electron microscopy (SEM) techniques. We show that the precipitation processes in our experiment lead to unusual morphologies of crystals corresponding to different growth stages, and the morphologies of the precipitated crystal aggregates ranging from the main rod-, cross-, star-, cauliflower-like morphologies to spherulitic structure. The complex and unusual morphologies of the precipitated calcite by strain HJ-1 may provide a reference point for better understanding the biomineralization mechanism of calcite, moreover, morphological transition of minerals revealed that the multi-ply crystals-aggregation mechanism for calcite growth in crystallisation media.

Electrophoretic deposition of nanostructured hydroxyapatite coating on AZ91 magnesium alloy implants with different surface treatments

NASA Astrophysics Data System (ADS)

Rojaee, Ramin; Fathi, Mohammadhossein; Raeissi, Keyvan

2013-11-01

Bio-absorbable magnesium (Mg) based alloys have been introduced as innovative orthopedic implants during recent years. It has been specified that rapid degradation of Mg based alloys in physiological environment should be restrained in order to be utilized in orthopedic trauma fixation and vascular intervention. In this developing field of healthcare materials, micro-arc oxidation (MAO), and MgF2 conversion coating were exploited as surface pre-treatment of AZ91 magnesium alloy to generate a nanostructured hydroxyapatite (n-HAp) coating via electrophoretic deposition (EPD) method. X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), and transmission electron microscopy (TEM) techniques were used to characterize the obtained powder and coatings. The potentiodynamic polarization tests were carried out to evaluate the corrosion behavior of the coated and uncoated specimens, and in vitro bioactivity evaluation were performed in simulated body fluid. Results revealed that the MAO/n-HAp coated AZ91 Mg alloy samples with a rough topography and lower corrosion current density leads to a lower Mg degradation rate accompanied by high bioactivity.

Engineering birnessite-type MnO2 nanosheets on fiberglass for pH-dependent degradation of methylene blue

NASA Astrophysics Data System (ADS)

Xin Zhang, Yu; Long Guo, Xiao; Huang, Ming; Dong Hao, Xiao; Yuan, Yuan; Hua, Chao

2015-08-01

We construct hierarchical MnO2 nanosheets @ fiberglass nanostructures via one-pot hydrothermal method without any surfactants. The morphology and structure of MnO2-modified fiberglass composites are examined by focus ion beam scanning electron microscopy (FIB/SEM), X-Ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR). The birnessite-type MnO2 nanosheets are observed to grow vertically on the surface of fiberglass. Furthermore, the birnessite-type MnO2-fiberglass composites exhibit good ability for degradation of methylene blue (MB) in different pH levels. In neutral solution (pH 6.5-7.0), it achieves a high removal rate of 96.1% (2 h, at 60 °C) in the presence of H2O2; and in acidic environment (pH 1.5), 96.8% of MB solution (20 mg/L, 100 mL) is decomposed by oxidation within only 5 min. In principles, the rational design of MnO2 nanosheets-decorated fiberglass architectures demonstrated the suitability of the low-cost MnO2-modified fiberglass nanostructure for water treatment.

Magnetic molecularly imprinted polymer for the selective extraction of quercetagetin from Calendula officinalis extract.

PubMed

Ma, Run-Tian; Shi, Yan-Ping

2015-03-01

A new magnetic molecularly imprinted polymers (MMIPs) for quercetagetin was prepared by surface molecular imprinting method using super paramagnetic core-shell nanoparticle as the supporter. Acrylamide as the functional monomer, ethyleneglycol dimethacrylate as the crosslinker and acetonitrile as the porogen were applied in the preparation process. Fourier transform infrared spectrometer (FT-IR), X-ray diffraction (XRD) and Vibrating sample magnetometer (VSM) were applied to characterize the MMIPs, and High performance liquid chromatography (HPLC) was utilized to analyze the target analytes. The selectivity of quercetagetin MMIPs was evaluated according to their recognition to template and its analogues. Excellent binding for quercetagetin was observed in MMIPs adsorption experiment, and the adsorption isotherm models analysis showed that the homogeneous binding sites were distributed on the surface of the MMIPs. The MMIPs were employed as adsorbents in solid phase extraction for the determination of quercetagetin in Calendula officinalis extracts. Furthermore, this method is fast, simple and could fulfill the determination and extraction of quercetagetin from herbal extract. Copyright © 2014 Elsevier B.V. All rights reserved.

Bluish green emitting carbon quantum dots synthesized from jackfruit (Artocarpus heterophyllus) and its sensing applications of Hg (II) and Cr (VI) ions

NASA Astrophysics Data System (ADS)

Rajendran, Kalimuthu; Rajendiran, Nagappan

2018-02-01

A simple, economical, and green method for the preparation of water soluble, high fluorescent carbon quantum dots (CQDs) has been prepared via hydrothermal process using jackfruit (Artocarpus heterophyllus) as a carbon source. The optical properties of synthesized CQDs were characterized by UV- visible and fluorescence spectroscopy. Fourier transform infrared spectroscopy (FT-IR), x-ray Diffraction (XRD) and high resolution transmission electron microscopy (HR-TEM) techniques were used to study the composition and size of the CQDs. The prepared CQDs were spherical in shape with an average size of 2.5 nm along with uniform distribution and showed bright bluish green emission properties, without any further surface modification. The prepared CQDs were exhibit high stability at neutral pH and showed high photo-stability under UV light irradiation at 365 nm. The obtained CQDs were effectively utilized as fluorescent probe for highly selective and sensitive detection of Hg2+ and Cr6+ ions in environmental samples with a limit of detection of about 8 and 10 nM respectively.

TiO2-PANI/Cork composite: A new floating photocatalyst for the treatment of organic pollutants under sunlight irradiation.

PubMed

Sboui, Mouheb; Nsib, Mohamed Faouzi; Rayes, Ali; Swaminathan, Meenakshisundaram; Houas, Ammar

2017-10-01

A novel photocatalyst based on TiO 2 -PANI composite supported on small pieces of cork has been reported. It was prepared by simple impregnation method of the polyaniline (PANI)-modified TiO 2 on cork. The TiO 2 -PANI/Cork catalyst shows the unique feature of floating on the water surface. The as-synthesized catalyst was characterized by X-ray diffraction (XRD), scanning electron micrograph (SEM), transmission electron microscopy (TEM), thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FT-IR), UV-vis diffuse reflectance spectra (UV-vis DRS) and the Brunauer-Emmett-Teller (BET) surface area analysis. Characterization suggested the formation of anatase highly dispersed on the cork surface. The prepared floating photocatalyst showed high efficiency for the degradation of methyl orange dye and other organic pollutants under solar irradiation and constrained conditions, i.e., no-stirring and no-oxygenation. The TiO 2 -PANI/Cork floating photocatalyst can be reused for at least four consecutive times without significant decrease of the degradation efficiency. Copyright © 2017. Published by Elsevier B.V.

Conversion of KCl into KBH4 by Mechano-Chemical Reaction and its Catalytic Decomposition

NASA Astrophysics Data System (ADS)

Bilen, Murat; Gürü, Metin; Çakanyildirim, Çetin

2017-07-01

Production of KBH4, in the presence of KCl, B2O3 and MgH2 by means of a mechanical reaction and a dehydrogenation kinetic, constitute the main parts of this study. Operating time and reactant ratio are considered as two parameters for the mechanical reaction to obtain the maximum yield. The production process was carried out in a ball milling reactor, and the product residue was purified with ethylene diamine (EDA) and subsequently characterized by Fourier Transform Infrared Spectroscopy (FT-IR) and x-ray Diffraction (XRD) analyses. Optimum time for mechano-chemical treatment and reactant ratio (MgH2/KCl) were obtained as 1000 min and 1.0, respectively. Synthesized and commercial KBH4 were compared by hydrolysis tests in the presence of Co1-xNix/Al2O3 heterogeneous catalyst. Hydrogen generation rates, activation energy and order of the KBH4 decomposition reaction were obtained as 1578 {mL}_{{{{H}}2 }} \\min^{ - 1} {g}_{{catalyst}}^{ - 1}, 39.2 kJ mol-1 and zero order, respectively.

Synthesis and property of novel MnO2@polypyrrole coaxial nanotubes as electrode material for supercapacitors

NASA Astrophysics Data System (ADS)

Yao, Wei; Zhou, Hui; Lu, Yun

2013-11-01

Novel MnO2@polypyrrole (PPy) coaxial nanotubes have been prepared via a simple and green approach without any surfactant and additional oxidant. Under the acidic condition, MnO2 nanotubes act as both template and oxidant to initiate the polymerization of pyrrole monomers on its fresh-activated surface. Fourier transform infrared spectra (FT-IR), X-ray diffraction patterns (XRD), thermo-gravimetric analysis data (TG) and X-ray photoelectron spectra (XPS) suggest the formation of composite structure of MnO2@PPy. Also, FESEM and TEM images intuitively confirm that the PPy shell is coated uniformly on the surface of MnO2 nanotubes. Adjusting the concentrations of sulfuric acid or adding oxidant can modulate the morphology of the products accordingly. Due to the synergic effect between MnO2 core and PPy shell, the MnO2@PPy coaxial nanotubes possess better rate capability, larger specific capacitance of 380 F g-1, doubling the specific capacitance of MnO2 nanotubes, and good capacitance retention of 90% for its initial capacitance after 1000 cycles.

Biosourced Polymetallic Catalysis: A Surprising and Efficient Means to Promote the Knoevenagel Condensation

PubMed Central

Deyris, Pierre-Alexandre; Bert, Valérie; Diliberto, Sébastien; Boulanger, Clotilde; Petit, Eddy; Legrand, Yves-Marie; Grison, Claude

2018-01-01

Zn hyperaccumulator (Arabidobsis halleri) and Zn accumulator Salix “Tordis” (Salix schwerinii × Salix viminalis) have shown their interest in the phytoextraction of polluted brownfields. Herein, we explore a novel methodology based on the chemical valorization of Zn-rich biomass produced by these metallophyte plants. The approach is based on the use of polymetallic salts derived from plants as bio-based catalysts in organic chemistry. The formed ecocatalysts were characterized via ICP-MS, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) in order to precise the chemical composition, structure, and behavior of the formed materials. The Doebner-Knoevenagel reaction was chosen as model reaction to study their synthetic potential. Significant differences to usual catalysts such as zinc (II) chloride are observed. They can principally be related to a mixture of unusual mineral species. DFT calculations were carried out on these salts in the context of the Gutmann theory. They allow the rationalization of experimental results. Finally, these new bio-based polymetallic catalysts illustrated the interest of this concept for green and sustainable catalysis. PMID:29637065

Biosourced Polymetallic Catalysis: A Surprising and Efficient Means to Promote the Knoevenagel Condensation.

PubMed

Deyris, Pierre-Alexandre; Bert, Valérie; Diliberto, Sébastien; Boulanger, Clotilde; Petit, Eddy; Legrand, Yves-Marie; Grison, Claude

2018-01-01

Zn hyperaccumulator ( Arabidobsis halleri ) and Zn accumulator Salix "Tordis" ( Salix schwerinii × Salix viminalis ) have shown their interest in the phytoextraction of polluted brownfields. Herein, we explore a novel methodology based on the chemical valorization of Zn-rich biomass produced by these metallophyte plants. The approach is based on the use of polymetallic salts derived from plants as bio-based catalysts in organic chemistry. The formed ecocatalysts were characterized via ICP-MS, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) in order to precise the chemical composition, structure, and behavior of the formed materials. The Doebner-Knoevenagel reaction was chosen as model reaction to study their synthetic potential. Significant differences to usual catalysts such as zinc (II) chloride are observed. They can principally be related to a mixture of unusual mineral species. DFT calculations were carried out on these salts in the context of the Gutmann theory. They allow the rationalization of experimental results. Finally, these new bio-based polymetallic catalysts illustrated the interest of this concept for green and sustainable catalysis.

Synthesis and characterization of TiO2 loaded cashew nut shell activated carbon and photocatalytic activity on BG and MB dyes under sunlight radiation

NASA Astrophysics Data System (ADS)

Ragupathy, S.; Raghu, K.; Prabu, P.

2015-03-01

Synthesis of titanium dioxide (TiO2) nanoparticles and TiO2 loaded cashew nut shell activated carbon (TiO2/CNSAC) had been undertaken using sol-gel method and their application in BG and MB dyes removal under sunlight radiation has been investigated. The synthesized photocatalysts were characterized by X-ray diffraction analysis (XRD), Fourier infra-red spectroscopy (FT-IR), UV-Vis-diffuse reflectance spectroscopy (DRS) and scanning electron microscopy (SEM) with energy dispersive X-ray analysis (EDX). The various experimental parameters like amount of catalyst, contact time for efficient dyes degradation of BG and MB were concerned in this study. Activity measurements performed under solar irradiation has shown good results for the photodegradation of BG and MB in aqueous solution. It was concluded that the higher photocatalytic activity in TiO2/CNSAC was due to parameters like band-gap, number of hydroxyl groups, surface area and porosity of the catalyst. The kinetic data were also described by the pseudo-first-order and pseudo-second-order kinetic models.

Preparation high photocatalytic activity of CdS/halloysite nanotubes (HNTs) nanocomposites with hydrothermal method

NASA Astrophysics Data System (ADS)

Xing, Weinan; Ni, Liang; Huo, Pengwei; Lu, Ziyang; Liu, Xinlin; Luo, Yingying; Yan, Yongsheng

2012-10-01

A novel nanocatalyst CdS/halloysite nanotubes (HNTs) was synthesized by hydrothermal method with direct growth of CdS nanoparticles on the surface of HNTs. The as-prepared photocatalysts had been characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), UV-vis diffuse reflectance spectra (UV-vis DRS), Fourier transform infrared (FT-IR) and the thermo gravimetric analysis (TGA). The photocatalytic activity of the sample was evaluated by the degradation of tetracycline (TC) under visible light irradiation. Benefit from the excellent properties of CdS and HNTs, the photocatalyst exhibited good photocatalytic activity and stability. In order to find out the optimum synthesis condition to obtain the best photocatalytic activity, a series of experiments were performed with different CdS loading capacity, different sources of sulfide and different hydrothermal temperatures, etc. The best photodegradation rate could reach 93% in 60 min under visible light irradiation. Therefore, the combination of CdS nanoparticles with HNTs endowed this material with a potential use in environmental treatments in industries.

Synthesis and electrochemical performance of polyaniline @MnO2/graphene ternary composites for electrochemical supercapacitors

NASA Astrophysics Data System (ADS)

Pan, Chao; Gu, Haiteng; Dong, Li

2016-01-01

We introduce a facile method to construct new ternary hierarchical nanocomposites by combining MnO2 coated one dimensional (1D) conducting polyaniline (PANI) nanowires with 2D graphene sheets (GNs). The hierarchical nanocomposite structures of PANI@MnO2/GNs (PMGNs) are further proved by X-ray diffraction (XRD), FT-IR, field emission scanning electron microscopy (FESEM), transmission electron microscope (TEM), thermogravimetric analysis (TGA), and X-ray photoelectron spectroscopy (XPS). The electrochemical characteristics of the electrodes made of the hierarchical structured PMGNs materials are determined by the CV and galvanostatic measurements. These electrochemical tests indicate that electrodes made of the nanostructured PMGNs exhibit an improved reversible capacitance of 695 F g-1 after 1000 cycles at a high current density of 4 A g-1. The ternary composites possess higher electrochemical capacitance than each individual component as supercapacitor electrode materials. Such intriguing electrochemical performance is mainly attributed to the synergistic effects of MnO2, PANI and graphene. The hierarchical ternary nanocomposites show excellent electrochemical properties for energy storage applications, which evidence their potential application as supercapacitors.

One-Pot Route towards Active TiO2 Doped Hierarchically Porous Cellulose: Highly Efficient Photocatalysts for Methylene Blue Degradation

PubMed Central

Sun, Xiaoxia; Wang, Kunpeng; Shu, Yu; Zou, Fangdong; Zhang, Boxing; Sun, Guangwu; Uyama, Hiroshi; Wang, Xinhou

2017-01-01

In this study, novel photocatalyst monolith materials were successfully fabricated by a non-solvent induced phase separation (NIPS) technique. By adding a certain amount of ethyl acetate (as non-solvent) into a cellulose/LiCl/N,N-dimethylacetamide (DMAc) solution, and successively adding titanium dioxide (TiO2) nanoparticles (NPs), cellulose/TiO2 composite monoliths with hierarchically porous structures were easily formed. The obtained composite monoliths possessed mesopores, and two kinds of macropores. Scanning Electron Microscope (SEM), Energy Dispersive Spectroscopy (EDS), Fourier Transform Infrared Spectroscopy (FT-IR), X-ray Diffraction (XRD), Brunauer-Emmett-Teller (BET), and Ultraviolet-visible Spectroscopy (UV-Vis) measurements were adopted to characterize the cellulose/TiO2 composite monolith. The cellulose/TiO2 composite monoliths showed high efficiency of photocatalytic activity in the decomposition of methylene blue dye, which was decomposed up to 99% within 60 min under UV light. Moreover, the composite monoliths could retain 90% of the photodegradation efficiency after 10 cycles. The novel NIPS technique has great potential for fabricating recyclable photocatalysts with highly efficiency. PMID:28772734

Growth, structural, thermal, dielectric and optical studies on HBST crystal: A potential THz emitter

NASA Astrophysics Data System (ADS)

Ma, Yuzhe; Teng, Bing; Cao, Lifeng; Zhong, Degao; Ji, Shaohua; Teng, Fei; Liu, Jiaojiao; Yao, Yuan; Tang, Jie; Tong, Jiaming

2018-02-01

The efficient organic nonlinear optical material 4-hydroxy benzaldehyde-N-methyl 4-stilbazolium tosylate (HBST) was grown from methanol by slope nucleation method combined with slow cooling (SNM-SC) for the first time. The optimum growth conditions based on the cooling rate was further investigated. The single crystal X-ray diffraction (XRD) revealed that the chromophores of HBST crystal make an angle of about 33° with respect to the a-axis, which is close to the optimum of Terahertz (THz)-wave generation and electro-optics applications. NMR and FT-IR spectral studies have been performed to ascertain various functional groups present in the sample. Futhermore, the thermal stability and decomposition stages were analyzed through TG-DTA and DSC techniques. The dielectric constant and dielectric loss of HBST crystal have been studied. Critical optical properties like the absorption coefficient, refractive index, cut-off wavelength and band gap energy were calculated. Photoluminescence (PL) exication studies indicated green emission occured at 507 nm. All the results of HBST crystal make it a promising candidate in the fields of optoelectronic and the generation of THz.

Structural, electrical conductivity and dielectric behavior of Na2SO4-LDT composite solid electrolyte.

PubMed

Iqbal, Mohd Z; Rafiuddin

2016-01-01

A series of composite materials of general molecular formula (1 - x) Na2SO4 - (x) LDT was prepared by solid state reaction method. The phase structure and functionalization of these materials were defined by X-ray diffraction (XRD) and Fourier-transform infrared spectroscopy (FT-IR) respectively. Differential thermal analysis (DTA) revealed that the hump of phase transition at 250 °C has decreased while its thermal stability was enhanced. Scanning electron microscopy signifies the presence of improved rigid surfaces and interphases that are accountable for the high ionic conduction due to dispersion of LDT particles in the composite systems. Arrhenius plots of the conductance show the maximum conductivity, σ = 4.56 × 10(-4) S cm(-1) at 500 °C for the x = 0.4 composition with the lowest activation energy 0.34 eV in the temperature range of 573-773 K. The value of dielectric constant was decreased with increasing frequency and follows the usual trend.

Pure keratin membrane and fibers from chicken feather.

PubMed

Ma, Bomou; Qiao, Xue; Hou, Xiuliang; Yang, Yiqi

2016-08-01

In this research, keratin was extracted from the disposable chicken feather using l-cysteine as reducing agent. Then, it was re-dissolved in the sodium carbonate-sodium bicarbonate buffer, and the pure keratin membrane and fiber were fabricated by doctor-blade casting process and wet spinning method, respectively. Scanning electron microscopy (SEM), fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD) and thermogravimetric analysis (TGA) were used to characterize the chemical and physical properties of resulting powder, membrane and fiber. Compared with the raw chicken feather, the regenerated keratin materials retain its chemical structure and thermal stability, their relative crystallinity is a little different depend on the shaping method, which leads to the difference in moisture regain. The mechanical results show that tensile strength of the keratin membrane researches 3.5MPa, have potential application in biomedical fields. However, the keratin fiber presents low tenacity, i.e. 0.5cN/dtex, this problem should be solved in order to apply the new fiber in textile and material science. Copyright © 2016 Elsevier B.V. All rights reserved.

HYDROTHERMAL SYNTHESIS OF α-MoO3 NANORODS FOR NO2 DETECTION

NASA Astrophysics Data System (ADS)

Bai, Shouli; Chen, Song; Tian, Yuan; Luo, Ruixian; Li, Dianqing; Chen, Aifan

2012-12-01

Thermodynamically stable molybdenum trioxide nanorods have been successfully synthesized by a simple hydrothermal process. The product exhibits high-quality, single-crystalline layered orthorhombic structure (α-MoO3), and aspect ratio over 20 by characterizations of X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HR-TEM) and Fourier transform infrared (FT-IR). The growth mechanism of α-MoO3 nanorods can be understood by electroneutral and dehydration reaction, which is highly dependent on solution acidity and hydrothermal temperature. The sensing tests show that the sensor based on MoO3 nanorods exhibits high sensitivity to NO2 and is not interferred by CO and CH4, which makes this kind sensor a competitive candidate for NO2 detection. The intrinsic sensing performance of MoO3 maybe arise from its nonstoichiometry of MoO3 owing to the presence of Mo5+ and oxygen vacancy in MoO3 lattice, which has been confirmed by X-ray photoelectron spectroscopy (XPS) analysis. The sensing mechanism of MoO3 for NO2 is also discussed.

Rheological and structural characterisation of film-forming solutions and biodegradable edible film made from kefiran as affected by various plasticizer types.

PubMed

Ghasemlou, Mehran; Khodaiyan, Faramarz; Oromiehie, Abdulrasoul

2011-11-01

The rheological properties of kefiran film-forming solutions, as well as the structural characterisation of the resulting films, were investigated as a function of various plasticizer types. The behaviours of the storage (G') and loss (G″) moduli as a function of frequency were typical of gel-like material, with the G' higher than the G″. Kefiran-based films, which may find application as edible films, were prepared by a casting and solvent-evaporation method. Possible interaction between the adjacent chains in the kefiran polymer and various plasticizers was proven by Fourier-transform infrared spectroscopy (FT-IR). The crystallinity of plasticized kefiran film was also analysed using X-ray diffraction (XRD); this revealed an amorphous-crystalline structure. These results were explained by the film's microstructure, which was analysed by atomic force microscopy (AFM) and scanning electron microscopy (SEM). The present study has helped determine possible interactions of kefiran, plasticizer and water molecules in determining film properties. Copyright © 2011 Elsevier B.V. All rights reserved.

Synthesis and characterization of biotin modified cholesteryl pullulan as a novel anticancer drug carrier.

PubMed

Yang, Wenzhi; Wang, Miaomiao; Ma, Lilan; Li, Haiying; Huang, Le

2014-01-01

A series of biotin modified cholesteryl pullulan (Bio-CHSP) conjugates with different degrees of substitution (DS) of biotin moiety were synthesized and characterized by Fourier transform infrared (FT-IR), proton nuclear magnetic resonance ((1)H NMR) and X-ray diffraction (XRD). Bio-CHSP conjugates were amphiphilic in nature and their self-aggregation behavior in aqueous media was evaluated by the fluorescence probe technique. Bio-CHSP self-aggregated nanoparticles (Bio-CHSP NPs) were prepared and analyzed by dynamic light scattering (DLS), zeta potential and transmission electron microscopy (TEM) technologies. These novel nanoparticles were almost spherical in shape, and their size, ranging from 178.8 to 100.0 nm. The safety of Bio-CHSP NPs was studied through single dose toxicity test in mice, and the result showed that Bio-CHSP NPs were well tolerated at the intravenous dose of 200 mg/kg in mice. Moreover, as a model anticancer drug, mitoxantrone loaded Bio-CHSP NPs were also prepared and characterized in this study. Copyright © 2013 Elsevier Ltd. All rights reserved.

Preparation, characterization and activity evaluation of heterostructure In(2)O(3)/In(OH)(3) photocatalyst.

PubMed

Shifu, Chen; Xiaoling, Yu; Huaye, Zhang; Wei, Liu

2010-08-15

In this paper, the heterostructure In(2)O(3)/In(OH)(3) photocatalyst was prepared by programmed thermal treatment of In(OH)(3) using In(NO(3))(3).9H(2)O as the precursor. Various characterization methods such as X-ray power diffraction (XRD), UV-vis diffuse reflectance spectroscopy (DRS), Fourier transform infrared spectrometry (FT-IR) and transmission electron microscopy (TEM) were employed to investigate the structure, morphologies, and optical properties. Terephthalic acid was used as a probe molecule to detect the generation of hydroxyl radicals (OH) on the surface of UV-illuminated photocatalyst by a photoluminescence (PL) technique. The results showed that the photocatalytic activity of the heterostructure In(2)O(3)/In(OH)(3) was higher than that of single In(2)O(3) or In(OH)(3). The increased photocatalytic activity may be attributed to the formation of the heterojunction between In(2)O(3) and In(OH)(3), which suppresses the recombination of photoexcited electrons-hole pairs. Copyright 2010 Elsevier B.V. All rights reserved.

Facile approach to synthesize magnesium oxide nanoparticles by using Clitoria ternatea—characterization and in vitro antioxidant studies

NASA Astrophysics Data System (ADS)

John Sushma, N.; Prathyusha, D.; Swathi, G.; Madhavi, T.; Deva Prasad Raju, B.; Mallikarjuna, K.; Kim, Hak-Sung

2016-03-01

Facile approach to synthesize the metal oxide nanoparticles is getting an increased attention in various biomedical applications such as, to treat antibiotic resistant diseases. Magnesium oxide nanoparticles (MgO·NPs) were synthesized by using Clitoria ternatea as the stabilizer in a green synthesis approach. The preliminary screening of MgO·NPs in the presence of C. ternatea extract was observed by UV-visible spectrophotometer. X-ray diffraction (XRD) pattern have proved the crystalline nature of the MgO·NPs; Photoluminescence (PL) measurement studies are used to identify the quality and defects in the crystal structure. FE-SEM with EDS has showed the size of 50-400 nm with specific binding energies. FT-IR has revealed the functional groups present in the plant extract and the peak at 521 cm-1 indicated the characteristic absorption bands of MgO·NPs. The DPPH activity and reducing power assay of biologically synthesized MgO·NPs could reach 65 % at a concentration of 150 µg/ml, respectively. From the results it was concluded that the biologically synthesized MgO·NPs exhibit good antioxidant activity.

Generation of conductivity through transfer charge properties, for polyesters and polyamides with characteristic functional groups

NASA Astrophysics Data System (ADS)

Gonzalez, Carmen; Tagle, Luis Hernan; Terraza, Claudio A.; Barriga, Andres; Cabrera, A. L.; Volkmann, Ulrich G.

2011-03-01

Electro-optic properties of σ -conjugated polymers, as polysilylene; are associated with electron conjugation in the silicon atom, which allows a significant delocalization of electrons along of the chain. Thus, the conductivity is intimately connected to the mobility of charge carriers, which in turn depends on the structure and morphology of the system. We report the characterization of polyesters (PEFs) and polyamides (PAFs). Film thicknesses were obtained by ellipsometry. The vibration frequencies of the groups were determined by FT-IR and corroborated by Raman spectroscopy. Structural information was obtained from X-Ray diffraction (XRD). The structural and surface morphology were studied by scanning electron microscope (SEM). Electrical conductivity of the polymers was measured before and after exposure to iodine vapor, for films of different thicknesses. Morphological differentiation was studied by energy dispersive microscopy (EDX), showing a regular distribution of iodine within the polymer. Preliminary conductivity measurements showed adverse effects when oxidation of the polymer films is induced These effects are related to a certain grade of disorder within the system

2,4-Dinitrophenylhydrazine functionalized sodium dodecyl sulfate-coated magnetite nanoparticles for effective removal of Cd(II) and Ni(II) ions from water samples.

PubMed

Sobhanardakani, Soheil; Zandipak, Raziyeh

2015-07-01

2,4-Dinitrophenylhydrazine immobilized on sodium dodecyl sulfate (SDS)-coated magnetite and was used for removal of Cd(II) and Ni(II) ions from aqueous solution. The prepared product was characterized by X-ray diffraction (XRD) analysis, Fourier transform infrared spectroscopy (FT-IR), and scanning electron microscopy (SEM). The size of the nanoparticles according to SEM was obtained around 20-35 nm. In batch tests, the effects of pH, contact time, initial metal concentration, and temperature were studied. The kinetic and equilibrium data were modeled with recently developed models. The adsorption kinetics and isotherms were well fitted by the fractal-like pseudo-second-order model and Langmuir-Freundlich model, respectively. Maximum adsorption capacity by this adsorbent is 255.1 mg g(-1) for Cd(II) ion and 319.6 mg g(-1) for Ni(II) ion at pH 7.0 and 25 °C. The method was successfully applied to the removal of metal cations in real samples (tap water, river water, and petrochemical wastewater).

Environmental performance, mechanical and microstructure analysis of concrete containing oil-based drilling cuttings pyrolysis residues of shale gas.

PubMed

Wang, Chao-Qiang; Lin, Xiao-Yan; He, Ming; Wang, Dan; Zhang, Si-Lan

2017-09-15

The overall objective of this research project is to investigate the feasibility of incorporating oil-based drilling cuttings pyrolysis residues (ODPR) and fly ash serve as replacements for fine aggregates and cementitious materials in concrete. Mechanical and physical properties, detailed environmental performances, and microstructure analysis were carried out. Meanwhile, the early hydration process and hydrated products of ODPR concrete were analyzed with X-ray diffraction (XRD), Fourier transform infrared (FT-IR), scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX). The results indicated that ODPR could not be categorize into hazardous wastes. ODPR had specific pozzolanic characteristic and the use of ODPR had certain influence on slump and compressive strength of concrete. The best workability and optimal compressive strength were achieved with the help of 35% ODPR. Environmental performance tests came to conclusion that ODPR as recycled aggregates and admixture for the preparation of concrete, from the technique perspective, were the substance of mere environmental contamination. Copyright © 2017 Elsevier B.V. All rights reserved.

Synthesis and characterization of the NiFe2O4@TEOS-TPS@Ag nanocomposite and investigation of its antibacterial activity

NASA Astrophysics Data System (ADS)

Allafchian, Ali R.; Jalali, S. A. H.; Amiri, R.; Shahabadi, Sh.

2016-11-01

In this study, the NiFe2O4 was embedded in (3-mercaptopropyl) trimethoxysilane (TPS) and tetraethyl orthosilicate (TEOS) using the sol-gel method. These compounds were used as the support of Ag nanoparticles (Ag NPs). The NiFe2O4@TEOS-TPS@Ag nanocomposites were obtained with the development of bonding between the silver atoms of Ag NPs and the sulfur atoms of TPS molecule. Field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR) were used for the characterization of the Ag nanocomposites. Also, the magnetic properties of these nanocomposites were studied by using a vibrating sample magnetometer (VSM) technique. The disk diffusion, minimum inhibition concentration (MIC) and minimum bactericidal concentrations (MBC) tests were used for the investigation of the antibacterial effect of this nanocomposite against bacterial strains. The synthesized nanocomposite presented high reusability and good antibacterial activity against gram-positive and gram-negative bacteria. Remarkably, this nanocomposite could be easily removed from the disinfected media by magnetic decantation.

Synthesis of magnetic activated carbon/α-Fe2O3 nanocomposite and its application in the removal of acid yellow 17 dye from water.

PubMed

Ranjithkumar, V; Sangeetha, S; Vairam, S

2014-05-30

The adsorption of acid yellow 17 dye on activated carbon/α-Fe2O3 nanocomposite prepared by simple pyrolytic method using iron(II) gluconate was investigated by batch technique. The composite was characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM), and vibrating sample magnetometry (VSM). The size of iron oxide nanoparticles formed from iron(II) gluconate precursor is in the range 5-17nm. The saturation magnetization (Ms), remanence (Mr) and coercivity (Hc) of the magnetic carbon nanocomposite is 5.6emu/g, 1.14emu/g and 448Oe, respectively. The adsorption data are found to fit well with Langmuir and, fairly well with Freundlich and Tempkin isotherms at higher concentration of dye (40-100mg/L). Kinetics data indicate that the adsorption of dye follows pseudo-second order kinetics model. Copyright © 2014 Elsevier B.V. All rights reserved.

Adsorption of an anionic dye on a novel low-cost mesoporous adsorbent: kinetic, thermodynamic and isotherm studies

NASA Astrophysics Data System (ADS)

Msaad, Asmaa; Belbahloul, Mounir; Zouhri, Abdeljalil

2018-05-01

Our activated carbon was prepared successfully using phosphoric acid as an activated agent. The activated carbon was characterized by Scanning Electron Micrograph (SEM), Brunauer-Emmett- Teller (BET), Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD). The aim of our study is to evaluate the adsorption capacity of Methyl Orange (MO) on Ziziphus lotus activated carbon. Adsorption isotherms were studied according to Langmuir and Freundlich Model, and adsorption kinetics according to pseudo-first and second-order. Results show that the maximum adsorption was reached in the first 10min at ambient temperature with a yield of 96.31%. The Langmuir isotherm shows a correlation coefficient of 99.4 % higher than Freundlich model and the adsorption kinetic model follow a pseudo-second-order with a maximum adsorption capacity of 769.23 mg/g. FTIR and X-Ray spectroscopy indicate that our activated carbon has an amorphous structure with the presence of functional groups, where BET analysis revealed a high surface area of 553 mg/g, which facilitate the adsorption process

Preparation and characterization of HA microflowers coating on AZ31 magnesium alloy by micro-arc oxidation and a solution treatment

NASA Astrophysics Data System (ADS)

Tang, Hui; Yu, Dezhen; Luo, Yan; Wang, Fuping

2013-01-01

Magnesium and its alloys are potential biodegradable implant materials due to their attractive biological properties. But the use of magnesium is still hampered by its poor corrosion resistance in physiological fluids. In this work, hydroxyapatite microflowers coating is fabricated by micro-arc oxidation and a solution treatment on AZ31 magnesium alloy. The microstructure and composition are analyzed by scanning electron microscopy (SEM), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR). The potentiodynamic polarization and electrochemical impedance spectroscopy are studied in simulated body fluid (SBF) solution, and the apatite-forming ability is studied also. The results show that the corrosion resistance of the magnesium alloy has been enhanced by MAO coating. And the solution treatment can improve the corrosion resistance of the MAO sample, by forming a barrier layer on the surface of the MAO coating, and by penetrating into the outer layer of the MAO film, sealing the micropores and micro-cracks existed in the MAO coating. In addition, the MAO-ST coating also exhibits a high ability to form apatite.

Crystal Analysis of Multi Phase Calcium Phosphate Nanoparticles Containing Different amount of Magnesium

NASA Astrophysics Data System (ADS)

Gozalian, Afsaneh; Behnamghader, Ali Asghar; Moshkforoush, Arash

In this study, Mg doped hydroxyapatite [(Ca, Mg)10(PO4)6(OH)2] and β-tricalcium phosphate nanoparticles were synthesized via sol gel method. Triethyl phosphite, calcium nitrate tetrahydrate and magnesium nitrate hexahydrate were used as P, Ca and Mg precursors. The ratio of (Ca+Mg)/P and the amount of magnesium (x) were kept constant at 1.67 and ranging x = 0 up to 3 in molecular formula of Ca10-xMgx (PO4)6(OH)2, respectively. Phase composition and chemical structure were performed using X-ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR). Phase percentages, crystallite size, degree of crystallinity and lattice parameters were investigated. The presence of magnesium led to form the Mg doped tricalcium phosphate (β-TCMP) and Mg doped hydroxyapatite (Mg-HA). Based on the results of this study, lattice parameters, degree of crystallinity and crystallite size decreased with magnesium content. In addition, with increasing magnesium content, the amount of CaO phase decreased whereas the amount of MgO phase increased significantly. Obtained results can be used for new biomaterials design.

Effects of sodium salt types on the intermolecular interaction of sodium alginate/antarctic krill protein composite fibers.

PubMed

Zhang, Rui; Guo, Jing; Liu, Yuanfa; Chen, Shuang; Zhang, Sen; Yu, Yue

2018-06-01

Sodium alginate (SA) and antarctic krill protein (AKP) were blended to fabricate the SA/AKP composite fibers by the conventional wet spinning method using 5% CaCl 2 as coagulation solution. The sodium salt was added to the SA/AKP solution to adjust the ionization degree and intermolecular interaction of composite system. The main purpose of this study is to investigate the influences of sodium salt types (NaCl, CH 3 COONa, Na 2 SO 4 ) on the intermolecular interaction of SA/AKP composite fibers. The intermolecular interaction, morphology, crystallinity, thermal stability and mechanical properties of SA/AKP composite fibers were analyzed by fourier transform infrared spectroscopy (FT-IR), scanning electron microscope (SEM), x-ray diffraction (XRD), thermogravimetric analysis (TGA). The results show that the types of sodium salt have obvious influences on the content of both β-sheet, intermolecular hydrogen bond, breaking strength and surface morphology in SA/AKP composite fibers, but have a negligible effect on the crystallinity and thermal stability. Copyright © 2018 Elsevier Ltd. All rights reserved.

Synthesis of Cu/SiO2 Core-Shell Particles Using Hyperbranched Polyester as Template and Dispersant

NASA Astrophysics Data System (ADS)

Han, Wensong

2017-07-01

Third-generation hyperbranched polyester (HBPE3) was synthesized by stepwise polymerization with N, N-diethylol-3-amine methylpropionate as AB2 monomer and pentaerythritol as core molecule. Then, Cu particles were prepared by reduction of copper nitrate with ascorbic acid in aqueous solution using HBPE3 as template. Finally, Cu/SiO2 particles were prepared by coating silica on the surface of Cu particles. The structure and morphology of the samples were characterized by Fourier-transform infrared (FT-IR) spectrometry, x-ray diffraction (XRD) analysis, transmission electron microscopy (TEM), scanning electron microscopy (SEM), and thermogravimetric analysis (TGA). The results confirmed the formation of the silica coating on the surface of Cu and that the Cu/SiO2 particles had spherical shape with particle size in the range of 0.8 μm to 2 μm. Compared with pure Cu, the synthesized Cu/SiO2 core-shell particles exhibited better oxidation resistance at high temperature. Moreover, the oxidation resistance of the Cu/SiO2 particles increased significantly with increasing tetraethyl orthosilicate (TEOS) concentration.

Synthesis and structural properties of (Y, Sr)(Ti, Fe, Nb)O3-δ perovskite nanoparticles fabricated by modified polymer precursor method

NASA Astrophysics Data System (ADS)

Miruszewski, T.; Gdaniec, P.; Karczewski, J.; Bochentyn, B.; Szaniawska, K.; Kupracz, P.; Prześniak-Welenc, M.; Kusz, B.

2016-09-01

The yttrium, iron and niobium doped-SrTiO3 powders have been successfully fabricated by a modified low-temperature synthesis method from a polymer complex. The usage of strontium hydroxide precursor instead of conventional strontium nitrate or strontium carbonate provides to the possibility of significant decrease of annealing temperature. It allows to prepare a material with sphere-shape grains of nanometric size (15-70 nm). The results of thermal analysis indicate that the crystallization of precursor takes place at different stages. The product after heat treatment at 600 °C for 3 h in air was also characterized by X-Ray diffraction method (XRD) and Fourier transform - infrared spectroscopy (FT-IR). After the crystallization and the impurity removal process, a single-phase material was obtained in case of all analyzed samples. The morphology of obtained nano-powders was also studied by a scanning electron microscopy (SEM). It can be concluded, that this method allows obtaining a perovskite phase of a metal doped SrTiO3 with nanometric particles.

Nanostructures formed by cyclodextrin covered procainamide through supramolecular self assembly - Spectral and molecular modeling study

NASA Astrophysics Data System (ADS)

Rajendiran, N.; Mohandoss, T.; Sankaranarayanan, R. K.

2015-02-01

Inclusion complexation behavior of procainamide (PCA) with two cyclodextrins (α-CD and β-CD) were analyzed by absorption, fluorescence, scanning electron microscope (SEM), transmission electron microscope (TEM), Raman image, FT-IR, differential scanning colorimeter (DSC), Powder X ray diffraction (XRD) and 1H NMR. Blue shift was observed in β-CD whereas no significant spectral shift observed in α-CD. The inclusion complex formation results suggest that water molecules also present in the inside of the CD cavity. The present study revealed that the phenyl ring of the PCA drug is entrapped in the CD cavity. Cyclodextrin studies show that PCA forms 1:2 inclusion complex with α-CD and β-CD. PCA:α-CD complex form nano-sized particles (46 nm) and PCA:β-CD complex form self-assembled to micro-sized tubular structures. The shape-shifting of 2D nanosheets into 1D microtubes by simple rolling mechanism were analysed by micro-Raman and TEM images. Thermodynamic parameters (ΔH, ΔG and ΔS) of inclusion process were determined from semiempirical PM3 calculations.

Ferrocene adsorbed into the porous octakis(hydridodimethylsiloxy)silsesquioxane after thermolysis in tetrahydrofuran media: An applied surface for ascorbic acid determination

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

Ribeiro do Carmo, Devaney, E-mail: docarmo@dfq.feis.unesp.br; Lataro Paim, Leonardo; Ramos Stradiotto, Nelson

Highlights: Black-Right-Pointing-Pointer Octakis(hydridodimethylsiloxi)silsesquioxane was synthesized and Ferrocene was adsorbed. Black-Right-Pointing-Pointer Polymeric net through electrostatic interactions was observed. Black-Right-Pointing-Pointer The novel materials presents electroacatalytic activity for Ascorbic acid. -- Abstract: Octakis(hydridodimethylsiloxi)silsesquioxane (Q{sub 8}M{sub 8}{sup H}) was synthesized and Ferrocene was adsorbed in a polymeric net through electrostatic interactions, with anion forming after the cleavage of any siloxy groups (ESFc). The nanostructured materials (Q{sub 8}M{sub 8}{sup H} and EsFc) were characterized by Fourier transform infrared spectra (FT-IR), nuclear magnetic resonance (NMR), X-ray diffraction (XRD), Thermogravimetric analyses and Voltammetric technique The cyclic voltammograms of the graphite paste electrode modified with ESFc showed onemore » redox couple with E{sup 0} Prime = 0.320 V (1.0 mol L{sup -1} NaCl, v = 50 mV s{sup -1}), with a diffusion-controlled process and the redox process shows electrocatalytic activity for the oxidation of ascorbic acid.« less

Copper nanoparticles mediated by chitosan: synthesis and characterization via chemical methods.

PubMed

Usman, Muhammad Sani; Ibrahim, Nor Azowa; Shameli, Kamyar; Zainuddin, Norhazlin; Yunus, Wan Md Zin Wan

2012-12-14

Herein we report a synthesis of copper nanoparticles (Cu-NPs) in chitosan (Cts) media via a chemical reaction method. The nanoparticles were synthesized in an aqueous solution in the presence of Cts as stabilizer and CuSO(4)·5H(2)O precursor. The synthesis proceeded with addition of NaOH as pH moderator, ascorbic acid as antioxidant and hydrazine( )as the reducing agent. The characterization of the prepared NPs was done using ultraviolet-visible spectroscopy, which showed a 593 nm copper band. The Field Emission Scanning Electron Microscope (FESEM) images were also observed, and found to be in agreement with the UV-Vis result, confirming the formation of metallic Cu-NPs. The mean size of the Cu-NPs was estimated to be in the range of 35-75 nm using X-ray diffraction. XRD was also used in analysis of the crystal structure of the NPs. The interaction between the chitosan and the synthesized NPs was studied using Fourier transform infrared (FT-IR) spectroscopy, which showed the capping of the NPs by Cts.

Preparation of nanobiochar as magnetic solid acid catalyst by pyrolysis-carbonization from oil palm empty fruit bunches

NASA Astrophysics Data System (ADS)

Jenie, S. N. Aisyiyah; Kristiani, Anis; Kustomo, Simanungkalit, Sabar; Mansur, Dieni

2017-11-01

Nanomaterials based on carbon exhibits unique properties, both physical and chemical, that can be utilized in various application, including catalyst. These nanomaterials were prepared through pyrolysis-carbonization process of biomass, oil palm empty fruit bunches. The effect of carbonization temperature in range of 500°C-600°C were also studied. The magnetic nanobiochar samples, MBC, were sulfonated by using sulfuric acid to increase their properties as solid acid catalyst. Their chemical and physical properties were characterized by Surface Area Analyzer and Porositymeter, X-Ray Diffraction, Scanning Electron Microscopy, Fourier Transform Infra-Red. The magnetic biochar samples obtained from carbonization at 873 K, MBC02-SO3H, was proven to have higher surface area, crystallinity properties and surface chemical composition after sulfonation process, which were confirmed by the BET, XRD and FT-IR analysis. Moreover, sample MBC02-SO3H exhibit promising catalytic acitivity in a catalysed esterification reaction, producing an ester yield of 64%. The result from this work opens new opportunities for the development of magnetic heterogenous acid catalyst from biomass waste.

Preparation and characterization of uniform nanosized cephradine by combination of reactive precipitation and liquid anti-solvent precipitation under high gravity environment.

PubMed

Zhong, Jie; Shen, Zhigang; Yang, Yan; Chen, Jianfeng

2005-09-14

In this work, a novel direct method, which was combined with reactive precipitation and liquid anti-solvent precipitation under high gravity environment, had been developed to prepare nanosized cephradine with narrow particle size distribution. Compared with commercial crude cephradine, the prepared cephradine showed a significant decrease in particle size, a significant increase in the specific surface area and shorter dissolving time when used for injection. The characteristic particle size was between 200-400 nm. The specific surface area increased from 2.95 to 10.87 m2/g after micronization. When the amount of L-arginin decreased from 0.25 to 0.18 g, the mixture of nanosized cephradine and L-arginine could still dissolve in 1 min. The X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR) analysis indicated that the physical characteristics and molecular states remained unchanged after the recrystallization process. This method had potential application in industrial fields because of its low cost, efficient processing and the ease of scaling-up.

Immobilization of ionophore and surface characterization studies of the titanium(III) ion in a PVC-membrane sensor.

PubMed

Rezayi, Majid; Heng, Lee Yook; Kassim, Anuar; Ahmadzadeh, Saeid; Abdollahi, Yadollah; Jahangirian, Hossein

2012-01-01

Novel ionophores comprising various hydroxide and amine structures were immobilized onto poly(vinyl chloride) (PVC) matrices, and these were examined to determine Ti(III) selectivity. To predict the selectivity of Ti(III), a PVC membrane was used to investigate the binding of Ti(III) to c-methylcalix[4]resorcinarene (CMCR). The study showed that the chelating ligand, CMCR, was coordinated selectively to Ti(III) at eight coordination sites involving the oxygen atoms at the interface of the membrane/solution. The membrane was prepared, based on CMCR as an ionophore, sodium tetrakis(4-fluorophenyl) borate (NaTFPB) as a lipophilic ionic additive, and dioctylphthalate (DOP) as a plasticizer. The immobilization of the ionophore and surface characterization studies revealed that the performance of CMCR-immobilized PVC was equivalent to that of mobile ionophores in supported liquid membranes (SLMs). The strengths of the ion-ionophore (CMCR-Ti(OH)(OH(2))(5) (2+)) interactions and the role of ionophores on membranes were studied via UV-Vis, Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and and X-ray diffraction (XRD).

Novel chemical synthesis and characterization of copper pyrovanadate nanoparticles and its influence on the flame retardancy of polymeric nanocomposites

NASA Astrophysics Data System (ADS)

Ghiyasiyan-Arani, Maryam; Masjedi-Arani, Maryam; Ghanbari, Davood; Bagheri, Samira; Salavati-Niasari, Masoud

2016-05-01

In this work, copper pyrovanadate (Cu3V2O7(OH)2(H2O)2) nanoparticles have been synthesized by a simple and rapid chemical precipitation method. Different copper-organic complexes were used to control the size and morphology of products. The morphology and structure of the as-synthesized products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectrum, electron dispersive X-ray spectroscopy (EDX), thermal gravimetric analysis (TGA), differential thermal analysis (DTA) and photoluminescence (PL) spectroscopy. The influence of copper pyrovanadate nanostructures on the flame retardancy of the polystyrene, poly vinyl alcohol and cellulose acetate was studied. Dispersed nanoparticles play the role of a magnetic barrier layer, which slows down product volatilization and prevents the flame and oxygen from the sample during decomposition of the polymer. Cu3V2O7(OH)2(H2O)2 is converted to Cu3V2O8 with an endothermic reaction which simultaneously releases water and decrease the temperature of the flame region.

Electrospun montmorillonite modified poly(vinylidene fluoride) nanocomposite separators for lithium-ion batteries

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

Fang, Changjiang; Yang, Shuli; Zhao, Xinfei

2016-07-15

Highlights: • Composite separators of PVDF and MMT for lithium-ion batteries were electrospun. • Thermal dimensional stability and tensile property of composite separators get improved. • Presence of montmorillonite promotes electrical properties of PVDF fibrous separators. • Batteries consisting of PVDF/MMT-5% separator achieve the best performance. - Abstract: Composite separators of poly(vinylidene fluoride) (PVDF) with different contents of montmorillonite (MMT) for Li-ion batteries have been fabricated by electrospinning. The morphology, function group, crystallinity, and mechanical properties of membranes were investigated by scanning electron microscope (SEM), Fourier Transform infrared spectra (FT-IR), differential scanning calorimetry (DSC), and tensile test, respectively. Interlayer spacingmore » of MMT in polymer was characterized by X-ray diffraction (XRD). In addition, the results of electrochemical measurements suggest that PVDF/MMT-5% composite membrane has maximum ionic conductivity of 4.2 mS cm{sup −1}, minimum interfacial resistance of 97 Ω, and excellent electrochemical stability. The cell comprising PVDF/MMT-5% composite membrane shows higher capacity and more stable cycle performance than the one using commercial Celgard PP membrane.« less

Enhancement of antioxidant and antibacterial properties for tannin acid/chitosan/tripolyphosphate nanoparticles filled electrospinning films: Surface modification of sliver nanoparticles.

PubMed

Zhan, Fuchao; Sheng, Feng; Yan, Xiangxing; Zhu, Yingrui; Jin, Weiping; Li, Jing; Li, Bin

2017-11-01

The tannin acid/chitosan/tripolyphosphate nanoparticles were encapsulated in polyvinyl alcohol (PVA)/poly-acrylic acid (PAA) electrospinning films by electrostatic spinning technology. To optimize the prepared condition, properties and morphology of nanoparticles were characterized by dynamic light scattering (DLS) and transmission electron microscope (TEM). The optimized initial concentration of tannin, chitosan and tripolyphosphate solutions were 1, 1, 0.5mg/ml, respectively, with adding proportion for 5:5:1. The average diameter of tannin acid/chitosan/tripolyphosphate nanoparticles was ∼80nm. The electrospinning films showed an excellent water-resistant property with 0.5wt%N,N'-Methylenebisacrylamide (MBA). Due to the antioxidant and antibacterial of tannic acid, the films possessed these properties. The antioxidant and antibacterial of these fibers significantly improved after in situ formation of silver nanoparticles (AgNPs). Electrospun films were characterized by scanning electron microscopy (SEM), Fourier transform infrared spectra (FT-IR), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). Copyright © 2017 Elsevier B.V. All rights reserved.

Transition metal ions effect on the properties and photocatalytic activity of nanocrystalline TiO2 prepared in an ionic liquid.

PubMed

Ghasemi, S; Rahimnejad, S; Setayesh, S Rahman; Rohani, S; Gholami, M R

2009-12-30

TiO(2) and transition metal (Cr, Mn, Fe, Co, Ni, Cu, and Zn) doped TiO(2) nanoparticles were synthesized by the sol-gel method using 2-hydroxylethylammonium formate as an ionic liquid. All the prepared samples were calcined at 500 degrees C and characterized by X-ray diffraction (XRD), BET surface area determination, energy dispersive X-ray (EDX) analysis, diffuse reflectance spectroscopy (DRS), and Fourier transformed infrared (FT-IR) techniques. The studies revealed that transition metal (TM) doped nanoparticles have smaller crystalline size and higher surface area than pure TiO(2). Dopant ions in the TiO(2) structure caused significant absorption shift into the visible region. The results of photodegradation of Acid Blue92 (AB92) in aqueous medium under UV light showed that photocatalytic activity of TiO(2) nanoparticles was significantly enhanced by the presence of some transition metal ions. Chemical Oxygen Demand (COD) of dye solutions were done at regular intervals gave a good idea about mineralization of dye.

Preparation and characterizaton of CaO nanoparticle for biodiesel production

NASA Astrophysics Data System (ADS)

Gupta, Jharna; Agarwal, Madhu

2016-04-01

Nanoparticle of CaO from calcium Nitrate (CaO/CaN) and Snail shell (CaO/SS) are successfully synthesized by method as described in the literature and used as an active and stable catalyst for the biodiesel production. These catalysts are characterized by Fourier-transform infrared spectra (FT-IR), X-ray diffraction (XRD), and thermal gravimetric analysis (TGA). The average crystalline size in nanometer was also calculated by Debye-Scherrer equation. The performance of the CaO/CaN and CaO/SS were tested for their catalytic activity via transesterification process and it was found that biodiesel yield has been increased from 93 to 96%. The optimum conditions for the highest yield were 8wt% catalyst loading, 65°C temperature, 12:1 methanol/oil molar ratio, and 6 h for reaction time. The nano catalyst from snail shell exhibits excellent catalytic activity and stability for the transesterification reaction, which suggested that this catalyst would be potentially used as a solid base nano catalyst for biodiesel production. In order to examine the reusability of catalyst developed from snail shell, five transesterification reaction cycles were also performed.

Surface modification of montmorillonite on surface Acid-base characteristics of clay and thermal stability of epoxy/clay nanocomposites.

PubMed

Park, Soo-Jin; Seo, Dong-Il; Lee, Jae-Rock

2002-07-01

In this work, the effect of surface treatments on smectitic clay was investigated in surface energetics and thermal behaviors of epoxy/clay nanocomposites. The pH values, X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FT-IR) were used to analyze the effect of cation exchange on clay surface and the exfoliation phenomenon of clay interlayer. The surface energetics of clay and thermal properties of epoxy/clay nanocomposites were investigated in contact angles and thermogravimetric analysis (TGA), respectively. From the experimental results, the surface modification of clay by dodecylammonium chloride led to the increases in both distance between silicate layers of about 8 A and surface acid values, as well as in the electron acceptor component (gamma(+)(s)) of surface free energy, resulting in improved interfacial adhesion between basic (or electron donor) epoxy resins and acidic (electron acceptor) clay interlayers. Also, the thermal stability of nanocomposites was highly superior to pure epoxy resin due to the presence of the well-dispersed clay nanolayer, which has a barrier property in a composite system.

Synthesis of N-doped potassium tantalate perovskite material for environmental applications

NASA Astrophysics Data System (ADS)

Rao, Martha Purnachander; Nandhini, Vellangattupalayam Ponnusamy; Wu, Jerry J.; Syed, Asad; Ameen, Fuad; Anandan, Sambandam

2018-02-01

Nitrogen containing potassium tantalate perovskite material has been synthesized by the solvothermal method using urea (CH4N2O) as a nitrogen source. The as-prepared sample was characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), diffuse reflectance spectroscopy (DRS), scanning electron microscope (SEM), and energy-dispersive X-ray spectroscopy (EDX) and X-ray photoelectron spectroscopy (XPS). The particle size of nitrogen containing KTaO3 observed from SEM images was found to be 100-150 nm. Doping KTaO3 with nitrogen causes reduction of band gap from 3.5 to 2.54 eV. The incorporation of Nitrogen into the crystal lattice of KTaO3 not only extended the absorption of light from UV (ultraviolet) region to visible region and also enhanced the photocatalytic activity. As prepared nitrogen containing KTaO3 samples exhibit cubic-like morphology and noticed efficient photocatalytic activity towards methylene blue dye degradation under visible light illumination. The intermediates formed during photodegradation were identified by mass spectrometry (GC-MS) and proposed suitable degradation pathway.

Enzymatic production of N-acetyl-d-glucosamine from crayfish shell wastes pretreated via high pressure homogenization.

PubMed

Wei, Guoguang; Zhang, Alei; Chen, Kequan; Ouyang, Pingkai

2017-09-01

This study presents an efficient pretreatment of crayfish shell using high pressure homogenization that enables N-acetyl-d-glucosamine (GlcNAc) production by chitinase. Firstly, the chitinase from Serratia proteamaculans NJ303 was screened for its ability to degrade crayfish shell and produce GlcNAc as the sole product. Secondly, high pressure homogenization, which caused the crayfish shell to adopt a fluffy netted structure that was characterized by Scanning electron microscope (SEM), Fourier transform infrared spectrometer (FT-IR), X-ray diffraction (XRD), was evaluated as the best pretreatment method. In addition, the optimal conditions of high pressure homogenization of crayfish shell were determined to be five cycles at a pressure of 400bar, which achieved a yield of 3.9g/L of GlcNAc from 25g/L of crayfish shell in a batch enzymatic reaction over 1.5h. The results showed high pressure homogenization might be an efficient method for direct utilization of crayfish shell for enzymatic production of GlcNAc. Copyright © 2017 Elsevier Ltd. All rights reserved.

Hybrid structure of polyaniline/ZnO nanograss and its application in dye-sensitized solar cell with performance improvement

NASA Astrophysics Data System (ADS)

Zhu, Shibu; Wei, Wei; Chen, Xiangnan; Jiang, Man; Zhou, Zuowan

2012-06-01

Polyaniline (PANI) hybridized ZnO photoanode for dye-sensitized solar cell (DSSC) was primarily prepared via a two-step process which involved hydrothermal growth of ZnO nanograss on the fluorine-doped tin oxide (FTO) substrate and subsequently chemisorption of PANI on the surfaces of the ZnO nanorods. The PANI hybridized ZnO nanograss films were characterized by scanning electron microscope (SEM), X-ray diffraction (XRD) and Fourier transform infrared spectra (FT-IR), and the results indicated that there were chemical interactions between PANI and ZnO. Both pure ZnO nanograss and PANI hybridized ZnO nanograss were applied to DSSC. The results of photoelectrochemical measurement showed that the photocurrent density of PANI (100 mg/L) hybridized ZnO nanograss photoanode was significantly enhanced, and the overall light-conversion efficiency increased by 60%. The electrochemical impedance spectra (EIS) displayed that the electron densities in photoanodes of PANI hybridized ZnO nanograss were larger than that in pure ZnO nanograss. This is ascribed to more effective charge separation and faster interfacial charge transferring occurred in the hybrid photoanode.

Energy transfer from Pr3+ to Gd3+ ions in BaB8O13 phosphor for phototherapy lamps

NASA Astrophysics Data System (ADS)

Tamboli, Sumedha; Nair, Govind B.; Dhoble, S. J.; Burghate, D. K.

2018-04-01

A series of BaB8O13 phosphors doped with different concentrations of Gd3+ ions and co-doped with Pr3+ ions were synthesized by solid state synthesis method. X-ray powder diffraction (XRD) analysis confirmed the formation of the compound in a crystalline and homogeneous form. Scanning Electron Microscopy (SEM) was performed to study the surface morphology of the compound and Fourier Transform Infrared (FT-IR) spectroscopy measurements determined the nature of bonding between elements of the compounds. The photoluminescence (PL) excitation spectra of BaB8O13:Gd3+ phosphor showed excitation peaks at 246 nm, 252 nm and 274 nm. The prominent emission peak was observed at 313 nm which is in narrow band ultraviolet B (NB-UVB) range. Energy transfer was achieved by co-doping Pr3+ ions with Gd3+ ions. PL decay time was also measured for BaB8O13: Gd3+, Pr3+ phosphor. Emission at 313 nm can be used for the treatment of skin diseases.

An efficient one-pot synthesis of 1,4-disubstituted 1,2,3-triazoles at room temperature by green synthesized Cu NPs using Otostegia persica leaf extract.

PubMed

Nasrollahzadeh, Mahmoud; Sajadi, S Mohammad; Mirzaei, Yousef

2016-04-15

In this study, copper nanoparticles (Cu NPs) were synthesized using a rapid, single step and completely green biosynthetic method by reduction of CuCl2 · 2H2O solution with aqueous extract of leaves of Otostegia persica containing flavonoid and other phenolics as a main factor which acts as reducing agent and efficient stabilizer. UV-vis spectra gave surface plasmon resonance (SPR) at 560 nm. The Cu NPs were characterized by transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD). A possible synthesis mechanism of Cu NPs was presented. In addition, we investigated the catalytic activity of Cu NPs for the one-pot synthesis of 1,4-disubstituted 1,2,3-triazoles under mild reaction conditions with good to excellent yields. The catalyst could be easily recovered by centrifugation and reused at least five recycles with no significant decreases in the yields. Copyright © 2016 Elsevier Inc. All rights reserved.

Synthesis of Fluorinated Graphene/CoAl-Layered Double Hydroxide Composites as Electrode Materials for Supercapacitors.

PubMed

Peng, Weijun; Li, Hongqiang; Song, Shaoxian

2017-02-15

CoAl-layered double hydroxide/fluorinated graphene (CoAl-LDH/FGN) composites were fabricated via a two-step hydrothermal method. The synthesized CoAl-LDH/FGN composites have been characterized by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), field-emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDS), and electrochemical measurements. The results indicated that the fluorinated carbon with various configuration forms were grafted onto the framework of graphene, and the C-F bond configuration and fluorine content could be tuned by the fluorination time. Most of semi-ionic C-F bonds were formed at an appropriate fluorination time and, then, converted into fluorine rich surface groups (such as CF 2 , CF 3 , etc.) which were electrochemically inactive as the fluorination time prolonged. Moreover, the CoAl-LDH/FGN composites prepared at the optimal fluorination time exhibited the highest specific capacitance (1222 F/g at 1 A/g), the best rate capability, and the most stable capacitance retention, which offered great promise as electrode materials for supercapacitors.

Solar photocatalytic degradation of isoproturon over TiO2/H-MOR composite systems.

PubMed

Sharma, Mangalampalli V Phanikrishna; Durgakumari, Valluri; Subrahmanyam, Machiraju

2008-12-30

The photocatalytic degradation and mineralization of isoproturon herbicide was investigated in aqueous solution containing TiO2 over H-mordenite (H-MOR) photocatalysts under solar light. The catalysts are characterized by X-ray diffraction (XRD), UV-Vis diffused reflectance spectra (UV-Vis DRS), Fourier transform-infra red spectra (FT-IR) and scanning electron microscopy (SEM) techniques. The effect of TiO2, H-MOR support and different wt% of TiO2 over the support on the photocatalytic degradation and influence of parameters such as TiO2 loading, catalyst amount, pH and initial concentration of isoproturon on degradation are evaluated. 15wt% TiO2/H-MOR composite is found to be optimum. The degradation reaction follows pseudo-first order kinetics and is discussed in terms of Langmuir-Hinshelwood (L-H) kinetic model. The extent of isoproturon mineralization studied with chemical oxygen demand (COD) and total organic carbon (TOC) measurements and approximately 80% mineralization occurred in 5h. A plausible mechanism is proposed based on the intermediates identified by liquid chromatography-mass spectroscopy (LC-MS).

Studies on growth, thermal, optical, vibrational properties and hyperpolarizability of a complex orthonitroaniline with picric acid

NASA Astrophysics Data System (ADS)

Anandhi, S.; Shyju, T. S.; Gopalakrishnan, R.

2010-11-01

The present article reports the growth of single crystals of a complex Orthonitroaniline with picric acid (2[C 6H 6N 2O 2]·C 6H 2(NO 2) 3OH) (ONAP) by solution growth (slow evaporation) method at room temperature. Single crystal XRD, UV-vis spectral analysis and TGA/DTA studies were carried out. FT-IR and Raman spectra were recorded to explore information of the functional groups. The high-resolution X-ray diffraction curve reveals the internal structural low angle boundaries. The PL spectrum of the title compound shows green emission. Dielectric behaviour was investigated at 33 and 70 °C. The dipole moment and first-order hyperpolarizability ( β) values were evaluated by using Gaussian 98 W software package with the help of B3LYP the density functional theory (DFT) method. The possible modes of vibrations are theoretically predicted by factor group analysis. The mechanical stability of the grown crystal was tested with Vicker's microhardness tester and the work hardening coefficient of the grown material was estimated.

New ZnO@Cardanol Porphyrin Composite Nanomaterials with Enhanced Photocatalytic Capability under Solar Light Irradiation

PubMed Central

Ribeiro, Viviane Gomes Pereira; Marcelo, Ana Maria Pereira; da Silva, Kássia Teixeira; da Silva, Fernando Luiz Firmino; Mota, João Paulo Ferreira; do Nascimento, João Paulo Costa; Sombra, Antonio Sérgio Bezerra; Clemente, Claudenilson da Silva; Mazzetto, Selma Elaine

2017-01-01

This work describes the synthesis, characterization, and photocatalytic activity of new composite nanomaterials based on ZnO nanostructures impregnated by lipophlilic porphyrins derived from cashew nut shell liquid (CNSL). The obtained nanomaterials were characterized by X-ray diffraction (XRD), UV-Vis diffuse reflectance spectroscopy (DRS), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), and steady-state photoluminescence spectra (PL). The results confirm nanostructures showing average diameter of 55 nm and an improved absorption in the visible region. Further, the FTIR analysis proved the existence of non-covalent interactions between the porphyrin molecules and ZnO. The photocatalytic activity of prepared photocatalysts was investigated by degradation of rhodamine B (RhB) in aqueous solution under visible light irradiation and natural sunlight. It was demonstrated that the photocatalytic activity increases in the presence of the porphyrins and, also, depends on the irradiation source. The development of composite photocatalysts based on porphyrins derived from CNSL provides an alternative approach to eliminate efficiently toxic wastes from water under ambient conditions. PMID:28934117

Solvothermal synthesis of well-dispersed MF2 (M = Ca,Sr,Ba) nanocrystals and their optical properties

NASA Astrophysics Data System (ADS)

Zhang, Xiaoming; Quan, Zewei; Yang, Jun; Yang, Piaoping; Lian, Hongzhou; Lin, Jun

2008-02-01

MF2 (M = Ca,Sr,Ba) nanocrystals (NCs) were synthesized via a solvothermal process in the presence of oleic acid and characterized by x-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectra, UV/vis absorption spectra, photoluminescence (PL) excitation and emission spectra, and lifetimes, respectively. In the synthetic process, oleic acid as a surfactant played a crucial role in confining the growth and solubility of the MF2 NCs. The as-prepared CaF2, SrF2 and BaF2 NCs present morphologies of truncated octahedron, cube and sheet in a narrow distribution, respectively. Possible growth mechanisms were proposed to explain these results. The as-prepared NCs are highly crystalline and can be well dispersed in cyclohexane to form stable and clear colloidal solutions, which demonstrate strong emission bands centred at 400 nm in photoluminescence (PL) spectra compared with the cyclohexane solvent. The PL properties of the colloidal solutions of the as-prepared NCs can be ascribed to the trap states of surface defects.

Graft polymerization of guar gum with acryl amide irradiated by microwaves for colonic drug delivery.

PubMed

Shahid, Muhammad; Bukhari, Shazia Anwer; Gul, Yousra; Munir, Hira; Anjum, Fozia; Zuber, Mohammad; Jamil, Tahir; Zia, Khalid Mahmood

2013-11-01

This article is aimed to discuss the modification of guar gum through microwave irradiation by varying the time of irradiation. The characterization of the modified products was carried out using FTIR spectroscopic analysis. The FT-IR spectrum of the pure guar gum (GG) sample showed a broad peak at 3298 cm(-1) while the modified GG sample displayed a peak at 1541 cm(-1) which was absent in the crude sample. The X-ray diffraction (XRD) analysis confirmed the increase in crystallinity due to grafting of the sample with polyacrylamide (GG-g-PAM). Scanning electron microscope (SEM) images revealed that granular form of guar gum was changed into fibrillar structure after grafting. Thermo-gravimetric analysis of the modified samples was also carried out and discussed. The role of guar gum as a matrix for controlled release of drug triamcinolone was evaluated. The GG-acrylamide grafted samples presented a correlation between drug release and time of microwave exposure. The results revealed that such modified product has potential applications in colonic drug delivery system. Copyright © 2013 Elsevier B.V. All rights reserved.

Formation of Ag nanoframes with facilitation of dithiols.

PubMed

Cheng, Fong-Yu; Hu, Kuo-Wei; Yeh, Chen-Sheng

2012-03-01

Two-dimensional Ag nanoprisms readily formed Ag triangular nanoframes upon electron beam irradiation. Following meso-2, 3-dimercaptosuccinicacid (DMSA) ripening behavior, continuous electron beam exposure transformed a solid nanoplate into a core/void/shell morphology, which then evolved into a hollow nanoframe structure. TEM was used to observe the ripening and etching processes of Ag nanoprisms as a function of DMSA concentration and electron irradiation time. X-ray diffraction (XRD) and FT-IR analysis were conducted to characterize the Ag nanoprism structure and surface before and after treatment with DMSA. X-ray photoelectron spectroscopy (XPS) was used to determine surface chemical compositions and indicated DMSA was adsorbed on the Ag nanoprisms in the form of Ag(+)-S(-). Raman measurements provided evidence of a disulfide group on Ag nanoprisms. Similar organosulfur structures such as mercaptosuccinic acid and 2-mercaptoacetic acid were also studied with results suggesting that the two S-H groups of dithiol DMSA played the crucial role in nanoframe fabrication. Using the same strategy with DMSA, the nano-architecture can be extended to 2D nanodiscs yielding nanorings.

Spectroscopic, Homo-Lumo and NLO studies of tetra fluoro phthalate doped Coumarin crystals using DFT method

NASA Astrophysics Data System (ADS)

Latha, B.; Kumaresan, P.; Nithiyanantham, S.; Sampathkumar, K.

2017-08-01

In the present examination, a methodical study has been done on the development of unadulterated and Coumarin doped Tetrafluoro Phthalate precious stones. Powder X-beam diffraction studies were done and the cross section parameters were computed by minimum square technique in pure and doped crystals. FT-IR, UV-Vis, Thermal, Micro-hardness and Dielectric studies were additionally done for the pure and doped crystals. The tentatively watched FT-IR and FT-Raman groups were allotted to various ordinary methods of the atom. The steadiness and charge delocalization of the particle were likewise concentrations were done by characteristic security orbital (NBO) examination. The HOMO-LUMO energies depict the charge exchange happens inside the particle. Atomic electrostatic potential has been broken down the electronic properties such as excitation energies, oscillator quality, wavelengths and HOMO-LUMO energies were acquired by time-subordinate DFT (TD-DFT) approach. The SHG of pure and doped TFP stones were examined through Nd:YAG Q-exchanged laser.

FT-IR characterization of articulated ceramic bricks with wastes from ceramic industries

NASA Astrophysics Data System (ADS)

Nirmala, G.; Viruthagiri, G.

The 30 ceramic test samples with the kaolinitic clay and ceramic rejects (in the as-received state and sintered at temperatures 900-1200 °C) were investigated through spectral studies in order to elucidate the possibility of recycling the wastes from the government ceramic industry of Vriddhachalam, Tamilnadu state, South India. A detailed attribution of all the spectroscopic frequencies in the spectra recorded in the 4000-400 cm-1 region was attempted and their assignment to different minerals was accomplished. X-ray diffraction analysis was performed to demonstrate the reliability of IR attributions. The indication of well-ordered kaolinite is by the band at 1115 cm-1 in the raw samples which tends to shift towards 1095 cm-1 in all the fired samples. The peaks at 563 cm-1 and 795 cm-1 can be assigned to anorthite and dickite respectively. The presence of quartz and anorthite is confirmed both by XRD and FTIR. The microstructural observations were done through the SEM images which visualized the vitrification of the fired bricks at higher temperatures. The refractory properties of the samples found through the XRF analysis are also appreciable. The present work suggests that the incorporation of the rejects into the clay mixture will be a valid route for the ceramic industries to reduce the costs of the ceramic process.

FT-IR characterization of articulated ceramic bricks with wastes from ceramic industries.

PubMed

Nirmala, G; Viruthagiri, G

2014-05-21

The 30 ceramic test samples with the kaolinitic clay and ceramic rejects (in the as-received state and sintered at temperatures 900-1200°C) were investigated through spectral studies in order to elucidate the possibility of recycling the wastes from the government ceramic industry of Vriddhachalam, Tamilnadu state, South India. A detailed attribution of all the spectroscopic frequencies in the spectra recorded in the 4000-400cm(-1) region was attempted and their assignment to different minerals was accomplished. X-ray diffraction analysis was performed to demonstrate the reliability of IR attributions. The indication of well-ordered kaolinite is by the band at 1115cm(-1) in the raw samples which tends to shift towards 1095cm(-1) in all the fired samples. The peaks at 563cm(-1) and 795cm(-1) can be assigned to anorthite and dickite respectively. The presence of quartz and anorthite is confirmed both by XRD and FTIR. The microstructural observations were done through the SEM images which visualized the vitrification of the fired bricks at higher temperatures. The refractory properties of the samples found through the XRF analysis are also appreciable. The present work suggests that the incorporation of the rejects into the clay mixture will be a valid route for the ceramic industries to reduce the costs of the ceramic process. Copyright © 2014 Elsevier B.V. All rights reserved.

Preparation, characterization, and optical properties of gold, silver, and gold-silver alloy nanoshells having silica cores.

PubMed

Kim, Jun-Hyun; Bryan, William W; Lee, T Randall

2008-10-07

This report describes the structural and optical properties of a series of spherical shell/core nanoparticles in which the shell is comprised of a thin layer of gold, silver, or gold-silver alloy, and the core is comprised of a monodispersed silica nanoparticle. The silica core particles were prepared using the Stöber method, functionalized with terminal amine groups, and then seeded with small gold nanoparticles (approximately 2 nm in diameter). The gold-seeded silica particles were coated with a layer of gold, silver, or gold-silver alloy via solution-phase reduction of an appropriate metal ion or mixture of metal ions. The size, morphology, and elemental composition of the composite nanoparticles were characterized by field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, thermal gravimetric analysis (TGA), dynamic light scattering (DLS), and transmission electron microscopy (TEM). The optical properties of the nanoparticles were analyzed by UV-vis spectroscopy, which showed strong absorptions ranging from 400 nm into the near-IR region, where the position of the plasmon band reflected not only the thickness of the metal shell, but also the nature of the metal comprising the shell. Importantly, the results demonstrate a new strategy for tuning the position of the plasmon resonance without having to vary the core diameter or the shell thickness.

Crystal structure determination of new antimitotic agent bis(p-fluorobenzyl)trisulfide.

PubMed

An, Haoyun; Hu, Xiurong; Gu, Jianming; Chen, Linshen; Xu, Weiming; Mo, Xiaopeng; Xu, Wanhong; Wang, Xiaobo; Xu, Xiao

2008-01-01

The purpose of this research was to investigate the physical characteristics and crystalline structure of bis(p-fluorobenzyl)trisulfide, a new anti-tumor agent. Methods used included X-ray single crystal diffraction, X-ray powder diffraction (XRPD), Fourier-transform infrared (FT-IR) spectroscopy, differential scanning calorimetric (DSC) and thermogravimetric (TG) analyses. The findings obtained with X-ray single crystal diffraction showed that a monoclinic unit cell was a = 12.266(1) A, b = 4.7757(4) A, c = 25.510(1) A, beta = 104.25(1) degrees ; cell volume = 1,448.4(2) A(3), Z = 4, and space group C2/c. The XRPD studies of the four crystalline samples, obtained by recrystallization from four different solvents, indicated that they had the same diffraction patterns. The diffraction pattern stimulated from the crystal structure data is in excellent agreement with the experimental results. In addition, the identical FT-IR spectra of the four crystalline samples revealed absorption bands corresponding to S-S and C-S stretching as well as the characteristic aromatic substitution. Five percent weight loss at 163.3 degrees C was observed when TG was used to study the decomposition process in the temperature range of 20-200 degrees C. DSC also allowed for the determination of onset temperatures at 60.4(1)-60.7(3) degrees C and peak temperatures at 62.1(3)-62.4(3) degrees C for the four crystalline samples studied. The results verified that the single crystal structure shared the same crystal form with the four crystalline samples investigated.

Differentiations of Chitin Content and Surface Morphologies of Chitins Extracted from Male and Female Grasshopper Species

PubMed Central

Kaya, Murat; Lelešius, Evaldas; Nagrockaitė, Radvilė; Sargin, Idris; Arslan, Gulsin; Mol, Abbas; Baran, Talat; Can, Esra; Bitim, Betul

2015-01-01

In this study, we used Fourier transform infrared spectroscopy (FT-IR), elemental analysis (EA), thermogravimetric analysis (TGA), X-ray diffractometry (XRD), and scanning electron microscopy (SEM) to investigate chitin structure isolated from both sexes of four grasshopper species. FT-IR, EA, XRD, and TGA showed that the chitin was in the alpha form. With respect to gender, two main differences were observed. First, we observed that the quantity of chitin was greater in males than in females and the dry weight of chitin between species ranged from 4.71% to 11.84%. Second, using SEM, we observed that the male chitin surface structure contained 25 – 90nm wide nanofibers and 90 – 250 nm nanopores, while no pores or nanofibers were observed in the chitin surface structure of the majority of females (nanofibers were observed only in M. desertus females). In contrast, the elemental analysis, thermal properties, and crystalline index values for chitin were similar in males and females. Also, we carried out enzymatic digestion of the isolated chitins using commercial chitinase from Streptomyces griseus. We observed that there were no big differences in digestion rate of the chitins from both sexes and commercial chitin. The digestion rates were for grasshoppers’ chitins; 88.45–95.48% and for commercial chitin; 94.95%. PMID:25635814

Enhanced dissolution and oral bioavailability of valsartan solid dispersions prepared by a freeze-drying technique using hydrophilic polymers.

PubMed

Xu, Wei-Juan; Xie, Hong-Juan; Cao, Qing-Ri; Shi, Li-Li; Cao, Yue; Zhu, Xiao-Yin; Cui, Jing-Hao

2016-01-01

This study aimed to improve the dissolution rate and oral bioavailability of valsartan (VAL), a poorly soluble drug using solid dispersions (SDs). The SDs were prepared by a freeze-drying technique with polyethylene glycol 6000 (PEG6000) and hydroxypropylmethylcellulose (HPMC 100KV) as hydrophilic polymers, sodium hydroxide (NaOH) as an alkalizer, and poloxamer 188 as a surfactant without using any organic solvents. In vitro dissolution rate and physicochemical properties of the SDs were characterized using the USP paddle method, differential scanning calorimetry (DSC), X-ray diffractometry (XRD) and Fourier transform-infrared (FT-IR) spectroscopy, respectively. In addition, the oral bioavailability of SDs in rats was evaluated by using VAL (pure drug) as a reference. The dissolution rates of the SDs were significantly improved at pH 1.2 and pH 6.8 compared to those of the pure drug. The results from DSC, XRD showed that VAL was molecularly dispersed in the SDs as an amorphous form. The FT-IR results suggested that intermolecular hydrogen bonding had formed between VAL and its carriers. The SDs exhibited significantly higher values of AUC 0-24 h and Cmax in comparison with the pure drug. In conclusion, hydrophilic polymer-based SDs prepared by a freeze-drying technique can be a promising method to enhance dissolution rate and oral bioavailability of VAL.

Electrical conductivity studies on Ammonium bromide incorporated with Zwitterionic polymer blend electrolyte for battery application

NASA Astrophysics Data System (ADS)

Parameswaran, V.; Nallamuthu, N.; Devendran, P.; Nagarajan, E. R.; Manikandan, A.

2017-06-01

Solid polymer blend electrolytes are widely studied due to their extensive applications particularly in electrochemical devices. Blending polymer makes the thermal stability, higher mechanical strength and inorganic salt provide ionic charge carrier to enhance the conductivity. In these studies, 50% polyvinyl alcohol (PVA), 50% poly (N-vinyl pyrrolidone) (PVP) and 2.5% L-Asparagine mixed with different ratio of the Ammonium bromide (NH4Br), have been synthesized using solution casting technique. The prepared PVA/PVP/L-Asparagine/doped-NH4Br polymer blend electrolyte films have been characterized by various analytical methods such as FT-IR, XRD, impedance spectroscopy, TG-DSC and scanning electron microscopy. FT-IR, XRD and TG/DSC analysis revealed the structural and thermal behavior of the complex formation between PVA/PVP/L-Asparagine/doped-NH4Br. The ionic conductivity and the dielectric properties of PVA/PVP/L-Asparagine/doped-NH4Br polymer blend electrolyte films were examined using impedance analysis. The highest ionic conductivity was found to be 2.34×10-4 S cm-1 for the m.wt. composition of 50%PVA:50%PVP:2.5%L-Asparagine:doped 0.15 g NH4Br at ambient temperature. Solid state proton battery is fabricated and the observed open circuit voltage is 1.1 V and its performance has been studied.

Stabilization of collagen with EDC/NHS in the presence of L-lysine: a comprehensive study.

PubMed

Usha, R; Sreeram, K J; Rajaram, A

2012-02-01

This paper reports the effect of L-lysine on the conformational, rheological, and thermal properties of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide (EDC) and N-hydroxysuccinimide (NHS) cross linked collagen and investigates the influence of l-lysine on the self assembly processes of collagen. In the absence of L-lysine, the rheological characterization of collagen cross linked with EDC/NHS showed an increase in shearing stress with shearing speed indicating that the collagen chains become rigid and the molecules are reluctant to flow. On the other hand, the increase in shearing stress with shearing speed is comparatively much less in the presence of L-lysine indicating a greater flexibility of the collagen molecules. The self assembly processes of collagen treated with EDC/NHS in the absence and presence of L-lysine were characterized using powder XRD, FT-IR, polarizing optical microscopy and kinetic studies. XRD studies show an increase in peak intensity and sharpness in the presence of L-lysine indicating the enhancement of crystallinity of collagen nano-fibrils. FT-IR results suggest that the incorporation of L-lysine in the EDC/NHS cross linking favors the molecular stability of collagen. From the present study, it is possible to conclude that the pre-treatment of collagen with L-lysine enhances EDC/NHS cross linking and can be used for biomaterial applications. Copyright © 2011 Elsevier B.V. All rights reserved.

Investigation of composition and structure of spongy and hard bone tissue using FTIR spectroscopy, XRD and SEM

NASA Astrophysics Data System (ADS)

Al-Akhras, M.-Ali H.; Hasan Qaseer, M. K.; Albiss, B. A.; Alebrhim, M. Anwar; Gezawa, Umar S.

2018-02-01

Valuable structural and chemical features can be obtained for spongy and hard bone by infrared spectroscopy and X-ray diffraction. A better understanding of chemical and structural differences between spongy and hard bone is a very important contributor to bone quality. Our data according to IR data showed that the collagen cross-links occurred to be higher in spongy bone, and crystallinity was lower in spongy bone. Deconvolution of the infrared band near 870 cm-1 reveals evidence for A2-type carbonate substitution on hydroxyapatite of spongy bone in addition to the A and B type carbonate substitution that are also found in hard bone. IR and XRD data confirmed the results of each other since full width at half maximum of 002-apatite pattern of XRD showed that the crystallinity was lower in spongy bone. The microstructure was examined by using scanning electron microscope and the result showed that the lattice of thin threads in spongy bone and is less dense than hard bone.

Anticancer and enhanced antimicrobial activity of biosynthesizd silver nanoparticles against clinical pathogens

NASA Astrophysics Data System (ADS)

Rajeshkumar, Shanmugam; Malarkodi, Chelladurai; Vanaja, Mahendran; Annadurai, Gurusamy

2016-07-01

The present investigation shows the biosynthesis of eco-friendly silver nanoparticles using culture supernatant of Enterococcus sp. and study the effect of enhanced antimicrobial activity, anticancer activity against pathogenic bacteria, fungi and cancer cell lines. Silver nanoparticles was synthesized by adding 1 mM silver nitrate into the 100 ml of 24 h freshly prepared culture supernatant of Enterococcus sp. and were characterized by UV-vis spectroscopy, X-ray diffraction (XRD), Transmission Electron Microscope (TEM), Selected Area Diffraction X-Ray (SAED), Energy Dispersive X Ray (EDX) and Fourier Transform Infra red Spectroscopy (FT-IR). The synthesized silver nanoparticles were impregnated with commercial antibiotics for evaluation of enhanced antimicrobial activity. Further these synthesized silver nanoparticles were assessed for its anticancer activity against cancer cell lines. In this study crystalline structured nanoparticles with spherical in the size ranges from 10 to 80 nm and it shows excellent enhanced antimicrobial activity than the commercial antibiotics. The in vitro assay of silver nanoparticles on anticancer have great potential to inhibit the cell viability. Amide linkages and carboxylate groups of proteins from Enterococcus sp. may bind with silver ions and convert into nanoparticles. The activities of commercial antibiotics were enhanced by coating silver nanoparticles shows significant improved antimicrobial activity. Silver nanoparticles have the great potential to inhibit the cell viability of liver cancer cells lines (HepG2) and lung cancer cell lines (A549).

Cu-based metal-organic framework/activated carbon composites for sulfur compounds removal

NASA Astrophysics Data System (ADS)

Fan, Hui-Ling; Shi, Rui-Hua; Zhang, Zhen-Rong; Zhen, Tian; Shangguan, Ju; Mi, Jie

2017-02-01

MOF-199 was modified by incorporating activated carbon (AC) during its synthesis under hydrothermal conditions to improve its performance in the removal of hydrogen sulfide (H2S) and dimethyl sulfide (CH3SCH3). A variety of different characterization techniques including X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, nitrogen adsorption/desorption isotherms, scanning electron microscopy (SEM), pyridine adsorption infrared spectroscopy (Py-IR), thermogravimetric- mass spectroscopy (TG-MS) and X-ray photoelectron spectroscopy (XPS) were used to analyze the fresh and exhausted composites. It was found that the composites, which have an amount of AC of less than 2%, had the same morphology as those of pristine MOF-199, but exhibited a more ordered crystallinity structure as well as higher surface area. The composite with 2% AC incorporation showed highest sulfur capacity of 8.46 and 8.53% for H2S and CH3SCH3, respectively, which increased by 51 and 41% compared to that of MOF-199. This improvement was attributed to the formation of more micropores and especially the increased number of unsaturated copper metal sites, as revealed by Py-IR. It is suggested the chemical reaction was apparent during adsorption of H2S, which resulted in the formation of CuS and the collapse of the MOF structure. Whereas reversible chemisorption was found for CH3SCH3 adsorption, as testified by TG-MS and fixed-bed regeneration. Exhausted MAC-2 can be almost totally regenerated by high temperature 180 °C nitrogen purge, indicating a promising adsorbent for CH3SCH3 removal.

Epitaxial growth of iridate pyrochlore Nd 2Ir 2O 7 films

DOE PAGES

Gallagher, J. C.; Esser, B. D.; Morrow, R.; ...

2016-02-29

Epitaxial films of the pyrochlore Nd 2Ir 2O 7 have been grown on (111)-oriented yttria-stabilized zirconia (YSZ) substrates by off-axis sputtering followed by post-growth annealing. X-ray diffraction (XRD) results demonstrate phase-pure epitaxial growth of the pyrochlore films on YSZ. Scanning transmission electron microscopy (STEM) investigation of an Nd 2Ir 2O 7 film with a short post-annealing provides insight into the mechanism for crystallization of Nd 2Ir 2O 7 during the post-annealing process. STEM images reveal clear pyrochlore ordering of Nd and Ir in the films. As a result, the epitaxial relationship between the YSZ and Nd 2Ir 2O 7 ismore » observed clearly while some interfacial regions show a thin region with polycrystalline Ir nanocrystals.« less

Evaluation of mechanical property and bioactivity of nano-bioglass 45S5 scaffold coated with poly-3-hydroxybutyrate.

PubMed

Montazeri, Mahbobeh; Karbasi, Saeed; Foroughi, Mohammad Reza; Monshi, Ahmad; Ebrahimi-Kahrizsangi, Reza

2015-02-01

One of the major challenges facing researchers of tissue engineering is scaffold design with desirable physical and mechanical properties for growth and proliferation of cells and tissue formation. In this research, firstly, nano-bioglass powder with grain sizes of 55-56 nm was prepared by melting method of industrial raw materials at 1,400 °C. Then the porous ceramic scaffold of bioglass with 30, 40 and 50 wt% was prepared by using the polyurethane sponge replication method. The scaffolds were coated with poly-3-hydroxybutyrate (P3HB) for 30 s and 1 min in order to increase the scaffold's mechanical properties. XRD, XRF, SEM, FE-SEM and FT-IR were used for phase and component studies, morphology, particle size and determination of functional groups, respectively. XRD and XRF results showed that the type of the produced bioglass was 45S5. The results of XRD and FT-IR showed that the best temperature to produce bioglass scaffold was 600 °C, in which Na2Ca2Si3O9 crystal is obtained. By coating the scaffolds with P3HB, a composite scaffold with optimal porosity of 80-87% in 200-600 μm and compression strength of 0.1-0.53 MPa was obtained. According to the results of compressive strength and porosity tests, the best kind of scaffold was produced with 30 wt% of bioglass immersed for 1 min in P3HB. To evaluate the bioactivity of the scaffold, the SBF solution was used. The selected scaffold (30 wt% bioglass/6 wt% P3HB) was maintained for up to 4 weeks in this solution at an incubation temperature of 37 °C. The XRD, SEM EDXA and AAS tests were indicative of hydroxyapatite formation on the surface of bioactive scaffold. This scaffold has some potential to use in bone tissue engineering.

CdO-NPs; synthesis from 1D new nano Cd coordination polymer, characterization and application as anti-cancer drug for reducing the viability of cancer cells

NASA Astrophysics Data System (ADS)

Afzalian Mend, Behnaz; Delavar, Mahmoud; Darroudi, Majid

2017-04-01

The hexagonal CdO nano-particles (CdO-NPs) was prepared using new nano Cd coordination polymer, [Cd(NO3)(bipy)(pzca)]n (1) as a precursor, through direct calcination process at 500 °C. The precursor (1) was synthesized by sonochemical method. The new nano compound (1) was characterized by IR spectroscopy, elemental analyses, X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and thermal gravimetric analyses. The structure of nano coordination polymer was determined by comparing the XRD pattern of nano and single-crystal of compound (1). The nano CdO was characterized by scanning electron microscopy (SEM) and X-ray powder diffraction (XRD). In addition, the activity and efficiency of nano CdO as an anti-cancer drug was studied on cancer cells with different concentration. The results shows that the viability of cancer cells reduced above 2 μg/mL of CdO-NPs concentration.

Unusual thermal expansion of Sr{sub 2}IrO{sub 4}: A variable temperature synchrotron X-ray diffraction study

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

Ranjbar, Ben; Kennedy, Brendan J.

The structure of Sr{sub 2}IrO{sub 4} has been studied between 20 and 1273 K using synchrotron X-ray diffraction. Sr{sub 2}IrO{sub 4} undergoes an apparently continuous transition from I4{sub 1}/acd to I4/mmm near 1123 K. The cooperative tilting of the corner sharing IrO{sub 6} octahedra in I4{sub 1}/acd results in highly anisotropic and unusual thermal expansion behavior with negative thermal expansion along the c-axis. - Graphical abstract: The progressive reduction in the magnitude of the tilting of the corner sharing IrO{sub 6} octahedra in Sr{sub 2}IrO{sub 4} results in negative thermal expansion along the c-axis before undergoing an apparently continuous transitionmore » from I4{sub 1}/acd to I4/mmm near 1123 K. - Highlights: • Thermal expansion of Sr{sub 2}IrO{sub 4} was studied using Synchrotron-XRD. • Unusual negative thermal expansion along c-axis observed. • I4{sub 1}/acd→I4/mmm phase transition detected near 1120 K. • Tilting of the corner sharing IrO{sub 6} octahedra related to the observed NTE.« less

Vibrational spectroscopic (FT-IR and FT-Raman) studies, HOMO-LUMO, NBO analysis and MEP of 6-methyl-1-({[(2E)-2-methyl-3-phenyl-prop-2-en-1-yl]oxy}methyl)-1,2,3,4-tetra-hydroquinazoline-2,4-dione, a potential chemotherapeutic agent, using density functional methods.

PubMed

Sebastian, Sr S H Roseline; Al-Tamimi, Abdul-Malek S; El-Brollosy, Nasser R; El-Emam, Ali A; Yohannan Panicker, C; Van Alsenoy, Christian

2015-01-05

6-Methyl-1-({[(2E)-2-methyl-3-phenyl-prop-2-en-1-yl]oxy}methyl)-1,2,3,4-tetra-hydro quinazoline-2,4-dione was prepared via treatment of silylated 6-methylquinazoline-2,4-dione with bis-[(E)-2-methyl-3-phenylallyloxy]methane. FT-IR and FT-Raman spectra were recorded and analyzed. The vibrational wavenumbers were computed using DFT methods and are assigned with the help of potential energy distribution method. The first hyperpolarizability, infrared intensities and Raman activities also reported. The geometrical parameters of the title compound obtained from XRD studies are in agreement with the calculated (B3LYP) values. The stability of the molecule arising from hyper-conjugative interaction and charge delocalization has been analyzed using NBO analysis. The HOMO and LUMO analysis are used to determine the charge transfer within the molecule. MEP was performed by the B3LYP method and from the MEP it is evident that the negative charge covers the CO group and the positive region is over the phenyl ring and NH group. Copyright © 2014 Elsevier B.V. All rights reserved.

Preparation and characterizations of SnO2 nanopowder and spectroscopic (FT-IR, FT-Raman, UV-Visible and NMR) analysis using HF and DFT calculations.

PubMed

Ayeshamariam, A; Ramalingam, S; Bououdina, M; Jayachandran, M

2014-01-24

In this work, pure and singe phase SnO2 Nano powder is successfully prepared by simple sol-gel combustion route. The photo luminescence and XRD measurements are made and compared the geometrical parameters with calculated values. The FT-IR and FT-Raman spectra are recorded and the fundamental frequencies are assigned. The optimized parameters and the frequencies are calculated using HF and DFT (LSDA, B3LYP and B3PW91) theory in bulk phase of SnO2 and are compared with its Nano phase. The vibrational frequency pattern in nano phase gets realigned and the frequencies are shifted up to higher region of spectra when compared with bulk phase. The NMR and UV-Visible spectra are simulated and analyzed. Transmittance studies showed that the HOMO-LUMO band gap (Kubo gap) is reduced from 3.47 eV to 3.04 eV while it is heated up to 800°C. The Photoluminescence spectra of SnO2 powder showed a peak shift towards lower energy side with the change of Kubo gap from 3.73 eV to 3.229 eV for as-prepared and heated up to 800°C. Crown Copyright © 2013. Published by Elsevier B.V. All rights reserved.

Comparative theoretical and experimental study on novel tri-quinoline system and its anticancer studies

NASA Astrophysics Data System (ADS)

Gayathri, Kasirajan; Radhika, Ramachandran; Shankar, Ramasamy; Malathi, Mahalingam; Savithiri, Krishnaswamy; Sparkes, Hazel A.; Howard, Judith A. K.; Mohan, Palathurai Subramaniam

2017-04-01

A novel compound 2-chloro-3,6-bis-(quinolin-8-yloxymethyl)-quinoline 3 bearing a tri-quinoline moiety has been synthesized from 2-chloro-3,6-dimethyl quinoline 1 and 8-hydroxy quinoline 2 using dry acetone and K2CO3 as a base. 3 has been characterized by using FT-IR, FT-Raman, UV-Vis, 1H NMR, 13C NMR spectra and single crystal X-ray diffraction methods. We have also made a combined experimental and theoretical study on the molecular structure, vibrational spectra, NMR, FT-IR, FT-Raman and UV-Vis spectra of 2-chloro-3,6-bis-(quinolin-8-yloxymethyl)-quinoline. The theoretical studies of the title compound have been evaluated by using density functional theory calculations using B3LYP/6-31+G(d,p) and M06-2X/6-31+G(d,p) level of theories. The calculated theoretical values were found to be in good agreement with the experimental findings. The single crystal structure 3 crystallized in the orthorhombic space group Pna21. The compound 3 exhibits higher cytotoxicity in human cervical cancer cell lines (HeLa) than human breast cancer cell lines (MCF7).

Synthesis and characterization of nano-sized zirconia powder synthesized by single emulsion-assisted direct precipitation.

PubMed

Chandra, Navin; Singh, Deepesh Kumar; Sharma, Meenakshi; Upadhyay, Ravi Kant; Amritphale, S S; Sanghi, S K

2010-02-15

For the first time, single reverse microemulsion-assisted direct precipitation route has been successfully used to synthesize tetragonal zirconia nanoparticles in narrow size range. The synthesized powder was characterized using FT-IR, XRD and HRTEM techniques. The zirconia nanoparticles obtained were spherical in shape and has narrow particle size distribution in the range of 13-31nm and crystallite size in the range of 13-23nm. Copyright 2009 Elsevier Inc. All rights reserved.