Monitoring cure of composite resins using frequency dependent electromagnetic sensing techniques
NASA Technical Reports Server (NTRS)
Kranbuehl, D. E.; Hoff, M. S.; Loos, A. C.; Freeman, W. T., Jr.; Eichinger, D. A.
1988-01-01
A nondestructive in situ measurement technique has been developed for monitoring and measuring the cure processing properties of composite resins. Frequency dependent electromagnetic sensors (FDEMS) were used to directly measure resin viscosity during cure. The effects of the cure cycle and resin aging on the viscosity during cure were investigated using the sensor. Viscosity measurements obtained using the sensor are compared with the viscosities calculated by the Loos-Springer cure process model. Good overall agreement was obtained except for the aged resin samples.
Analysis of curing process and thermal properties of phenol-urea-formaldehyde cocondensed resins
Bunchiro Tomita; Masahiko Ohyama; Atsushi Itoh; Kiyoto Doi; Chung-Yun Hse
1994-01-01
The curing processes of resols, urea-formaldehyde (UF) resins, their mechanical blends, and phenol-urea cocondensed resins, as well as the reaction of 2,4,6-trimethylolphenol with urea were investiiated with the torsional braid analysis method. The thermal stabilities of these resins after curing also were compared. The results were as follows: (1) In the curing...
NASA Technical Reports Server (NTRS)
Loos, Alfred C.; Weideman, Mark H.; Long, Edward R., Jr.; Kranbuehl, David E.; Kinsley, Philip J.; Hart, Sean M.
1991-01-01
A model was developed which can be used to simulate infiltration and cure of textile composites by resin transfer molding. Fabric preforms were resin infiltrated and cured using model generated optimized one-step infiltration/cure protocols. Frequency dependent electromagnetic sensing (FDEMS) was used to monitor in situ resin infiltration and cure during processing. FDEMS measurements of infiltration time, resin viscosity, and resin degree of cure agreed well with values predicted by the simulation model. Textile composites fabricated using a one-step infiltration/cure procedure were uniformly resin impregnated and void free. Fiber volume fraction measurements by the resin digestion method compared well with values predicted using the model.
2013-03-01
remain nonvolatile during the entire fiber-infusion process and curing operation. The resin must offer several days of storage life before the prepreg ...shipboard handling and in-flight cyclic loading. The raw materials for the new resin and the process for making and curing the prepreg must be affordable
Effects of Amine and Anhydride Curing Agents on the VARTM Matrix Processing Properties
NASA Technical Reports Server (NTRS)
Grimsley, Brian W.; Hubert, Pascal; Song, Xiaolan; Cano, Roberto J.; Loos, Alfred C.; Pipes, R. Byron
2002-01-01
To ensure successful application of composite structure for aerospace vehicles, it is necessary to develop material systems that meet a variety of requirements. The industry has recently developed a number of low-viscosity epoxy resins to meet the processing requirements associated with vacuum assisted resin transfer molding (VARTM) of aerospace components. The curing kinetics and viscosity of two of these resins, an amine-cured epoxy system, Applied Poleramic, Inc. VR-56-4 1, and an anhydride-cured epoxy system, A.T.A.R.D. Laboratories SI-ZG-5A, have been characterized for application in the VARTM process. Simulations were carried out using the process model, COMPRO, to examine heat transfer, curing kinetics and viscosity for different panel thicknesses and cure cycles. Results of these simulations indicate that the two resins have significantly different curing behaviors and flow characteristics.
Matrix Characterization and Development for the Vacuum Assisted Resin Transfer Molding Process
NASA Technical Reports Server (NTRS)
Grimsley, B. W.; Hubert, P.; Hou, T. H.; Cano, R. J.; Loos, A. C.; Pipes, R. B.
2001-01-01
The curing kinetics and viscosity of an epoxy resin system, SI-ZG-5A, have been characterized for application in the vacuum assisted resin transfer molding (VARTM) process. Impregnation of a typical carbon fiber perform provided the test bed for the characterization. Process simulations were carried out using the process model, COMPRO, to examine heat transfer and curing kinetics for a fully impregnated panel, neglecting resin flow. The predicted viscosity profile and final degree of cure were found to be in good agreement with experimental observations.
Phenoxy resins containing pendent ethynyl groups and cured resins obtained therefrom
NASA Technical Reports Server (NTRS)
Hergenrother, P. M. (Inventor)
1985-01-01
Phenoxy resins containing pendent ethynyl groups, the process for preparing the same, and the cured resin products obtained therefrom are disclosed. Upon the application of heat, the ethynyl groups react to provide branching and crosslinking with the cure temperature being lowered by using a catalyst if desired but not required. The cured phenoxy resins containing pendent ethynyl groups have improved solvent resistance and higher use temperature than linear uncrosslinked phenoxy resins and are applicable for use as coatings, films, adhesives, composited matrices and molding compounds.
Solidifying process and flame retardancy of epoxy resin cured with boron-containing phenolic resin
NASA Astrophysics Data System (ADS)
Deng, Peng; Shi, Yan; Liu, Yuansen; Liu, Yuan; Wang, Qi
2018-01-01
For the sake of improving the charring performance and flame retardancy of epoxy resin (EP), boron-containing phenolic resin (BPR) instead of a conventional curing agent, linear phenolic resin (LPR) was employed to cure EP. Of several possible chemical structures for BPR, the existence of benzyl hydroxy groups in BPR chains has been confirmed using 1H nuclear magnetic resonance spectroscopy. The resonance of these groups may reasonably explain the higher curing reactivity of BPR-cured EP than that of LPR-cured EP. Thermogravimetric analysis, observation of the morphologies of the char residues and X-ray photoelectron spectroscopic were performed to characterize the charring process. Due to the presence of B2O3 produced on the char surface from decomposition of phenyl borates and the facile high self-crosslinking reaction of BPR, a more continuous and stronger char barrier was formed for BPR-cured EP compared to that for the LPR-cured EP system. Therefore the former exhibited much better flame retardancy. In addition, BPR-cured EP also displayed better dynamic mechanical properties, than those observed for LPR-cured EP. It is not subject to the significant lowering the glass transition temperature of the polymer which accompanies curing with LPR. This suggests that BPR cured resin may meet the requirement for utilization at high temperature.
A criterion for maximum resin flow in composite materials curing process
NASA Astrophysics Data System (ADS)
Lee, Woo I.; Um, Moon-Kwang
1993-06-01
On the basis of Springer's resin flow model, a criterion for maximum resin flow in autoclave curing is proposed. Validity of the criterion was proved for two resin systems (Fiberite 976 and Hercules 3501-6 epoxy resin). The parameter required for the criterion can be easily estimated from the measured resin viscosity data. The proposed criterion can be used in establishing the proper cure cycle to ensure maximum resin flow and, thus, the maximum compaction.
Masahiko Ohyama; Bunchiro Tomita; Chung-Yun Hse
1995-01-01
The curing processes and thermal properties of resol-type phenol-urea-formaldehyde cocondensed resins, which were prepared by alkaline treatments of the cocondensed resins once synthesized from UF-concentrate and phenol, were investigated by torsional braid analysis. The resol-type cocondensed resins displayed almost the same curing behaviors and heat-resistance as a...
Resin impregnation process for producing a resin-fiber composite
NASA Technical Reports Server (NTRS)
Palmer, Raymond J. (Inventor); Moore, William E. (Inventor)
1994-01-01
Process for vacuum impregnation of a dry fiber reinforcement with a curable resin to produce a resin-fiber composite, by drawing a vacuum to permit flow of curable liquid resin into and through a fiber reinforcement to impregnate same and curing the resin-impregnated fiber reinforcement at a sufficient temperature and pressure to effect final curing. Both vacuum and positive pressure, e.g. autoclave pressure, are applied to the dry fiber reinforcement prior to application of heat and prior to any resin flow to compact the dry fiber reinforcement, and produce a resin-fiber composite of reduced weight, thickness and resin content, and improved mechanical properties. Preferably both a vacuum and positive pressure, e.g. autoclave pressure, are also applied during final curing.
Dsouza, Roshan; Subhash, Hrebesh; Neuhaus, Kai; Kantamneni, Ramakrishna; McNamara, Paul M; Hogan, Josh; Wilson, Carol; Leahy, Martin
2016-01-01
Monitoring the curing kinetics of light-activated resin is a key area of research. These resins are used in restorative applications and particularly in dental applications. They can undergo volumetric shrinkage due to poor control of the depth dependent curing process, modulated by the intensity and duration of the curing light source. This often results in the formation of marginal gaps, causing pain and damage to the restoration site. In this study, we demonstrate the capabilities of a correlation method applied using a multiple references optical coherence tomography (MR-OCT) architecture to monitor the curing of the resin. A MR-OCT system is used in this study to monitor the curing of the resin. The system operates at the center wavelength of 1310 nm with an A-scan rate of 1200 A-scans per second. The axial and lateral resolution of the system is ∼13 μm and ∼27 μm. The method to determine the intensity correlation between adjacent B-frames is based on the Pearson correlation coefficient for a region of interest. Calculating the correlation coefficient for multiple B-frames related to the first B-frame at regular spaced time points, shows for a noncured resin a reduction of the correlation coefficient over time due to Brownian motion. The time constant of the reduction of the correlation value is a measure for the progress of the polymerization during LED light irradiation of the resin. The proposed approach is potentially a low-cost, powerful and unique optical imaging modality for measuring the curing behavior of dental resin and other resins, coatings, and adhesives in medical and industrial applications. To demonstrate the proposed method to monitor the curing process, a light-activated resin composite from GRADIA DIRECT ANTERIOR (GC Corporation, Japan) is studied. The curing time of resin was measured and monitored as a function of depth. The correlation coefficient method is highly sensitive to Brownian motion. The process of curing results in a change in intensity as measured by the MR-OCT signal and hence can be monitored using this method. These results show that MR-OCT has the potential to measure the curing time and monitor the curing process as a function of depth. Moreover, MR-OCT as a product has potential to be compact, low-cost and to fit into a smartphone. Using such a device for monitoring the curing of the resin will be suitable for dentists in stationary and mobile clinical settings. © 2015 Wiley Periodicals, Inc.
NASA Technical Reports Server (NTRS)
Sreekantamurthy, Thammaiah; Hudson, Tyler B.; Hou, Tan-Hung; Grimsley, Brian W.
2016-01-01
Composite cure process induced residual strains and warping deformations in composite components present significant challenges in the manufacturing of advanced composite structure. As a part of the Manufacturing Process and Simulation initiative of the NASA Advanced Composite Project (ACP), research is being conducted on the composite cure process by developing an understanding of the fundamental mechanisms by which the process induced factors influence the residual responses. In this regard, analytical studies have been conducted on the cure process modeling of composite structural parts with varied physical, thermal, and resin flow process characteristics. The cure process simulation results were analyzed to interpret the cure response predictions based on the underlying physics incorporated into the modeling tool. In the cure-kinetic analysis, the model predictions on the degree of cure, resin viscosity and modulus were interpreted with reference to the temperature distribution in the composite panel part and tool setup during autoclave or hot-press curing cycles. In the fiber-bed compaction simulation, the pore pressure and resin flow velocity in the porous media models, and the compaction strain responses under applied pressure were studied to interpret the fiber volume fraction distribution predictions. In the structural simulation, the effect of temperature on the resin and ply modulus, and thermal coefficient changes during curing on predicted mechanical strains and chemical cure shrinkage strains were studied to understand the residual strains and stress response predictions. In addition to computational analysis, experimental studies were conducted to measure strains during the curing of laminated panels by means of optical fiber Bragg grating sensors (FBGs) embedded in the resin impregnated panels. The residual strain measurements from laboratory tests were then compared with the analytical model predictions. The paper describes the cure process procedures and residual strain predications, and discusses pertinent experimental results from the validation studies.
Differential Curing In Fiber/Resin Laminates
NASA Technical Reports Server (NTRS)
Webster, Charles N.
1989-01-01
Modified layup schedule counteracts tendency toward delamination. Improved manufacturing process resembles conventional process, except prepregs partially cured laid on mold in sequence in degree of partial cure decreases from mold side to bag side. Degree of partial cure of each layer at time of layup selected by controlling storage and partial-curing temperatures of prepreg according to Arrhenius equation for rate of gel of resin as function of temperature and time from moment of mixing. Differential advancement of cure in layers made large enough to offset effect of advance bag-side heating in oven or autoclave. Technique helps prevent entrapment of volatile materials during manufacturing of fiber/resin laminates.
Epoxy foams using multiple resins and curing agents
Russick, Edward M.; Rand, Peter B.
2000-01-01
An epoxy foam comprising a plurality of resins, a plurality of curing agents, at least one blowing agent, at least one surfactant and optionally at least one filler and the process for making. Preferred is an epoxy foam comprising two resins of different reactivities, two curing agents, a blowing agent, a surfactant, and a filler. According to the present invention, an epoxy foam is prepared with tailorable reactivity, exotherm, and pore size by a process of admixing a plurality of resins with a plurality of curing agents, a surfactant and blowing agent, whereby a foamable mixture is formed and heating said foamable mixture at a temperature greater than the boiling temperature of the blowing agent whereby said mixture is foamed and cured.
Electron Beam Cured Epoxy Resin Composites for High Temperature Applications
NASA Technical Reports Server (NTRS)
Janke, Christopher J.; Dorsey, George F.; Havens, Stephen J.; Lopata, Vincent J.; Meador, Michael A.
1997-01-01
Electron beam curing of Polymer Matrix Composites (PMC's) is a nonthermal, nonautoclave curing process that has been demonstrated to be a cost effective and advantageous alternative to conventional thermal curing. Advantages of electron beam curing include: reduced manufacturing costs; significantly reduced curing times; improvements in part quality and performance; reduced environmental and health concerns; and improvement in material handling. In 1994 a Cooperative Research and Development Agreement (CRADA), sponsored by the Department of Energy Defense Programs and 10 industrial partners, was established to advance the electron beam curing of PMC technology. Over the last several years a significant amount of effort within the CRADA has been devoted to the development and optimization of resin systems and PMCs that match the performance of thermal cured composites. This highly successful materials development effort has resulted in a board family of high performance, electron beam curable cationic epoxy resin systems possessing a wide range of excellent processing and property profiles. Hundreds of resin systems, both toughened and untoughened, offering unlimited formulation and processing flexibility have been developed and evaluated in the CRADA program.
An infiltration/cure model for manufacture of fabric composites by the resin infusion process
NASA Technical Reports Server (NTRS)
Weideman, Mark H.; Loos, Alfred C.; Dexter, H. Benson; Hasko, Gregory H.
1992-01-01
A 1-D infiltration/cure model was developed to simulate fabrication of advanced textile composites by the resin film infusion process. The simulation model relates the applied temperature and pressure processing cycles, along with the experimentally measured compaction and permeability characteristics of the fabric preforms, to the temperature distribution, the resin degree of cure and viscosity, and the infiltration flow front position as a function of time. The model also predicts the final panel thickness, fiber volume fraction, and resin mass for full saturation as a function of compaction pressure. Composite panels were fabricated using the RTM (Resin Transfer Molding) film infusion technique from knitted, knitted/stitched, and 2-D woven carbon preforms and Hercules 3501-6 resin. Fabric composites were fabricated at different compaction pressures and temperature cycles to determine the effects of the processing on the properties. The composites were C-scanned and micrographed to determine the quality of each panel. Advanced cure cycles, developed from the RTM simulation model, were used to reduce the total cure cycle times by a factor of 3 and the total infiltration times by a factor of 2.
Modeling the curing process of thermosetting resin matrix composites
NASA Technical Reports Server (NTRS)
Loos, A. C.
1986-01-01
A model is presented for simulating the curing process of a thermosetting resin matrix composite. The model relates the cure temperature, the cure pressure, and the properties of the prepreg to the thermal, chemical, and rheological processes occurring in the composite during cure. The results calculated with the computer code developed on the basis of the model were compared with the experimental data obtained from autoclave-curved composite laminates. Good agreement between the two sets of results was obtained.
Fiber optic sensor design for chemical process and environmental monitoring
NASA Astrophysics Data System (ADS)
Mahendran, R. S.; Harris, D.; Wang, L.; Machavaram, V. R.; Chen, R.; Kukureka, St. N.; Fernando, G. F.
2007-07-01
Cure monitoring is a term that is used to describe the cross-linking reactions in a thermosetting resin system. Advanced fiber reinforced composites are being used increasingly in a number of industrial sectors including aerospace, marine, sport, automotive and civil engineering. There is a general realization that the processing conditions that are used to manufacture the composites can have a major influence on its hot-wet mechanical properties. This paper is concerned with the design and demonstration of a number of sensor designs for in-situ cure monitoring of a model thermosetting resin system. Simple fixtures were constructed to enable a pair of cleaved optical fibers with a defined gap between the end-faces to be held in position. The resin system was introduced into this gap and the cure kinetics were followed by transmission infrared spectroscopy. A semi-empirical model was used to describe the cure process using the data obtained at different cure temperatures. The same sensor system was used to detect the ingress of moisture in the cured resin system.
Acetylene terminated matrix resins
NASA Technical Reports Server (NTRS)
Goldfarb, I. J.; Lee, Y. C.; Arnold, F. E.; Helminiak, T. E.
1985-01-01
The synthesis of resins with terminal acetylene groups has provided a promising technology to yield high performance structural materials. Because these resins cure through an addition reaction, no volatile by-products are produced during the processing. The cured products have high thermal stability and good properties retention after exposure to humidity. Resins with a wide variety of different chemical structures between the terminal acetylene groups are synthesized and their mechanical properties studied. The ability of the acetylene cured polymers to give good mechanical properties is demonstrated by the resins with quinoxaline structures. Processibility of these resins can be manipulated by varying the chain length between the acetylene groups or by blending in different amounts of reactive deluents. Processing conditions similar to the state-of-the-art epoxy can be attained by using backbone structures like ether-sulfone or bis-phenol-A. The wide range of mechanical properties and processing conditions attainable by this class of resins should allow them to be used in a wide variety of applications.
NASA Technical Reports Server (NTRS)
Hou, Tan-Hung
2014-01-01
For the fabrication of resin matrix fiber reinforced composite laminates, a workable cure cycle (i.e., temperature and pressure profiles as a function of processing time) is needed and is critical for achieving void-free laminate consolidation. Design of such a cure cycle is not trivial, especially when dealing with reactive matrix resins. An empirical "trial and error" approach has been used as common practice in the composite industry. Such an approach is not only costly, but also ineffective at establishing the optimal processing conditions for a specific resin/fiber composite system. In this report, a rational "processing science" based approach is established, and a universal cure cycle design protocol is proposed. Following this protocol, a workable and optimal cure cycle can be readily and rationally designed for most reactive resin systems in a cost effective way. This design protocol has been validated through experimental studies of several reactive polyimide composites for a wide spectrum of usage that has been documented in the previous publications.
Development of new and improved polymer matrix resin systems, phase 1
NASA Technical Reports Server (NTRS)
Hsu, M. S.
1983-01-01
Vinystilbazole (vinylstryrylpyridine) and vinylpolystyrulpyridine were prepared for the purpose of modifying bismaleimide composite resins. Cure studies of resins systems were investigated by differential scanning calorimetry. The vinylstyrylpyridine-modified bismaleimide composite resins were found to have lower cure and gel temperatures, and shorter cure times than the corresponding unmodified composite resins. The resin systems were reinforced with commercially avialable satin-weave carbon cloth. Prepregs were fabricated by solvent or hot melt techniques. Thermal stability, flammability, moisture absorption, and mechanical properties of the composites (such as flexural strength, modulus, tensile and short beam shear strength) were determined. Composite laminates showed substantial improvements in both processability and mechanical properties compared to he bismaleimide control systems. The vinylstyrylpyridine modified bismaleimide resins can be used as advanced matrix resins for graphite secondary structures where ease of processing, fireworthiness, and high temperature stability are required for aerospace applications.
NASA Astrophysics Data System (ADS)
Golestanian, Hossein
This research focuses on modeling Resin Transfer Molding process for manufacture of composite parts with woven fiber mats. Models are developed to determine cure dependent stiffness matrices for composites manufactured with two types of woven fiber mats. Five-harness carbon and eight-harness fiberglass mats with EPON 826 resin composites are considered. The models presented here take into account important material/process parameters with emphasis on; (1) The effects of cure-dependent resin mechanical properties, (2) Fiber undulation due to the weave of the fiber fill and warp bundles, and (3) Resin interaction with the fiber bundles at a microscopic scale. Cure-dependent mechanical properties were then used in numerical models to determine residual stresses and deformation in the composite parts. The complete cure cycle was modeled in these analyses. Also the cool down stage after the composite cure was analyzed. The effect of 5% resin shrinkage on residual stresses and deformations was also investigated. In the second part of the study, Finite Element models were developed to simulate mold filling in RTM processes. Resin flow in the fiber mats was modeled as flow through porous media. Physical models were also developed to investigate resin flow behavior into molds of rectangular and irregular shapes. Silicone fluids of 50 and 100 centistoke viscosities as well as EPON 826 epoxy resin were used in the mold filling experiments. The reinforcements consisted of several layers of woven fiberglass and carbon fiber mats. The effects of injection pressure, fluid viscosity, type of reinforcement, and mold geometry on mold filling times were investigated. Fiber mat permeabilities were determined experimentally for both types of reinforcements. Comparison of experimental and numerical resin front positions indicated the importance of edge effects in resin flow behavior in small cavities. The resin front positions agreed well for the rectangular mold geometry.
Co-Curing of CFRP-Steel Hybrid Joints Using the Vacuum Assisted Resin Infusion Process
NASA Astrophysics Data System (ADS)
Streitferdt, Alexander; Rudolph, Natalie; Taha, Iman
2017-10-01
This study focuses on the one-step co-curing process of carbon fiber reinforced plastics (CFRP) joined with a steel plate to form a hybrid structure. In this process CFRP laminate and bond to the metal are realized simultaneously by resin infusion, such that the same resin serves for both infusion and adhesion. For comparison, the commonly applied two-step process of adhesive bonding is studied. In this case, the CFRP laminate is fabricated in a first stage through resin infusion of Non Crimp Fabric (NCF) and joined to the steel plate in a further step through adhesive bonding. For this purpose, the commercially available epoxy-based Betamate 1620 is applied. CFRP laminates were fabricated using two different resin systems, namely the epoxy (EP)-based RTM6 and a newly developed fast curing polyurethane (PU) resin. Results show comparable mechanical performance of the PU and EP based CFRP laminates. The strength of the bond of the co-cured samples was in the same order as the samples adhesively bonded with the PU resin and the structural adhesive. The assembly adhesive with higher ductility showed a weaker performance compared to the other tests. It could be shown that the surface roughness had the highest impact on the joint performance under the investigated conditions.
INTEGRATION OF COST MODELS AND PROCESS SIMULATION TOOLS FOR OPTIMUM COMPOSITE MANUFACTURING PROCESS
DOE Office of Scientific and Technical Information (OSTI.GOV)
Pack, Seongchan; Wilson, Daniel; Aitharaju, Venkat
Manufacturing cost of resin transfer molded composite parts is significantly influenced by the cycle time, which is strongly related to the time for both filling and curing of the resin in the mold. The time for filling can be optimized by various injection strategies, and by suitably reducing the length of the resin flow distance during the injection. The curing time can be reduced by the usage of faster curing resins, but it requires a high pressure injection equipment, which is capital intensive. Predictive manufacturing simulation tools that are being developed recently for composite materials are able to provide variousmore » scenarios of processing conditions virtually well in advance of manufacturing the parts. In the present study, we integrate the cost models with process simulation tools to study the influence of various parameters such as injection strategies, injection pressure, compression control to minimize high pressure injection, resin curing rate, and demold time on the manufacturing cost as affected by the annual part volume. A representative automotive component was selected for the study and the results are presented in this paper« less
Differences in interfacial bond strengths of graphite fiber-epoxy resin composites
NASA Technical Reports Server (NTRS)
Needles, H. L.
1985-01-01
The effect of epoxy-size and degree of cure on the interfacial bonding of an epoxy-amine-graphite fiber composite system is examined. The role of the fiber-resin interface in determining the overall mechanical properties of composites is poorly understood. A good interfacial adhesive bond is required to achieve maximum stress transfer to the fibers in composites, but at the same time some form of energy absorbing interfacial interaction is needed to achieve high fracture toughening. The incompatibility of these two processes makes it important to understand the nature and basic factors involved at the fiber-resin interface as stress is applied. The mechanical properties including interlaminar shear values for graphite fiber-resin composites are low compared to glass and boron-resin composites. These differences have been attributed to poor fiber-matrix adhesion. Graphite fibers are commonly subjected to post-treatments including application of organic sizing in order to improve their compatibility with the resin matrix and to protect the fiber tow from damage during processing and lay-up. In such processes, sized graphite fiber tow is impregnated with epoxy resin and then layed-up i nto the appropriate configuration. Following an extended ambient temperature cure, the graphite-resin composite structure is cured at elevated temperature using a programmed temperature sequence to cure and then cool the product.
High Temperature Transfer Molding Resins: Status of PETI-298 and PETI-330
NASA Technical Reports Server (NTRS)
Connell, John W.; Smith, Joseph G., Jr.; Hergenrother, Paul M.; Criss, Jim M.
2003-01-01
Two phenylethynyl terminated oligomers designated PETI-298 and PETI-330 were developed at the NASA Langley Research Center and have emerged as leading candidates for composite applications requiring high temperature performance (i.e. greater than or equal to 288 C for 1000 hours) combined with the ability to be readily processed into composites without the use of an autoclave or complex/lengthy cure or post-cure cycle. These high performance/high temperature composites are potentially useful on advanced aerospace vehicles in structural applications and as aircraft engine components such as inlet frames and compressor vanes. The number designation (i.e. 298, 330) refers to the glass transition temperature in degrees Celsius as determined on neat resin cured for 1 hour at 371 C. The resins are processable by non-autoclave techniques such as resin transfer molding (RTM), vacuum assisted RTM (VARTM) and resin infusion (RI). Both resins exhibit low complex melt viscosities (0.1-10 poise) at 280 C and are stable for greater than or equal to 2 hours at this temperature. Typically, the resins are melted, de-gassed and infused or injected at 280 C and subsequently cured at 371 C for 1-2 hours. Virtually no volatiles are evolved during the cure process. The resin synthesis is straightforward and has been scaled-up to 25 kg batches. The chemistry of PETI-298 and PETI-330 and the RTM AS-4 and T-650 carbon fabric laminate properties, and those of BMI-5270 for comparison, are presented.
Structure Property Relationships of Biobased Epoxy Resins
NASA Astrophysics Data System (ADS)
Maiorana, Anthony Surraht
The thesis is about the synthesis, characterization, development, and application of epoxy resins derived from sustainable feedstocks such as lingo-cellulose, plant oils, and other non-food feedstocks. The thesis can be divided into two main topics 1) the synthesis and structure property relationship investigation of new biobased epoxy resin families and 2) mixing epoxy resins with reactive diluents, nanoparticles, toughening agents, and understanding co-curing reactions, filler/matrix interactions, and cured epoxy resin thermomechanical, viscoelastic, and dielectric properties. The thesis seeks to bridge the gap between new epoxy resin development, application for composites and advanced materials, processing and manufacturing, and end of life of thermoset polymers. The structures of uncured epoxy resins are characterized through traditional small molecule techniques such as nuclear magnetic resonance, high resolution mass spectrometry, and infrared spectroscopy. The structure of epoxy resin monomers are further understood through the process of curing the resins and cured resins' properties through rheology, chemorheology, dynamic mechanical analysis, tensile testing, fracture toughness, differential scanning calorimetry, scanning electron microscopy, thermogravimetric analysis, and notched izod impact testing. It was found that diphenolate esters are viable alternatives to bisphenol A and that the structure of the ester side chain can have signifi-cant effects on monomer viscosity. The structure of the cured diphenolate based epoxy resins also influence glass transition temperature and dielectric properties. Incorporation of reactive diluents and flexible resins can lower viscosity, extend gel time, and enable processing of high filler content composites and increase fracture toughness. Incorpora-tion of high elastic modulus nanoparticles such as graphene can provide increases in physical properties such as elastic modulus and fracture toughness. The synthesis of epoxy resins with aliphatic esters in the main chain of the polymer allow for chemical recycling under alkaline conditions and changing the hydrophobicity and access of main chain esters influences the rate of polymer degradation. The thesis further provides strategies and concepts that will allow for future researchers to rapidly understand how to manipulate epoxy resins for specific end uses and supplements current understanding of epoxy curing agents, accelerators, and interactions with fillers.
Chai, Mei; Tang, Xuyan; Liang, Guangku
2015-12-01
To investigate clinical effect of individual light-curing resin tray as edge plastic material in complete denture modulo. A total of 30 patients with poor condition for alveolar ridge of mandible were chosen individual tray with individual light-curing resin tray for material edge shaping or traditional individual impression tray for edge shaping cream to produce complete denture. The operability, questionnaire about denture retention, comfort, mucosal cases and chewing function in the process of shaping the edge were investigated three months later after wearing dentures. There was no significant difference in retention, comfort, mucosa and the chewing function between the two mandibular denture impression methods. However, the patients with individual light-curing resin tray as edge shaping material felt better in the process than that in the patients with die-cream as the edge shaping material (P<0.05). Furthermore, the manipulation with individual light-curing resin tray as edge shaping material is easy for doctor. Although the clinical effect of Individual light-curing resin tray material as the edge shaping material is equal to that of impression cream, it saves time and human resource. Moreover, it is more acceptable for the patients and thus it can be spread in clinics.
New processable modified polyimide resins for adhesive and matrix applications
NASA Technical Reports Server (NTRS)
Landman, D.
1985-01-01
A broad product line of bismaleimide modified epoxy adhesives which are cured by conventional addition curing methods is described. These products fill a market need for 232 C (450 F) service adhesives which are cured in a manner similar to conventional 177 C (350 F) epoxy adhesives. The products described include film adhesives, pastes, and a primer. Subsequent development work has resulted in a new bismaleimide modified epoxy resin which uses a unique addition curing mechanism. This has resulted in products with improved thermomechanical properties compared to conventional bismaleimide epoxy resins. A film adhesive, paste, and matrix resin for composites using this new technology are described. In all cases, the products developed are heat cured by using typical epoxy cure cycles i.e., 1 hour at 177 C (350 F) followed by 2 hours postcure at 246 C (475 F).
The synthesis and dynamics research of new curing agent for epoxy resin
NASA Astrophysics Data System (ADS)
Peng, Yongli; Huang, Hengyu; Sun, Yong
2017-05-01
Two-step synthesis of trimellitic anhydride trimellitic anhydride n - butyl ester (TMNB) was introduced which could be used as an epoxy resin curing agent. The kinetics of the curing reaction was analyzed by N-order model and autocatalytic model. The curing kinetics parameters, the results show that the curing activation energy (Ea) of this system was 35.79kJ / mol. The kinetic equation of curing was d/a d t =2.1061 ×104e x p (-35.79/R T ) α0.5163(l-α ) 0.366 . Combined with β-1 / T extrapolation and experimental adjustment to obtain the resin system curing process: 75°C for 1h, 140°C for 3h, 160°C for 2h.
Fiber-optic sensor design for chemical process and environmental monitoring
NASA Astrophysics Data System (ADS)
Mahendran, R. S.; Wang, L.; Machavaram, V. R.; Pandita, S. D.; Chen, R.; Kukureka, S. N.; Fernando, G. F.
2009-10-01
"Curing" is a term that is used to describe the cross-linking reactions in a thermosetting resin system. Advanced fiber-reinforced composites are being used increasingly in a number of industrial sectors including aerospace, marine, sport, automotive and civil engineering. There is a general realization that the processing conditions that are used to manufacture the composite can have a major influence on its hot-wet mechanical properties. This paper is concerned with the design and demonstration of a number of sensor designs for in situ monitoring of the cross-linking reactions of a commercially available thermosetting resin system. Simple fixtures were constructed to enable a pair of cleaved optical fibers with a defined gap between the end-faces to be held in position. The resin system was introduced into this gap and the cure kinetics were followed by transmission infrared spectroscopy. A semi-empirical model was used to describe the cure process using the data obtained at different cure temperatures. The same sensor system was used to detect the ingress of moisture into the cured resin system.
RTM Production Monitoring of the A380 Hinge Arm Droop Nose Mechanism: A Multi-Sensor Approach.
Chiesura, Gabriele; Lamberti, Alfredo; Yang, Yang; Luyckx, Geert; Van Paepegem, Wim; Vanlanduit, Steve; Vanfleteren, Jan; Degrieck, Joris
2016-06-14
This research presents a case study of production monitoring on an aerospace composite component: the hinge arm of the droop nose mechanism on the Airbus A380 wing leading edge. A sensor network composed of Fibre Bragg Gratings, capacitive sensors for cure monitoring and thermocouples was embedded in its fibre reinforced lay-up and measurements were acquired throughout its Resin Transfer Moulding production process. Two main challenges had to be overcome: first, the integration of the sensor lines in the existing Resin Transfer Moulding mould without modifying it; second, the demoulding of the component without damaging the sensor lines. The proposed embedding solution has proved successful. The wavelength shifts of the Fibre Bragg Gratings were observed from the initial production stages, over the resin injection, the complete curing of the resin and the cooling-down prior to demoulding. The sensors proved to be sensitive to detecting the resin flow front, vacuum and pressure increase into the mould and the temperature increase caused by the resin curing. Measurements were also acquired during the post-curing cycle. Residual strains during all steps of the process were derived from the sensors' wavelength shift, showing values up to 0.2% in compression. Moreover, the capacitive sensors were able to follow-up the curing degree during the production process. The sensors proved able to detect the resin flow front, whereas thermocouples could not measure an appreciable increase of temperature due to the fact that the resin had the same temperature as the mould.
RTM Production Monitoring of the A380 Hinge Arm Droop Nose Mechanism: A Multi-Sensor Approach
Chiesura, Gabriele; Lamberti, Alfredo; Yang, Yang; Luyckx, Geert; Van Paepegem, Wim; Vanlanduit, Steve; Vanfleteren, Jan; Degrieck, Joris
2016-01-01
This research presents a case study of production monitoring on an aerospace composite component: the hinge arm of the droop nose mechanism on the Airbus A380 wing leading edge. A sensor network composed of Fibre Bragg Gratings, capacitive sensors for cure monitoring and thermocouples was embedded in its fibre reinforced lay-up and measurements were acquired throughout its Resin Transfer Moulding production process. Two main challenges had to be overcome: first, the integration of the sensor lines in the existing Resin Transfer Moulding mould without modifying it; second, the demoulding of the component without damaging the sensor lines. The proposed embedding solution has proved successful. The wavelength shifts of the Fibre Bragg Gratings were observed from the initial production stages, over the resin injection, the complete curing of the resin and the cooling-down prior to demoulding. The sensors proved to be sensitive to detecting the resin flow front, vacuum and pressure increase into the mould and the temperature increase caused by the resin curing. Measurements were also acquired during the post-curing cycle. Residual strains during all steps of the process were derived from the sensors’ wavelength shift, showing values up to 0.2% in compression. Moreover, the capacitive sensors were able to follow-up the curing degree during the production process. The sensors proved able to detect the resin flow front, whereas thermocouples could not measure an appreciable increase of temperature due to the fact that the resin had the same temperature as the mould. PMID:27314347
Monitoring the Cure State of Thermosetting Resins by Ultrasound.
Lionetto, Francesca; Maffezzoli, Alfonso
2013-09-05
The propagation of low intensity ultrasound in a curing resin, acting as a high frequency oscillatory excitation, has been recently proposed as an ultrasonic dynamic mechanical analysis (UDMA) for cure monitoring. The technique measures sound velocity and attenuation, which are very sensitive to changes in the viscoelastic characteristics of the curing resin, since the velocity is related to the resin storage modulus and density, while the attenuation is related to the energy dissipation and scattering in the curing resin. The paper reviews the results obtained by the authors' research group in the last decade by means of in-house made ultrasonic set-ups for both contact and air-coupled ultrasonic experiments. The basics of the ultrasonic wave propagation in polymers and examples of measurements of the time-evolution of ultrasonic longitudinal modulus and chemical conversion of different thermosetting resins are presented. The effect of temperature on the cure kinetics, the comparison with rheological, low frequency dynamic mechanical and calorimetric results, and the correlation between ultrasonic modulus and crosslinking density will be also discussed. The paper highlights the reliability of ultrasonic wave propagation for monitoring the physical changes taking place during curing and the potential for online monitoring during polymer and polymer matrix composite processing.
Monitoring the Cure State of Thermosetting Resins by Ultrasound
Lionetto, Francesca; Maffezzoli, Alfonso
2013-01-01
The propagation of low intensity ultrasound in a curing resin, acting as a high frequency oscillatory excitation, has been recently proposed as an ultrasonic dynamic mechanical analysis (UDMA) for cure monitoring. The technique measures sound velocity and attenuation, which are very sensitive to changes in the viscoelastic characteristics of the curing resin, since the velocity is related to the resin storage modulus and density, while the attenuation is related to the energy dissipation and scattering in the curing resin. The paper reviews the results obtained by the authors’ research group in the last decade by means of in-house made ultrasonic set-ups for both contact and air-coupled ultrasonic experiments. The basics of the ultrasonic wave propagation in polymers and examples of measurements of the time-evolution of ultrasonic longitudinal modulus and chemical conversion of different thermosetting resins are presented. The effect of temperature on the cure kinetics, the comparison with rheological, low frequency dynamic mechanical and calorimetric results, and the correlation between ultrasonic modulus and crosslinking density will be also discussed. The paper highlights the reliability of ultrasonic wave propagation for monitoring the physical changes taking place during curing and the potential for online monitoring during polymer and polymer matrix composite processing. PMID:28788306
Fast Curing of Composite Wood Products
DOE Office of Scientific and Technical Information (OSTI.GOV)
Dr. Arthur J. Ragauskas
2006-04-26
The overall objective of this program is to develop low temperature curing technologies for UF and PF resins. This will be accomplished by: • Identifying the rate limiting UF and PF curing reactions for current market resins; • Developing new catalysts to accelerate curing reactions at reduced press temperatures and times. In summary, these new curing technologies will improve the strength properties of the composite wood products and minimize the detrimental effects of wood extractives on the final product while significantly reducing energy costs for wood composites. This study is related to the accelerated curing of resins for wood compositesmore » such as medium density fiberboard (MDF), particle board (PB) and oriented strandboard (OSB). The latter is frequently manufactured with a phenol-formaldehyde resin whereas ureaformaldehyde (UF) resins are usually used in for the former two grades of composite wood products. One of the reasons that hinder wider use of these resins in the manufacturing of wood composites is the slow curing speed as well as inferior bondability of UF resin. The fast curing of UP and PF resins has been identified as an attractive process development that would allow wood to be bonded at higher moisture contents and at lower press temperatures that currently employed. Several differing additives have been developed to enhance cure rates of PF resins including the use of organic esters, lactones and organic carbonates. A model compound study by Conner, Lorenz and Hirth (2002) employed 2- and 4-hydroxymethylphenol with organic esters to examine the chemical basis for the reported enhanced reactivity. Their studies suggested that the enhance curing in the presence of esters could be due to enhanced quinone methide formation or enhanced intermolecular SN2 reactions. In either case the esters do not function as true catalysts as they are consumed in the reaction and were not found to be incorporated in the polymerized resin product. An alternative approach to accelerated PF curing can be accomplished with the addition amines or amides. The later functionality undergoes base catalyzed hydrolysis yielding the corresponding carboxyl ate and free amine which rapidly reacts with the phenolic methylol groups facilitating polymerization and curing of the PF resin (Pizzi, 1997).« less
In-situ measurement of thermoset resin degree of cure using embedded fiber optic
NASA Astrophysics Data System (ADS)
Breglio, Giovanni; Cusano, Andrea; Cutolo, Antonello; Calabro, Antonio M.; Cantoni, Stefania; Di Vita, Gandolfo; Buonocore, Vincenzo; Giordano, Michele; Nicolais, Luigi, II
1999-12-01
In this work, a fiber optic sensor based on Fresnel principle is presented. It is used to monitor the variations of the refractive index due to the cure process of an epoxy based resin. These materials are widely used in polymer- matrix composites. The process of thermoset matrix based composite involves mass and heat transfer coupled with irreversible chemical reactions inducing physical changes: the transformation of a fluid resin into a rubber and then into a solid glass. To improve the quality and the reliability of these materials key points are the cure monitoring and the optimization of the manufacturing process. To this aim, the fiber optic embedded sensor has been designed, developed and tested. Preliminary results on sensor capability to monitor the cure kinetics are shown. Correlation between the sensor output and conversion advancement has been proposed following the Lorentz-Lorenz law. Isothermal data form the sensor have been compared with calorimetric analysis of an epoxy based resin.
Phenylethynyl Containing Polyarylene Ethers/Polyimides Resin Infiltration of Composites
NASA Technical Reports Server (NTRS)
Dunn, DeRome O.
1998-01-01
The following tasks were performed at NCA&TSU during the second year in performance of the grant. LaRC-LV-1 13 resin was synthesized at NCA&TSU. In order to perform the synthesis, glassware and needed apparatus were purchased with grant funds along with the appropriate monomers. It was found that the LaRC-LV-1 13 resin was easily synthesized by the NMP solvent/toluene imminization/distilled water precipitation process. However, in use this resin exhibited a bubbling/foaming behavior during cure that was detrimental leading to the production of composite panels having a high void content. Composite panels were fabricated using compression molding and resin transfer molding (RTM) techniques. Initial fiber volume determinations were computed at NCA&TSU along with NASA-Langley measured c-scans on the panels produced. The initial results indicated a unsatisfactory level of approximately 20% by volume of voids. Testing of uniaxial coupons in compression to failure also agreed with these results. The uniaxial coupons delaminated as the major mode of failure indicative of an unacceptably low level of resin and to much void content in the final composites produced. In discussions with Dr. Brian Jensen, it was suggested the void fraction needs to be reduced to at least 2% by volume for a useful composite. The panels produced used both resin synthesized at NASA-Langley and NCA&TSU. In reviewing our progress over the past year, it was noted that the resin as formulated by the current synthesis process bubbled at elevated temperature. This was especially observed in neat resin slugs cured at the recommended one, four and eight hour cure temperatures. Pressurized cures where then performed with pressures up to 200 psi and simultaneously the lowest eight hour cure temperatures. Although this procedure reduced the amount of bubbles to some extent in the neat resin slugs it did not completely eliminate them. The cure reaction appears to be very energetic even at the lowest recommended cure temperature. Currently, the pressurized cure apparatus developed at NCA&TSU is limited to 200 psi.
Development and characterization of soy-based epoxy resins and pultruded FRP composites
NASA Astrophysics Data System (ADS)
Zhu, Jiang
This dissertation focuses on the development, manufacture and characterization of novel soy-based epoxy FRP composites. Use of alternative epoxy resin systems derived from a renewable resource holds potential for low cost raw materials for the polymer and composite industries. Epoxidized Allyl Soyate (EAS) and Epoxidized Methyl Soyate (EMS) were developed from soybean oil with two chemical modification procedures: transesterification and epoxidation. This research investigates the curing characteristics and thermal and mechanical properties of the neat soyate resin systems. The derived soyate resins have higher reactivity and superior performance compared to commercially available epoxidized soybean oil. An efficient two-step curing method was developed in order to utilize these soyate resins to their full potential. The epoxy co-resin systems with varied soyate resin content were successfully used to fabricate composite material through pultrusion. The pultrusion resin systems with 30 wt% soyate resins yielded improved, or comparable mechanical properties with neat commercial resins. A finite element analysis of the heat transfer and curing process was performed to study the processing characterization on glass/epoxy composite pultrusion. This model can be used to establish baseline process variables and will benefit subsequent optimization. This research demonstrates that soy-based resins, especially EAS, show considerable promise as an epoxy resin supplement for use in polymer and composite structural applications. The new products derived from soybean oil can provide competitive performance, low cost and environmental advantages.
Double-Vacuum-Bag Process for Making Resin-Matrix Composites
NASA Technical Reports Server (NTRS)
Bradford, Larry J.
2007-01-01
A double-vacuum-bag process has been devised as a superior alternative to a single-vacuum-bag process used heretofore in making laminated fiber-reinforced resin-matrix composite-material structural components. This process is applicable to broad classes of high-performance matrix resins including polyimides and phenolics that emit volatile compounds (solvents and volatile by-products of resin-curing chemical reactions) during processing. The superiority of the double-vacuum-bag process lies in enhanced management of the volatile compounds. Proper management of volatiles is necessary for making composite-material components of high quality: if not removed and otherwise properly managed, volatiles can accumulate in interior pockets as resins cure, thereby forming undesired voids in the finished products. The curing cycle for manufacturing a composite laminate containing a reactive resin matrix usually consists of a two-step ramp-and-hold temperature profile and an associated single-step pressure profile as shown in Figure 1. The lower-temperature ramp-and-hold step is known in the art as the B stage. During the B stage, prepregs are heated and volatiles are generated. Because pressure is not applied at this stage, volatiles are free to escape. Pressure is applied during the higher-temperature ramp-and-hold step to consolidate the laminate and impart desired physical properties to the resin matrix. The residual volatile content and fluidity of the resin at the beginning of application of consolidation pressure are determined by the temperature and time parameters of the B stage. Once the consolidation pressure is applied, residual volatiles are locked in. In order to produce a void-free, high-quality laminate, it is necessary to design the curing cycle to obtain the required residual fluidity and the required temperature at the time of application of the consolidation pressure.
Effect of curing mode on the micro-mechanical properties of dual-cured self-adhesive resin cements.
Ilie, Nicoleta; Simon, Alexander
2012-04-01
Light supplying to luting resin cements is impeded in several clinical situations, causing us to question whether materials can properly be cured to achieve adequately (or adequate) mechanical properties. The aim of this study was therefore to analyse the effect of light on the micro-mechanical properties of eight popular dual-cured self-adhesive resin cements by comparing them with two conventional, also dual-cured, resin cements. Four different curing procedures were applied: auto-polymerisation (dark curing) and light curing (LED unit, Freelight 2, 20 s) by applying the unit directly on the samples' surface, at a distance of 5 and 10 mm. Twenty minutes after curing, the samples were stored for 1 week at 37°C in a water-saturated atmosphere. The micro-mechanical properties-Vickers hardness, modulus of elasticity, creep and elastic/plastic deformation-were measured. Data were analysed with multivariate ANOVA followed by Tukey's test and partial eta-squared statistics (p < 0.05). A very strong influence of the material as well as filler volume and weight on the micro-mechanical properties was measured, whereas the influence of the curing procedure and type of cement-conventional or self-adhesive-was generally low. The influence of light on the polymerisation process was material dependent, with four different behaviour patterns to be distinguished. As a material category, significantly higher micro-mechanical properties were measured for the conventional compared to the self-adhesive resin cements, although this difference was low. Within the self-adhesive resin cements group, the variation in micro-mechanical properties was high. The selection of suitable resin cements should be done by considering, besides its adhesive properties, its micro-mechanical properties and curing behaviour also.
Turbine superalloy component defect repair with low-temperature curing resin
Hunt, David W.; Allen, David B.
2015-09-08
Voids, cracks or other similar defects in substrates of thermal barrier coated superalloy components, such as turbine blades or vanes, are filled with resin, without need to remove substrate material surrounding the void by grinding or other processes. The resin is cured at a temperature under 200.degree. C., eliminating the need for post void-filling heat treatment. The void-filled substrate and resin are then coated with a thermal barrier coating.
Acetylene-chromene terminated resins as high temperature thermosets
NASA Technical Reports Server (NTRS)
Godschalx, J. P.; Inbasekaran, M. N.; Bartos, B. R.; Scheck, D. M.; Laman, S. A.
1990-01-01
A novel phase transfer catalyzed process for the preparation of propargyl ethers has been developed. The propargyl ethers serve as precursors to a new class of thermosetting resins called acetylene-chromene terminated (ACT) resins. Heat treatment of a solution of propargyl ethers with various catalysts, followed by removal of solvent leads to the ACT resins via partial conversion of the propargyl ether groups to chromenes. This process reduces the energy content of the resin systems and reduces the amount of shrinkage found during cure. Due to the presence of the solvent the process is safe and gives rise to low viscosity products suitable for resin transfer molding and filament winding type applications. Due to the high glass transition temperature, high modulus, and low moisture uptake the cured resins display better than 232 C/wet performance. The thermal stability of the ACT resins in air at 204 C is superior to that of conventional bismaleimide resins. The resins also display excellent electrical properties.
Modeling the VARTM Composite Manufacturing Process
NASA Technical Reports Server (NTRS)
Song, Xiao-Lan; Loos, Alfred C.; Grimsley, Brian W.; Cano, Roberto J.; Hubert, Pascal
2004-01-01
A comprehensive simulation model of the Vacuum Assisted Resin Transfer Modeling (VARTM) composite manufacturing process has been developed. For isothermal resin infiltration, the model incorporates submodels which describe cure of the resin and changes in resin viscosity due to cure, resin flow through the reinforcement preform and distribution medium and compaction of the preform during the infiltration. The accuracy of the model was validated by measuring the flow patterns during resin infiltration of flat preforms. The modeling software was used to evaluate the effects of the distribution medium on resin infiltration of a flat preform. Different distribution medium configurations were examined using the model and the results were compared with data collected during resin infiltration of a carbon fabric preform. The results of the simulations show that the approach used to model the distribution medium can significantly effect the predicted resin infiltration times. Resin infiltration into the preform can be accurately predicted only when the distribution medium is modeled correctly.
High Temperature Transfer Molding Resins Based on 2,3,3',4'-Biphenyltetracarboxylic Dianhydride
NASA Technical Reports Server (NTRS)
Smith, J. G., Jr.; Connell, J. W.; Hergenrother, P. M.; Yokota, R.; Criss, J. M.
2002-01-01
As part of an ongoing effort to develop materials for resin transfer molding (RTM) processes to fabricate high performance/high temperature composite structures, phenylethynyl containing imides have been under investigation. New phenylethynyl containing imide compositions were prepared using 2,3,3',4'-biphenyltetracarboxylic dianhydride (a-BPDA) and evaluated for cured glass transition temperature (Tg), melt flow behavior, and for processability into flat composite panels via RTM. The a-BPDA imparts a unique combination of properties that are desirable for high temperature transfer molding resins. In comparison to its symmetrical counterpart (i.e. 3,3',4,4'-biphenyltetracarboxylic dianhydride), a-BPDA affords oligomers with lower melt viscosities and when cured, higher Tgs. Several candidates exhibited the appropriate combination of properties such as a low and stable melt viscosity required for RTM processes, high cured Tg, and moderate toughness. The chemistry, physical, and composite properties of select resins will be discussed.
NASA Astrophysics Data System (ADS)
Chehura, E.; Skordos, A. A.; Ye, C.-C.; James, S. W.; Partridge, I. K.; Tatam, R. P.
2005-04-01
Fibre Bragg gratings (FBGs) fabricated in linearly birefringent fibres were embedded in glass fibre/epoxy composites and in the corresponding unreinforced resin to monitor the effective transverse strain development during the cure process. The optical fibres containing the FBG sensors were aligned either normal or parallel to the reinforcement fibres in unidirectional glass fibre/epoxy prepregs. The chemical cure kinetics of the epoxy resin system used were studied using differential scanning calorimetry, in order to investigate the correlation between the strain monitoring results and the evolution of the curing reaction. A non-parametric cure kinetics model was developed and validated for this purpose. The effective transverse strain measured by the FBGs demonstrated high sensitivity to the degree of cure as a result of the densification of the resin caused by the curing reaction. The effective compressive transverse strain developed during the reaction, and thus the corresponding sensitivity to chemical changes, was higher in the case of the sensing fibre aligned normal to the reinforcement fibres than in the case of the sensor fibre parallel to the reinforcement fibres. Small but measurable sensitivity to cure induced changes was observed in the case of the unreinforced resin.
Thermochemical tests on resins: Char resistance of selected phenolic cured epoxides
NASA Technical Reports Server (NTRS)
Keck, F. L.
1982-01-01
Curing epoxy resins with novalac phenolic resins is a feasible approach for increasing intact char of the resin system. Char yields above 40% at 700 C were achieved with epoxy novalac (DEN 438)/novalac phenolic (BRWE 5833) resin systems with or without catalyst such as ethyl tri-phenyl phosphonium iodide. These char yields are comparable to commercially used epoxy resin systems like MY-720/DDS/BF3. Stable prepregs are easily made from a solvent solution of the epoxy/phenolic system and this provides a feasible process for fabrication of same into commercial laminates.
Low Melt Viscosity Resins for Resin Transfer Molding
NASA Technical Reports Server (NTRS)
Harris, Frank W.
2002-01-01
In recent years, resin transfer molding (RTM) has become one of the methods of choice for high performance composites. Its cost effectiveness and ease of fabrication are major advantages of RTM. RTM process usually requires resins with very low melt viscosity (less than 10 Poise). The optimum RTM resins also need to display high thennal-oxidative stability, high glass transition temperature (T(sub g)), and good toughness. The traditional PMR-type polyimides (e.g. PMR-15) do not fit this requirement, because the viscosities are too high and the nadic endcap cures too fast. High T(sub g), low-melt viscosity resins are highly desirable for aerospace applications and NASA s Reusable Launch Vehicle (RLV) program. The objective of this work is to prepare low-melt viscosity polyimide resins for RTM or resin film infusion (RFI) processes. The approach involves the synthesis of phenylethynyl-terminated imide oligomers. These materials have been designed to minimize their melt viscosity so that they can be readily processed. During the cure, the oligomers undergo both chain extension and crosslinking via the thermal polymerization of the phenylethynyl groups. The Phenylethynyl endcap is preferred over the nadic group due to its high curing temperature, which provides broader processing windows. This work involved the synthesis and polymerization of oligomers containing zig-zag backbones and twisted biphenyl structures. Some A-B type precursors which possessed both nitro and anhydride functionality, or both nitro and amine functionality, were also synthesized in order to obtain the well defined oligomers. The resulting zig-zag structured oligomers were then end-capped with 4-phenylethynylphthalic anhydride (PEPA) for further cure. The properties of these novel imide oligomers are evaluated.
Application of mass spectrometry to process control for polymer material in autoclave curing
NASA Technical Reports Server (NTRS)
Smith, A. C.
1983-01-01
Mass spectrometer analysis of gas samples collected during a cure cycle of polymer materials can be used as a process control technique. This technique is particularly helpful in studying the various types of solvents and resin systems used in the preparation of polymer materials and characterizing the chemical composition of different resin systems and their mechanism of polymerization.
Murthy, S Srinivasa; Murthy, Gargi S
2015-01-01
Background: Dentistry in general and prosthodontics in particular is evolving at greater pace, but the denture base resins poly methyl methacrylate. There has been vast development in modifying chemically and the polymerization techniques for better manipulation and enhancement of mechanical properties. One such invention was introduction of visible light cure (VLC) denture base resin. Argon ion lasers have been used extensively in dentistry, studies has shown that it can polymerize restorative composite resins. Since composite resin and VLC resin share the same photo initiator, Argon laser is tested as activator for polymerizing VLC resin. In the Phase 1 study, the VLC resin was evaluated for exposure time for optimum polymerization using argon ion laser and in Phase 2; flexural strength, impact strength, surface hardness and surface characteristics of laser cured resin was compared with light cure and conventional heat cure resin. Materials and Methods: Phase 1; In compliance with American Dental Association (ADA) specification no. 12, 80 samples were prepared with 10 each for different curing time using argon laser and evaluated for flexural strength on three point bend test. Results were compared to established performance requirement specified. Phase 2, 10 specimen for each of the mechanical properties (30 specimen) were polymerized using laser, visible light and heat and compared. Surface and fractured surface of laser, light and heat cured resins were examined under scanning electron microscope (SEM). Results: In Phase 1, the specimen cured for 7, 8, 9 and 10 min fulfilled ADA requirement. 8 min was taken as suitable curing time for laser curing. Phase 2 the values of mechanical properties were computed and subjected to statistical analysis using one-way ANOVA and Tukey post-hoc test. The means of three independent groups showed significant differences between any two groups (P < 0.001). Conclusion: Triad VLC resin can be polymerized by argon ion laser with 1 W/mm2 power and exposure time of 8 min to satisfy ADA specification. Impact strength, surface hardness of laser cure was better than light cure and heat cure resin. Flexural strength of light cure was better than laser cure and heat cure resin. The SEM study showed similar density on surface, the fractured surface of heat cure resin was dense and compact. PMID:26124596
No-Oven, No-Autoclave Composite Processing
NASA Technical Reports Server (NTRS)
Rauscher, Michael D.
2015-01-01
Very large composite structures, such as those used in NASA's Space Launch System, push the boundaries imposed by current autoclaves. New technology is needed to maintain composite performance and free manufacturing engineers from the restraints of curing equipment size limitations. Recent efforts on a Phase II project by Cornerstone Research Group, Inc. (CRG), have advanced the technology and manufacturing readiness levels of a unique two-part epoxy resin system. Designed for room-temperature infusion of a dry carbon preform, the system includes a no-heat-added cure that delivers 350 F composite performance in a matter of hours. This no-oven, no-autoclave (NONA) composite processing eliminates part-size constraints imposed by infrastructure and lowers costs by increasing throughput and reducing capital-specific, process-flow bottlenecks. As a result of the Phase II activity, NONA materials and processes were used to make high-temperature composite tooling suitable for further production of carbon-epoxy laminates and honeycomb/ sandwich-structure composites with an aluminum core. The technology platform involves tooling design, resin infusion processing, composite part design, and resin chemistry. The various technology elements are combined to achieve a fully cured part. The individual elements are not unusual, but they are combined in such a way that enables proper management of the heat generated by the epoxy resin during cure. The result is a self-cured carbon/ epoxy composite part that is mechanically and chemically stable at temperatures up to 350 F. As a result of the successful SBIR effort, CRG has launched NONA Composites as a spinoff subsidiary. The company sells resin to end users, fabricates finished goods for customers, and sells composite tooling made with NONA materials and processes to composite manufacturers.
Measuring UV Curing Parameters of Commercial Photopolymers used in Additive Manufacturing.
Bennett, Joe
2017-12-01
A testing methodology was developed to expose photopolymer resins and measure the cured material to determine two key parameters related to the photopolymerization process: E c (critical energy to initiate polymerization) and D p (penetration depth of curing light). Five commercially available resins were evaluated under exposure from 365 nm and 405 nm light at varying power densities and energies. Three different methods for determining the thickness of the cured resin were evaluated. Caliper measurements, stylus profilometry, and confocal laser scanning microscopy showed similar results for hard materials while caliper measurement of a soft, elastomeric material proved inaccurate. Working curves for the five photopolymers showed unique behavior both within and among the resins as a function of curing light wavelength. E c and D p for the five resins showed variations as large as 10×. Variations of this magnitude, if unknown to the user and not controlled for, will clearly affect printed part quality. This points to the need for a standardized approach for determining and disseminating these, and perhaps, other key parameters.
Method of controlling a resin curing process. [for fiber reinforced composites
NASA Technical Reports Server (NTRS)
Webster, Charles Neal (Inventor); Scott, Robert O. (Inventor)
1989-01-01
The invention relates to an analytical technique for controlling the curing process of fiber-reinforced composite materials that are formed using thermosetting resins. The technique is the percent gel method and involves development of a time-to-gel equation as a function of temperature. From this equation a rate-of-gel equation is then determined, and a percent gel is calculated which is the product of rate-of-gel times time. Percent gel accounting is used to control the proper pressure application point in an autoclave cure process to achieve desired properties in a production composite part.
A development of visible light cured FRP plate denture.
Kimura, H; Teraoka, F
1990-12-01
A FRP denture base, which was made from visible light curing prepreg, was developed. The visible light cured FRP denture base had advantages with respect to an adequate strength, bonding strength of acrylic base resin, esthetic properties and ease to manipulation. The matrix resin of Bis-GMA/UDMA/3 G at 48/48/4 was determined from the results of the bending test and manipulation processing. The sateen weave's glasscloth was used for the reinforcement of the prepreg. The adaptability of the FRP plate denture was better than that of the resin base denture constructed with microwave heating.
Aziz, Hawraa Khalid
2018-01-01
The criteria of conventional curing of polymethyl methacrylate do not match the standard properties of the denture base materials. This research was conducted to investigate the addition of TiO 2 nano practical on impact strength, thermal conductivity and color stability of acrylic resin cured by microwave in comparison to the conventional cured of heat-polymerized acrylic resin. 120 specimens made of high impact acrylic resin were divided into two main groups according to the type of curing (water bath, microwave), then each group was subdivided into two groups according to the addition of 3% TiO 2 nano-fillers and control group (without the addition of TiO 2 0%). Each group was subdivided according to the type of test into 3 groups with 10 specimens for each group. Data were statistically analyzed using Student t-test to detect the significant differences between tested and control groups at significance level ( P <0.05). According to curing type methods, the results showed that there was a significant decrease in impact strength of microwaved cured resin, but there was no significant difference in the thermal conductivity and color stability of resin. In addition, by using nanofiller, there was a significant increase in the impact strength and color stability with the addition of 3% TiO 2 nanofillers, but no significant difference was found in the thermal conductivity of the acrylic resin. The microwave curing of acrylic resin had no change in the color stability and thermal conductivity in comparison to the water bath, but the impact strength was decreased. The addition of 3% TiO 2 improved the impact and the color stability, but the thermal conductivity did not change.
[Effect of Radii barrier sleeves on cure depth of composite resin].
Wang, Binping; DU, Yongxiu
2009-01-01
To explore the effect of Radii barrier sleeves on the cure depth of composite resin. Cylinder mold was prepared, and the resin was filled strictly into the mold. The surface was flattened and then cured with plastic engraver's knife.The depth of composite resin which was cured by QHL75TM with or without Radii barrier sleeves was compared. The cure depth of composite resin which were cured by QHL75TM with or without Radii barrier sleeves of photo-curing machine was 4.38 mm and 4.27 mm respectively,with no statistical difference. The cure depth of composite resin is not influenced by Radii barrier sleeves under the same light condition.
NASA Technical Reports Server (NTRS)
Smith, J. G., Jr.; Connell, J. W.; Hergenrother, P. M.
1997-01-01
As part of a program to develop high temperature/high performance structural resins for aeronautical applications, imide oligomers containing terminal phenylethynyl groups with calculated number average molecular weights of 1250, 2500 and 5000 g/mol were prepared, characterized, and evaluated as adhesives and composite matrix resins. The goal of this work was to develop resin systems that are processable using conventional processing equipment into void free composites that exhibit high mechanical properties with long term high temperature durability, and are not affected by exposure to common aircraft fluids. The imide oligomers containing terminal phenylethynyl groups were fabricated into titanium adhesive specimens and IM-7 carbon fiber laminates under 0.1 - 1.4 MPa for 1 hr at 350-371 C. The lower molecular weight oligomers exhibited higher cured Tg, better processability, and better retention of mechanical properties at elevated temperature without significantly sacrificing toughness or damage tolerance than the higher molecular weight oligomer. The neat resin, adhesive and composite properties of the cured polymers will be presented.
Room Temperature Curing Resin Systems for Graphite/Epoxy Composite Repair.
1979-12-01
ROOM TEMPERATURE CURING RESIN SYSTEMS FOR GRAPHITE/EPOXY COMPOS--ETC(UI DEC 79 0 J CRABTREE N62269-79-C-G224 UNCLASSIFIE O80-46 NADC -781 1-6 NL END...Room Temperature Curing Resin Sys-U3 linal for Graphite/Epoxy Composite Repair •.Dec *79 NOR- -46h: V111IT NUM8ER(s) 4362269-79- ,722 S. PERFORMING...repair, composite repair room temperature cure resin , moderate temperature cure resins , epoxies, adhesives, vinyl eater polymers, anaerobic curing polymers
An Efficient Modelling Approach for Prediction of Porosity Severity in Composite Structures
NASA Technical Reports Server (NTRS)
Bedayat, Houman; Forghani, Alireza; Hickmott, Curtis; Roy, Martin; Palmieri, Frank; Grimsley, Brian; Coxon, Brian; Fernlund, Goran
2017-01-01
Porosity, as a manufacturing process-induced defect, highly affects the mechanical properties of cured composites. Multiple phenomena affect the formation of porosity during the cure process. Porosity sources include entrapped air, volatiles and off-gassing as well as bag and tool leaks. Porosity sinks are the mechanisms that contribute to reducing porosity, including gas transport, void shrinkage and collapse as well as resin flow into void space. Despite the significant progress in porosity research, the fundamentals of porosity in composites are not yet fully understood. The highly coupled multi-physics and multi-scale nature of porosity make it a complicated problem to predict. Experimental evidence shows that resin pressure history throughout the cure cycle plays an important role in the porosity of the cured part. Maintaining high resin pressure results in void shrinkage and collapse keeps volatiles in solution thus preventing off-gassing and bubble formation. This study summarizes the latest development of an efficient FE modeling framework to simulate the gas and resin transport mechanisms that are among the major phenomena contributing to porosity.
Processing factors affecting the clarity of a rapid-curing clear acrylic resin.
Keng, S B; Cruickshanks-Boyd, D W; Davies, E H
1979-10-01
The difficulty in repeatedly producing unblemished, clear acrylic resin in the dental laboratory has hindered its wider use, despite its many advantages over coloured material. Recently, rapid-cure dental acrylics have been introduced, which are available in both clear and coloured forms. This investigation examined various factors which may influence the production of unblemished, rapid-curing, clear acrylic resin. Utilizing a quantitative assessment of clarity, the most important factor influencing the clarity of the resin is shown to be the choice of separating medium. Tin-foil produces extremely high clarity, but alginate mould separator causes surface blanching. However, this surface blanching can be removed by polishing. Porosity, caused by too rapid curing, and stone model dryness are of only secondary importance. Possible water contamination of the monomer liquid due to accidental exposure only affects clarity at very high levels of contamination.
Dispersion stability in carbon nanotube modified polymers and its effect on the fracture toughness
NASA Astrophysics Data System (ADS)
Mirjalili, Vahid; Yourdkhani, Mostafa; Hubert, Pascal
2012-08-01
In this paper, the dispersion stability of multiwall carbon nanotubes (MWNTs) mixed with an epoxy resin is studied. An instrumented optical microscope with a hot stage was used to study the evolution of the carbon nanotubes (CNTs) dispersion during the cure of the resin. A new image processing approach is then introduced to quantify dispersion and identify the source of dispersion degradation during the cure. The results showed that the reduction of the resin viscosity at temperatures greater than 100 °C caused an irreversible re-agglomeration of the CNTs in the matrix. It was shown that the fine-tuning of the ratio and type of curing agent as well as the curing temperature directly affect the dispersion stability of MWNTs in the epoxy polymer. The dispersion quality was then directly correlated to the fracture toughness of the modified resin and a maximum of 20% improvement was achieved.
Composite Curing Process Nondestructive Evaluation
1988-06-01
3.5.3.2.1 Background (Arrheuius Equation) 50 3.5.3.2.2 Intepretation of AWG Data . . . 50 3.6 SIGNAL PROCESSING AND DATA OUTPUT .. ............ 52 4.0 RESIN...conventional methods: o permits in-situ measurement of fluorescence in remote, hostile environments o provides immunity to electromagnetic interferences...These devices are very sensitive to changes during material cure because sound escapes from the waveguide to the resin dependent on the relative
Process simulations for manufacturing of thick composites
NASA Astrophysics Data System (ADS)
Kempner, Evan A.
The availability of manufacturing simulations for composites can significantly reduce the costs associated with process development. Simulations provide a tool for evaluating the effect of processing conditions on the quality of parts produced without requiring numerous experiments. This is especially significant in parts that have troublesome features such as large thickness. The development of simulations for thick walled composites has been approached by examining the mechanics of resin flow and fiber deformation during processing, applying these evaluations to develop simulations, and evaluating the simulation with experimental results. A unified analysis is developed to describe the three-dimensional resin flow and fiber preform deformation during processing regardless of the manufacturing process used. It is shown how the generic governing evaluations in the unified analysis can be applied to autoclave molding, compression molding, pultrusion, filament winding, and resin transfer molding. A comparison is provided with earlier models derived individually for these processes. The evaluations described for autoclave curing were used to produce a one-dimensional cure simulation for autoclave curing of thick composites. The simulation consists of an analysis for heat transfer and resin flow in the composite as well as bleeder plies used to absorb resin removed from the part. Experiments were performed in a hot press to approximate curing in an autoclave. Graphite/epoxy laminates of 3 cm and 5 cm thickness were cured while monitoring temperatures at several points inside the laminate and thickness. The simulation predicted temperatures fairly closely, but difficulties were encountered in correlation of thickness results. This simulation was also used to study the effects of prepreg aging on processing of thick composites. An investigation was also performed on filament winding with prepreg tow. Cylinders were wound of approximately 12 mm thickness with pressure gages at the mandrel-composite interface. Cylinders were hoop wound with tensions ranging from 13-34 N. An analytical model was developed to calculate change in stress due to relaxation during winding. Although compressive circumferential stresses occurred throughout each of the cylinders, the magnitude was fairly low.
NASA Astrophysics Data System (ADS)
Martin, Ffion A.; Warrior, Nicholas A.; Simacek, Pavel; Advani, Suresh; Hughes, Adrian; Darlington, Roger; Senan, Eissa
2018-03-01
Very short manufacture cycle times are required if continuous carbon fibre and epoxy composite components are to be economically viable solutions for high volume composite production for the automotive industry. Here, a manufacturing process variant of resin transfer moulding (RTM), targets a reduction of in-mould manufacture time by reducing the time to inject and cure components. The process involves two stages; resin injection followed by compression. A flow simulation methodology using an RTM solver for the process has been developed. This paper compares the simulation prediction to experiments performed using industrial equipment. The issues encountered during the manufacturing are included in the simulation and their sensitivity to the process is explored.
FTIR Monitoring Of Curing Of Composites
NASA Technical Reports Server (NTRS)
Druy, Mark A.; Stevenson, William A.; Young, Philip R.
1990-01-01
Infrared-sensing optical fiber system developed to monitor principal infrared absorption bands resulting from vibrations of atoms and molecules as chemical bonds form when resin cured. System monitors resin chemistry more directly. Used to obtain Fourier transform infrared (FTIR) spectrum from graphite fiber/polyimide matrix resin prepreg. Embedded fiber optic FTIR sensor used to indicate state of cure of thermosetting composite material. Developed primarily to improve quality of advanced composites, many additional potential applications exist because principal of operation applicable to all organic materials and most inorganic gases. Includes monitoring integrities of composite materials in service, remote sensing of hazardous materials, and examination of processes in industrial reactors and furnaces.
Thermal Curing Process Monitoring of the Composite Material Using the FBG sensor
NASA Astrophysics Data System (ADS)
Zhang, Youhong; Chang, Xinlong; Zhang, Xiaojun; He, Xiangyong
2018-03-01
The raw composite material will suffer complex chemical and morphological changes during the thermal curing process, and it is difficult to monitor the curing process and curing effect. In this paper, the FBG sensor was embedded in the raw composite material to monitor the whole curing process. The experiment results showed that the FBG sensor can monitor the resin transformation and residual deformation of the composite material, and the FBG sensor can be applied to monitor the thermal curing process of the composite structure.
Dental composite polymerization: a three different sources comparison
NASA Astrophysics Data System (ADS)
Sozzi, Michele; Fornaini, Carlo; Lagori, Giuseppe; Merigo, Elisabetta; Cucinotta, Annamaria; Vescovi, Paolo; Selleri, Stefano
2015-02-01
The introduction of photo-activators, with absorption spectra in the violet region, in composite resins raised interest in the use of 405 nm diode lasers for polymerization. The purpose of this research is the evaluation of the resins polymerization by means of violet diode laser compared to traditional lamps. Two different resins have been used for the experiments: Filtek Supreme XT flow (3M ESPE, USA) and Tetric Evo flow (Ivoclar, Vivadent). The photo-activator used is Camphoroquinone, alone, or in combination with Lucirin TPO. The resins have been cured with an halogen lamp (Heliolux DXL, Vivadent Ivoclar, Austria), a broadband LED curing light (Valo Ultradent, USA) and a 405 nm laser (Euphoton, Italy). The measure of cure depth, of the volumetric shrinkage, and the conversion degree (DC%) of the double bond during the curing process have been evaluated. A composite layer of 3 mm was cured in Filtek Supreme resin (Camphoroquinone activator), lower if compared to the use of the other two light sources. Tests on Tetric Evo (Camphoroquinone + Lucirin) didn't show any improvement of the use of laser compared to the halogen lamp and the broadband LED. By measuring the volumetric shrinkage the laser induced the lower change with both the composites. In terms of DC% the lower performance was obtained with the laser. Considering that the polymerization process strongly depends on the kind of composite used the effectiveness of 405 nm laser proved to be lower than halogen lamps and broadband LEDs.
A theoretical study of resin flows for thermosetting materials during prepreg processing
NASA Technical Reports Server (NTRS)
Hou, T. H.
1984-01-01
A flow model which describes the process of resin consolidation during prepreg lamination was developed. The salient features of model predictions were explored. It is assumed that resin flows in all directions originate from squeezing action between two approaching adjacent fiber/fabric layers. In the horizontal direction, a squeezing flow between two nonporous parallel plates is analyzed, while in the vertical direction a poiseuille type pressure flow through porous media is assumed. Proper force and mass balance was established for the whole system which is composed of these two types of flow. A flow parameter, CF, shows to be a measure of processibility for the curing resin. For a given external load-F the responses of resin flow during prepreg lamination, as measured by CF, are categorized into three regions: (1) the low CF region where resin flows are inhibited by the high chemoviscosity during initial curing stages; (2) the median CF region where resin flows are properly controllable; and (3) the high CF region where resin flows are ceased due to fiber/fabric compression effects. Resin losses in both directions are calculated. Potential uses of this model and quality control of incoming prepreg material are discussed.
Oberholzer, T G; Makofane, M E; du Preez, I C; George, R
2012-06-01
Pulpal temperature changes induced by modern high powered light emitting diodes (LEDs) are of concern when used to cure composite resins. This study showed an increase in pulp chamber temperature with an increase in power density for all light cure units (LCU) when used to bulk cure composite resin. Amongst the three LEDs tested, the Elipar Freelight-2 recorded the highest temperature changes. Bulk curing recorded a significantly larger rise in pulp chamber temperature change than incrementally cured resin for all light types except for the Smartligh PS. Both the high powered LED and the conventional curing units can generate heat. Though this temperature rise may not be sufficient to cause irreversible pulpal damage, it would be safer to incrementally cure resins.
Pahlevan, Ayob; Tabatabaei, Masumeh Hasani; Arami, Sakineh; Valizadeh, Sara
2016-01-01
Objectives: Different light curing units are used for polymerization of composite resins. The aim of this study was to evaluate the degree of conversion (DC) and temperature rise in hybrid and low shrinkage composite resins cured by LED and Argon Laser curing lights. Materials and Methods: DC was measured using FTIR spectroscopy. For measuring temperature rise, composite resin samples were placed in Teflon molds and cured from the top. The thermocouple under samples recorded the temperature rise. After initial radiation and specimens reaching the ambient temperature, reirradiation was done and temperature was recorded again. Both temperature rise and DC data submitted to one-way ANOVA and Tukey-HSD tests (5% significance). Results: The obtained results revealed that DC was not significantly different between the understudy composite resins or curing units. Low shrinkage composite resin showed a significantly higher temperature rise than hybrid composite resin. Argon laser caused the lowest temperature rise among the curing units. Conclusion: Energy density of light curing units was correlated with the DC. Type of composite resin and light curing unit had a significant effect on temperature rise due to polymerization and curing unit, respectively. PMID:27843507
Pahlevan, Ayob; Tabatabaei, Masumeh Hasani; Arami, Sakineh; Valizadeh, Sara
2016-01-01
Different light curing units are used for polymerization of composite resins. The aim of this study was to evaluate the degree of conversion (DC) and temperature rise in hybrid and low shrinkage composite resins cured by LED and Argon Laser curing lights. DC was measured using FTIR spectroscopy. For measuring temperature rise, composite resin samples were placed in Teflon molds and cured from the top. The thermocouple under samples recorded the temperature rise. After initial radiation and specimens reaching the ambient temperature, reirradiation was done and temperature was recorded again. Both temperature rise and DC data submitted to one-way ANOVA and Tukey-HSD tests (5% significance). The obtained results revealed that DC was not significantly different between the understudy composite resins or curing units. Low shrinkage composite resin showed a significantly higher temperature rise than hybrid composite resin. Argon laser caused the lowest temperature rise among the curing units. Energy density of light curing units was correlated with the DC. Type of composite resin and light curing unit had a significant effect on temperature rise due to polymerization and curing unit, respectively.
NASA Technical Reports Server (NTRS)
Kranbuehl, D.; Kingsley, P.; Hart, S.; Loos, A.; Hasko, G.; Dexter, B.
1992-01-01
In-situ frequency dependent electromagnetic sensors (FDEMS) and the Loos resin transfer model have been used to select and control the processing properties of an epoxy resin during liquid pressure RTM impregnation and cure. Once correlated with viscosity and degree of cure the FDEMS sensor monitors and the RTM processing model predicts the reaction advancement of the resin, viscosity and the impregnation of the fabric. This provides a direct means for predicting, monitoring, and controlling the liquid RTM process in-situ in the mold throughout the fabrication process and the effects of time, temperature, vacuum and pressure. Most importantly, the FDEMS-sensor model system has been developed to make intelligent decisions, thereby automating the liquid RTM process and removing the need for operator direction.
Viswanathan, R; Shashibhushan, K K; Subba Reddy, V V
2011-12-01
To evaluate and compare shear bond strengths of composite resins to primary enamel and dentine when the adhesives are pre-cured (light cured before the application of the resin) or co-cured (adhesive and the resin light cured together). Buccal surfaces of 80 caries-free primary molars were wet ground to create bonding surfaces on enamel and dentine and specimens mounted on acrylic blocks. Two bonding agents (Prime and Bond NT® and Xeno III®) were applied to either enamel or dentine as per manufacturer's instructions. In 40 specimens, the bonding agent was light cured immediately after the application (pre-cured). The other 40 specimens were not light cured until the composite resin application (co-cured). Resin composite cylinders were made incrementally using acrylic moulds over the adhesives and light cured. Specimens were stored in deionised water for 24 hours at room temperature. Shear bond strength was measured using an Instron universal testing machine (in MPa) and was analysed with Student's unpaired t test. Light curing the adhesive separately produced significantly higher bond strengths to primary dentine than co-curing (p<0.001). At the same time light curing the adhesive separately did not produce significantly different bond strengths to primary enamel (p>0.05). Curing sequence had no significant effect on shear bond strength of adhesives on the primary enamel. Pre-curing adhesives before curing composite resins produced greater shear bond strength to primary dentine.
Mechanical impedance measurements for improved cost-effective process monitoring
NASA Astrophysics Data System (ADS)
Clopet, Caroline R.; Pullen, Deborah A.; Badcock, Rodney A.; Ralph, Brian; Fernando, Gerard F.; Mahon, Steve W.
1999-06-01
The aerospace industry has seen a considerably growth in composite usage over the past ten years, especially with the development of cost effective manufacturing techniques such as Resin Transfer Molding and Resin Infusion under Flexible Tooling. The relatively high cost of raw material and conservative processing schedules has limited their growth further in non-aerospace technologies. In-situ process monitoring has been explored for some time as a means to improving the cost efficiency of manufacturing with dielectric spectroscopy and optical fiber sensors being the two primary techniques developed to date. A new emerging technique is discussed here making use of piezoelectric wafers with the ability to sense not only aspects of resin flow but also to detect the change in properties of the resin as it cures. Experimental investigations to date have shown a correlation between mechanical impedance measurements and the mechanical properties of cured epoxy systems with potential for full process monitoring.
Morotomi, Takahiko; Hirata-Tsuchiya, Shizu; Washio, Ayako; Kitamura, Chiaki
2016-01-01
To assess the effects of different curing stages of 4-META/MMA-TBB resin on osteoblasts and gingival keratinocytes. The MC3T3-E1 murine pre-osteoblastic cell line and GE-1 murine gingival epithelial cell line were cultured with mixtures of Super-Bond C&B at different curing stages, and the cell viability was assessed. The alkaline phosphatase (ALP) activity of the MC3T3-E1 cells was also assessed. The majority of the MC3T3-E1 cells died and showed no ALP activity when cultured with 4-META/MMA-TBB resin during the initial curing phase (1 min of curing). A later curing phase of the 4-META/MMA-TBB resin (7 min of curing) showed cytotoxicity at day 1, but the toxic effect was temporary and the proliferative capacity and ALP activity in the cells were similar to control cells at day 7. Completely cured 4-META/MMA-TBB resin (after 1 or 12 h of curing) did not affect the cell viability or ALP activity of the MC3T3-E1 cells. In contrast, 4-META/MMA-TBB resin showed no effect on the GE-1 cells at any stage of curing. Although 4-META/MMA-TBB resin during the initial curing phase shows toxic effects on MC3T3-E1 cells, that cytotoxicity is minimal at later curing phases. In contrast, neither the uncured nor cured resins affected the GE-1 cells.
Determining resin/fiber content of laminates
NASA Technical Reports Server (NTRS)
Garrard, G. G.; Houston, D. W.
1979-01-01
Article discusses procedure where hydrazine is used to extract graphite fibers from cured polyimide resin. Method does not attack graphite fibers and is faster than hot-concentrated-acid digestion process.
Shimamoto, Daisuke; Hotta, Yuji
2018-01-01
The interfacial adhesion of recycled carbon fiber (CF) reinforced epoxy composite heated by microwave (MW) irradiation were investigated by changing the curing state of the epoxy resin. The recycled CF was recovered from the composite, which was prepared by vacuum-assisted resin transfer molding, by thermal degradation at 500 or 600 °C. Thermogravimetric analysis showed that the heating at 600 °C caused rough damage to the CF surface, whereas recycled CF recovered at 500 °C have few defects. The interfacial shear strength (IFSS) between recycled CF and epoxy resin was measured by a single-fiber fragmentation test. The test specimen was heated by MW after mixing the epoxy resin with a curing agent or pre-curing, in order to investigate the curing effects on the matrix resin. The IFSSs of the MW-irradiated samples were significantly varied by the curing state of the epoxy resin and the surface condition of recycled CF, resulting that they were 99.5 to 131.7% of oven heated samples Furthermore, rheological measurements showed that the viscosity and shrinking behaviors of epoxy resin were affected based on the curing state of epoxy resin before MW irradiation. PMID:29587422
Tominaga, Yuichi; Shimamoto, Daisuke; Hotta, Yuji
2018-03-26
The interfacial adhesion of recycled carbon fiber (CF) reinforced epoxy composite heated by microwave (MW) irradiation were investigated by changing the curing state of the epoxy resin. The recycled CF was recovered from the composite, which was prepared by vacuum-assisted resin transfer molding, by thermal degradation at 500 or 600 °C. Thermogravimetric analysis showed that the heating at 600 °C caused rough damage to the CF surface, whereas recycled CF recovered at 500 °C have few defects. The interfacial shear strength (IFSS) between recycled CF and epoxy resin was measured by a single-fiber fragmentation test. The test specimen was heated by MW after mixing the epoxy resin with a curing agent or pre-curing, in order to investigate the curing effects on the matrix resin. The IFSSs of the MW-irradiated samples were significantly varied by the curing state of the epoxy resin and the surface condition of recycled CF, resulting that they were 99.5 to 131.7% of oven heated samples Furthermore, rheological measurements showed that the viscosity and shrinking behaviors of epoxy resin were affected based on the curing state of epoxy resin before MW irradiation.
Evaluation of experimental epoxy monomers
NASA Technical Reports Server (NTRS)
Hodges, W. T.; St.clair, T. L.; Pratt, J. R.; Ficklin, R.
1985-01-01
Future generation aircraft need higher performance polymer matrices to fully achieve the weight savings possible with composite materials. New resins are being formulated in an effort to understand basic polymer behavior and to develop improved resins. Some polymer/curing agent combinations that could be useful are difficult to process. In the area of epoxies, a major problem is that some components have physical properties which make them difficult to utilize as matrix resins. A previous study showed that the use of ultrasonic energy can be advantageous in the mixing of curing agents into a standard epoxy resin, such as MY 720 (Ciba-Geigy designation). This work is expanded to include three novel epoxides.
Cui, Yong; Hou, Xiaopeng; Wang, Wenliang; Chang, Jianmin
2017-06-18
In this study, bio-oil from the fast pyrolysis of renewable biomass was used as the raw material to synthesize bio-oil phenol formaldehyde (BPF) resin-a desirable resin for fabricating phenolic-based material. During the synthesis process, paraformaldehyde was used to achieve the requirement of high solid content and low viscosity. The properties of BPF resins were tested. Results indicated that BPF resin with the bio-oil addition of 20% had good performance on oxygen index and bending strength, indicating that adding bio-oil could modify the fire resistance and brittleness of PF resin. The thermal curing behavior and heat resistance of BPF resins were investigated by differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA). Results showed that adding bio-oil had an impact on curing characteristics and thermal degradation process of PF resin, but the influence was insignificant when the addition was relatively low. The chemical structure and surface characteristics of BPF resins were determined by Fourier transform infrared (FTIR) spectroscopy and scanning electron microscopy (SEM). The analysis demonstrated that adding bio-oil in the amount of 20% was able to improve the crosslinking degree and form more hydrocarbon chains in PF resin.
Toughened epoxy resin system and a method thereof
Janke, C.J.; Dorsey, G.F.; Havens, S.J.; Lopata, V.J.
1998-03-10
Mixtures of epoxy resins with cationic initiators are curable under high energy ionizing radiation such as electron beam radiation, X-ray radiation, and gamma radiation. The composition of this process consists of an epoxy resin, a cationic initiator such as a diaryliodonium or triarylsulfonium salt of specific anions, and a toughening agent such as a thermoplastic, hydroxy-containing thermoplastic oligomer, epoxy-containing thermoplastic oligomer, reactive flexibilizer, rubber, elastomer, or mixture thereof. Cured compositions have high glass transition temperatures, good mechanical properties, and good toughness. These properties are comparable to those of similar thermally cured epoxies.
Toughened epoxy resin system and a method thereof
Janke, Christopher J.; Dorsey, George F.; Havens, Stephen J.; Lopata, Vincent J.
1998-01-01
Mixtures of epoxy resins with cationic initiators are curable under high energy ionizing radiation such as electron beam radiation, X-ray radiation, and gamma radiation. The composition of this process consists of an epoxy resin, a cationic initiator such as a diaryliodonium or triarylsulfonium salt of specific anions, and a toughening agent such as a thermoplastic, hydroxy-containing thermoplastic oligomer, epoxy-containing thermoplastic oligomer, reactive flexibilizer, rubber, elastomer, or mixture thereof. Cured compositions have high glass transition temperatures, good mechanical properties, and good toughness. These properties are comparable to those of similar thermally cured epoxies.
Cure Cycle Optimization of Rapidly Cured Out-Of-Autoclave Composites.
Dong, Anqi; Zhao, Yan; Zhao, Xinqing; Yu, Qiyong
2018-03-13
Out-of-autoclave prepreg typically needs a long cure cycle to guarantee good properties as the result of low processing pressure applied. It is essential to reduce the manufacturing time, achieve real cost reduction, and take full advantage of out-of-autoclave process. The focus of this paper is to reduce the cure cycle time and production cost while maintaining high laminate quality. A rapidly cured out-of-autoclave resin and relative prepreg were independently developed. To determine a suitable rapid cure procedure for the developed prepreg, the effect of heating rate, initial cure temperature, dwelling time, and post-cure time on the final laminate quality were evaluated and the factors were then optimized. As a result, a rapid cure procedure was determined. The results showed that the resin infiltration could be completed at the end of the initial cure stage and no obvious void could be seen in the laminate at this time. The laminate could achieve good internal quality using the optimized cure procedure. The mechanical test results showed that the laminates had a fiber volume fraction of 59-60% with a final glass transition temperature of 205 °C and excellent mechanical strength especially the flexural properties.
Cure Cycle Optimization of Rapidly Cured Out-Of-Autoclave Composites
Dong, Anqi; Zhao, Yan; Zhao, Xinqing; Yu, Qiyong
2018-01-01
Out-of-autoclave prepreg typically needs a long cure cycle to guarantee good properties as the result of low processing pressure applied. It is essential to reduce the manufacturing time, achieve real cost reduction, and take full advantage of out-of-autoclave process. The focus of this paper is to reduce the cure cycle time and production cost while maintaining high laminate quality. A rapidly cured out-of-autoclave resin and relative prepreg were independently developed. To determine a suitable rapid cure procedure for the developed prepreg, the effect of heating rate, initial cure temperature, dwelling time, and post-cure time on the final laminate quality were evaluated and the factors were then optimized. As a result, a rapid cure procedure was determined. The results showed that the resin infiltration could be completed at the end of the initial cure stage and no obvious void could be seen in the laminate at this time. The laminate could achieve good internal quality using the optimized cure procedure. The mechanical test results showed that the laminates had a fiber volume fraction of 59–60% with a final glass transition temperature of 205 °C and excellent mechanical strength especially the flexural properties. PMID:29534048
Fiber Reinforced Polyester Resins Polymerized by Microwave Source
NASA Astrophysics Data System (ADS)
Visco, A. M.; Calabrese, L.; Cianciafara, P.; Bonaccorsi, L.; Proverbio, E.
2007-12-01
Polyester resin based composite materials are widely used in the manufacture of fiberglass boats. Production time of fiberglass laminate components could be strongly reduced by using an intense energy source as well as microwaves. In this work a polyester resin was used with 2% by weight of catalyst and reinforced with chopped or woven glass fabric. Pure resin and composite samples were cured by microwaves exposition for different radiation times. A three point bending test was performed on all the cured samples by using an universal testing machine and the resulting fracture surfaces were observed by means of scanning electron microscopy (SEM). The results of mechanical and microscopy analyses evidenced that microwave activation lowers curing time of the composite while good mechanical properties were retained. Microwaves exposition time is crucial for mechanical performance of the composite. It was evidenced that short exposition times suffice for resin activation while long exposure times cause fast cross linking and premature matrix fracture. Furthermore high-radiation times induce bubbles growth or defects nucleation within the sample, decreasing composite performance. On the basis of such results microwave curing activation of polyester resin based composites could be proposed as a valid alternative method for faster processing of laminated materials employed for large-scale applications.
Esposito Corcione, Carola; Freuli, Fabrizio; Frigione, Mariaenrica
2014-01-01
The curing reaction of a commercial cold-curing structural epoxy resin, specifically formulated for civil engineering applications, was analyzed by thermal analysis as a function of the curing time and the sample thickness. Original and remarkable results regarding the effects of curing time on the glass transition temperature and on the residual heat of reaction of the cold-cured epoxy were obtained. The influence of the sample thickness on the curing reaction of the cold-cured resin was also deeply investigated. A highly exothermal reaction, based on a self-activated frontal polymerization reaction, was supposed and verified trough a suitable temperature signal acquisition system, specifically realized for this measurement. This is one of the first studies carried out on the curing behavior of these peculiar cold-cured epoxy resins as a function of curing time and thickness. PMID:28788215
Corcione, Carola Esposito; Freuli, Fabrizio; Frigione, Mariaenrica
2014-09-22
The curing reaction of a commercial cold-curing structural epoxy resin, specifically formulated for civil engineering applications, was analyzed by thermal analysis as a function of the curing time and the sample thickness. Original and remarkable results regarding the effects of curing time on the glass transition temperature and on the residual heat of reaction of the cold-cured epoxy were obtained. The influence of the sample thickness on the curing reaction of the cold-cured resin was also deeply investigated. A highly exothermal reaction, based on a self-activated frontal polymerization reaction, was supposed and verified trough a suitable temperature signal acquisition system, specifically realized for this measurement. This is one of the first studies carried out on the curing behavior of these peculiar cold-cured epoxy resins as a function of curing time and thickness.
American Society of Composites, 32nd Technical Conference
DOE Office of Scientific and Technical Information (OSTI.GOV)
Aitharaju, Venkat; Yu, Hang; Zhao, Selina
Resin transfer molding (RTM) has become increasingly popular for the manufacturing of composite parts. To enable high volume manufacturing and obtain good quality parts at an acceptable cost to automotive industry, accurate process simulation tools are necessary to optimize the process conditions. Towards that goal, General Motors and the ESI-group are involved in developing a state of the art process simulation tool for composite manufacturing in a project supported by the Department of Energy. This paper describes the modeling of various stages in resin transfer molding such as resin injection, resin curing, and part distortion. An instrumented RTM system locatedmore » at the General Motors Research and Development center was used to perform flat plaque molding experiments. The experimental measurements of fill time, in-mold pressure versus time, cure variation with time, and part deformation were compared with the model predictions and very good correlations were observed.« less
High temperature polymerization monitoring of an epoxy resin using ultrasound
NASA Astrophysics Data System (ADS)
Maréchal, P.; Ghodhbani, N.; Duflo, H.
2018-05-01
In this study, the real time ultrasonic monitoring is investigated to quantify changes in physical and mechanical properties during the manufacture of composite structures. In this context, an experimental transmission was developed with the aim of characterizing a high temperature polymerization reaction and post-curing properties using an ultrasonic method. First, the monitoring of ultrasonic parameters of a thermosetting resin is carried out in a device reproducing the experimental conditions for manufacturing a composite material with a process known as RTM, that is to say an isothermal polymerization at T = 160°C. During this curing, the resin is changing from its initial viscous liquid state to its final viscous solid state. Between those states, a glassy transition stage is observed, during which the physical properties are strongly changing, i.e. an increase of the ultrasonic velocity up to its steady value and a transient increase of the ultrasonic attenuation. Second, the ultrasonic inspection of the thermosetting resin is performed during a heating and cooling process to study the temperature sensitivity after curing. This type of characterization leads to identifying the ultrasonic properties dependence before, during and after the glassy transition temperature Tg . Eventually, this study is composed of two complementary parts: the first is useful for the curing optimization, while the second one is fruitful for the post-processing characterization in a temperature range including the glassy transition temperature Tg .
X.-M. Wang; B. Riedl; A.W. Christiansen; R.L. Geimer
1994-01-01
Phenol-formaldehyde (PF) resin is a widely used adhesive in the manufacture of wood composites. However, curing behaviour of the resin under various environmental conditions is not well known. A differential scanning calorimeter was employed to characterize the degree of resin cure in this study. Resin-impregnated glass cloth samples with varied moisture contents (0,31...
Chemoviscosity modeling for thermosetting resins - I
NASA Technical Reports Server (NTRS)
Hou, T. H.
1984-01-01
A new analytical model for chemoviscosity variation during cure of thermosetting resins was developed. This model is derived by modifying the widely used WLF (Williams-Landel-Ferry) Theory in polymer rheology. Major assumptions involved are that the rate of reaction is diffusion controlled and is linearly inversely proportional to the viscosity of the medium over the entire cure cycle. The resultant first order nonlinear differential equation is solved numerically, and the model predictions compare favorably with experimental data of EPON 828/Agent U obtained on a Rheometrics System 4 Rheometer. The model describes chemoviscosity up to a range of six orders of magnitude under isothermal curing conditions. The extremely non-linear chemoviscosity profile for a dynamic heating cure cycle is predicted as well. The model is also shown to predict changes of glass transition temperature for the thermosetting resin during cure. The physical significance of this prediction is unclear at the present time, however, and further research is required. From the chemoviscosity simulation point of view, the technique of establishing an analytical model as described here is easily applied to any thermosetting resin. The model thus obtained is used in real-time process controls for fabricating composite materials.
Latent Hardeners for the Assembly of Epoxy Composites
NASA Technical Reports Server (NTRS)
Palmieri, Frank; Wohl, Christopher J.; Connell, John W.; Mercado, Zoar; Galloway, Jordan
2016-01-01
Large-scale composite structures are commonly joined by secondary bonding of molded-and-cured thermoset components. This approach may result in unpredictable joint strengths. In contrast, assemblies made by co-curing, although limited in size by the mold, result in stable structures, and are certifiable for commercial aviation because of structural continuity through the joints. Multifunctional epoxy resins were prepared that should produce fully-cured subcomponents with uncured joining surfaces, enabling them to be assembled by co-curing in a subsequent out-of-autoclave process. Aromatic diamines were protected by condensation with a ketone or aldehyde to form imines. Properties of the amine-cured epoxy were compared with those of commercially available thermosetting epoxy resins and rheology and thermal analysis were used to demonstrate the efficacy of imine protection. Optimum conditions to reverse the protecting chemistry in the solid state using moisture and acid catalysis were determined. Alternative chemistries were also investigated. For example, chain reaction depolymerization and photoinitiated catalysts would be expected to minimize liberation of volatile organic content upon deprotection and avoid residual reactive species that could damage the resin. Results from the analysis of protected and deprotected resins will be presented.
Lima, Ana Paula Barbosa; Vitti, Rafael Pino; Amaral, Marina; Neves, Ana Christina Claro; da Silva Concilio, Lais Regiane
2018-04-01
This study evaluated the dimensional stability of a complete-arch prosthesis processed by conventional method in water bath or microwave energy and polymerized by two different curing cycles. Forty maxillary complete-arch prostheses were randomly divided into four groups (n = 10): MW1 - acrylic resin cured by one microwave cycle; MW2 - acrylic resin cured by two microwave cycles: WB1 - conventional acrylic resin polymerized using one curing cycle in a water bath; WB2 - conventional acrylic resin polymerized using two curing cycles in a water bath. For evaluation of dimensional stability, occlusal vertical dimension (OVD) and area of contact points were measured in two different measurement times: before and after the polymerization method. A digital caliper was used for OVD measurement. Occlusal contact registration strips were used between maxillary and mandibular dentures to measure the contact points. The images were measured using the software IpWin32, and the differences before and after the polymerization methods were calculated. The data were statistically analyzed using the one-way ANOVA and Tukey test (α = .05). he results demonstrated significant statistical differences for OVD between different measurement times for all groups. MW1 presented the highest OVD values, while WB2 had the lowest OVD values ( P <.05). No statistical differences were found for area of contact points among the groups ( P =.7150). The conventional acrylic resin polymerized using two curing cycles in a water bath led to less difference in OVD of complete-arch prosthesis.
Cork-resin ablative insulation for complex surfaces and method for applying the same
NASA Technical Reports Server (NTRS)
Walker, H. M.; Sharpe, M. H.; Simpson, W. G. (Inventor)
1980-01-01
A method of applying cork-resin ablative insulation material to complex curved surfaces is disclosed. The material is prepared by mixing finely divided cork with a B-stage curable thermosetting resin, forming the resulting mixture into a block, B-stage curing the resin-containing block, and slicing the block into sheets. The B-stage cured sheet is shaped to conform to the surface being insulated, and further curing is then performed. Curing of the resins only to B-stage before shaping enables application of sheet material to complex curved surfaces and avoids limitations and disadvantages presented in handling of fully cured sheet material.
Early hardness of self-adhesive resin cements cured under indirect resin composite restorations.
Giráldez, Isabel; Ceballos, Laura; Garrido, Miguel A; Rodríguez, Jesús
2011-04-01
To determine the influence of curing mode on the surface hardness of seven resin cements used to lute indirect composite restorations. Seven commercial dual-curing resin cements were tested: two were total-etch (RelyX ARC [3M ESPE, St. Paul, MN, USA] and Variolink II [Ivoclar Vivadent, Schaan, Liechtenstein]); one was self-etch (Multilink Automix [Ivoclar Vivadent]), and four were self-adhesive (RelyX Unicem [3M ESPE], Maxcem Elite [Kerr Corp., Orange, CA, USA], SmartCem2 [Dentsply, Detrey, GmbH, Konstanz, Germany], and G-Cem [GC CORPORATION, Itabashi-Ku, Tokyo, Japan]). Three specimens (0.5 × 6.5mm) of each material were prepared for each of three experimental groups: Group 1 (cements allowed to self cure); Group 2 (cements light-cured for 40 seconds); and Group 3 (cements light-cured for 80 seconds). All specimens were cured through a 4-mm-thick composite cylinder (Filtek Z250-A3). Surface microhardness numbers were determined at 20 min after preparation. Results were analyzed by two-way analysis of variance and Student-Newman-Keuls tests (p<0.05). Superficial hardness was significantly influenced by the resin cement tested (p<0.0001), the curing mode (p<0.0001), and their interaction (p<0.0001). RelyX ARC exhibited the highest mean microhardness values regardless of the curing mode. Light-curing significantly increased the microhardness of all resin cements studied, and these values increased even further with a doubling of irradiation time. Self-adhesive cements exhibited different behavior according to the curing mode. RelyX Unicem was highly sensitive to light irradiation, showing the lowest mean values in the self-curing mode. After light irradiation for 40 or 80 seconds, Maxcem Elite exhibited the lowest mean hardness values of all the resin cements tested. The microhardness of resin cements is highly dependent on the brand. Dual-curing resin cements should always be light irradiated for longer periods than that recommended by manufacturers. Dual-curing resin cements should always be light-cured for longer irradiation times, as light irradiation for 80 seconds yields the highest microhardness values in comparison with self-curing or light irradiation for 40 seconds. However, some self-adhesive resin cements exhibit low microhardness values when used to cement 4-mm-thick indirect composite restorations regardless of the curing mode applied. © 2011, COPYRIGHT THE AUTHORS. JOURNAL COMPILATION © 2011, WILEY PERIODICALS, INC.
Anisotropy of Photopolymer Parts Made by Digital Light Processing
Monzón, Mario; Ortega, Zaida; Hernández, Alba; Paz, Rubén; Ortega, Fernando
2017-01-01
Digital light processing (DLP) is an accurate additive manufacturing (AM) technology suitable for producing micro-parts by photopolymerization. As most AM technologies, anisotropy of parts made by DLP is a key issue to deal with, taking into account that several operational factors modify this characteristic. Design for this technology and photopolymers becomes a challenge because the manufacturing process and post-processing strongly influence the mechanical properties of the part. This paper shows experimental work to demonstrate the particular behavior of parts made using DLP. Being different to any other AM technology, rules for design need to be adapted. Influence of build direction and post-curing process on final mechanical properties and anisotropy are reported and justified based on experimental data and theoretical simulation of bi-material parts formed by fully-cured resin and partially-cured resin. Three photopolymers were tested under different working conditions, concluding that post-curing can, in some cases, correct the anisotropy, mainly depending on the nature of photopolymer. PMID:28772426
NASA Technical Reports Server (NTRS)
Alston, William B.
1986-01-01
PRM (polymerization of monomeric reactants) methodology was used to prepare thirty different polyimide oligomeric resins. Monomeric composition as well as chain length between sites of crosslinks were varied to examine their effects on glass transition temperature (Tg) of the cured/postcured resins. An almost linear correlation of Tg versus molecular distance between the crosslinks was observed. An attempt was made to correlate Tg with initial mechanical properties (flexural strength and interlaminar shear strength) of unidirectional graphite fiber composites prepared with these resins. However, the scatter in mechanical strength data prevented obtaining as clear a correlation as was observed for the structural modification/crosslink distance versus Tg. Instead, only a range of composite mechanical properties was obtained at the test temperatures studied (room temperature, 288 and 316 C). Perhaps more importantly, what did become apparent during the attempted correlation study was: (1) that PMR methodology could be used to prepare composites from resins that contain a wide variety of monomer modifications, and (2) that these composites almost invariably provided satisfactory initial mechanical properties as long as the resins selected were melt processable.
NASA Technical Reports Server (NTRS)
Alston, W. B.
1986-01-01
PRM (polymerization of monomeric reactants) methodology was used to prepare thirty different polyimide oligomeric resins. Monomeric composition as well as chain length between sites of crosslinks were varied to examine their effects on glass transition temperature (Tg) of the cured/postcured resins. An almost linear correlation of Tg versus molecular distance between the crosslinks was observed. An attempt was made to correlate Tg with initial mechanical properties (flexural strength and interlaminar shear strength) of unidirectional graphite fiber composites prepared with these resins. However, the scatter in mechanical strength data prevented obtaining as clear a correlation as was observed for the structural modification/crosslink distance versus Tg. Instead, only a range of composite mechanical properties was obtained at the test temperatures studied (room temperature, 288 and 316 C). Perhaps more importantly, what did become apparent during the attempted correlation study was: (1) that PMR methodology could be used to prepare composites from resins that contain a wide variety of monomer modifications, and (2) that these composites almost invariably provided satisfactory initial mechanical properties as long as the resins selected were melt processable.
Chemoviscosity modeling for thermosetting resins, 2
NASA Technical Reports Server (NTRS)
Hou, T. H.
1985-01-01
A new analytical model for simulating chemoviscosity of thermosetting resin was formulated. The model is developed by modifying the Williams-Landel-Ferry (WLF) theory in polymer rheology for thermoplastic materials. By assuming a linear relationship between the glass transition temperature and the degree of cure of the resin system under cure, the WLF theory can be modified to account for the factor of reaction time. Temperature dependent functions of the modified WLF theory constants were determined from the isothermal cure data of Lee, Loos, and Springer for the Hercules 3501-6 resin system. Theoretical predictions of the model for the resin under dynamic heating cure cycles were shown to compare favorably with the experimental data reported by Carpenter. A chemoviscosity model which is capable of not only describing viscosity profiles accurately under various cure cycles, but also correlating viscosity data to the changes of physical properties associated with the structural transformations of the thermosetting resin systems during cure was established.
The Modification of a Tetrafunctional Epoxy and Its Curing Reaction
Yu, Mingming; Feng, Bin; Xie, Wang; Fang, Lin; Li, Hong; Liu, Liqi; Ren, Musu; Sun, Jinliang; Zhang, Jiabao; Hu, Hefeng
2015-01-01
Recent experimental results showed that the Tg of cured resin scarcely decreased and the impact strength of resins increased by over 50% when a tetrafunctional epoxy named N,N,N',N'-tetraglycidyl-4,4'-diaminodiphenyl ether (TGDDE) was introduced to an appropriate flexible chain from a dimer fatty acid (DFA). In order to understand the reason for this phenomenon, the modification and the chemical structure of the prepolymer together with the curing reaction and the viscoelasticity of the cured resins were studied in detail in the present work. The results indicated that the modification would help the prepolymer improve its molecular mobility. As a result, the resins could be further cured, resulting in the cross-linking density increasing. This is because the curing efficiency was increased, but the tetrafunctional epoxy was not cured completely due to its large steric hindrance. Moreover, the flexibility of some parts of the networks was improved, which was beneficial for the toughness of the cured resins. Therefore, the toughness of the tetrafunctional resin was improved with little influence on the thermal properties when the epoxies were modified with an appropriate content of DFA.
Light-Cured Self-Etch Adhesives Undergo Hydroxyapatite-Triggered Self-Cure
Liu, Y.; Bai, X.; Liu, Y.W.; Wang, Y.
2015-01-01
Light cure is a popular mode of curing for dental adhesives. However, it suffers from inadequate light delivery when the restoration site is less accessible, in which case a self-cure mechanism is desirable to salvage any compromised polymerization. We previously reported a novel self-cure system mediated by ethyl 4-(dimethylamino)-benzoate (4E) and hydroxyapatite (HAp). The present work aims to investigate if such self-cure phenomenon takes place in adhesives that underwent prior inadequate light cure and to elucidate if HAp released from the dental etching process is sufficient to trigger it. Model self-etch adhesives were formulated with various components, including bis[2-methacryloyloxy)ethyl]-phosphate (2MP) as acidic monomer and trimethylbenzoyl-diphenylphosphine oxide (TPO) as photoinitiator. In vitro evolution of degree of conversion (DC) of HAp-incorporated adhesives was monitored by infrared spectroscopy during light irradiation and dark storage. Selected adhesives were allowed to etch and extract HAp from enamel, light-cured in situ, and stored in the dark, after which Raman line mapping was used to obtain spatially resolved DC across the enamel-resin interface. Results showed that TPO+4E adhesives reached DC similar to TPO-only counterparts upon completion of light irradiation but underwent another round of initiation that boosted DC to ~100% regardless of HAp level or prior light exposure. When applied to enamel, TPO-only adhesives had ~80% DC in resin, which gradually descended to ~50% in enamel, whereas TPO+4E adhesives consistently scored ~80% DC across the enamel-resin interface. These observations suggest that polymerization of adhesives that underwent insufficient light cure is salvaged by the novel self-cure mechanism, and such salvaging effect can be triggered by HAp released from dental substrate during the etching process. PMID:26635279
Light-Cured Self-Etch Adhesives Undergo Hydroxyapatite-Triggered Self-Cure.
Liu, Y; Bai, X; Liu, Y W; Wang, Y
2016-03-01
Light cure is a popular mode of curing for dental adhesives. However, it suffers from inadequate light delivery when the restoration site is less accessible, in which case a self-cure mechanism is desirable to salvage any compromised polymerization. We previously reported a novel self-cure system mediated by ethyl 4-(dimethylamino)-benzoate (4E) and hydroxyapatite (HAp). The present work aims to investigate if such self-cure phenomenon takes place in adhesives that underwent prior inadequate light cure and to elucidate if HAp released from the dental etching process is sufficient to trigger it. Model self-etch adhesives were formulated with various components, including bis[2-methacryloyloxy)ethyl]-phosphate (2MP) as acidic monomer and trimethylbenzoyl-diphenylphosphine oxide (TPO) as photoinitiator. In vitro evolution of degree of conversion (DC) of HAp-incorporated adhesives was monitored by infrared spectroscopy during light irradiation and dark storage. Selected adhesives were allowed to etch and extract HAp from enamel, light-cured in situ, and stored in the dark, after which Raman line mapping was used to obtain spatially resolved DC across the enamel-resin interface. Results showed that TPO+4E adhesives reached DC similar to TPO-only counterparts upon completion of light irradiation but underwent another round of initiation that boosted DC to ~100% regardless of HAp level or prior light exposure. When applied to enamel, TPO-only adhesives had ~80% DC in resin, which gradually descended to ~50% in enamel, whereas TPO+4E adhesives consistently scored ~80% DC across the enamel-resin interface. These observations suggest that polymerization of adhesives that underwent insufficient light cure is salvaged by the novel self-cure mechanism, and such salvaging effect can be triggered by HAp released from dental substrate during the etching process. © International & American Associations for Dental Research 2015.
Ma, Yu-juan; Cui, Hua-peng; Li, Hai-yang
2011-04-01
To analyze the amount and tendency of methyl methacrylate (MMA) released from autopolymerized denture base polymer (self-curing resin) during processing using time-of-flight mass spectrometer (TOF-MS). Self-curing resin was mixed in the container using a ratio of 2 g of powder to 1 g of liquid in accordance with the manufacturer's instructions for 40 s as a specimen. The amount of MMA released from the specimen was continuously monitored and simultaneously recorded every minute by TOF-MS since immediately after mixing. A total of five specimens were monitored. The amount of MMA increased dramatically at 11 min [(45.2 ± 3.5) mg/L] after mixing, and reached the highest level at 13 min [(228.9 ± 22.6) mg/L], then become stable at 23 min [(8.8 ± 2.3) mg/L] after mixing. The releasing tendency of MMA could be analyzed accurately with continuously monitoring during processing. The amount of MMA released from self-curing resin changed rapidly and the processing was complicated and changeful.
Singh, Sunint; Palaskar, Jayant N.; Mittal, Sanjeev
2013-01-01
Background: Conventional heat cure poly methyl methacrylate (PMMA) is the most commonly used denture base resin despite having some short comings. Lengthy polymerization time being one of them and in order to overcome this fact microwave curing method was recommended. Unavailability of specially designed microwavable acrylic resin made it unpopular. Therefore, in this study, conventional heat cure PMMA was polymerized by microwave energy. Aim and Objectives: This study was designed to evaluate the surface porosities in PMMA cured by conventional water bath and microwave energy and compare it with microwavable acrylic resin cured by microwave energy. Materials and Methods: Wax samples were obtained by pouring molten wax into a metal mold of 25 mm × 12 mm × 3 mm dimensions. These samples were divided into three groups namely C, CM, and M. Group C denotes conventional heat cure PMMA cured by water bath method, CM denotes conventional heat cure PMMA cured by microwave energy, M denotes specially designed microwavable acrylic denture base resin cured by microwave energy. After polymerization, each sample was scanned in three pre-marked areas for surface porosities using the optical microscope. As per the literature available, this instrument is being used for the first time to measure the porosity in acrylic resin. It is a reliable method of measuring area of surface pores. Portion of the sample being scanned is displayed on the computer and with the help of software area of each pore was measured and data were analyzed. Results: Conventional heat cure PMMA samples cured by microwave energy showed maximum porosities than the samples cured by conventional water bath method and microwavable acrylic resin cured by microwave energy. Higher percentage of porosities was statistically significant, but well within the range to be clinically acceptable. Conclusion: Within the limitations of this in-vitro study, conventional heat cure PMMA can be cured by microwave energy without compromising on its property such as surface porosity. PMID:24015000
Kaneko, K
1989-09-01
A heating method using micro-waves was utilized to obtain strong thermosetting resin for crown and bridge. The physical and mechanical properties of the thermosetting resin were examined. The resin was cured in a shorter time by the micro-waves heating method than by the conventional heat curing method and the working time was reduced markedly. The base resins of the thermosetting resin for crown and bridge for the micro-waves heating method were 2 PA and diluent 3 G. A compounding volume of 30 wt% for diluent 3 G was considered good the results of compressive strength, bending strength and diametral tensile strength. Grams of 200-230 of the filler compounded to the base resins of 2 PA-3 G system provided optimal compressive strength, bending strength and diametral tensile strength. A filler gram of 230 provided optimal hardness and curing shrinkage rate, the coefficient of thermal expansion became smaller with the increase of the compounding volume of the filler. The trial thermosetting resin for crown and bridge formed by the micro-waves heating method was not inferior to the conventional resin by the heat curing method or the light curing method.
Sm, Mousavinasab; M, Atai; N, Salehi; A, Salehi
2016-12-01
The degree of conversion depends on the material composition, light source properties, distance from light source, light intensity, curing time, and other factors such as shade and translucency. In the present study, we evaluated the effects of different light-curing modes and shades of methacrylate and silorane-based resin composites on the degree of conversion of resin composites (DC). The methacrylate-based (Filtek Z250, 3M, ESPE) and low-shrinkage silorane-based (Filtek P90, 3M, ESPE) resin composites were used in three groups as follows: group 1-Filtek Z250 (shade A3), group 2-Filtek Z250 (shade B2), and group 3-Filtek P90 (shade A3). We used a light-emitting diode (LED) curing unit for photopolymerization. 10 samples were prepared in each group to evaluate the degree of conversion; 5 samples were cured using soft-start curing mode, and the other 5 were cured using standard curing mode. The DC of the resin composites was measured using Fourier Transform Infrared Spectroscopy (FTIR). The data were analyzed using Kruskal Wallis and one-way ANOVA statistical tests. The degree of conversion of silorane-based resin composite was 70 - 75.8% and that of methacrylate-based resin composites was 60.2 - 68.2% (p = 0.009). The degree of conversion of the composite with brighter colour (B2) was statistically more than the darker composite (A3). Higher degree of conversion was achieved applying the standard curing mode. The results of the study showed that the colour and type of the resin composite and also the curing mode influence the degree of conversion of resin composites.
Factors affecting marginal integrity of class II bulk-fill composite resin restorations
Savadi Oskoee, Siavash; Bahari, Mahmoud; Jafari Navimipour, Elmira; Ajami, Amir Ahmad; Ghiasvand, Negar; Savadi Oskoee, Ayda
2017-01-01
Background. Bulk-fill composite resins are a new type of resin-based composite resins, claimed to have the capacity to be placed in thick layers, up to 4 mm. This study was carried out to evaluate factors affecting gap formation in Cl II cavities restored using the bulk-fill technique. Methods. A total of 60 third molars were used in this study. Two Cl II cavities were prepared in each tooth, one on the mesial aspect 1 mm coronal to the CEJ and one on the distal aspect 1 mm apical to the CEJ. The teeth were divided into 4 groups: A: The cavities were restored using the bulk-fill technique with Filtek P90 composite resin and its adhesive system and light-cured with quartz tungsten halogen (QTH) light-curing unit. B: The cavities were restored similar to that in group A but light-cured with an LED light-curing unit. C: The cavities were restored using the bulk-fill technique with X-tra Fil composite resin and Clearfil SE Bond adhesive system and light-cured with a QTH curing unit. D: The cavities were restored similar to that in group C but light-cured with an LED light-curing unit. The gaps were examined under a stereomicroscope at ×60. Data were analyzed with General Linear Model test. In cases of statistical significance (P<0.05), post hoc Bonferroni test was used for further analyses. Results. The light-curing unit type had no effect on gap formation. However, the results were significant in relation to the composite resin type and margin location (P<0.001). The cumulative effects of light-curing unit*gingival margin and light-curing unit*composite resin type were not significant; however, the cumulative effect of composite rein type*gingival margin was significant (P=0.04) Conclusion. X-tra Fil composite exhibited smaller gaps compared with Filtek P90 composite with both light-curing units. Both composite resins exhibited smaller gaps at enamel margins. PMID:28748051
Closed hollow bulb obturator--one-step fabrication: a clinical report.
Buzayan, Muaiyed M; Ariffin, Yusnidar T; Yunus, Norsiah
2013-10-01
A method is described for the fabrication of a closed hollow bulb obturator prosthesis using a hard thermoforming splint material and heat-cured acrylic resin. The technique allowed the thickness of the thermoformed bulb to be optimized for weight reduction, while the autopolymerized seal area was covered in heat-cured acrylic resin, thus eliminating potential leakage and discoloration. This technique permits the obturator prosthesis to be processed to completion from the wax trial denture without additional laboratory investing, flasking, and processing. © 2013 by the American College of Prosthodontists.
Selecting the process variables for filament winding
NASA Technical Reports Server (NTRS)
Calius, E.; Springer, G. S.
1986-01-01
A model is described which can be used to determine the appropriate values of the process variables for filament winding cylinders. The process variables which can be selected by the model include the winding speed, fiber tension, initial resin degree of cure, and the temperatures applied during winding, curing, and post-curing. The effects of these process variables on the properties of the cylinder during and after manufacture are illustrated by a numerical example.
Samimi, Pooran; Alizadeh, Mehdi; Shirban, Farinaz; Davoodi, Amin; Khoroushi, Maryam
2016-01-01
Dual-cured composite resins are similar to self-cured composite resins in some of their clinical applications due to inadequate irradiation, lack of irradiation, or delayed irradiation. Therefore, incompatibility with self-etch adhesives (SEAs) should be taken into account with their use. On the other, the extent of dentin dehydration has a great role in the quality of adhesion of these resin materials to dentin. The aim of this study was to investigate the effect of dentin dehydration and composite resin polymerization mode on bond strength of two SEAs. A total of 120 dentinal specimens were prepared from extracted intact third molars. Half of the samples were dehydrated in ethanol with increasing concentrations. Then Clearfil SE Bond (CSEB) and Prompt L-Pop (PLP) adhesives were applied in the two groups. Cylindrical composite resin specimens were cured using three polymerization modes: (1) Immediate light-curing, (2) delayed light-curing after 20 min, and (3) self-curing. Bond strength was measured using universal testing machine at a crosshead speed of 1 mm/min. Data were analyzed with two-way ANOVA and Duncan post hoc tests. Statistical significance was defined at P < 0.05. There were no significant differences for CSEB subgroups with hydrated and dehydrated dentin samples between the three different curing modes (P > 0.05). PLP showed significant differences between subgroups with the lowest bond strength in hydrated dentin with delayed light-curing and self-cured mode of polymerization. Within the limitations of this study, a delay in composite resin light-curing or using chemically cured composite resin had a deleterious effect on dentin bond strength of single-step SEAs used in the study.
Samimi, Pooran; Alizadeh, Mehdi; Shirban, Farinaz; Davoodi, Amin; Khoroushi, Maryam
2016-01-01
Background: Dual-cured composite resins are similar to self-cured composite resins in some of their clinical applications due to inadequate irradiation, lack of irradiation, or delayed irradiation. Therefore, incompatibility with self-etch adhesives (SEAs) should be taken into account with their use. On the other, the extent of dentin dehydration has a great role in the quality of adhesion of these resin materials to dentin. The aim of this study was to investigate the effect of dentin dehydration and composite resin polymerization mode on bond strength of two SEAs. Materials and Methods: A total of 120 dentinal specimens were prepared from extracted intact third molars. Half of the samples were dehydrated in ethanol with increasing concentrations. Then Clearfil SE Bond (CSEB) and Prompt L-Pop (PLP) adhesives were applied in the two groups. Cylindrical composite resin specimens were cured using three polymerization modes: (1) Immediate light-curing, (2) delayed light-curing after 20 min, and (3) self-curing. Bond strength was measured using universal testing machine at a crosshead speed of 1 mm/min. Data were analyzed with two-way ANOVA and Duncan post hoc tests. Statistical significance was defined at P < 0.05. Results: There were no significant differences for CSEB subgroups with hydrated and dehydrated dentin samples between the three different curing modes (P > 0.05). PLP showed significant differences between subgroups with the lowest bond strength in hydrated dentin with delayed light-curing and self-cured mode of polymerization. Conclusion: Within the limitations of this study, a delay in composite resin light-curing or using chemically cured composite resin had a deleterious effect on dentin bond strength of single-step SEAs used in the study. PMID:27041894
Katsumasa Miyake; Bunichiro Tomita; Chung-Yun Hse; George E. Myers
1989-01-01
A new curing system for urea-formaldehyde (UF) resins was investigated using poly(methacryloyl hydrazide) as the curing reagent. Results were as follows: 1) Gel time and the water-soluble part of cured resins were determined as function of pH and molar ratio [hydrazide group/(free formaldehyde+methylol group)]. It was found that the reaction in this system proceeds for...
Composite Structures and Materials Research at NASA Langley Research Center
NASA Technical Reports Server (NTRS)
Starnes, James H., Jr.; Dexter, H. Benson; Johnston, Norman J.; Ambur, Damodar R.; Cano, roberto J.
2003-01-01
A summary of recent composite structures and materials research at NASA Langley Research Center is presented. Fabrication research to develop low-cost automated robotic fabrication procedures for thermosetting and thermoplastic composite materials, and low-cost liquid molding processes for preformed textile materials is described. Robotic fabrication procedures discussed include ply-by-ply, cure-on-the-fly heated placement head and out-of-autoclave electron-beam cure methods for tow and tape thermosetting and thermoplastic materials. Liquid molding fabrication processes described include Resin Film Infusion (RFI), Resin Transfer Molding (RTM) and Vacuum-Assisted Resin Transfer Molding (VARTM). Results for a full-scale composite wing box are summarized to identify the performance of materials and structures fabricated with these low-cost fabrication methods.
Composite Structures and Materials Research at NASA Langley Research Center
NASA Technical Reports Server (NTRS)
Starnes, James H., Jr.; Dexter, H. Benson; Johnston, Norman J.; Ambur, Damodar R.; Cano, Roberto J.
2001-01-01
A summary of recent composite structures and materials research at NASA Langley Research Center is presented. Fabrication research to develop low-cost automated robotic fabrication procedures for thermosetting and thermoplastic composite materials, and low-cost liquid molding processes for preformed textile materials is described. Robotic fabrication procedures discussed include ply-by-ply, cure-on-the-fly heated placement head and out-of-autoclave electron-beam cure methods for tow and tape thermosetting and thermoplastic materials. Liquid molding fabrication processes described include Resin Film Infusion (RFI) Resin Transfer Molding (RTM) and Vacuum-Assisted Resin Transfer Molding (VARTM). Results for a full-scale composite wing box are summarized to identify the performance of materials and structures fabricated with these low-cost fabrication methods.
NASA Technical Reports Server (NTRS)
Miller, Sandi G.; Roberts, Gary D.; Copa, Christine C.; Bail, Justin L.; Kohlman, Lee W.; Binienda, Wieslaw K.
2011-01-01
The hygrothermal aging characteristics of an epoxy resin were characterized over 1 year, which included 908 temperature and humidity cycles. The epoxy resin quickly showed evidence of aging through color change and increased brittleness. The influence of aging on the material s glass transition temperature (Tg) was evaluated by Differential Scanning Calorimetry (DSC) and Dynamic Mechanical Analysis (DMA). The Tg remained relatively constant throughout the year long cyclic aging profile. The chemical composition was monitored by Fourier Transform Infrared Spectroscopy (FTIR) where evidence of chemical aging and advancement of cure was noted. The tensile strength of the resin was tested as it aged. This property was severely affected by the aging process in the form of reduced ductility and embrittlement. Detailed chemical evaluation suggests many aging mechanisms are taking place during exposure to hygrothermal conditions. This paper details the influence of processes such as: advancement of cure, chemical degradation, and physical aging on the chemical and physical properties of the epoxy resin.
Hoorizad Ganjkar, Maryam; Heshmat, Haleh; Hassan Ahangari, Reza
2017-01-01
Statement of the Problem: Increasing the thickness of the veneering porcelain may affect the polymerization of resin cements. Incomplete polymerization of resin cements can lead to compromised quality of restoration and decrease the longevity of indirect restorations. Purpose: This study sought to assess the effect of IPS Empress porcelain thickness on the degree of conversion of light-cure and dual-cure resin cements using Fourier transform infrared spectroscopy. Materials and Method: In this experimental study, IPS Empress porcelain discs (A2 shade) with 10mm diameter and 0.5, 1 and 1.5 mm thicknesses were fabricated. Choice2 (Bisco, USA) and Nexus3 (Kerr, USA) resin cements were light cured through the three porcelain thicknesses in two groups of 3 samples using a LED light-curing unit (LEDemetron II; Kerr, USA). The control group samples were cured individually with no porcelain disc. The degree of conversion of resin cements was determined using FTIR (Bruker; Equinox55, Germany). The data were analyzed using Dunn’s test. Results: The degree of conversion (in percent) beneath the 0.5, 1.5 and 2 mm thicknesses of IPS Empress was 68.67±0.88, 71.06±0.94 and 72.51±0.41 for Choice2 resin cement and 69.60±2.12, 69.64±1.63 and 69.24±2.12 for Nexus3, respectively. Porcelain thickness and type of resin cement had no significant effect on degree of conversion (p≥ 0.05). Conclusion: It seems that increasing the porcelain thickness by up to 1.5 mm has no adverse effect on degree of conversion of both dual cure and light cure resin cements evaluated in this study. PMID:28280757
Flury, Simon; Lussi, Adrian; Hickel, Reinhard; Ilie, Nicoleta
2014-04-01
The aim of this study was to investigate micromechanical properties of five dual-curing resin cements after different curing modes including light curing through glass ceramic materials. Vickers hardness (VH) and indentation modulus (Y HU) of Panavia F2.0, RelyX Unicem 2 Automix, SpeedCEM, BisCem, and BeautiCem SA were measured after 1 week of storage (37 °C, 100 % humidity). The resin cements were tested following self-curing or light curing with the second-generation light-emitting diode (LED) curing unit Elipar FreeLight 2 in Standard Mode (1,545 mW/cm(2)) or with the third-generation LED curing unit VALO in High Power Mode (1,869 mW/cm(2)) or in XtraPower Mode (3,505 mW/cm(2)). Light curing was performed directly or through glass ceramic discs of 1.5 or 3 mm thickness of IPS Empress CAD or IPS e.max CAD. VH and Y HU were analysed with Kruskal-Wallis tests followed by pairwise Wilcoxon rank sum tests (α = 0.05). RelyX Unicem 2 Automix resulted in the highest VH and Y HU followed by BeautiCem SA, BisCem, SpeedCEM, and finally Panavia F2.0. Self-curing of RelyX Unicem 2 Automix and SpeedCEM lowered VH and Y HU compared to light curing whereas self-curing of Panavia F2.0, BisCem, and BeautiCem SA led to similar or significantly higher VH and Y HU compared to light curing. Generally, direct light curing resulted in similar or lower VH and Y HU compared to light curing through 1.5-mm-thick ceramic discs. Light curing through 3-mm-thick discs of IPS e.max CAD generally reduced VH and Y HU for all resin cements except SpeedCEM, which was the least affected by light curing through ceramic discs. The resin cements responded heterogeneously to changes in curing mode. The applied irradiances and light curing times adequately cured the resin cements even through 1.5-mm-thick ceramic discs. When light curing resin cements through thick glass ceramic restorations, clinicians should consider to prolong the light curing times even with LED curing units providing high irradiances.
Optimal cure cycle design of a resin-fiber composite laminate
NASA Technical Reports Server (NTRS)
Hou, Jean W.; Hou, Tan H.; Sheen, Jeen S.
1987-01-01
Fibers reinforced composites are used in many applications. The composite parts and structures are often manufactured by curing the prepreg or unmolded material. The magnitudes and durations of the cure temperature and the cure pressure applied during the cure process have significant consequences on the performance of the finished product. The goal of this study is to exploit the potential of applying the optimization technique to the cure cycle design. The press molding process of a polyester is used as an example. Various optimization formulations for the cure cycle design are investigated. Recommendations are given for further research in computerizing the cure cycle design.
Processing and Properties of a Phenolic Composite System
NASA Technical Reports Server (NTRS)
Hou, Tan-Hung; Bai, J. M.; Baughman, James M.
2006-01-01
Phenolic resin systems generate water as a reaction by-product via condensation reactions during curing at elevated temperatures. In the fabrication of fiber reinforced phenolic resin matrix composites, volatile management is crucial in producing void-free quality laminates. A commercial vacuum-bag moldable phenolic prepreg system was selected for this study. The traditional single-vacuum-bag (SVB) process was unable to manage the volatiles effectively, resulting in inferior voidy laminates. However, a double vacuum bag (DVB) process was shown to afford superior volatile management and consistently yielded void-free quality parts. The DVB process cure cycle (temperature /pressure profiles) for the selected composite system was designed, with the vacuum pressure application point carefully selected, to avoid excessive resin squeeze-outs and achieve the net shape and target resin content in the final consolidated laminate parts. Laminate consolidation quality was characterized by optical photomicrography for the cross sections and measurements of mechanical properties. A 40% increase in short beam shear strength, 30% greater flexural strength, 10% higher tensile and 18% higher compression strengths were obtained in composite laminates fabricated by the DVB process.
Kimura, H; Yu, P Y; Teraoka, F; Sugita, M
1989-09-01
To develop the visible light-cured FRP denture base, we investigated the physical properties and the warp of FRP plate by using various combinations of matrix resin and reinforcement. From the results of the bending test, hardness test and manipulation processing, the matrix resin of Bis-GMA/UDMA/3 G at 48/48/4 wt% was determined. The sateen weave's glasscloth as the reinforcement of the prepreg was used. The maximum plies included FRP of 0.5 mm, 0.8 and 1.0 mm thickness have the same maximum bending strengths of 45 kgf/mm2, which is about 5 times larger than that of conventional acrylic resin. The warp of these FRP plates were not found.
Oligosilylarylnitrile: The Thermoresistant Thermosetting Resin with High Comprehensive Properties.
Wang, Mingcun; Ning, Yi
2018-04-11
One of the highest thermoresistant thermosetting resins ever studied so far, oligosilylarylnitrile resin, was investigated first in this study. Oligosilylarylnitrile was synthesized by lithium-reduced Wurtz-Fittig condensation reaction, and the prepared viscous resin exhibited moderate rheological behaviors while heated purely or together with 20% polysilazane as a cross-linking agent. The thermal curing temperatures were found by differential scanning calorimetry at 268 °C (pure) and 158 °C (with the polysilazane cross-linking agent), which is comparably close to that of polysilylarylacetylene resin (normally at 220-250 °C) but much lower than those of polyimide and phthalonitrile resins (normally >300 °C), indicating the admirable material processability of oligosilylnitrile. The cured oligosilylarylnitrile resins have extremely high thermal resistance, indicated by the results of thermogravimetric analysis (the mass residue at 800 °C is >90% under N 2 ) and dynamic mechanical analysis (the glass-transition temperature is >420 °C). The mechanical property of the oligosilylarylnitrile-matrixed silica-cloth reinforced laminate is comparably close to those of polyimide and phthalonitrile but much higher than that of polysilylarylacetylene, indicating the enviable thermal and mechanical properties of oligosilylnitrile. Thus, among the high-temperature resins ever studied so far, the oligosilylarylnitrile resin was found to have the almost best comprehensive characteristics of processability and properties.
Wang, Yiru; Liu, Wanshuang; Qiu, Yiping; Wei, Yi
2018-04-27
Imidazole cured epoxy resin systems were evaluated for one-component, fast-curing resins for liquid molding of automotive composite parts according to industry requirements. It was demonstrated that an epoxy resin-1-(cyanoethyl)-2-ethyl-4-methylimidazol(EP-1C2E4MIM) system would cure in a few minutes at 120 °C, while exhibiting acceptable pot life, viscosity profiles, and low water absorption. Moreover, this system yielded high T g parts with mechanical properties similar to the amine-epoxy systems, which are the mainstream two-component epoxy resin systems for automobiles.
Wang, Yiru; Qiu, Yiping; Wei, Yi
2018-01-01
Imidazole cured epoxy resin systems were evaluated for one-component, fast-curing resins for liquid molding of automotive composite parts according to industry requirements. It was demonstrated that an epoxy resin-1-(cyanoethyl)-2-ethyl-4-methylimidazol(EP-1C2E4MIM) system would cure in a few minutes at 120 °C, while exhibiting acceptable pot life, viscosity profiles, and low water absorption. Moreover, this system yielded high Tg parts with mechanical properties similar to the amine-epoxy systems, which are the mainstream two-component epoxy resin systems for automobiles. PMID:29702575
Effect of laminate edge conditions on the formation of microvoids in composite laminates
NASA Astrophysics Data System (ADS)
Anderson, J. P.; Altan, M. C.
2015-05-01
Manufacturing defects such as microvoids are common in thermoset composite components and are known to negatively affect their strength. The resin pressure developed in and the resin flow out from the laminates during cure have been reported to be the primary factors influencing the final void content of a composite component. In this work, the effect of laminate edge conditions during the cure process on the formation of microvoids was experimentally investigated. This was achieved by fabricating eight-ply laminates from TenCate® BT250/7781 prepreg in a hot-press at a constant cure pressure of 170 kPa while limiting the laminate perimeter available for resin flow by 0%, 25%, 50%, 75%, and 100%. The individual plies of these five laminates were conditioned at 99% relative humidity before curing to maximize the moisture present in the lay-up before fabrication. The presence of moisture in the lay-ups was expected to promote void formation and allow the effect of restricting flow at the edges of a laminate to be better identified. The restriction of resin outflow was found to cause the average characteristic void diameter to decrease by 17% and void content to rise by 33%. This phenomenon was identified to be a result of the outflow restriction increasing the number of voids trapped within the laminate and indicates that for laminates cured at low pressures resin outflow is the dominant mechanism for void reduction.
Stress and flow analyses of ultraviolet-curable resin during curing
NASA Astrophysics Data System (ADS)
Umezaki, Eisaku; Okano, Akira; Koyama, Hiroto
2014-06-01
The stress and flow generated in ultraviolet (UV)-curable resin during curing in molds were measured to investigate their relationship. The specimens were molds consisting of glass plates and acrylic bars, and UV-curable liquid resin. The specimens were illuminated from above with UV rays. Photoelastic and visual images were separately obtained at a constant time interval using cameras during curing. To help obtain the visual images, acrylic powder was mixed with the liquid resin. The stress was obtained from the photoelastic images by a digital photoelastic technique with phase stepping, and the flow was obtained from the visual images by a particle-tracking velocimetry technique. Results indicate that the stress generated in the UV-curable resin during curing depends on the degree of contact between the mold and the cured area of the resin, and is hardly related to the flow.
NASA Technical Reports Server (NTRS)
Rheineck, A. E.; Heskin, R. A.; Hill, L. W.
1972-01-01
The solubility and/or swelling of cured epoxy resins was studied using the solubility parameter method. Determination of solubility parameters were found in order to select solvents for solvent-assisted degradation of cured epoxy polymers used in spacecraft. A method for improving recovery of seeded spores is suggested for assay of buried contaminants. Three commercial epoxy resins were cured using four different alkyl amines. For each resin-amine combination, three levels of amine were used, corresponding to 1/3, 2/3, and all of the amine required to react with the oxirane groups of the resin. The solubility parameters of the 36 resulting model compounds were determined in poorly and moderately hydrogen-bonded solvents. No strongly hydrogen-bonded solvents caused dissolution or swelling. The tolerance of cured resins is discussed in terms of polymer structure.
NASA Technical Reports Server (NTRS)
Pearce, E.; Lin, S. C.
1981-01-01
The effects of resin composition, curing conditions fillers, and flame retardant additives on the flammability of diglycidyl ether of bisphenol-A (DGEBA) as measured by the oxygen index is examined. The oxygen index of DGEBA cured with various curing agents was between 0.198 to 0.238. Fillers and flame retardant additives can increase the oxygen index dependent on the material and the amount used. Changes in the basic cured resin properties can be anticipated with the addition of noncompatible additives. High flame resistant epoxy resins with good stability and mechanical properties are investigated.
Effect of bench time polymerization on depth of cure of dental composite resin
NASA Astrophysics Data System (ADS)
Harahap, K.; Yudhit, A.; Sari, F.
2017-07-01
The aim of this research was to investigate the effect of bench time before light cured polymerization on the depth of cure of dental composite resin. Nanofiller composite resin (Filtek Z350 XT,3M, ESPE,China) was used in this study. Sixty samples of nanofiller composite resin were made and divided into control and test groups with bench time for 0, 15, 30, 45, and 60 min. For the test group, composite resins were stored in refrigerator with 4°C temperatures. Meanwhile, for the control groups, the composite resin was stored at room temperature. The samples were prepared using metal mould with size diameter of 6 mm and 4 mm in thickness. Samples were cured for 20 s by using visible blue light curing unit. Part of samples that unpolymerized were removed by using a plastic spatula. The remaining parts of samples were measured by digital caliper and noted as depth of cure (mm). Data were analyzed to one-way ANOVA and LSD tests (p≤0.05). Results showed there was no significance differences between test groups (p=0.5). A 60 minutes bench time group showed the highest depth of cure value among test group, and it was almost similar with control group value. It can be concluded that longer bench time can increase the depth of cure of composite resin.
[Curing mode of universal adhesives affects the bond strength of resin cements to dentin].
Fu, Z R; Tian, F C; Zhang, L; Han, B; Wang, X Y
2017-02-18
To determine the effects of curing mode of one-step and two-step universal adhesives on the micro-tensile bond strength (μTBS) of different dual-cure resin cements to dentin. One-step universal adhesive Single Bond Universal (SBU), and two-step universal adhesive OptiBond Versa (VSA) were chosen as the subjects, one-step self-etching adhesive OptiBond All in One (AIO) and two-step self-etching adhesive Clearfil SE Bond (SEB) were control groups, and two dual-cure resin cements RelyX Ultimate (RLX) and Nexus 3 Universal (NX3) were used in this study. In this study, 80 extracted human molars were selected and the dentin surface was exposed using diamond saw. The teeth were divided into 16 groups according to the adhesives (AIO, SBU, SEB, VSA), cure modes of adhesives (light cure, non-light cure) and resin cements (RLX, NX3). The adhesives were applied on the dentin surface following the instruction and whether light cured or not, then the resin cements were applied on the adhesives with 1 mm thickness and light cured (650 mW/cm(2) for 20 s. A resin was built up (5 mm) on the cements and light cured layer by layer. After water storage for 24 h, the specimens were cut into resin-cement-dentin strips with a cross sectional area of 1 mm×1 mm and the μTBS was measured. Regarding one-step universal adhesive (SBU) light cured, the μTBS with RLX [(35.45±7.04) MPa] or NX3 [(26.84±10.39) MPa] were higher than SBU non-light cured with RLX [(17.93±8.93) MPa)] or NX3 [(10.07±5.89) MPa, P<0.001]. Compared with AIO, light-cured SBU combined with RLX presented higher μTBS than AIO group [(35.45±7.04) MPa vs. (24.86±8.42) MPa, P<0.05]. When SBU was not lighted, the μTBS was lower than AIO [(17.93±8.93) MPa vs. (22.28±7.57) MPa, P<0.05]. For two-step universal adhesive (VSA) and control adhesive (SEB), curing mode did not affect the μTBS when used with either RLX or NX3 (25.98-32.24 MPa, P>0.05). Curing mode of one-step universal adhesive may affect the μTBS between dual-cure resin cements and dentin, while for two-step universal adhesive, the curing mode and the type of resin cements did not influence the μTBS.
Molding cork sheets to complex shapes
NASA Technical Reports Server (NTRS)
Sharpe, M. H.; Simpson, W. G.; Walker, H. M.
1977-01-01
Partially cured cork sheet is easily formed to complex shapes and then final-cured. Temperature and pressure levels required for process depend upon resin system used and final density and strength desired. Sheet can be bonded to surface during final cure, or can be first-formed in mold and bonded to surface in separate step.
Synthesis and properties of a bio-based epoxy resin with high epoxy value and low viscosity.
Ma, Songqi; Liu, Xiaoqing; Fan, Libo; Jiang, Yanhua; Cao, Lijun; Tang, Zhaobin; Zhu, Jin
2014-02-01
A bio-based epoxy resin (denoted TEIA) with high epoxy value (1.16) and low viscosity (0.92 Pa s, 258C) was synthesized from itaconic acid and its chemical structure was confirmed by 1H NMR and 13C NMR spectroscopy. Its curing reaction with poly(propylene glycol) bis(2-aminopropyl ether) (D230) and methyl hexahydrophthalic anhydride (MHHPA) was investigated. For comparison, the commonly used diglycidyl ether of bisphenol A (DGEBA) was also cured with the same curing agents. The results demonstrated that TEIA showed higher curing reactivity towards D230/MHHPA and lower viscosity compared with DGEBA, resulting in the better processability. Owing to its high epoxy value and unique structure, comparable or better glass transition temperature as well as mechanical properties could be obtained for the TEIA-based network relative to the DGEBA-based network. The results indicated that itaconic acid is a promising renewable feedstock for the synthesis of bio-based epoxy resin with high performance.
NASA Astrophysics Data System (ADS)
Zhang, J. X.; Y Ren, Z.; Zheng, G.; Wang, H. F.; Jiang, L.; Fu, Y.; Yang, W. Q.; He, H. H.
2017-12-01
In this work, hydroxylated tung oil (HTO) modified high temperature resistant resin containing boron and benzoxazine was synthesized. HTO and ethylenediamine was used to toughen the boron phenolic resin with specific reaction. The structure of product was studied by Fourier-transform infrared spectroscopy(FTIR), and the heat resistance was tested by Differential Scanning Calorimetry (DSC) and Thermogravimetric Analysis(TGA). The results indicated that the conjugated triene structure of HTO was involved in the crosslinking of the heating curing progress, and in addition, the open-loop polymerization reaction of benzoxazine resin during heating can effectively reduce the curing temperature of the resin and reduce the release of small molecule volatiles, which is advantageous to follow-up processing. DSC data showed that the initial decomposition temperature of the resin is 350-400 °C, the carbon residue rate under 800 °C was 65%. It indicated that the resin has better heat resistance than normal boron phenolic resin. The resin can be used as an excellent ablative material and anti-friction material and has a huge application market in many fields.
Cytotoxicity of Light-Cured Dental Materials according to Different Sample Preparation Methods
Lee, Myung-Jin; Kim, Mi-Joo; Kwon, Jae-Sung; Lee, Sang-Bae; Kim, Kwang-Mahn
2017-01-01
Dental light-cured resins can undergo different degrees of polymerization when applied in vivo. When polymerization is incomplete, toxic monomers may be released into the oral cavity. The present study assessed the cytotoxicity of different materials, using sample preparation methods that mirror clinical conditions. Composite and bonding resins were used and divided into four groups according to sample preparation method: uncured; directly cured samples, which were cured after being placed on solidified agar; post-cured samples were polymerized before being placed on agar; and “removed unreacted layer” samples had their oxygen-inhibition layer removed after polymerization. Cytotoxicity was evaluated using an agar diffusion test, MTT assay, and confocal microscopy. Uncured samples were the most cytotoxic, while removed unreacted layer samples were the least cytotoxic (p < 0.05). In the MTT assay, cell viability increased significantly in every group as the concentration of the extracts decreased (p < 0.05). Extracts from post-cured and removed unreacted layer samples of bonding resin were less toxic than post-cured and removed unreacted layer samples of composite resin. Removal of the oxygen-inhibition layer resulted in the lowest cytotoxicity. Clinicians should remove unreacted monomers on the resin surface immediately after restoring teeth with light-curing resin to improve the restoration biocompatibility. PMID:28772647
Flow monitoring of microwave pre-heated resin in LCM processes
NASA Astrophysics Data System (ADS)
Rubino, F.; Paradiso, V.; Carlone, P.
2017-10-01
Liquid composite molding is manufacturing techniques that involve the injection or infusion of catalyzed liquid resin into a mold to impregnate a dry fiber preform. The challenges of LCM processes are related to the obtaining of a complete wetting of the reinforcement as well as a reduction of the void to obtain a final product with high mechanical properties. The heating of the resin prior the injection into the mold cavity has proven to be useful to improve the LCM processes. The increasing of temperature results in a reduction of resin viscosity and allows the resin to flow more easily through the reinforcement; the cure stage is also improved resulting in a reduction of global process time required. Besides the conventional solutions to heat up the resin based on the thermal conduction, in-line microwave heating is a suitable method to heat dielectric materials providing an even temperature distribution through the resin, thereby avoiding a thermal gradient between the surface and the core of liquid resin, which could result in a premature and uncontrolled cure. In the present work, an in-line microwave system, manually controlled, have been coupled with a VARTM apparatus to heat the resin before the infusion. In addition, parallel-plate dielectric sensors and pressure sensors, embedded into the mold, were employed to track the flow front through the fiber reinforcement in two distinct cases: unheated resin and pre-heated resin. The aim of work was to assess the effectiveness of microwave pre-heating to improve the macro and micro-impregnation of dry preform. The obtained results showed capability of in-line microwave heating to shorten the impregnation of dry fabric and provide a homogeneous wetting of fibers.
Post-irradiation hardening of dual-cured and light-cured resin cements through machinable ceramics.
Yoshida, Keiichi; Atsuta, Mitsuru
2006-10-01
To evaluate the surface hardness (Knoop Hardness Number) of the thin layer in three light-cured and dual-cured resin cements irradiated through or not through 2.0 mm thick machinable ceramics. A piece of adhesive polyethylene tape with a circular hole was positioned on the surface of the ceramic plate to control the cement layer (approximately 50 microm). The cement paste was placed on the ceramic surface within the circle. The ceramic plate with resin cement paste was placed on a clear micro cover glass over a zirconia ceramic block to obtain a flat surface, and the material was polymerized using a visible-light-curing unit. The surface hardness was recorded at a series of time intervals up to 5 days, starting from the end of a light-irradiation period. The hardness steadily increased with post-irradiation time and tended towards a maximum, usually reached after 1 or 2 days. In all cases, the increase in hardness was relatively rapid over the first 30 minutes and continued at a lower rate thereafter. The dual-cured resin cement for each material showed a significantly higher hardness value than the light-cured resin cement irradiated either through or not through ceramics at all post-irradiation times. The resin cements cured through ceramic for each material were significantly less hard compared with those cured not through ceramics at all post-irradiation times.
Wear Resistance of 3D Printing Resin Material Opposing Zirconia and Metal Antagonists.
Park, Ji-Man; Ahn, Jin-Soo; Cha, Hyun-Suk; Lee, Joo-Hee
2018-06-20
3D printing offers many advantages in dental prosthesis manufacturing. This study evaluated the wear resistance of 3D printing resin material compared with milling and conventional resin materials. Sixty substrate specimens were prepared with three types of resin materials: 3D printed resin, milled resin, and self-cured resin. The 3D printed specimens were printed at a build angle of 0° and 100 μm layer thickness by digital light processing 3D printing. Two kinds of abraders were made of zirconia and CoCr alloy. The specimens were loaded at 5 kg for 30,000 chewing cycles with vertical and horizontal movements under thermocycling condition. The 3D printed resin did not show significant difference in the maximal depth loss or the volume loss of wear compared to the milled and the self-cured resins. No significant difference was revealed depending on the abraders in the maximal depth loss or the volume loss of wear. In SEM views, the 3D printed resin showed cracks and separation of inter-layer bonds when opposing the metal abrader. The results suggest that the 3D printing using resin materials provides adequate wear resistance for dental use.
Digital micromirror device (DMD)-based 3D printing of poly(propylene fumarate) scaffolds.
Mott, Eric J; Busso, Mallory; Luo, Xinyi; Dolder, Courtney; Wang, Martha O; Fisher, John P; Dean, David
2016-04-01
Our recent investigations into the 3D printing of poly(propylene fumarate) (PPF), a linear polyester, using a DMD-based system brought us to a resin that used titanium dioxide (TiO2) as an ultraviolet (UV) filter for controlling cure depth. However, this material hindered the 3D printing process due to undesirable lateral or "dark" curing (i.e., in areas not exposed to light from the DMD chip). Well known from its use in sunscreen, another UV filter, oxybenzone, has previously been used in conjunction with TiO2. In this study we hypothesize that combining these two UV filters will result in a synergistic effect that controls cure depth and avoids dark cure. A resin mixture (i.e., polymer, initiator, UV filters) was identified that worked well. The resin was then further characterized through mechanical testing, cure testing, and cytotoxicity testing to investigate its use as a material for bone tissue engineering scaffolds. Results show that the final resin eliminated dark cure as shown through image analysis. Mechanically the new scaffolds proved to be far weaker than those printed from previous resins, with compressive strengths of 7.8 ± 0.5 MPa vs. 36.5 ± 1.6 MPa, respectively. The new scaffolds showed a 90% reduction in elastic modulus and a 74% increase in max strain. These properties may be useful in tissue engineering applications where resorption is required. Initial cytotoxicity evaluation was negative. As hypothesized, the use of TiO2 and oxybenzone showed synergistic effects in the 3D printing of PPF tissue engineering scaffolds. Copyright © 2015 Elsevier B.V. All rights reserved.
Curing of epoxy resins with 1-/di(2-chloroethoxyphosphinyl)methyl/-2,4- and -2,6-diaminobenzene
NASA Technical Reports Server (NTRS)
Mikroyannidis, J. A.; Kourtides, D. A.
1984-01-01
Fire resistant compositions were prepared using 1-di(2-chloroethoxy-phosphinyl)methyl-2,4- and -2,6-diaminobenzene (DCEPD) as a curing agent for typical epoxy resins such as EPON 828 (Shell), XD 7342 (Dow), and My 720 (Ciba Geigy). In addition, compositions of these three epoxy resins with common curing agents such as m-phenylenediamine (MPD) or 4,4'-diaminodiphenylsulphone (DDS) were studied to compare their reactions with those of DCEPD. The reactivity of the three curing agents toward the epoxy resins, measured by differential calorimetry (DSC), was of the order MPD DCEPD DDS. The relatively lower reactivity of DCEPD toward epoxy resins was attributed to electronic effects.
Adhesion at the interface in cured graphite fiber epoxy-amine resin composites
NASA Technical Reports Server (NTRS)
Needles, Howard L.; Alger, Kenneth W.; Okamoto, Robert
1987-01-01
The effect of high temperature curing on the interface between unsized or epoxy-sized graphite fiber tow and epoxy-amine resin was examined by scanning electron microscopy of compression and freeze fractured specimens. Little or no adhesion was found between the unsized graphite fiber tows and the epoxy-amine resin on curing at 165 C for 17 hrs. Epoxy-sized graphite fibers showed a similar lack of adhesion between the fiber tows and the epoxy-amine resin at 3 and 17 hr cures, although good penetration of the resin into the sized fiber tows had occurred. Interfacial bond strengths for the composites could not be effectively measured by compression fracture of specimens.
Curing of epoxy resins with 1-DI(2-chloroethoxyphosphinyl) methyl-2,4 and -2,6-diaminobenzene
NASA Technical Reports Server (NTRS)
Mikroyannidis, J. A.; Kourtides, D. A.
1983-01-01
Fire resistant compositions were prepared using 1-di(2-chloroethoxy-phosphinyl)methyl-2,4- and -2,6-diaminobenzene (DCEPD) as a curing agent for typical epoxy resins such as EPON 828 (Shell), XD 7342 (Dow), and My 720 (Ciba Geigy). In addition, compositions of these three epoxy resins with common curing agents such as m-phenylenediamine (MPD) or 4,4'-diaminodiphenylsulphone (DDS) were studied to compare their reactions with those of DCEPD. The reactivity of the three curing agents toward the epoxy resins, measured by differential calorimetry (DSC), was of the order MPD DCEPD DDS. The relatively lower reactivity of DCEPD toward epoxy resins was attributed to electronic effects.
High-Temperature Graphite/Phenolic Composite
NASA Technical Reports Server (NTRS)
Seal, Ellis C.; Bodepudi, Venu P.; Biggs, Robert W., Jr.; Cranston, John A.
1995-01-01
Graphite-fiber/phenolic-resin composite material retains relatively high strength and modulus of elasticity at temperatures as high as 1,000 degrees F. Costs only 5 to 20 percent as much as refractory materials. Fabrication composite includes curing process in which application of full autoclave pressure delayed until after phenolic resin gels. Curing process allows moisture to escape, so when composite subsequently heated in service, much less expansion of absorbed moisture and much less tendency toward delamination. Developed for nose cone of external fuel tank of Space Shuttle. Other potential aerospace applications for material include leading edges, parts of nozzles, parts of aircraft engines, and heat shields. Terrestrial and aerospace applications include structural firewalls and secondary structures in aircraft, spacecraft, and ships. Modified curing process adapted to composites of phenolic with other fiber reinforcements like glass or quartz. Useful as high-temperature circuit boards and electrical insulators.
Tsujimoto, Akimasa; Barkmeier, Wayne W; Takamizawa, Toshiki; Latta, Mark A; Miyazaki, Masashi
2017-03-31
The purpose of this study was to investigate the depth of cure, flexural properties and volumetric shrinkage of low and high viscosity bulk-fill giomers and resin composites. Depth of cure and flexural properties were determined according to ISO 4049, and volumetric shrinkage was measured using a dilatometer. The depths of cure of giomers were significantly lower than those of resin composites, regardless of photo polymerization times. No difference in flexural strength and modulus was found among either high or low viscosity bulk fill materials. Volumetric shrinkage of low and high viscosity bulk-fill resin composites was significantly less than low and high viscosity giomers. Depth of cure of both low and high viscosity bulk-fill materials is time dependent. Flexural strength and modulus of high viscosity or low viscosity bulk-fill giomer or resin composite materials are not different for their respective category. Resin composites exhibited less polymerization shrinkage than giomers.
Studies on chemoviscosity modeling for thermosetting resins
NASA Technical Reports Server (NTRS)
Bai, J. M.; Hou, T. H.; Tiwari, S. N.
1987-01-01
A new analytical model for simulating chemoviscosity of thermosetting resins has been formulated. The model is developed by modifying the well-established Williams-Landel-Ferry (WLF) theory in polymer rheology for thermoplastic materials. By introducing a relationship between the glass transition temperature Tg(t) and the degree of cure alpha(t) of the resin system under cure, the WLF theory can be modified to account for the factor of reaction time. Temperature dependent functions of the modified WLF theory constants C sub 1 (t) and C sub 2 (t) were determined from the isothermal cure data. Theoretical predictions of the model for the resin under dynamic heating cure cycles were shown to compare favorably with the experimental data. This work represents progress toward establishing a chemoviscosity model which is capable of not only describing viscosity profiles accurately under various cure cycles, but also correlating viscosity data to the changes of physical properties associated with the structural transformation of the thermosetting resin systems during cure.
Chemoviscosity modeling for thermosetting resin systems, part 3
NASA Technical Reports Server (NTRS)
Hou, T. H.; Bai, J. M.
1988-01-01
A new analytical model for simulating chemoviscosity resin has been formulated. The model is developed by modifying the well established Williams-Landel-Ferry (WLF) theory in polymer rheology for thermoplastic materials. By introducing a relationship between the glass transition temperature (T sub g (t)) and the degree of cure alpha(t) of the resin system under cure, the WLF theory can be modified to account for the factor of reaction time. Temperature-dependent functions of the modified WLF theory parameters C sub 1 (T) and C sub 2 (T) were determined from the isothermal cure data. Theoretical predictions of the model for the resin under dynamic heating cure cycles were shown to compare favorably with the experimental data. This work represents a progress toward establishing a chemoviscosity model which is capable of not only describing viscosity profiles accurately under various cure cycles, but also correlating viscosity data to the changes of physical properties associated with the structural transformations of the thermosetting resin systems during cure.
Insufficient cure under the condition of high irradiance and short irradiation time.
Feng, Li; Carvalho, Ricardo; Suh, Byoung I
2009-03-01
To investigate if and why a plasma arc curing (PAC) light tends to undercure methacrylate-based resins or resin composites. Model dimethacrylate resins, commercial dental adhesives, and commercial resin composites were cured using a PAC light and a halogen light with the similar radiant exposures but different combinations of irradiance and irradiation time. The degree of double bond conversion (DC) was measured with FTIR spectroscopy and analyzed as a function of radiant exposure. The PAC light produced a lower DC than the halogen light for the model resin with the lowest viscosity and for three of the four adhesives. With a high irradiance, the PAC light could cure three of the four composites as thoroughly as its halogen counterpart. When the irradiance was reduced, however, three composites yielded a lower DC. Insufficient cure by PAC lights or any curing lights with very high irradiance is likely to happen when too short an irradiation time is used. It is because under higher irradiance, the lifetime of free radicals is shorter.
VARTM Model Development and Verification
NASA Technical Reports Server (NTRS)
Cano, Roberto J. (Technical Monitor); Dowling, Norman E.
2004-01-01
In this investigation, a comprehensive Vacuum Assisted Resin Transfer Molding (VARTM) process simulation model was developed and verified. The model incorporates resin flow through the preform, compaction and relaxation of the preform, and viscosity and cure kinetics of the resin. The computer model can be used to analyze the resin flow details, track the thickness change of the preform, predict the total infiltration time and final fiber volume fraction of the parts, and determine whether the resin could completely infiltrate and uniformly wet out the preform.
Attar, Hanaa El; Elhiny, Omnia; Salem, Ghada; Abdelrahman, Ahmed; Attia, Mazen
2016-12-15
To test the solubility of dual cure resin modified resin cement in a food simulating solution and the shear bond strength compared to conventional Glass ionomer cement. The materials tested were self-adhesive dual cure resin modified cement and Glass Ionomer (GIC). Twenty Teflon moulds were divided into two groups of tens. The first group was injected and packed with the modified resin cement, the second group was packed with GIC. To test the solubility, each mould was weighed before and after being placed in an analytical reagent for 30 days. The solubility was measured as the difference between the initial and final drying mass. To measure the Shear bond strength, 20 freshly extracted wisdom teeth were equally divided into two groups and embedded in self-cure acrylic resin. Four mm sections of stainless steel bands were cemented to the exposed buccal surfaces of teeth under a constant load of 500 g. Shear bond strength was measured using a computer controlled materials testing machine and the load required to deband the samples was recorded in Newtons. GIC showed significantly higher mean weight loss and an insignificant lower Shear bond strength, compared to dual cure resin Cement. It was found that dual cure resin modified cement was less soluble than glass ionomer cement and of comparable bond strength rendering it more useful clinically for orthodontic band cementation.
Multi-Response Optimization of Resin Finishing by Using a Taguchi-Based Grey Relational Analysis
Shafiq, Faizan; Sarwar, Zahid; Jilani, Muhammad Munib; Cai, Yingjie
2018-01-01
In this study, the influence and optimization of the factors of a non-formaldehyde resin finishing process on cotton fabric using a Taguchi-based grey relational analysis were experimentally investigated. An L27 orthogonal array was selected for five parameters and three levels by applying Taguchi’s design of experiments. The Taguchi technique was coupled with a grey relational analysis to obtain a grey relational grade for evaluating multiple responses, i.e., crease recovery angle (CRA), tearing strength (TE), and whiteness index (WI). The optimum parameters (values) for resin finishing were the resin concentration (80 g·L−1), the polyethylene softener (40 g·L−1), the catalyst (25 g·L−1), the curing temperature (140 °C), and the curing time (2 min). The goodness-of-fit of the data was validated by an analysis of variance (ANOVA). The optimized sample was characterized by Fourier-transform infrared (FTIR) spectroscopy, thermogravimetric analysis (TGA), and scanning electron microscope (SEM) to better understand the structural details of the resin finishing process. The results showed an improved thermal stability and confirmed the presence of well deposited of resin on the optimized fabric surface. PMID:29543724
Rapid Prototyping of Composite Structures
NASA Technical Reports Server (NTRS)
Colton, Jonathan S.
1998-01-01
This progress report for the project Rapid Production of Composite Structures covers the period from July 14, 1997 to June 30, 1998. It will present a short overview of the project, followed by the results to date and plans for the future. The goal of this research is to provide a minimum 100x reduction in the time required to produce arbitrary, laminated products without the need for a separate mold or an autoclave. It will accomplish this by developing the science underlying the rapid production of composite structures, specifically those of carbon fiber-epoxy materials. This scientific understanding will be reduced to practice in a demonstration device that will produce a part on the order of 12" by 12" by 6". Work in the past year has focussed on developing an understanding of the materials issues and of the machine design issues. Our initial goal was to use UV cureable resins to accomplish full cure on the machine. Therefore, we have centered our materials work around whether or not UV cureable resins will work. Currently, the answer seems to be that they will not work, because UV light cannot penetrate the carbon fibers, and because no "shadow" curing seems to occur. As a result, non-UV cureable resins are being investigated. This has resulted in a change in the machine design focus. We are now looking into a "dip and place" machine design, whereby a prepreg layer would have one side coated with a curing agent, and then would be placed onto the previous layer. This would lead to cure at the interface, but not to the top of the layer. The formulation of the resins to accomplish this task at room or slightly elevated temperatures is being investigated, as is the machine design needed to apply the curing agent and then cure or partially cure the part. A final, out-of-autoclave, post-cure may be needed with this strategy, as final cure on the machine may not be possible, as it was for the initial UV cure strategy. The remainder of this report details the progress in the materials and machine design areas. Materials Development The material system must be designed to fulfill the following requirements: to reduce the time and labor requirements of typical cure cycles; to reduce the thermal stresses developed during conventional heat curing; and to develop a structure that the build sequence requires. In order to accomplish these goals, there have been parallel tracks of investigation. One area has tested photopolymerizable (ultraviolet (UV) curable) materials and combinations of these materials with standard heat curing resins. The second area has investigated resins that cure rapidly at room or low heat temperatures. The main goal of these investigations has been to identify a system that will rapidly set or cure at room temperature during a tape lay-up process and hold its structure during a post-cure cycle.
High performance mixed bisimide resins and composites based thereon
NASA Technical Reports Server (NTRS)
Parker, J. A.; ations.
1986-01-01
Mixtures of bismaleimide/biscitraconirnide resins produces materials which have better handling, processing or mechanical and thermal properties, particularly in graphite composites, than materials made with the individual resins. The mechanical strength of cured graphite composites prepared from a 1:1 copolymer of such bisimide resins is excellent at both ambient and elevated temperatures. The copolymer mixture provides improved composites which are lighter than metals and replace metals in many aerospace applications.
Asal, S A; Al-AlShiekh, H M
2017-12-01
Although light-activated resins (Eclipse) have been reported to possess superior physical and mechanical properties compared with the heat-cured acrylic resins (Lucitone-199), a few studies have compared overdentures with a locator attachment constructed from heat-cured acrylic resins with those constructed from light-activated resins. This clinical study was designed to compare the performance of a mandibular implant-supported overdenture constructed from a heat-cured acrylic resin (Lucitone-199) with that of an overdenture constructed from a light-activated resin (Eclipse). Ten participants received two identical mandibular implant-retained overdentures (Lucitone-199 and Eclipse) opposing one maxillary denture in a random order. Each mandibular overdenture was delivered and worn for 6 months, and two weeks of rest was advised between wears to minimize any carryover effects. Three questionnaires were devised. The first questionnaire (patient evaluation) focused on evaluating different aspects of the denture and overall satisfaction. The second questionnaire (professional dentist evaluation) was based on a clinical evaluation of soft tissues, complications, and the applied technique. The third questionnaire (technician evaluation) involved ranking the different manufacturing steps of the denture and overall preferences. The obtained data was statistically analyzed using an independent sample t-test and the Wilcoxon rank-sum test. The clinician and technician preferred the Eclipse dentures because of their technical aspects, whereas the patients preferred the Lucitone-199 dentures for their aesthetic properties. Implant-supported overdentures constructed from a heat-cured acrylic resin showed superior aesthetics and had a better odor compared with those constructed from a light-cured resin.
Significance of wood extractives for wood bonding.
Roffael, Edmone
2016-02-01
Wood contains primary extractives, which are present in all woods, and secondary extractives, which are confined in certain wood species. Extractives in wood play a major role in wood-bonding processes, as they can contribute to or determine the bonding relevant properties of wood such as acidity and wettability. Therefore, extractives play an immanent role in bonding of wood chips and wood fibres with common synthetic adhesives such as urea-formaldehyde-resins (UF-resins) and phenol-formaldehyde-resins (PF-resins). Extractives of high acidity accelerate the curing of acid curing UF-resins and decelerate bonding with alkaline hardening PF-resins. Water-soluble extractives like free sugars are detrimental for bonding of wood with cement. Polyphenolic extractives (tannins) can be used as a binder in the wood-based industry. Additionally, extractives in wood can react with formaldehyde and reduce the formaldehyde emission of wood-based panels. Moreover, some wood extractives are volatile organic compounds (VOC) and insofar also relevant to the emission of VOC from wood and wood-based panels.
Composite Pressure Vessel Including Crack Arresting Barrier
NASA Technical Reports Server (NTRS)
DeLay, Thomas K. (Inventor)
2013-01-01
A pressure vessel includes a ported fitting having an annular flange formed on an end thereof and a tank that envelopes the annular flange. A crack arresting barrier is bonded to and forming a lining of the tank within the outer surface thereof. The crack arresting barrier includes a cured resin having a post-curing ductility rating of at least approximately 60% through the cured resin, and further includes randomly-oriented fibers positioned in and throughout the cured resin.
Facile fabrication of superhydrophobic films with fractal structures using epoxy resin microspheres
NASA Astrophysics Data System (ADS)
Quan, Yun-Yun; Zhang, Li-Zhi
2014-02-01
A simple method has been developed to fabricate superhydrophobic surfaces with fractal structures with epoxy resin microspheres (ERMs). The ERMs is produced by phase separation in an epoxy-amine curing system with a silica sol (SS) dispersant. The transparent epoxy solution becomes cloudy and turns into epoxy suspension (ES) in this process. The fractal structure (two tier structure) generated by synthetic epoxy resin microspheres (ERMs) and deposited nanoincrutations on the surfaces of these ERMs, which have been observed by scanning electron microscope (SEM). The curing time of ES is an important condition to obtain films with good comprehensive performances. Superhydrophobic films can be prepared by adding extra SS into ES with a curing time longer than 5 h. The optimal curing time is 10 h to fabricate a film with good mechanical stability and high superhydrophobicity. In addition, a surface with anti-wetting property of impacting microdroplets can be fabricated by prolonging the curing time of ES to 24 h. The gradually decreased hydrophilic groups resulted from a longer curing time enable the surface to have smaller surface adhesions to water droplets, which is the main reason to keep its superhydrophobicity under impacting conditions. The coated surface is highly hydrophobic and the impacting water droplets are bounced off from the surface.
DE SOUZA, Grace; BRAGA, Roberto Ruggiero; CESAR, Paulo Francisco; LOPES, Guilherme Carpena
2015-01-01
Resin-based cements have been frequently employed in clinical practice to lute indirect restorations. However, there are numerous factors that may compromise the clinical performance of those cements. The aim of this literature review is to present and discuss some of the clinical factors that may affect the performance of current resin-based luting systems. Resin cements may have three different curing mechanisms: chemical curing, photo curing or a combination of both. Chemically cured systems are recommended to be used under opaque or thick restorations, due to the reduced access of the light. Photo-cured cements are mainly indicated for translucent veneers, due to the possibility of light transmission through the restoration. Dual-cured are more versatile systems and, theoretically, can be used in either situation, since the presence of both curing mechanisms might guarantee a high degree of conversion (DC) under every condition. However, it has been demonstrated that clinical procedures and characteristics of the materials may have many different implications in the DC of currently available resin cements, affecting their mechanical properties, bond strength to the substrate and the esthetic results of the restoration. Factors such as curing mechanism, choice of adhesive system, indirect restorative material and light-curing device may affect the degree of conversion of the cement and, therefore, have an effect on the clinical performance of resin-based cements. Specific measures are to be taken to ensure a higher DC of the luting system to be used. PMID:26398507
[Surface characteristics of the acrylic resins according to the polishing methods].
Vitalariu, Anca Mihaela; Lazăr, Lenuţa; Buruiană, Tinca; Diaconu, Diana; Tatarciuc, Monica Silvia
2011-01-01
The objective of this study was to evaluate the effect of the polishing technique and glazing on the porosity of the dental resins. The studied resins were: Castapress/Vertex, Prothyl Hot/Zermack, Rapid Simplified/Vertex, Duracryl Plus/Spofa Dental, Vertex-Soft/Vertex, Superacryl Plus/Spofa Dental. Thirty specimens, five for every resin, of 50/25/2 cm in size were done. One surface of each sample was polished with extrahard tungsten carbide burs, the other surface being polished with extrahard extrafine and diamond burs. The final polishing was done using a conventional method: pumice, water and lathe bristle brush for 90 seconds, 1500 rpm and soft leather polishing wheel for 90 seconds, 3000 rpm. Twenty surfaces were glazed after polishing with Glaze/Bosworth. Vertex Soft specimens were not polished because this is a resilient material. Surface porosity of the acrylic resin specimens was measured by optical microscopy. The lowest porosity was obtained by conventional polishing combined with glazing techniques. No differences between glazed and non/glazed self-curing resin specimens were noticed, but there were differences between self-curing and heat-curing resins. Conventional lathe polishing method is an effective and reliable technique for polishing dental resins. Specimens of self-curing resin had a higher porosity than heat curing resin following the same surface treatment. Higher surface smoothness was obtained by conventional lathe polishing completed by glazing.
NASA Astrophysics Data System (ADS)
Kim, Yun Hae; Han, Joong Won; Kim, Don Won; Choi, Byung Keun; Murakami, R.
Delamination can be observed in the sound areas during and/or after a couple times exposure to the elevated curing temperature due to the repeated repair condition. This study was conducted for checking the degree of degradation of properties of the cured parts and delamination between skin prepreg and honeycomb core. Specimens with glass honeycomb sandwich construction and glass/epoxy prepreg were prepared. The specimens were cured 1 to 5 times at 260°F in an autoclave and each additionally exposed 50, 100 and 150 hours in the 260°F oven. Each specimen was tested for tensile strength, compressive strength, flatwise tensile strength and interlaminar shear strength. To monitor the characteristics of the resin itself, the cured resin was tested using DMA and DSC. As a results, the decrease of Tg value were observed in the specific specimen which is exposed over 50 hrs at 260°F. This means the change or degradative of resin properties is also related to the decrease of flatwise tensile properties. Accordingly, minimal exposure on the curing temperature is recommended for parts in order to prevent the delation and maintain the better condition.
Imide modified epoxy matrix resins
NASA Technical Reports Server (NTRS)
Scola, D. A.; Pater, R. H.
1981-01-01
High char yield epoxy using novel bisimide amines (BIA's) as curing agents with a state of the art epoxy resin was developed. Stoichiometric quantities of the epoxy resin and the BIA's were studied to determine the cure cycle required for preparation of resin specimens. The bisimide cured epoxies were designated IME's (imide modified epoxy). The physical, thermal and mechanical properties of these novel resins were determined. The levels of moisture absorption exhibited by the bisimide amine cured expoxies (IME's) were considerably lower than the state of the art epoxies. The strain-to-failure of the control resin system was improved 25% by replacement of DDS with 6F-DDS. Each BIA containing resin exhibited twice the char yield of the control resin MY 720/DDS. Graphite fiber reinforced control (C) and IME resins were fabricated and characterized. Two of the composite systems showed superior properties compared to the other Celion 6000/IME composite systems and state of the art graphite epoxy systems. The two systems exhibited excellent wet shear and flexural strengths and moduli at 300 and 350 F.
Rajagopal, Praveen; Chitre, Vidya; Aras, Meena A
2012-01-01
Traditionally, inlay casting waxes have been used to fabricate patterns for castings. Newer resin pattern materials offer greater rigidity and strength, allowing easier laboratory and intraoral adjustment without the fear of pattern damage. They also claim to possess a greater dimensional stability when compared to inlay wax. This study attempted to determine and compare the marginal accuracy of patterns fabricated from an inlay casting wax, an autopolymerized pattern resin and a light polymerized pattern resin on storage off the die for varying time intervals. Ten patterns each were fabricated from an inlay casting wax (GC Corp., Tokyo, Japan), an autopolymerized resin pattern material (Pattern resin, GC Corp, Tokyo, Japan) and a light-cured resin pattern material (Palavit GLC, Hereaus Kulzer GmbH, Germany). The completed patterns were stored off the die at room temperature. Marginal gaps were evaluated by reseating the patterns on their respective dies and observing it under a stereomicroscope at 1, 12, and 24 h intervals after pattern fabrication. The results revealed that the inlay wax showed a significantly greater marginal discrepancy at the 12 and 24 h intervals. The autopolymerized resin showed an initial (at 1 h) marginal discrepancy slightly greater than inlay wax, but showed a significantly less marginal gap (as compared to inlay wax) at the other two time intervals. The light-cured resin proved to be significantly more dimensionally stable, and showed minimal change during the storage period. The resin pattern materials studied, undergo a significantly less dimensional change than the inlay waxes on prolonged storage. They would possibly be a better alternative to inlay wax in situations requiring high precision or when delayed investment (more than 1 h) of patterns can be expected.
Foam, Foam-resin composite and method of making a foam-resin composite
NASA Technical Reports Server (NTRS)
MacArthur, Doug E. (Inventor); Cranston, John A. (Inventor)
1995-01-01
This invention relates to a foam, a foam-resin composite and a method of making foam-resin composites. The foam set forth in this invention comprises a urethane modified polyisocyanurate derived from an aromatic amino polyol and a polyether polyol. In addition to the polyisocyanurate foam, the composite of this invention further contains a resin layer, wherein the resin may be epoxy, bismaleimide, or phenolic resin. Such resins generally require cure or post-cure temperatures of at least 350.degree. F.
Development of LaRC 160/NR150B2 polyimide graphite hybrid composites. [for shuttle applications
NASA Technical Reports Server (NTRS)
Maximovich, M. G.; Bergren, O.; Lockerby, S.
1980-01-01
A method for co-curing NR150B2 and LaRC 160 prepregs into hybrid composites was developed. The processing characteristics and the properties of the hybrid composites were compared with those of laminates fabricated from the individual component prepregs. Resin forms were selected and optimized and a new NR150 formulation was investigated. The new formulation greatly facilitated the processing and the performance of this system. Quality control techniques were evaluated and developed, high quality laminates were fabricated from both individual resin systems, and hybrid laminates were successfully co-cured. Optimum hybrid forms were investigated and several novel approaches were explored. An optimum hybrid system was developed that utilizes a LaRC curing schedule but shows no degradation of mechanical properties after aging 500 hr in air at 260 C.
Heat stability of cured urea-formaldehyde resins by measuring formaldehyde emission
Shin-ichiro Tohmura; Chung-Yun Hse; Mitsuo Higuchi
1999-01-01
A test method for measuring formaldehyde from urea-formaldehyde (UF) resins at high temperaÂtures was developed and used to assess the influence of the reaction pH at synthesis on the formaldehyde emission during cure and heat stability of the cured resins without water. Additionally, 13C-CP/MAS solid-state nuclear magnetic resonance (NMR)...
Foxton, R M; Nakajima, M; Tagami, J; Miura, H
2005-02-01
The regional tensile bond strengths of two dual-cure composite resin core materials to root canal dentine using either a one or two-step self-etching adhesive were evaluated. Extracted premolar teeth were decoronated and their root canals prepared to a depth of 8 mm and a width of 1.4 mm. In one group, a one-step self-etching adhesive (Unifil Self-etching Bond) was applied to the walls of the post-space and light-cured for 10 s. After which, the post-spaces were filled with the a dual-cure composite resin (Unifil Core) and then half the specimens were light-cured for 60 s and the other half placed in darkness for 30 min. In the second group, a self-etching primer (ED Primer II) was applied for 30 s, followed by an adhesive resin (Clearfil Photo Bond), which was light-cured for 10 s. The post-spaces were filled with a dual-cure composite resin (DC Core) and then half the specimens were light-cured for 60 s and the other half placed in darkness for 30 min. Chemical-cure composite resin was placed on the outer surfaces of all the roots, which were then stored in water for 24 h. They were serially sliced perpendicular to the bonded interface into 8, 0.6 mm-thick slabs, and then transversely sectioned into beams, approximately 8 x 0.6 x 0.6 mm, for the microtensile bond strength test (muTBS). Data were divided into two (coronal/apical half of post-space) and analysed using three-way anova and Scheffe's test (P < 0.05). Failure modes were observed under an scanning electron microscope (SEM) and statistically analysed. Specimens for observation of the bonded interfaces were prepared in a similar manner as for bond strength testing, cut in half and embedded in epoxy resin. They were then polished to a high gloss, gold sputter coated, and after argon ion etching, observed under an SEM. For both dual-cure composite resins and curing strategies, there were no significant differences in muTBS between the coronal and apical regions (P > 0.05). In addition, both dual-cure composite resins exhibited no significant differences in muTBS irrespective of whether polymerization was chemically or photoinitiated (P > 0.05). Both dual-cure composite resins exhibited good bonding to root canal dentin, which was not dependent upon region or mode of polymerization.
Dielectric cure monitoring: Preliminary studies
NASA Technical Reports Server (NTRS)
Goldberg, B. E.; Semmel, M. L.
1984-01-01
Preliminary studies have been conducted on two types of dielectric cure monitoring systems employing both epoxy resins and phenolic composites. An Audrey System was used for 23 cure monitoring runs with very limited success. Nine complete cure monitoring runs have been investigated using a Micromet System. Two additional measurements were performed to investigate the Micromet's sensitivity to water absorption in a post-cure carbon-phenolic material. While further work is needed to determine data significance, the Micromet system appears to show promise as a feedback control device during processing.
Munikamaiah, Ranganath L; Jain, Saket K; Pal, Kapil S; Gaikwad, Ajay
2018-03-01
Silver colloidal nanoparticles have been incorporated into acrylic resins to induce antimicrobial properties. However, as additives, they can influence the mechanical properties of the final product. Mechanical properties are also dependent on different curing cycles. The aim of this study was to evaluate flexural strength of a denture base resin incorporated with different concentrations of silver colloidal nanoparticles subjected to two different curing cycles. Lucitone 199 denture base resin was used into which silver colloidal nanoparticles were incorporated at 0.5 and 5% by polymer mass. Specimens devoid of nanoparticles were used as controls. A total of 60 specimens were fabricated and divided into two groups. Each group was divided into three subgroups consisting of 10 specimens each. The specimens were fabricated according to American Dental Association (ADA) specification No. 12 and tested for flexural strength using universal testing machine. Silver colloidal nanoparticle incorporation at 0.5% concentration increased the mean flexural strength in both curing cycles by 7.5 and 4.4%, respectively, when compared with the control group. The study suggested that the mean flexural strength value of 0.5% silver colloidal nanoparticles in denture base resin was above the value of the control group both in short and long curing cycles, which makes it clinically suitable as a denture base material. However, at 5% concentration, the statistically significant amount of decrease in flexural strength compared with the value of control group both in short and long curing cycles gives it a questionable prognosis. The specimens incorporated with the antimicrobial agent 0.5% silver colloidal nanoparticles and processed by long curing cycles showed significant increase in its flexural strength compared with the control group, which makes it clinically suitable as a denture base material.
Kanie, Takahito; Arikawa, Hiroyuki; Fujii, Koichi; Ban, Seiji
2004-09-01
The purpose of this study was to investigate the flexural properties of denture base resin reinforced using glass fiber cloth and a urethane oligomer. The five types of oligomer used in this study were S5, S9, S3, U4, and U6, which have varying functional groups and viscosities. The flexural properties of S9 with glass fiber cloth could not be measured because S9 is elastic. In the heat-cured resin reinforced with S9, the reinforcement peeled away from the resin. In the self- and light-cured resins reinforced with S9, the flexural properties increased significantly. When reinforced with the other four oligomers (S5, S3, U4, and U6), the flexural strength and flexural modulus of the self-, heat-, and light-cured resins increased significantly (p<0.01).
Applications of Blue Light-curing Acrylic Resin to Forensic Sample Preparation and Microtomy.
Groves, Ethan; Palenik, Christopher S
2016-03-01
This study discusses the results of an evaluation of a one-part blue light-curing acrylic resin for embedding trace evidence prior to the preparation of thin sections with a microtome. Through a comparison to several epoxy resins, the physical properties relevant to both trace evidence examination and analytical microscopy in general, including as viscosity, clarity, color, hardness, and cure speed, were explored. Finally, thin sections from paint samples embedded in this acrylic resin were evaluated to determine if, through smearing or impregnation, the resin contributed to the infrared spectra. The results of this study show that blue light-curing acrylic resins provide the desired properties of an embedding medium, generate high-quality thin sections, and can significantly simplify the preparation of paint chips, fibers and a multitude of other types of microscopic samples in the forensic trace evidence laboratory. © 2015 American Academy of Forensic Sciences.
Effect of substituted phenylnadimides on processing and properties of PMR polyimide composites
NASA Technical Reports Server (NTRS)
Alston, W. B.; Lauver, R. W.
1985-01-01
Three nitrophenylnadimide cure initiators and two phenylnadimides (without nitros) were evaluated as additives to PMR-15 resins and Celion 6000 graphite fiber composites. The results of a resin screening study eliminated all of the additives except 3-nitrophenylnadimide (NO2PN) for use as a low temperature curing additive for PMR-15. Thus, NO2PN and the two control additives were investigated in PMR-15 formulations from which Celion 6000 graphite fiber/PMR-15 composites were processed both with low temperature (274 C) and normal (316 C) cure cycles. Comparisons of the two processing cycles, the resultant glass transition temperatures (Tg), the ambient, 274 and 316 C composite mechanical properties determined before and after 316 C postcure, the 316 C thermo-oxidative weight losses and the retention of 316 C composite mechanical properties are presented. Empirical correlations of the type and amount of nadimide additives with processing parameters, Tg, composite mechanical properties, composite thermo-oxidative stability and long term retention of 316 C composite mechanical properties are also presented.
NASA Astrophysics Data System (ADS)
LMP, Campos; Boaro, LC; LKG, Santos; Parra, DF; Lugão, AB
2015-10-01
Dental restorative composites are activated by visible light and the polymerization process, known as direct technique, is initiated by absorbing light in a specific wavelength range (450-500 nm). However this technique presented some disadvantages. If light is not inserted correctly, layers uncured can cause countless damage to restoration, especially with regard to mechanical properties. A clinical alternative used to reduce the shortcomings of direct application is the use of composite resins for indirect application. These composites are adaptations of resins prepared for direct use, with differences mainly in the healing process. Besides the traditional photoactivation, indirect application composites may be submitted to particular curing conditions, such as a slow curing rate, heating, vacuum, and inert-gas pressure leading to an oxygen-free environment. However few studies have been conducted on the process of post-curing by ionizing radiation at low doses. On this sense the purpose of this study was to evaluate possible interactions of ionizing radiation in the post-curing process of the experimental composites based on BisGMA/TEGDMA filled with silica Aerosil OX-50 silanized. Characterization of the experimental composites was performed by thermogravimetry analysis, infrared spectroscopy, elastic modulus and flexural strength. Statistical analysis of results was calculated by one-way ANOVA/Tukey's test. Cross-linking of the polymeric matrix caused by ionizing radiation, influenced the thermal stability of irradiated specimens. FTIR analysis showed that the ionizing radiation induced a post-cure reaction in the specimens. The irradiation dose influenced directly the mechanical properties that showed a strong positive correlation between flexural strength and irradiation and between modulus strength and irradiation.
Attar, Hanaa El; Elhiny, Omnia; Salem, Ghada; Abdelrahman, Ahmed; Attia, Mazen
2016-01-01
AIM: To test the solubility of dual cure resin modified resin cement in a food simulating solution and the shear bond strength compared to conventional Glass ionomer cement. MATERIALS AND METHOD: The materials tested were self-adhesive dual cure resin modified cement and Glass Ionomer (GIC). Twenty Teflon moulds were divided into two groups of tens. The first group was injected and packed with the modified resin cement, the second group was packed with GIC. To test the solubility, each mould was weighed before and after being placed in an analytical reagent for 30 days. The solubility was measured as the difference between the initial and final drying mass. To measure the Shear bond strength, 20 freshly extracted wisdom teeth were equally divided into two groups and embedded in self-cure acrylic resin. Four mm sections of stainless steel bands were cemented to the exposed buccal surfaces of teeth under a constant load of 500 g. Shear bond strength was measured using a computer controlled materials testing machine and the load required to deband the samples was recorded in Newtons. RESULTS: GIC showed significantly higher mean weight loss and an insignificant lower Shear bond strength, compared to dual cure resin Cement. CONCLUSION: It was found that dual cure resin modified cement was less soluble than glass ionomer cement and of comparable bond strength rendering it more useful clinically for orthodontic band cementation. PMID:28028417
Distance and protective barrier effects on the composite resin degree of conversion
Coutinho, Margareth; Trevizam, Natália Carvalho; Takayassu, Renata Nakase; Leme, Ariene Arcas; Soares, Giulliana Panfiglio
2013-01-01
Context: The food wrap films are used to cover the tip of curing light units in order to avoid contamination and prevent damage to the light guide. However, their effects on resin polymerization are not fully known. Aims: We investigated the effects on restoration efficiency of a food wrap protective barrier used on the tip of curing light units. Materials and Methods: For each treatment, five replications were performed, a total of 60 bovine incisor. The degree of conversion (%DC) of restorations with the composite resin Opallis EA2 was evaluated using 3 curing light devices (Optilux 501, Optilight and Ultra LED) and 2 curing distances (0 and 5 mm). The composite resin was tested for restoration of cavities in bovine crowns. %DC values were measured by the Fourier transform infrared spectroscopy-attenuated total reflectance technique. Statistical Analysis Used: The data were analyzed using 3-way ANOVA and Tukey's test. Results: Use of the protective film lowered %DC (F = 4.13; P = 0.05), and the effects of curing distance were associated to the curing light device (F = 3.61; P = 0.03). Conclusions: The distance from the light curing tip and use of a translucent protective barrier on the light-cure device can both impair composite resin %DC. PMID:24015001
Rubber-Modified Epoxies. I. Cure, Transitions, and Morphology.
1984-10-01
thermosetting systems has been developed. An aromatic tetrafunctional diamine-cured diglycidyl ether of bis- phenol A epoxy resin [maximum glass transition...systems has been developed. An aromatic tetrafunctional diamine-cured digly- cidyl ether of bisphenol A epoxy resin [maximum glass transition...epoxy resins are brittle materials. The crack resistance can be improved by the addition of reactive liquid rubber to uncured neat epoxy systems (1-3
Measurements of volatile compound contents in resins using a moisture analyzer.
Hashimoto, Masanori; Nagano, Futami; Endo, Kazuhiko; Ohno, Hiroki
2010-02-01
The contents of volatile adhesive compounds, such as water, solvents, and residual unpolymerized monomers, affect the integrity and durability of adhesive bonding. However, there is no method available that can be used to rapidly assess the residual solvent or water contents of adhesive resins. This study examined the effectiveness of a digital moisture analyzer to measure the volatile compound contents of resins. Five self-etching adhesives and seven experimental light-cured resins prepared with different contents (0, 10, and 20% by weight) of water or solvents (acetone and ethanol) were examined in this study. The resins were prepared using different methods (with and without air blast or light-curing) to simulate the clinical conditions of adhesive application. Resin weight changes (% of weight loss) were determined as the residual volatile compound contents, using the moisture analyzer. After the measurements, the resin films were examined using a scanning electron microscope. The weight changes of the resins were found to depend on the amount of water or solvents evaporating from the resin. Water and solvents were evaporated by air blast or light-curing, but some of the water and solvents remained in the cured resin. The moisture analyzer is easy to operate and is a useful instrument for using to measure the residual volatile compound contents of adhesive resin.
NASA Astrophysics Data System (ADS)
Ma, Qing; Zhao, Zijian; Yi, Songlin; Wang, Tianlong
In this study, Chinese Fir was impregnated with unsaturated polyester resin to enhance its properties. Samples 20 mm × 20 mm × 20 mm in size were split into different sections with epoxy resin and tinfoil and subjected to an impregnation experiment under various parameters. Vacuum degree was -0.04 MPa, -0.06 MPa or -0.08 MPa and vacuum duration was 15 min, 30 min, or 45 min. The results indicated that impregnation weight percent gain is linearly dependent on curing weight percent gain. Vacuum duration appears to have less influence on the curing weight percent gain than vacuum degree, and impregnation was most successful at the transverse section compared to other sections. The optimal impregnation parameters were 30 min modification under -0.08 MPa vacuum followed by 120 min at atmospheric pressure for samples 200 mm × 100 mm × 20 mm in size. Uneven distribution of weight percent gain and cracking during the curing process suggested that 30 min post-processing at -0.09 MPa vacuum was the most effective way to complete the impregnation process. The sample's bending strength and modulus of elasticity increased after impregnation treatment. Bending strength after impregnation without post-processing reached 112.85%, but reached 71.65% with vacuum-processing; modulus of elasticity improved 67.13% and 58.28% without and with post-processing, respectively.
Influence of curing protocol and ceramic composition on the degree of conversion of resin cement.
Lanza, Marcos Daniel Septimio; Andreeta, Marcello Rubens Barsi; Pegoraro, Thiago Amadei; Pegoraro, Luiz Fernando; Carvalho, Ricardo Marins De
2017-01-01
Due to increasing of aesthetic demand, ceramic crowns are widely used in different situations. However, to obtain long-term prognosis of restorations, a good conversion of resin cement is necessary. To evaluate the degree of conversion (DC) of one light-cure and two dual-cure resin cements under a simulated clinical cementation of ceramic crowns. Prepared teeth were randomly split according to the ceramic's material, resin cement and curing protocol. The crowns were cemented as per manufacturer's directions and photoactivated either from occlusal suface only for 60 s; or from the buccal, occlusal and lingual surfaces, with an exposure time of 20 s on each aspect. After cementation, the specimens were stored in deionized water at 37°C for 7 days. Specimens were transversally sectioned from occlusal to cervical surfaces and the DC was determined along the cement line with three measurements taken and averaged from the buccal, lingual and approximal aspects using micro-Raman spectroscopy (Alpha 300R/WITec®). Data were analyzed by 3-way ANOVA and Tukey test at =5%. Statistical analysis showed significant differences among cements, curing protocols and ceramic type (p<0.001). The curing protocol 3x20 resulted in higher DC for all tested conditions; lower DC was observed for Zr ceramic crowns; Duolink resin cement culminated in higher DC regardless ceramic composition and curing protocol. The DC of resin cement layers was dependent on the curing protocol and type of ceramic.
Accelerated cure of phenol-formaldehyde resins : studies with model compounds
Anthony H. Conner; Linda F. Lorenz; Kolby C. Hirth
2002-01-01
2-Hydroxymethylphenol (2-HMP) and 4-hydroxymethylphenol (4-HMP) were used as model compounds to study the reactions that occur during cure of phenol-formaldehyde (PF) resin to which cure accelerators (ethyl formate, propylene carbonate, g-butyrolactone, and triacetin) have been added. The addition of cure accelerators significantly increased the rate of condensation...
Novais, Veridiana Resende; Raposo, Luís Henrique Araújo; Miranda, Rafael Resende de; Lopes, Camila de Carvalho Almança; Simamoto, Paulo Cézar; Soares, Carlos José
2017-01-01
The aim of this study was to assess the performance of resin cements when different curing modes are used, by evaluating the degree of conversion and bond strength to a ceramic substrate. Three resin cements were evaluated, two dual-cured (Variolink II and RelyX ARC) and one light-cured (Variolink Veneer). The dual-cured resin cements were tested by using the dual activation mode (base and catalyst) and light-activation mode (base paste only). For degree of conversion (DC) (n=5), a 1.0 mm thick feldspathic ceramic disc was placed over the resin cement specimens and the set was light activated with a QTH unit. After 24 h storage, the DC was measured with Fourier transform infrared spectroscopy (FTIR). For microshear bond strength testing, five feldspathic ceramic discs were submitted to surface treatment, and three cylindrical resin cement specimens were bonded to each ceramic surface according to the experimental groups. After 24 h, microshear bond testing was performed at 0.5 mm/min crosshead speed until the failure. Data were submitted to one-way ANOVA followed by Tukey test (p<0.05). Scanning electron microscopy (SEM) was used for classifying the failure modes. Higher DC and bond strength values were shown by the resin cements cured by using the dual activation mode. The Variolink II group presented higher DC and bond strength values when using light-activation only when compared with the Variolink Veneer group. The base paste of dual-cured resin cements in light-activation mode can be used for bonding translucent ceramic restorations of up to or less than 1.0 mm thick.
Ramos-Tonello, Carla M; Lisboa-Filho, Paulo N; Arruda, Larisa B; Tokuhara, Cintia K; Oliveira, Rodrigo C; Furuse, Adilson Y; Rubo, José H; Borges, Ana Flávia S
2017-07-01
This study has investigated the influence of Titanium dioxide nanotubes (TiO 2 -nt) addition to self-adhesive resin cement on the degree of conversion, water sorption, and water solubility, mechanical and biological properties. A commercially available auto-adhesive resin cement (RelyX U200™, 3M ESPE) was reinforced with varying amounts of nanotubes (0.3, 0.6, 0.9wt%) and evaluated at different curing modes (self- and dual cure). The DC in different times (3, 6, 9, 12 and 15min), water sorption (Ws) and solubility (Sl), 3-point flexural strength (σf), elastic modulus (E), Knoop microhardness (H) and viability of NIH/3T3 fibroblasts were performed to characterize the resin cement. Reinforced self-adhesive resin cement, regardless of concentration, increased the DC for the self- and dual-curing modes at all times studied. The concentration of the TiO 2 -nt and the curing mode did not influence the Ws and Sl. Regarding σf, concentrations of both 0.3 and 0.9wt% for self-curing mode resulted in data similar to that of dual-curing unreinforced cement. The E increased with the addition of 0.9wt% for self-cure mode and H increased with 0.6 and 0.9wt% for both curing modes. Cytotoxicity assays revealed that reinforced cements were biocompatible. TiO 2 -nt reinforced self-adhesive resin cement are promising materials for use in indirect dental restorations. Taken together, self-adhesive resin cement reinforced with TiO 2 -nt exhibited physicochemical and mechanical properties superior to those of unreinforced cements, without compromising their cellular viability. Copyright © 2017 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
Chemoviscosity modeling for thermosetting resin systems, 4
NASA Technical Reports Server (NTRS)
Hou, T. H.; Huang, Joan Y. Z.
1989-01-01
An experimental study on the changes of chemorheological properties has been conducted and analyzed on commercial Hercules 3501-6 resin system cured under several isothermal conditions between 375 and 435 K. For the cure temperatures equal to or greater than 385 K, the storage modulus curing curves, G prime (t), exhibited abrupt changes in slope which occurred at various times depending on the curing temperatures and were attributed to the onset of gelation reactions. The crossover points between G prime (t) and G double prime (t) curves were observed for curing temperatures equal to or greater than 400 K. The gelation and the crossover points obtained from the chemorheological measurements, therefore, defined two characteristic resin states during cure. Approximately the same value for the degree of cure was reached by the advancement of the reaction at each of these states. The temperature dependency of the viscosities for the characteristic resin states and the rate constants of increase in moduli at different stages of curing were analyzed. Various G prime (t) and G double prime (t) isothermal curing curves were also shown to be capable of being superimposed on one another by the principle of time-temperature superposition. The resultant shift factors a sub t(t) and a Eta(T) were shown to follow the Arrhenius type relationship. Values of the activation energy suggested that the reaction kinetics, instead of the diffusion mechanism, was the limiting step in the overall resin advancement for the cure at temperatures equal to or greater than 385 K.
Bortolotto, Tissiana; Melian, Karla; Krejci, Ivo
2013-10-01
The present study attempted to find a simple direct adhesive restorative technique for the restoration of Class 2 cavities. A self-etch adhesive system with a dual-cured core buildup composite resin (paste 1 + paste 2) was evaluated in its ability to restore proximo-occlusal cavities with margins located on enamel and dentin. The groups were: A, cavity filling (cf) with paste 1 (light-curing component) by using a layering technique; B, cf by mixing both pastes, bulk insertion, and dual curing; and C, cf by mixing both pastes, bulk insertion, and chemical curing. Two control groups (D, negative, bulk; and E, positive, layering technique) were included by restoring cavities with a classic three-step etch-and-rinse adhesive and a universal restorative composite resin. SEM margin analysis was performed before and after thermomechanical loading in a chewing simulator. Percentages (mean ± SD) of "continuous margins" were improved by applying the material in bulk and letting it self cure (54 ± 6) or dual cure (59 ± 9), and no significant differences were observed between these two groups and the positive control (44 ± 19). The present study showed that the dual-cured composite resin tested has the potential to be used as bulk filling material for Class 2 restorations. When used as filling materials, dual-cure composite resins placed in bulk can provide marginal adaptation similar to light-cured composites applied with a complex stratification technique.
Cationic cure kinetics of a polyoxometalate loaded epoxy nanocomposite
DOE Office of Scientific and Technical Information (OSTI.GOV)
Anderson, Benjamin J.
2012-08-06
The reaction cure kinetics of a novel polyoxometalate (POM) loaded epoxy nanocomposite is described. The POM is dispersed in the epoxy resin up to volume fractions of 0.1. Differential scanning calorimetry measurements show the cure of the epoxy resin to be sensitive to the POM loading. A kinetics study of the cure exotherm confirms that POM acts as a catalyst promoting cationic homopolymerization of the epoxy resin. The cure reaction is shown to propagate through two cure regimes. A fast cure at short time is shown to be propagation by the activated chain end (ACE) mechanism. A slow cure atmore » long time is shown to be propagation by the activated monomer (AM) mechanism. The activation energies for the fast and slow cure regimes agree well with other epoxy based systems that have been confirmed to propagate by the ACE and AM mechanisms.« less
Contributions on the Study of the Compressive Strength of the Light-Cured Composite Resins
Manolea, H.; Degeratu, Sonia; Deva, V.; Coles, Evantia; Draghici, Emma
2009-01-01
The mechanical properties of the light-cured composite resins are related to the material composition, but also vary according to the light-source characteristics used for polymerization. In this study we followed the compressive strength variation for a light-cured composite resin according to the time of exposure to the curing light. With that end in view,18 test pieces were made from a light-cured hybrid composite material (Filtek Z250). The test pieces where then submitted to a compressive force by a mechanical properties universal testing machine. Our results didn’t show an increase of the compressive strength according to the light-curing time increasing, than only in the light-curing time limit indicated by the manufacturer. A longer light-curing time may induce a shrinkage polymerization growth with the formation of internal tensions inside the material. The composite materials light-curing in short layers as long as there is indicated by the manufacturer seems to be a safer method to make the best from a resin qualities, then an exaggerated increase of the light-curing time. The light-curing is indicated to be done in the direction of the compressive forces. To confirm this supposition other mechanical tests are also necessary PMID:24778814
Process for epoxy foam production
Celina, Mathias C [Albuquerque, NM
2011-08-23
An epoxy resin mixture with at least one epoxy resin of between approximately 60 wt % and 90 wt %, a maleic anhydride of between approximately 1 wt % and approximately 30 wt %, and an imidazole catalyst of less than approximately 2 wt % where the resin mixture is formed from at least one epoxy resin with a 1-30 wt % maleic anhydride compound and an imidazole catalyst at a temperature sufficient to keep the maleic anhydride compound molten, the resin mixture reacting to form a foaming resin which can then be cured at a temperature greater than 50.degree. C. to form an epoxy foam.
Nontoxic Resins Advance Aerospace Manufacturing
NASA Technical Reports Server (NTRS)
2009-01-01
The 2008 NASA Commercial Invention of the Year, PETI-330, is a polyimide matrix resin that performs well at high temperatures and is easily processed into composites in a simple, short curing cycle. Invented by scientists at Langley Research Center, PETI-330 is now licensed to Ube Industries, based in Japan with its American headquarters in New York. In addition to being durable and lightweight, the resin is also nontoxic, which makes it safe for workers to handle. PETI-330 was created specifically for heat-resistant composites formed with resin transfer molding and resin infusion, which formerly could only be used with low temperature resin systems.
Asada, Chikako; Basnet, Sunita; Otsuka, Masaya; Sasaki, Chizuru; Nakamura, Yoshitoshi
2015-03-01
A low molecular weight lignin from various lignocellulosic materials was used for the synthesis of bio-based epoxy resins. The lignin extracted with methanol from steam-exploded samples (steaming time of 5 min at steam pressure of 3.5 MPa) from different biomasses (i.e., cedar, eucalyptus, and bamboo) were functionalized by the reaction with epichlorohydrin, catalyzed by a water-soluble phase transfer catalyst tetramethylammonium chloride, which was further reacted with 30 wt% aqueous NaOH for ring closure using methyl ethyl ketone as a solvent. The glycidylated products of the lignin with good yields were cured to epoxy polymer networks with bio-based curing agents i.e., lignin itself and a commercial curing agent TD2131. Relatively good thermal properties of the bio-based epoxy network was obtained and thermal decomposition temperature at 5% weight loss (Td5) of cedar-derived epoxy resin was higher than that derived from eucalyptus and bamboo. The bio-based resin satisfies the stability requirement of epoxy resin applicable for electric circuit boards. The methanol-insoluble residues were enzymatically hydrolyzed to produce glucose. This study indicated that the biomass-derived methanol-soluble lignin may be a promising candidate to be used as a substitute for petroleum-based epoxy resin derived from bisphenol A, while insoluble residues may be processed to give a bioethanol precursor i.e., glucose. Copyright © 2015 Elsevier B.V. All rights reserved.
Monitoring Prepregs As They Cure
NASA Technical Reports Server (NTRS)
Young, P. R.; Gleason, J. R.; Chang, A. C.
1986-01-01
Quality IR spectra obtained in dynamic heating environment. New technique obtains quality infrared spectra on graphite-fiber-reinforced, polymeric-matrix-resin prepregs as they cure. Technique resulted from modification of diffuse reflectance/Fourier transform infrared (DR/FTIR) technique previously used to analyze environmentally exposed cured graphite composites. Technique contribute to better understanding of prepreg chemistry/temperature relationships and development of more efficient processing cycles for advanced materials.
Arikawa, Hiroyuki; Kanie, Takahito; Fujii, Koichi; Ban, Seiji
2005-12-01
The purpose of this study was to investigate the effect of radiation light characteristics--of different types of clinical light-curing unit--on polymerization efficiency, as determined by the surface hardness of light-cured paint-on resins. Four shades of paint-on resin for shade modification of restorative resins were used. Materials were cured using one laboratory and three clinical light-curing units with different light sources, namely tungsten-halogen, LED, plasma arc, and xenon flash lamps. Knoop hardness measurements were taken at both the top and bottom surfaces of the specimens to assess the mechanical properties and degree of polymerization. Both LED and plasma arc light units caused significantly poorer surface hardness than the halogen and laboratory xenon lights. In addition, the transparent shade was more sensitive to surface hardness than other chromatic shades. Our results indicated that the polymerization efficiency of paint-on resin was significantly influenced by the radiation light characteristics of clinical light-curing units.
Saini, Rajesh; Kotian, Ravindra; Madhyastha, Prashanthi; Srikant, N
2016-01-01
The objective of this study was to compare the sorption and solubility of heat-cure and self-cure acrylic resins in different solutions. One heat-cure acrylic resin (Trevalon) and one self-cure acrylic resin (Rapid Repair) were studied. Five groups of square-shaped specimens (20 mm × 20 mm × 2 mm) were prepared for each acrylic resin and then immersed in five solutions: distilled water, artificial saliva, denture cleansing solution, distilled water, and denture cleaning solution for 12 h alternatively, artificial saliva and denture cleaning solution for 12 h alternatively at 37 ± 2°C, and tested sorption and solubility by weight gain/loss method, respectively, after 1, 6, and 11 weeks. The data were analyzed by one-way analysis of variance followed by post hoc Tukey's test. Water sorption mean values varied from 17.5 ± 0.88 to 27.25 ± 1.04 μg/mm 3 for heat cure and from 12.75 ± 0.55 to 19.75 ± 1.04 μg/mm 3 for self-cure in the different solutions after different interval periods of 1, 6, and 11 weeks. These values were statistically significant (P< 0.001). Water solubility mean values varied from 0.25 ± 0.55 to 1.5 ± 0.55 μg/mm 3 for heat cure and from 1.5 ± 0.55 to 6.5 ± 0.55 μg/mm 3 for self-cure in the different solutions after different interval periods of 1, 6, and 11 weeks. These values were statistically not significant (P > 0.05). There was no linear correlation between sorption and solubility values. Overall, analysis of results showed the maximum sorption value in denture cleansing solution followed by alternative soaking in distilled water and artificial saliva. Least sorption was observed with artificial saliva followed by distilled water. Both heat-cure and self-cure acrylic resins showed varying water sorption and solubility. The results of both water sorption and solubility showed compliance with the International Standards Organization specification. No correlation was found between water sorption and solubility. Artificial saliva solution is a better storage medium than distilled water and denture cleansing solution for both heat-cure and self-cure acrylic resins.
Jianming, Yuan; Ying, Tang; Feng, Pan; Weixing, Xu
2016-12-01
This study aims to compare the marginal accuracy of single crowns fabricated using self-curing resin, Luxatemp, and computer aided design/computer aided manufacturing (CAD/CAM) methods in clinical application. A total of 30 working dies, which were obtained from 30 clinical teeth prepared with full crown as standard, were created and made into 30 self-curing resin, Luxatemp, and CAD/CAM single crowns. The restorations were seated on the working dies, and stereomicroscope was used to observe and measure the thickness of reference points. One-way analysis of variance, which was performed using SPSS 19.0 software package, compared the marginal gap widths of self-curing resin, Luxatemp, and CAD/CAM provisional crowns. The mean marginal gap widths of the fabricated self-curing resin, Luxatemp, and CAD/CAM were (179.06±33.24), (88.83±9.56), and (43.61±7.27) μm, respectively. A significant difference was observed among the three provisional crowns (P<0.05). The marginal gap width of CAD/CAM provisional crown was lower than that of the self-curing resin and Luxatemp. Thus, the CAD/CAM provisional crown offers a better remediation effect in clinical application.
Cekic-Nagas, Isil; Egilmez, Ferhan; Ergun, Gulfem
2010-01-01
Objectives: The aim of this study was to compare the microhardness of five different resin composites at different irradiation distances (2 mm and 9 mm) by using three light curing units (quartz tungsten halogen, light emitting diodes and plasma arc). Methods: A total of 210 disc-shaped samples (2 mm height and 6 mm diameter) were prepared from different resin composites (Simile, Aelite Aesthetic Enamel, Clearfil AP-X, Grandio caps and Filtek Z250). Photoactivation was performed by using quartz tungsten halogen, light emitting diode and plasma arc curing units at two irradiation distances (2 mm and 9 mm). Then the samples (n=7/per group) were stored dry in dark at 37°C for 24 h. The Vickers hardness test was performed on the resin composite layer with a microhardness tester (Shimadzu HMV). Data were statistically analyzed using nonparametric Kruskal Wallis and Mann-Whitney U tests. Results: Statistical analysis revealed that the resin composite groups, the type of the light curing units and the irradiation distances have significant effects on the microhardness values (P<.05). Conclusions: Light curing unit and irradiation distance are important factors to be considered for obtaining adequate microhardness of different resin composite groups. PMID:20922164
High-Flow, High-Molecular-Weight, Addition-Curing Polyimides
NASA Technical Reports Server (NTRS)
Chuang, Kathy C.; Vannucci, Raymond D.
1993-01-01
In developed series of high-flow PMR-type polyimide resins, 2, 2'-bis(trifluoromethyl)-4, 4'-diaminobiphenyl (BTDB) substituted for 1, 4-pheylenediamine in PMR-II formulation. Polyimides designated either as PMR-12F when nadic ester (NE) end caps used, or as V-CAP-12F when p-aminostyrene end caps used. High-molecular-weight, addition-curing polyimides based on BTBD and HFDE highly processable high-temperature matrix resins used to make composite materials with excellent retention of properties during long-term exposure to air at 650 degrees F or higher temperature. Furthermore, 12F addition-curing polyimides useful for electronic applications; fluorinated rigid-rod polyimides known to exhibit low thermal expansion coefficients as well as low absorption of moisture.
Process for applying a superconductive powder to a wide variety of substrates
NASA Astrophysics Data System (ADS)
Hooker, Matthew W.; Wise, Stephanie A.; Tran, Sang Q.
1992-12-01
A fine superconducting powder such as YBa2Cu3O(7-x), wherein x is less than one, is blended into a liquid mixture comprising an epoxy resin and a thinner. This liquid mixture with the blended superconducting powder is coated onto a substrate. Next, the thinner is evaporated and the remaining coating cured, resulting in a coating of cured epoxy resin having superconducting powder suspended therein. This coating exhibits the Meissner effect, i.e., it expels a magnetic flux which protects the substrate from external magnetic interference. Since the coated substrate need only be heated for evaporation and curing at relatively low temperatures compared to firing, the superconducting coating can be applied to a wide variety of different materials.
Chemoviscosity modeling for thermosetting resins
NASA Technical Reports Server (NTRS)
Tiwari, S. N.; Hou, T. H.; Bai, J. M.
1985-01-01
A chemoviscosity model, which describes viscosity rise profiles accurately under various cure cycles, and correlates viscosity data to the changes of physical properties associated with structural transformations of the thermosetting resin system during cure, was established. Work completed on chemoviscosity modeling for thermosetting resins is reported.
Bismaleimide resins for flame resistant honeycomb sandwich panels
NASA Technical Reports Server (NTRS)
Stenzenberger, H. D.
1978-01-01
Bismaleimide resins are prime candidates for nonflammable aircraft interior panels. Three resin types with different structures and processing characteristics were formulated. Resin M 751 was used to fabricate 100 kg of glass fabric prepregs which were used for the preparation of face sheets for honeycomb sandwich panels. Prepreg characteristics and curing cycles for laminate fabrication are provided. In order to advance beyond the current solvent resin technology for fibre and fabric impregnation, a hot melt solvent-less resin system was prepared and characterized. Preliminary tests were performed to develop a wet bonding process for the fabrication of advanced sandwich honeycomb panels by use of polybismaleimide glass fabric face sheets and polybismaleimide Nomex honeycomb core. B-stage material was used for both the core and the face sheet, providing flatwise tensile properties equivalent to those obtained by the state-of-the-art 3-step process which includes an epoxy adhesive resin.
Moharam, Lamiaa-Mahmoud; Salem, Haidy-Nabil; Elgamily, Hanaa-Mahmoud
2018-04-01
The aim of this study was to evaluate the effect of chlorhexidine digluconate incorporation on the degree of conversion of an experimental adhesive resin. The experimental resin was prepared from 70 wt% bisphenol A glycerolate dimethacrylate, 30 wt% hydroxyethyl methacrylate, silanized SiO2 nanofillers, 0.5% of camphorquinone and ethyl 4-dimethylaminebenzoate (binary photo-initiator system). Five chlorhexidine digluconate concentrations (0, 0.5, 1, 2 and 4 wt%) were then incorporated into the experimental resin. Thirty Potassium Bromide pellets were prepared then divided into six groups (n=5/group), repre¬senting the tested adhesive resins (Single Bond 2, 0, 0.5, 1, 2 and 4 wt% chlohexidine-incorporated experimental adhesive resins), that were applied to the pellets without light-curing (uncured specimens). Another 30 pellets were prepared and treated with the previous materials then light-cured using LED light-curing device (cured specimens). Degree of conversion of the uncured and the cured specimens were evaluated using FTIR analysis. Adper Single Bond 2 showed the highest degree of conversion mean values followed by 0.5 wt% chlorhexidine concentration then 2 wt% followed by 4 wt% then 1 wt% concentrations, while 0 wt% concentration showed the lowest mean values. Chlorhexidine digluconate had slight significant influence on the efficiency of polymerization of the experimental adhesive resin. Key words: Chlorhexidine digluconate, different concentrations, degree of conversion, experimental adhesive resin.
Evaluation of compatibility between different types of adhesives and dual-cured resin cement.
Franco, Eduardo B; Lopes, Lawrence G; D'alpino, Paulo H P; Pereira, José C; Mondelli, Rafael F L; Navarro, Maria F L
2002-01-01
The objective of this in vitro study was to evaluate the bonding compatibility between different adhesives and a dual-cured resin cement, using a conventional tensile bond test. The adhesives used were: Prime & Bond (PB) (Dentsply) (PB), Scotchbond Multi Purpose (SB) (3M), and the activator Self Cure (SC) (Dentsply). The dual-curing resin cement used was Enforce (EF) (Dentsply). Six groups with five specimens in each were tested: G1: EF/PB/EF (light cured); G2: EF/SB/EF (light cured); G3: EF/PB+SC/EF (light cured); G4: EF/PB+SC/EF (only chemically cured); G5: EF/EF (light cured); G6: EF/EF (only chemically cured). The resin cement was applied in two stainless steel molds with a cone-shaped perforation measuring 4 mm in diameter and 1 mm in thickness, and the adhesive was applied between them. Ten minutes after specimens were cured, the tensile strength was measured in a universal testing machine at a crosshead speed of 0.5 mm/min. The mean values (MPa) +/- SD obtained in each experimental group were: G1: 1.4 +/- 0.2; G2: 1.3 +/- 0.2; G3: 1.2 +/- 0.4; G4: 0.8 +/- 0.2; G5: 1.2 +/- 0.1; G6: 0.7 +/- 0.1. The results were statistically evaluated using nonparametric Kruskal-Wallis and Dunn tests (p < or = 0.05). Statistically significant differences among groups were found only between G1 and G4, and G1 and G6. There was no incompatibility among the different adhesives used with dual-cured resin cement. The lowest tensile bond strength values occurred in the absence of photoactivation.
NASA Astrophysics Data System (ADS)
Möginger, B.; Kehret, L.; Hausnerova, B.; Steinhaus, J.
2016-05-01
3D-Printing is an efficient method in the field of additive manufacturing. In order to optimize the properties of manufactured parts it is essential to adapt the curing behavior of the resin systems with respect to the requirements. Thus, effects of resin composition, e.g. due to different additives such as thickener and curing agents, on the curing behavior have to be known. As the resin transfers from a liquid to a solid glass the time dependent ion viscosity was measured using DEA with flat IDEX sensors. This allows for a sensitive measurement of resin changes as the ion viscosity changes two to four decades. The investigated resin systems are based on the monomers styrene and HEMA. To account for the effects of copolymerization in the calculation of the reaction kinetics it was assumed that the reaction can be considered as a homo-polymerization having a reaction order n≠1. Then the measured ion viscosity curves are fitted with the solution of the reactions kinetics - the time dependent degree of conversion (DC-function) - for times exceeding the initiation phase representing the primary curing. The measured ion viscosity curves can nicely be fitted with the DC-function and the determined fit parameters distinguish distinctly between the investigated resin compositions.
Depth of cure of resin composites: is the ISO 4049 method suitable for bulk fill materials?
Flury, Simon; Hayoz, Stefanie; Peutzfeldt, Anne; Hüsler, Jürg; Lussi, Adrian
2012-05-01
To evaluate if depth of cure D(ISO) determined by the ISO 4049 method is accurately reflected with bulk fill materials when compared to depth of cure D(new) determined by Vickers microhardness profiles. D(ISO) was determined according to "ISO 4049; Depth of cure" and resin composite specimens (n=6 per group) were prepared of two control materials (Filtek Supreme Plus, Filtek Silorane) and four bulk fill materials (Surefil SDR, Venus Bulk Fill, Quixfil, Tetric EvoCeram Bulk Fill) and light-cured for either 10s or 20s. For D(new), a mold was filled with one of the six resin composites and light-cured for either 10 s or 20 s (n=22 per group). The mold was placed under a microhardness indentation device and hardness measurements (Vickers hardness, VHN) were made at defined distances, beginning at the resin composite that had been closest to the light-curing unit (i.e. at the "top") and proceeding toward the uncured resin composite (i.e. toward the "bottom"). On the basis of the VHN measurements, Vickers hardness profiles were generated for each group. D(ISO) varied between 1.76 and 6.49 mm with the bulk fill materials showing the highest D(ISO). D(new) varied between 0.2 and 4.0 mm. D(new) was smaller than D(ISO) for all resin composites except Filtek Silorane. For bulk fill materials the ISO 4049 method overestimated depth of cure compared to depth of cure determined by Vickers hardness profiles. Copyright © 2012 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
de Moraes Porto, Isabel Cristina Celerino; Ramos de Brito, Andréia Cristina; Parolia, Abhishek
2013-01-01
Background: Among the advice on prevent cross-infection was included usage of mechanical barriers on tips of photoactivation units. However, questions about the use of protective barriers placed on the light-curing unit's tips and the possibility of interference with the ability of guaranteeing an effective polymerization of composite resins need to be clarified. Aims: The aim of this study was to evaluate the effect of cross infection control barriers used on the light-curing device tips on the cure depth of composite resin. Materials and Methods: Power density measurements from the light-cure unit were recorded with a radiometer on ten separate occasions with different types and placement modes of each barrier (low-density polyethylene and polyvinyl chloride (PVC) film – smooth and folds) and no-barrier (control). Cure depth of TPH™ Spectrum™ resin, A2-A4, was evaluated by the scraping test. Statistical Analysis: The data were analyzed using Student's t-test or ANOVA one-way with Tukey's test (α =0.05). Results: Same type of barrier and different shades (A2, A4) of composite exhibited significant difference in the cure depth among all groups (P < 0.05). Both low-density polyethylene and PVC film folded barriers produced a significant reduction in the light intensity (P < 0.05). Conclusions: Regarding the resin shade, there was a significant reduction in the cure depth of A4 composite resin (dark shade) but this reduction is not enough to cause any adverse effect on the material's clinical performance. Therefore, disposable barriers can be recommended for use over the end of the light guide. PMID:23833455
Porwal, Anand; Khandelwal, Meenakshi; Punia, Vikas; Sharma, Vivek
2017-01-01
Aim: The purpose of this study was to evaluate the effect of different denture cleansers on the color stability, surface hardness, and roughness of different denture base resins. Materials and Methods: Three denture base resin materials (conventional heat cure resin, high impact resin, and polyamide denture base resin) were immersed for 180 days in commercially available two denture cleansers (sodium perborate and sodium hypochlorite). Color, surface roughness, and hardness were measured for each sample before and after immersion procedure. Statistical Analysis: One-way analysis of variance and Tukey's post hoc honestly significant difference test were used to evaluate color, surface roughness, and hardness data before and after immersion in denture cleanser (α =0.05). Results: All denture base resins tested exhibited a change in color, surface roughness, and hardness to some degree in both denture cleansers. Polyamides resin immersed in sodium perborate showed a maximum change in color after immersion for 180 days. Conventional heat cure resin immersed in sodium hypochlorite showed a maximum change in surface roughness and conventional heat cure immersed in sodium perborate showed a maximum change in hardness. Conclusion: Color changes of all denture base resins were within the clinically accepted range for color difference. Surface roughness change of conventional heat cure resin was not within the clinically accepted range of surface roughness. The choice of denture cleanser for different denture base resins should be based on the chemistry of resin and cleanser, denture cleanser concentration, and duration of immersion. PMID:28216847
Influence of curing protocol and ceramic composition on the degree of conversion of resin cement
Lanza, Marcos Daniel Septimio; Andreeta, Marcello Rubens Barsi; Pegoraro, Thiago Amadei; Pegoraro, Luiz Fernando; Carvalho, Ricardo Marins De
2017-01-01
Abstract Due to increasing of aesthetic demand, ceramic crowns are widely used in different situations. However, to obtain long-term prognosis of restorations, a good conversion of resin cement is necessary. Objective: To evaluate the degree of conversion (DC) of one light-cure and two dual-cure resin cements under a simulated clinical cementation of ceramic crowns. Material and Methods: Prepared teeth were randomly split according to the ceramic's material, resin cement and curing protocol. The crowns were cemented as per manufacturer's directions and photoactivated either from occlusal suface only for 60 s; or from the buccal, occlusal and lingual surfaces, with an exposure time of 20 s on each aspect. After cementation, the specimens were stored in deionized water at 37°C for 7 days. Specimens were transversally sectioned from occlusal to cervical surfaces and the DC was determined along the cement line with three measurements taken and averaged from the buccal, lingual and approximal aspects using micro-Raman spectroscopy (Alpha 300R/WITec®). Data were analyzed by 3-way ANOVA and Tukey test at =5%. Results: Statistical analysis showed significant differences among cements, curing protocols and ceramic type (p<0.001). The curing protocol 3x20 resulted in higher DC for all tested conditions; lower DC was observed for Zr ceramic crowns; Duolink resin cement culminated in higher DC regardless ceramic composition and curing protocol. Conclusion: The DC of resin cement layers was dependent on the curing protocol and type of ceramic. PMID:29211292
Polymerisation characteristics of resin composites polymerised with different curing units.
Danesh, Gholamreza; Davids, Hendrick; Reinhardt, Klaus-Jürgen; Ott, Klaus; Schäfer, Edgar
2004-08-01
The aim of this study was to compare the plasma arc light source Apollo 95E and the conventional halogen lamp Elipar Visio regarding a number of polymerisation characteristics of different resin composites. Four different resin composites (Arabesk Top, Herculite XRV, Pertac II, Tetric) were irradiated using the Apollo 95E unit for one, two or three cycles of 3 s and using the Elipar Visio unit for 40 s. The investigated polymerisation characteristics were: flexural strength and modulus of elasticity, bond strength to dentine, depth of polymerisation, and quantity of remaining double bonds. The data were treated statistically by analysis of variance and by Scheffé test. The modulus of elasticity and the flexural strength resulting from curing with Apollo 95E for 1 x 3 s were equal to or less than those resulting from curing with Elipar Visio. The bond strength to dentine and the depth of polymerisation with Apollo 95E used for 1 x 3 s were equal to or less than that obtained with the conventional lamp, depending on the resin composite. Irradiation of Herculite XRV resulted in a higher quantity of remaining double bonds than did Elipar Visio. In general, two or three curing cycles of 3 s with Apollo 95E were necessary to produce mechanical properties not significantly worse than with 40 s of conventional curing. The efficiency of plasma arc curing with Apollo 95E strongly depends on the resin composite. For most resin composites tested, plasma arc curing for 3 s resulted in inferior mechanical properties as compared to conventional curing.
Kim, L U; Kim, J W; Kim, C K
2006-09-01
To prepare a dental composite that has a low amount of curing shrinkage and excellent mechanical strength, various 2,2-bis[4-(2-hydroxy-3-methacryloyloxy propoxy) phenyl] propane (Bis-GMA) derivatives were synthesized via molecular structure design, and afterward, properties of their mixtures were explored. Bis-GMA derivatives, which were obtained by substituting methyl groups for hydrogen on the phenyl ring in the Bis-GMA, exhibited lower curing shrinkage than Bis-GMA, whereas their viscosities were higher than that of Bis-GMA. Other Bis-GMA derivatives, which contained a glycidyl methacrylate as a molecular end group exhibited reduced curing shrinkage and viscosity. Methoxy substitution for hydroxyl groups on the Bis-GMA derivatives was performed for the further reduction of the viscosity and curing shrinkage. Various resin mixtures, which had the same viscosity as the commercial one, were prepared, and their curing shrinkage was examined. A resin mixture containing 2,2-bis[3,5-dimethyl, 4-(2-methoxy-3-methacryloyloxy propoxy) phenyl] propane] (TMBis-M-GMA) as a base resin and 4-tert-butylphenoxy-2-methyoxypropyl methacrylate (t-BP-M-GMA) as a diluent exhibited the lowest curing shrinkage among them. The composite prepared from this resin mixture also exhibited the lowest curing shrinkage along with enhanced mechanical properties.
Coating Characterization with the Quartz Crystal Microbalance
NASA Astrophysics Data System (ADS)
Sturdy, Lauren F.
The quartz crystal microbalance is a sensitive tool that can be used to measure the mass, modulus and phase angle of films of appropriate thicknesses. It is can be applied to systems with very varied properties, from liquid to solid, and under many different conditions. In this thesis its capabilities have been used to study the properties of several different systems of relevance to the coatings, art conservation, and rubber communities, in the process of which new techniques and tools were developed to analyze data and improve QCM data collection and experimental design. Alkyd resins, which have been used in artists' paints since the twentieth century, are the subject of the first studies. Alkyds are oil-modified polyesters. These resins are of interest because of their relatively recent use in art and how little is known of the mechanical properties in the early stages of cure. The QCM was shown to be sensitive to the curing process, changes in temperature, and mass change due to exposure to water. Kinetic studies during the first days of curing showed that the curing process can be divided into three regions. The first is dominated by solvent evaporation. In the second, oxygen absorption dominates and the mechanical properties change rapidly. The final stage extends from when the film is touch dry after about a day to years and is characterized by mass loss and continued increases in the modulus. Studying the curing at different temperatures revealed that the reactions do proceed much more rapidly at higher temperatures and an overall energy of activation was calculated for the curing process. The mechanical properties of alkyd resins containing zinc oxide, a white pigment, were studied with the QCM, nanoindentation and dynamic mechanical analysis. These measurements showed increases in the modulus with the inclusion of zinc oxide, and the QCM data showed that the second region started at earlier times as the pigment concentration was increased. Linseed oil is one of the starting materials for many alkyd resins and should cure similarly since the primary curing mechanisms are the same. It takes longer to cure than alkyds because it begins with no initial polymerization. Linseed oil was harder to study, as obtaining even films was difficult, multiple peaks at a single harmonic were observed, and the material properties during the early stages of curing led to a region where viscoelastic properties could not be calculated. To facilitate studying linseed oil, a multiple peak fitting method was developed to extract data from unusual peak shapes. With this ability, measurements at short times could be obtained despite poor film quality. Although linseed oil begins as a softer material than alkyds, its curing follows the same patterns as alkyd resins, exhibiting mass gain followed by mass loss, and sharp increases in modulus and decreases in phase angle during the early stages of curing. Having demonstrated the ability of the QCM to monitor curing, the QCM was also applied to uncrosslinked rubber systems. Rubbers, like the drying oils, contain double bonds which can react with oxygen, so first the oxidation of these materials was studied. In further studies oxidation was undesirable, so protocols were developed to limit oxidation. Measurements were made of homopolymers at different temperatures and the QCM measurements appear to be consistent with time-temperature superposition results obtained at lower frequencies. Blends of the various rubbers were studied and compared with models. The mechanical properties measured by the QCM were between the Voigt and Reuss predictions for most blends studied. Modeling the expected QCM response of layered rubbers matched the predictions of the Reuss model but not the measured values of the rubber blends, suggesting that the QCM is sensitive to different morphologies. Measurements with the QCM expanded our understanding of a variety of systems and proved to be a useful tool to measure mechanical changes during processes which are difficult to study by other methods.
Use of 2,5-dimethyl-2,5-hexane diamine as a curing agent for epoxy resins. [Patent application
Rinde, J.A.; Newey, H.A.
Primary diamines are prepared for use as a curing agent for epoxy resins. These curing agents can be used to form epoxy resin mixtures useful in filament winding and preimpregnated fiber molding and in formulating film adhesives, powder coatings and molding powders. The epoxy mixtures form for such uses a room temperature non-reacting, intermediate stable state which has a latent cross-linking capability.
Adhesives and method for making the same
Dorsey, George F.
1991-01-01
A thermosetting mixture for use as an adhesive, as well as other applications, that is substantially nonmutagenic. This mixture is based upon a thermosetting resin selected from polyurethane and epoxy resins, using an improved curing agent that does not contain mutagenic components. Specifically, the curing agent is a multi-mixture of substituted alkylanilines produced by an improved process. These alkylanilines are formed by condensation of at least two 2,6-dialkylanilines with a formaldehyde in an acid solution. Upon purification, at least three aromatic diamines are formed that are used for the curing agent with the polyurethane and epoxy resisn. Pot life, green strength and ultimate strength are comparable to adhesives of the prior art that contain mutagenic constituents. Although several dianilines are described, the preferred curing agents are formed using 2,6-diethylaniline (DEA) and 2,6-diisopropylaniline (DIPA), where the mole % of DEA and DIPA is 38-48 and 62-52, respectively. Curing agents within the preferred range have been designated as "Asilamine 4852" and "Asilamine 4555".
Preform Characterization in VARTM Process Model Development
NASA Technical Reports Server (NTRS)
Grimsley, Brian W.; Cano, Roberto J.; Hubert, Pascal; Loos, Alfred C.; Kellen, Charles B.; Jensen, Brian J.
2004-01-01
Vacuum-Assisted Resin Transfer Molding (VARTM) is a Liquid Composite Molding (LCM) process where both resin injection and fiber compaction are achieved under pressures of 101.3 kPa or less. Originally developed over a decade ago for marine composite fabrication, VARTM is now considered a viable process for the fabrication of aerospace composites (1,2). In order to optimize and further improve the process, a finite element analysis (FEA) process model is being developed to include the coupled phenomenon of resin flow, preform compaction and resin cure. The model input parameters are obtained from resin and fiber-preform characterization tests. In this study, the compaction behavior and the Darcy permeability of a commercially available carbon fabric are characterized. The resulting empirical model equations are input to the 3- Dimensional Infiltration, version 5 (3DINFILv.5) process model to simulate infiltration of a composite panel.
NASA Astrophysics Data System (ADS)
Meier, R.; Kirdar, C.; Rudolph, N.; Zaremba, S.; Drechsler, K.
2014-05-01
Efficient production and consumption of energy are of greatest importance for contemporary industries and their products. This has led to an increasing application of lightweight materials in general and of Carbon Fiber Reinforced Plastics (CFRP) in particular. However, broader application of CFRP is often limited by high costs and manual labor production processes. These constraints are addressed by Liquid Composite Molding (LCM) processes. In LCM a dry fibrous preform is placed into a cavity and infiltrated mostly by thermoset resins; epoxy resins are wide spread in CFRP applications. One crucial parameter for a fast mold filling is the viscosity of the resin, which is affected by the applied shear rates as well as temperature and curing time. The work presented focuses on the characterization of the shear thinning behavior of epoxy resins. Furthermore, the correlation with the conditions in vibration assisted LCM processes, where additional shear rates are created during manufacture, is discussed. Higher shear rates result from high frequencies and/or high amplitudes of the vibration motions which are created by a vibration engine mounted on the mold. In rheological investigations the shear thinning behavior of a representative epoxy resin is studied by means of rotational and oscillatory experiments. Moreover, possible effects of shear rates on the chemical curing reaction are studied. Here, the time for gelation is measured for different levels of shear rates in a pre-shearing phase. Based on the rheological studies, the beneficial effect of vibration assistance in LCM processes with respect to mold filling can further be predicted and utilized.
Cure Kinetics of Benzoxazine/Cycloaliphatic Epoxy Resin by Differential Scanning Calorimetry
NASA Astrophysics Data System (ADS)
Gouni, Sreeja Reddy
Understanding the curing kinetics of a thermoset resin has a significant importance in developing and optimizing curing cycles in various industrial manufacturing processes. This can assist in improving the quality of final product and minimizing the manufacturing-associated costs. One approach towards developing such an understanding is to formulate kinetic models that can be used to optimize curing time and temperature to reach a full cure state or to determine time to apply pressure in an autoclave process. Various phenomenological reaction models have been used in the literature to successfully predict the kinetic behavior of a thermoset system. The current research work was designed to investigate the cure kinetics of Bisphenol-A based Benzoxazine (BZ-a) and Cycloaliphatic epoxy resin (CER) system under isothermal and nonisothermal conditions by Differential Scanning Calorimetry (DSC). The cure characteristics of BZ-a/CER copolymer systems with 75/25 wt% and 50/50 wt% have been studied and compared to that of pure benzoxazine under nonisothermal conditions. The DSC thermograms exhibited by these BZ-a/CER copolymer systems showed a single exothermic peak, indicating that the reactions between benzoxazine-benzoxazine monomers and benzoxazine-cycloaliphatic epoxy resin were interactive and occurred simultaneously. The Kissinger method and isoconversional methods including Ozawa-Flynn-Wall and Freidman were employed to obtain the activation energy values and determine the nature of the reaction. The cure behavior and the kinetic parameters were determined by adopting a single step autocatalytic model based on Kamal and Sourour phenomenological reaction model. The model was found to suitably describe the cure kinetics of copolymer system prior to the diffusion-control reaction. Analyzing and understanding the thermoset resin system under isothermal conditions is also important since it is the most common practice in the industry. The BZ-a/CER copolymer system with 75/25 wt% ratio which exhibited high glass transition temperature compared to polybenzoxazine was investigated under isothermal conditions. The copolymer system exhibited the maximum reaction rate at an intermediate degree of cure (20 to 40%), indicating that the reaction was autocatalytic. Similar to the nonisothermal cure kinetics, Kamal and Sourour phenomenological reaction model was adopted to determine the kinetic behavior of the system. The theoretical values based on the developed model showed a deviation from the obtained experimental values, which indicated the change in kinetics from a reaction-controlled mechanism to a diffusion-controlled mechanism with increasing reaction conversion. To substantiate the hypothesis, Fournier et al's diffusion factor was introduced into the model, resulting in an agreement between the theoretical and experimental values. The changes in cross-linking density and the glass transition temperature (Tg) with increasing epoxy concentration were investigated under Dynamic Mechanical Analyzer (DMA). The BZ-a/CER copolymer system with the epoxy content of less than 40 wt% exhibited the greatest Tg and cross-linking density compared to benzoxazine homopolymer and other ratios.
1974-10-01
polyester chains. Cross-linking, normally known as the curing process, is brought about by free radicals supplied by a catalyst, usually an organic...peroxide. Cure is normally carried out at room temperature, but a higher tenmerature may be used, depending on the reactivity of the catalyst. In the...selection of an elevated cure temperature permits wide versatility and a large measure of control over the proces-ing of these resins. Since the direct
High-Performance, Low-Energy-Curing Resins.
1984-03-01
with a phenolic resin 0. Quinlivan, private communication). Although in this system, the phenolic resin requires curing well above room temperature...34 -4 JOHN T. QUINLIVAN received a B.S. degree from Gonzaga University and M.A. *1 and Ph.D. degrees in chemistry from Princeton University. After
Cure shrinkage in casting resins
DOE Office of Scientific and Technical Information (OSTI.GOV)
Spencer, J. Brock
2015-02-01
A method is described whereby the shrinkage of a casting resin can be determined. Values for the shrinkage of several resin systems in frequent use by Sandia have been measured. A discussion of possible methods for determining the stresses generated by cure shrinkage and thermal contraction is also included.
A semi-empirical approach for the chemoviscosity modeling of reactive resin system
NASA Technical Reports Server (NTRS)
Hou, T. H.; Bai, J. M.
1988-01-01
A new analytical model for simulating chemoviscosity of a thermosetting resin is presented. The model is developed on the basis of the Williams-Landel-Ferry (WLF, 1955) polymer rheology theory for the thermoplastic materials, which was modified to account for the factor of reaction time by introducing a relationship between the glass transition temperature and the degree of cure of the resin system. Theoretical predictions of the chemoviscosity profiles under dynamic curing conditions are shown to compare favorably with the experimental data obtained on the Hercules 3501-6 resin system cured under seven isothermal conditions.
Linda F. Lorenz; Anthony C. Conner
2000-01-01
Fast curing phenol-formaldehyde (PF) resins could potentially allow wood to be bonded at higher moisture contents and at lower press temperatures than those currently used commercially. Recent reports in the literature have shown that the addition of esters, lactones, or organic carbonates increased the curing rate of PF resins. Several mechanisms have been proposed to...
Dogar, A; Altintas, S C; Kavlak, S; Guner, A
2012-12-01
To evaluate the effect of quartz-fibre posts on the depth of polymerization of a dual-cure resin cement using Raman spectroscopy and to determine the physical properties of the polymerized cement using a dynamic mechanical analyzer (DMA). Twenty-five fibre and 25 CrNi posts were used to evaluate depth of polymerization. Posts were cemented with dual-cure resin into root canals formed from silicone moulds, without using bonding or etching agents. After polymerization, resin layers on each sample were removed using a curette and cut into three equal parts (apical, middle and coronal). All resin specimens for every third were gathered and crushed. Resin powder samples were analysed using Dynamic Mechanical Analysis and Raman spectroscopy for each third. The numerical data revealed that the thermal transitions of the materials took place at higher temperatures from the apical to the coronal sections in both groups. C=C double bond intensity was lower in fibre post-resin cement samples when compared to their intensity in metal post-resin cement samples. Dual-cured resin cements had more rigid properties and better polymerization for fibre posts when compared with metal posts. Polymerization quantity was affected by position in the canal. © 2012 International Endodontic Journal.
Flexural properties of ethyl or methyl methacrylate-UDMA blend polymers.
Kanie, Takahito; Kadokawa, Akihiko; Arikawa, Hiroyuki; Fujii, Koichi; Ban, Seiji
2010-10-01
Light-curing polyethyl methacrylate (PEMA)-urethane dimethacrylate (UDMA) resins and polymethyl methacrylate (PMMA)-UDMA resins were prepared by two processes. For first step, PEMA or PMMA powders were fully dissolved in ethyl methacrylate (EMA) or methyl methacrylate (MMA) and then the PEMA-EMA/PMMA-MMA mixtures were mixed with UDMA. The flexural properties of cured PEMA-UDMA and PMMA-UDMA polymers were measured using two PEMA (Mw: 300,000-400,000 and 650,000-1,000,000) and three PMMA (Mw: 30,000-60,000, 350,000 and 650,000-1,000,000) powders with different molecular weight, four mixing ratios of PMMA-MMA, and three mixing ratios of PMMA-MMA mixture and UDMA oligomer. Polymers with PMMA(Mw: 350,000) MMA=25/50, and with PMMA(Mw: 350,000)-MMA/UDMA=1/2 and =1/1, showed no-fracture in a flexural test at 1 mm/min and flexural strength and flexural modulus showed no significant difference compared with those of commercially available heat- and self-curing acrylic resins (p>0.01). Within limitation of this investigation, methyl methacrylate-UDMA blend polymer of this composition is available for denture base resin.
Epoxy Grout With Silica Thickener
NASA Technical Reports Server (NTRS)
Mcclung, C. E.
1984-01-01
Grout cures quickly, even in presence of hydraulic oil. Grout is mixture of aggregate particles, finely-divided silica, epoxy resin, and triethylenetetramine curing agent, with mixture containing about 85 percent silica and aggregate particle sand 15 percent resin and curing agent. Silica is thickening agent and keeps grout from sagging.
[Disintegration of visible light-cured composite resins caused by long-term water immersion].
Hino, T; Arai, K
1989-05-01
The purpose of this study is to clarify a cause of disintegration of composite resins by long-term immersion in distilled water. Three kinds of visible light-cured composite resins (Heliosit, Plurafil Super and Visio Dispers) and one conventional composite resin (Clearfil F II) were prepared as the specimens with a 20 mm diameter and 1 mm thickness. These specimens were immersed in distilled water at 37 +/- 1 degree C for 3 years. These specimens were analysed and observed by a comprehensive multi analyzer and scanning electron microscope. The other hand residues in distilled water were analysed by infrared (IR) and nuclear magnetic resonance (NMR) spectrometers. The surface layer of all four composite resins showed signs of disintegration. The composite resins with abundant dissolved substances had disintegrated markedly, and such disintegration occurred deep inside the specimens. In IR and 1H-NMR spectra of dissolved substances, two visible light-cured composite resins (Heliosit and Plurafil Super) could be detected unreacted monomers, but one visible light-cured composite resin (Visio Dispers) and one conventional composite resin (Clearfil F II) could not be detected them. In 1H-NMR spectra of dissolved substances of all four composite resins, new signals not composed originally were observed. The progress of disintegration were demonstrated clearly. The dissolved substances were shown as the disintegrated substance between resin matrixs and silane coupling agents. It is suggested that the disintegration of composite resins by long-term water immersion is derived from hydrolysis.
Hybrid self-healing matrix using core-shell nanofibers and capsuleless microdroplets.
Lee, Min Wook; An, Seongpil; Lee, Changmin; Liou, Minho; Yarin, Alexander L; Yoon, Sam S
2014-07-09
In this work, we developed novel self-healing anticorrosive hierarchical coatings that consist of several components. Namely, as a skeleton we prepared a core-shell nanofiber mat electrospun from emulsions of cure material (dimethyl methylhydrogen siloxane) in a poly(acrylonitrile) (PAN) solution in dimethylformamide. In these nanofibers, cure is in the core, while PAN is in the shell. The skeleton deposited on a protected surface is encased in an epoxy-based matrix, which contains emulsified liquid droplets of dimethylvinyl-terminated dimethylsiloxane resin monomer. When such hierarchical coatings are damaged, cure is released from the nanofiber cores and the resin monomer, released from the damaged matrix, is polymerized in the presence of cure. This polymerization and solidification process takes about 1-2 days and eventually heals the damaged material when solid poly(dimethylsiloxane) resin is formed. The self-healing effect was demonstrated using an electrochemical analogue of the scanning vibrating electrode technique. Damaged samples were left for 2 days. After that, the electric current through a damaged coating was found to be negligibly small for the samples with self-healing properties. On the other hand, for the samples without self-healing properties, the electric current was significant.
Feasibility study for the development of low temperature curing adhesives
NASA Technical Reports Server (NTRS)
Green, H. E.; Sutherland, J. D.; Sheppard, C. H.
1974-01-01
The feasibility of a new approach for the development of stable, easily handled, room temperature (293 K - 311 K) curing adhesives was studied and demonstrated. The work concentrated on a family of unsaturated amide/ester resins. Twelve candidate resins were synthesized and tested for completeness of cure at room temperature, adhesion to aluminum and titanium, shear strength, moisture resistance and heat stability. The three most promising candidate resins were selected and recommended for further development.
NASA Astrophysics Data System (ADS)
Ruey Ong, Huei; Maksudur Rahman Khan, Md.; Ramli, Ridzuan; Shein Hong, Chi; Yunus, Rosli Mohd
2018-03-01
An alkyd resin has been synthesized from palm oil that reacted with glycerol and phthalic anhydride by alcoholysis-polyesterification process and co-catalyzed by CuO nanoparticle. The CuO nanoparticle was pre-prepared in the glycerol via sol gel method, which creates a new reaction condition for resin preparation. The resins were characterized by fourier transform infrared spectroscopy (FTIR), where a new ester linkage bond (C-O-C) was noticed for resin sample. The antimicrobial activity and the curing behaviour of the resin were determined by Kirby-Bauer and differential scanning calorimeter technique. It was found that, the addition of CuO speeded up the reaction rate and played antimicrobial role. Moreover, it shortens the reaction time of alcoholysis and polyesterification process.
Phenylethynyl Containing Reactive Additives
NASA Technical Reports Server (NTRS)
Connell, John W. (Inventor); Smith, Joseph G., Jr. (Inventor); Hergenrother, Paul M. (Inventor)
2002-01-01
Phenylethynyl containing reactive additives were prepared from aromatic diamines containing phenylethynyl groups and various ratios of phthalic anhydride and 4-phenylethynylphthalic anhydride in glacial acetic acid to form the imide in one step or in N-methyl-2-pyrrolidi none to form the amide acid intermediate. The reactive additives were mixed in various amounts (10% to 90%) with oligomers containing either terminal or pendent phenylethynyl groups (or both) to reduce the melt viscosity and thereby enhance processability. Upon thermal cure, the additives react and become chemically incorporated into the matrix and effect an increase in crosslink density relative to that of the host resin. This resultant increase in crosslink density has advantageous consequences on the cured resin properties such as higher glass transition temperature and higher modulus as compared to that of the host resin.
Phenylethynyl Containing Reactive Additives
NASA Technical Reports Server (NTRS)
Connell, John W. (Inventor); Smith, Joseph G., Jr. (Inventor); Hergenrother, Paul M. (Inventor)
2002-01-01
Phenylethynyl containing reactive additives were prepared from aromatic diamine, containing phenylethvnvl groups and various ratios of phthalic anhydride and 4-phenylethynviphthalic anhydride in glacial acetic acid to form the imide in one step or in N-methyl-2-pvrrolidinone to form the amide acid intermediate. The reactive additives were mixed in various amounts (10% to 90%) with oligomers containing either terminal or pendent phenylethynyl groups (or both) to reduce the melt viscosity and thereby enhance processability. Upon thermal cure, the additives react and become chemically incorporated into the matrix and effect an increase in crosslink density relative to that of the host resin. This resultant increase in crosslink density has advantageous consequences on the cured resin properties such as higher glass transition temperature and higher modulus as compared to that of the host resin.
Soft Polymers for Building up Small and Smallest Blood Supplying Systems by Stereolithography
Meyer, Wolfdietrich; Engelhardt, Sascha; Novosel, Esther; Elling, Burkhard; Wegener, Michael; Krüger, Hartmut
2012-01-01
Synthesis of a homologous series of photo-polymerizable α,ω-polytetrahydrofuranether-diacrylate (PTHF-DA) resins is described with characterization by NMR, GPC, DSC, soaking and rheometrical measurements. The curing speeds of the resins are determined under UV light exposure. Young’s modulus and tensile strength of fully cured resins show flexible to soft material attributes dependent on the molar mass of the used linear PTHF-diacrylates. Structuring the materials by stereo lithography (SL) and multiphoton polymerization (MPP) leads to tubes and bifurcated tube systems with a diameter smaller than 2 mm aimed at small to smallest supplying systems with capillary dimensions. WST-1 biocompatibility tests ofm polymer extracts show nontoxic characteristics of the adapted polymers after a washing process. Some polymers show shape memory effect (SME). PMID:24955530
Oto, Tatsuki; Yasuda, Genta; Tsubota, Keishi; Kurokawa, Hiroyasu; Miyazaki, Masashi; Platt, Jeffrey A
2009-01-01
This study examined the influence of power density on dentin bond strength and polymerization behavior of dual-cured direct core foundation resin systems. Two commercially available dual-cured direct core foundation resin systems, Clearfil DC Core Automix with Clearfil DC Bond and UniFil Core with Self-Etching Bond, were studied. Bovine mandibular incisors were mounted in autopolymerizing resin and the facial dentin surfaces were ground wet on 600-grit SiC paper. Dentin surfaces were treated according to manufacturer's recommendations. The resin pastes were condensed into the mold and cured with the power densities of 0 (no irradiation), 100, 200, 400 and 600 mW/cm2. Ten specimens per group were stored in 37 degrees C water for 24 hours, then shear tested at a crosshead speed of 1.0 mm/minute in a universal testing machine. An ultrasonic measurement device was used to measure the ultrasonic velocities through the core foundation resins. The power densities selected were 0 (no irradiation), 200, and 600 mW/cm2, and ultrasonic velocity was calculated. ANOVA and Tukey HSD tests were performed at a level of 0.05. The highest bond strengths were obtained when the resin pastes were cured with the highest power density for both core foundation systems (16.8 +/- 1.9 MPa for Clearfil DC Core Automix, 15.6 +/- 2.9 MPa for UniFil Core). When polymerized with the power densities under 200 mW/cm2, significantly lower bond strengths were observed compared to those obtained with the power density of 600 mW/cm2. As the core foundation resins hardened, the sonic velocities increased and this tendency differed among the power density of the curing unit. When the sonic velocities at three minutes after the start of measurements were compared, there were no significant differences among different irradiation modes for UniFil Core, while a significant decrease in sonic velocity was obtained when the resin paste was chemically polymerized compared with dual-polymerization for Clearfil DC Core Automix. The data suggests that the dentin bond strengths and polymerization behavior of the dual-cured, direct core foundation systems are still affected by the power density of the curing unit. With a careful choice of the core foundation systems and power density of the curing unit, the benefit of using resin composites to endodontically-treated teeth might be acceptable.
In-situ Frequency Dependent Dielectric Sensing of Cure
NASA Technical Reports Server (NTRS)
Kranbuehl, David E.
1996-01-01
With the expanding use of polymeric materials as composite matrices, adhesives, coatings and films, the need to develop low cost, automated fabrication processes to produce consistently high quality parts is critical. Essential to the development of reliable, automated, intelligent processing is the ability to continuously monitor the changing state of the polymeric resin in-situ in the fabrication tool. This final report discusses work done on developing dielectric sensing to monitor polymeric material cure and which provides a fundamental understanding of the underlying science for the use of frequency dependent dielectri sensors to monitor the cure process.
NASA Technical Reports Server (NTRS)
Scola, D. A.
1982-01-01
Bisimide amines (BIAs), which are presently used as curing agents in a state-of-the-art epoxy resin, are oligomeric and polymeric mixtures. A series of composites consisting of the novel BIA-cured epoxy resin reinforced with Celion 6000 graphite fibers were fabricated and evaluated, and the ten-degree, off-axis uniaxial tensile and shear properties of these composites were determined. The use of the intralaminar shear strain-to-failure was used in the calculation of resin shear strain-to-failure. Study results indicate that several of these novel composite systems exhibit shear strain properties that are superior to those of the control composite system of the present experiments, which employed a sulfone curing agent.
Roy, Konda Karthik; Kumar, Kanumuru Pavan; John, Gijo; Sooraparaju, Sujatha Gopal; Nujella, Surya Kumari; Sowmya, Kyatham
2018-01-01
Aim: The aim of this study is to compare and to evaluate effect of curing light and curing modes on the nanohybrid composite resins with conventional Bis-GMA and novel tricyclodecane (TCD) monomers. Methodology: Two nanohybrid composites, IPS empress direct and charisma diamond were used in this study. Light-emitting diode (LED)-curing unit and quartz-tungsten-halogen (QTH)-curing unit which were operated into two different modes: continuous and soft start. Based on the composite resin, curing lights, and mode of curing used, the samples were divided into 8 groups. After polymerization, the samples were stored for 48 h in complete darkness at 37°C and 100% humidity. The Vickers hardness (VK) of the surface was determined with Vickers indenter by the application of 200 g for 15 s. Three VK readings were recorded for each sample surface both on top and bottom surfaces. For all the specimens, the three hardness values for each surface were averaged and reported as a single value. The mean VK and hardness ratio were calculated. The depth of cure was assessed based on the hardness ratio. Results: Comparison of mean hardness values and hardness ratios was done using ANOVA with post hoc Tukey's test. Conclusion: Both QTH- and LED-curing units had shown the adequate depth of cure. Soft-start-curing mode in both QTH- and LED-curing lights had effectively increased microhardness than the continuous mode of curing. TCD monomer had shown higher hardness values compared with conventional Bis-GMA-containing resin. PMID:29628651
Use of near-IR to monitor the influence of external heating on dental composite photopolymerization.
Trujillo, Marianela; Newman, Sheldon M; Stansbury, Jeffrey W
2004-10-01
This study was conducted to determine the effect of modest external heating on the photopolymerization kinetics and conversion of commercial dental composite restorative materials. A transmission-mode, real-time near-infrared spectroscopic technique was used to monitor the photopolymerization process in the composite materials at various temperatures between 23 and 70 degrees C. Several light curing units, differing in spectral output and power densities were compared at the different cure temperatures. Several significantly different commercial composites were compared for their response. Regardless of the curing light or composite material used, photopolymerization at a moderate curing temperature of 54.5 degrees C resulted in significantly higher immediate and final conversion values compared with room temperature photocuring. Contrary to the room temperature cured materials, at the elevated cure temperature the extent of post-cure was minor and different curing lights produced very uniform conversion values within a given material. The time required to reach a given level of conversion, established as full conversion with the room temperature cure, was reduced typically by 80-90% using the elevated curing conditions. Complementary kinetic studies confirmed the effect of cure temperature on increasing the polymerization rate in dental composites as significant. Increasing the temperature of composite resin within potentially biologically compatible limits can significantly influences resin polymerization. These increased rates and conversion could lead to improved properties of composite restorative materials.
Effect of various infection-control methods for light-cure units on the cure of composite resins.
Chong, S L; Lam, Y K; Lee, F K; Ramalingam, L; Yeo, A C; Lim, C C
1998-01-01
This study (1) compared the curing-light intensity with various barrier infection-control methods used to prevent cross contamination, (2) compared the Knoop hardness value of cured composite resin when various barrier control methods were used, and (3) correlated the hardness of the composite resin with the light-intensity output when different infection-control methods were used. The light-cure unit tips were covered with barriers, such as cellophane wrap, plastic gloves, Steri-shields, and finger cots. The control group had no barrier. Composite resins were then cured for each of the five groups, and their Knoop hardness values recorded. The results showed that there was significant statistical difference in the light-intensity output among the five groups. However, there was no significant statistical difference in the Knoop hardness values among any of the groups. There was also no correlation between the Knoop hardness value of the composite resin with the light-intensity output and the different infection-control methods. Therefore, any of the five infection-control methods could be used as barriers for preventing cross-contamination of the light-cure unit tip, for the light-intensity output for all five groups exceeded the recommended value of 300 W/m2. However, to allow a greater margin of error in clinical situations, the authors recommend that the plastic glove or the cellophane wrap be used to wrap the light-cure tip, since these barriers allowed the highest light-intensity output.
Par, Matej; Spanovic, Nika; Bjelovucic, Ruza; Skenderovic, Hrvoje; Gamulin, Ozren; Tarle, Zrinka
2018-06-17
The aim of this work was to investigate the curing potential of an experimental resin composite series with the systematically varying amount of bioactive glass 45S5 by evaluating the degree of conversion, light transmittance and depth of cure. Resin composites based on a Bis-GMA/TEGDMA resin with a total filler load of 70 wt% and a variable amount of bioactive glass (0-40 wt%) were prepared. The photoinitiator system was camphorquinone and ethyl-4-(dimethylamino) benzoate. The degree of conversion and light transmittance were measured by Raman spectroscopy and UV-vis spectroscopy, respectively. The depth of cure was evaluated according to the classical ISO 4049 test. The initial introduction of bioactive glass into the experimental series diminished the light transmittance while the further increase in the bioactive glass amount up to 40 wt% caused minor variations with no clear trend. The curing potential of the experimental composites was similar to or better than that of commercial resin composites. However, unsilanized bioactive glass fillers demonstrated the tendency to diminish both the maximum attainable conversion and the curing efficiency at depth. Experimental composite materials containing bioactive glass showed a clinically acceptable degree of conversion and depth of cure. The degree of conversion and depth of cure were diminished by bioactive glass fillers in a dose-dependent manner, although light transmittance was similar among all of the experimental composites containing 5-40 wt% of bioactive glass. Reduced curing potential caused by the bioactive glass has possible consequences on mechanical properties and biocompatibility. Copyright © 2018 Elsevier Ltd. All rights reserved.
NASA Technical Reports Server (NTRS)
Curley, Michael J. (Inventor); Sarkisov, Sergey S. (Inventor)
2008-01-01
A refractometer computer controls the rotation of a rotary plate upon which are mounted a prism optically coupled via an optical window to a spectroscopic cell holding a resin exhibiting a dynamic refractive index during photocuring. The computer system positions the prism and spectroscopic cell relative to a visible light laser which illuminates the prism-resin interface at selected incidence angles. A photodetector mounted on the plate generates a signal to the computer proportional to intensity of an internally reflected light beam. A curing light is selectively transmitted through the prism and into the photocurable resin. The refractometer determines the intensity of the internally reflected beam a selected incidence angles and determines the effective refractive index curve of the resin at an uncured state and, optionally, at a completely cured state. Next, an amount of uncured resin and selected optical components to be joined by the resin is placed in the spectroscopic cell and irradiated with the UV light. The refractometer is fixed at a selected incidence angle and measures the intensity of an internally reflected light beam of light throughout the cure cycle. The refractometer determines the resin's refractive index of the polymeric mixture by means of extrapolation of a horizontal shift in the effective refractive index curve of the resin from an uncured state to a selected point in the cure cycle.
Preparation and properties studies of UV-curable silicone modified epoxy resin composite system.
Yu, Zhouhui; Cui, Aiyong; Zhao, Peizhong; Wei, Huakai; Hu, Fangyou
2018-01-01
Modified epoxy suitable for ultraviolet (UV) curing is prepared by using organic silicon toughening. The curing kinetics of the composite are studied by dielectric analysis (DEA), and the two-phase compatibility of the composite is studied by scanning electron microscopy (SEM). The tensile properties, heat resistance, and humidity resistance of the cured product are explored by changing the composition ratio of the silicone and the epoxy resin. SEM of silicone/epoxy resin shows that the degree of cross-linking of the composites decreases with an increase of silicone resin content. Differential thermal analysis indicates that the glass transition temperature and the thermal stability of the composites decrease gradually with an increase of silicone resin content. The thermal degradation rate in the high temperature region, however, first decreases and then increases. In general, after adding just 10%-15% of the silicone resin and exposing to light for 15 min, the composite can still achieve a better curing effect. Under such conditions, the heat resistance of the cured product decreases a little. The tensile strength is kept constant so that elongation at breakage is apparently improved. The change rate after immersion in distilled water at 60°C for seven days is small, which shows excellent humidity resistance.
NASA Technical Reports Server (NTRS)
Serafini, T. T.; Delvigs, P.; Vannucci, R. D. (Inventor)
1981-01-01
A curing for a polyepoxide is described which contains a divalent aryl radical such as phenylene a tetravalent aryl radical such as a tetravalent benzene radical. An epoxide is cured by admixture with the curing agent. The cured epoxy product retains the usual properties of cured epoxides and, in addition, has a higher char residue after burning, on the order of 45% by weight. The higher char residue is of value in preventing release to the atmosphere of carbon fibers from carbon fiber-epoxy resin composites in the event of burning of the composite.
Nano-Composites: Relationships Between Nano-Structure and Mechanical Properties: Phase II
2006-01-01
was pre-reacted with the DEGBA resin to give a 40 wt.% CTBN -epoxy adduct: ‘Albipox 1000’ from Hanse Chemie, Geesthacht, Germany. The curing agent was...not lead to a decrease in the modulus of the composite. Nor does it lead to a significant increase in the viscosity of the epoxy resin , which would...preclude the use of low-cost manufacturing routes, such as a vacuum-assisted resin -transfer moulding (VARTM) process. Keywords Epoxy
Temperature rise during polymerization of different cavity liners and composite resins
Karatas, Ozcan; Turel, Verda; Bayindir, Yusuf Ziya
2015-01-01
Objective: The purpose of this study was to evaluate the thermal insulating properties of different light curing cavity liners and composite resins during light emitting diode (LED) curing. Materials and Methods: Sixty-four dentin discs, 1 mm thick and 8 mm in diameter, were prepared. Specimens were divided into four groups. Calcium hydroxide (Ca[OH]2), resin-modified glass ionomer cement, flowable composite and adhesive systems were applied to dentin discs according to the manufacturers’ instructions. The rise in temperature during polymerization with a LED curing unit (LCU) was measured using a K-type thermocouple connected to a data logger. Subsequently, all specimens were randomly divided into one of two groups. A silorane-based composite resin and a methacrylate-based composite resin were applied to the specimens. Temperature rise during polymerization of composite resins with LCU were then measured again. Data were analyzed using one-way ANOVA and post hoc Tukey analyses. Results: There were significant differences in temperature rise among the liners, adhesives, and composite resins (P < 0.05). Silorane-based composite resin exhibited significantly greater temperature rises than methacrylate-based resin (P < 0.05). The smallest temperature rises were observed in Ca(OH)2 specimens. Conclusion: Thermal insulating properties of different restorative materials are important factors in pulp health. Bonding agents alone are not sufficient to protect pulp from thermal stimuli throughout curing. PMID:26751112
Resin cement color stability and its influence on the final shade of all-ceramics.
Kilinc, Evren; Antonson, Sibel A; Hardigan, Patrick C; Kesercioglu, Atilla
2011-07-01
Adhesive resin cements may go through internal discoloration, which may show-through and affect the appearance of translucent all-ceramic restorations. This in vitro study evaluated the amount of resin cement color change and its effect on the final shade of the all-ceramics. Three different resin cements in both light and dual-cure forms were included in the study (Nexus-2/Kerr; Appeal/Ivoclar Vivadent; Calibra/Dentsply). All resin cements contained veneered (IPS Empress Esthetic, ETC1 shade, 20 mm × 1 mm ingot discs) and uncovered groups (n=10/group), all luted on white backgrounds (acetalpolyoxymethylene/Delrin(®)). Curing was performed according to ISO standards with a calibrated LED curing-light (Flashlite 1401). Samples were stored in 37°C distilled water at dark. Spectrophotometric baseline color measurements (Color Eye 7000A) were performed from the samples' top surfaces at 24h (D65 illuminator). Samples were subjected to 65 h of accelerated ageing (Atlas Ci4000). Further color measurements from the same areas were recorded in CIEL*a*b* coordinates where a ΔE data above 3 was accepted as visible discoloration (OptiviewLite-1.9software). Statistical analysis was performed using a nested random effects model and Tukey's post hoc analysis. Light-cure groups showed better color stability in all three resins but only in Appeal resin cement, the dual-cure group discolored significantly more (p<0.001). More discoloration was recorded on uncovered cement groups that represented the exposed cement at the margins. There was no visible color change (ΔE>3) through the ceramic surface on any veneered group. All resin cements showed varying degrees of discoloration after accelerated ageing however their actual color change was partially masked by the ceramic. Dual-cure resin cements may affect aesthetics on restoration margins if directly exposed. Copyright © 2011 Elsevier Ltd. All rights reserved.
Kim, Hyun-Jin; Bagheri, Rafat; Kim, Young Kyung; Son, Jun Sik; Kwon, Tae-Yub
2017-01-01
This study investigated the influence of curing mode (dual- or self-cure) on the surface energy and sorption/solubility of four self-adhesive resin cements (SARCs) and one conventional resin cement. The degree of conversion (DC) and surface energy parameters including degree of hydrophilicity (DH) were determined using Fourier transform infrared spectroscopy and contact angle measurements, respectively (n = 5). Sorption and solubility were assessed by mass gain or loss after storage in distilled water or lactic acid for 60 days (n = 5). A linear regression model was used to correlate between the results (%DC vs. DH and %DC/DH vs. sorption/solubility). For all materials, the dual-curing consistently produced significantly higher %DC values than the self-curing (p < 0.05). Significant negative linear regressions were established between the %DC and DH in both curing modes (p < 0.05). Overall, the SARCs showed higher sorption/solubility values, in particular when immersed in lactic acid, than the conventional resin cement. Linear regression revealed that %DC and DH were negatively and positively correlated with the sorption/solubility values, respectively. Dual-curing of SARCs seems to lower the sorption and/or solubility in comparison with self-curing by increased %DC and occasionally decreased hydrophilicity. PMID:28772489
Efficiency of light curing units in a government dental school.
Nassar, Hani M; Ajaj, Reem; Hasanain, Fatin
2018-01-01
The light intensity of a light-curing unit is a crucial factor that affects the clinical longevity of resin composites. This study aimed to investigate the efficiency of light-curing units in use at a local governmental dental school for curing conventional and bulk-fill resin materials. A total of 166 light-curing units at three locations were examined, and the brand, type, clinic location, diameter of curing tip, tip cleanliness (using a visual score), and the output (in mW/cm 2 using a digital radiometer) were recorded. Only 23.5% of the units examined had clean tips, with the graduate student clinical area containing the highest percentage of clean tips. Further, tips with poor cleanliness score values were associated with significantly lower output intensities. A small percentage (9.4%) of units was capable of producing intensities higher than 1,200 mW/cm 2 and lower than 600 mW/cm 2 (7.6%). The majority of the low intensity units were located in the undergraduate student area, which also contained the highest number of units with intensities between 900 and 1,200 mW/cm 2 . The output of all the units in service was satisfactory for curing conventional resin composites, and most units were capable of curing bulk-fill resin materials.
Resin transfer molding of textile preforms for aircraft structural applications
NASA Technical Reports Server (NTRS)
Hasko, Gregory H.; Dexter, H. Benson; Weideman, Mark H.
1992-01-01
The NASA LaRC is conducting and supporting research to develop cost-effective fabrication methods that are applicable to primary composite aircraft structures. One of the most promising fabrication methods that has evolved is resin transfer molding (RTM) of dry textile material forms. RTM has been used for many years for secondary structures, but has received increased emphasis because it is an excellent method for applying resin to damage-tolerant textile preforms at low cost. Textile preforms based on processes such as weaving, braiding, knitting, stitching, and combinations of these have been shown to offer significant improvements in damage tolerance compared to laminated tape composites. The use of low-cost resins combined with textile preforms could provide a major breakthrough in achieving cost-effective composite aircraft structures. RTM uses resin in its lowest cost form, and storage and spoilage costs are minimal. Near net shape textile preforms are expected to be cost-effective because automated machines can be used to produce the preforms, post-cure operations such as machining and fastening are minimized, and material scrap rate may be reduced in comparison with traditional prepreg molding. The purpose of this paper is to discuss experimental and analytical techniques that are under development at NASA Langley to aid the engineer in developing RTM processes for airframe structural elements. Included are experimental techniques to characterize preform and resin behavior and analytical methods that were developed to predict resin flow and cure kinetics.
Curing kinetics and thermomechanical properties of latent epoxy/carbon fiber composites
NASA Astrophysics Data System (ADS)
Dalle Vacche, S.; Michaud, V.; Demierre, M.; Bourban, P.-E.; Månson, J.-A. E.
2016-07-01
In this work, resins based on diglycidyl ether of bisphenol A (DGEBA) epoxy and a latent hardener, dicyandiamide (DICY), as well as carbon fiber (CF) composites based on them, were prepared with three commercial accelerators: a methylene bis (phenyl dimethyl urea), a cycloaliphatic substituted urea, and a modified polyamine. The curing kinetics of the three DGEBA/DICY/accelerator systems were investigated by chemorheology and differential scanning calorimetry (DSC), in isothermal and over temperature change conditions. Differences in the reaction onset temperature, and in the glass transition temperature (Tg) were highlighted. For curing of thick resin samples, a slow curing cycle at the lowest possible temperature was used, followed by high temperature (160 - 180 °C) post-curing. Indeed, fast curing at higher temperatures caused the formation of hot spots and led to local burning of the samples. The obtained thermomechanical properties, assessed by ultimate tensile testing and dynamic mechanical analysis (DMA) in single cantilever configuration, were all in the expected range for epoxy resins, with tensile moduli close to 3 GPa and Tg > 140 °C. The longterm stability of these resins at room temperature was verified by DSC. Composite samples were prepared by hand lay-up by manually impregnating four layers of 5-harness satin CF textile, and curing in vacuum bag. Impregnation quality and void content were assessed by optical microscopy. The flexural properties of the post-cured composites were assessed by three-point bending test at room temperature and showed no relevant differences, all composites having bending moduli of 45 - 50 GPa. Finally, composites cured with a faster high temperature curing cycle (20 min at 140 °C) were prepared with the DGEBA/DICY/ methylene bis (phenyl dimethyl urea) system, obtaining similar properties as with the slower curing cycle, showing that the prepreg system allowed more flexibility in terms of curing cycle than the bulk resin samples.
Steinhaus, Johannes; Hausnerova, Berenika; Haenel, Thomas; Großgarten, Mandy; Möginger, Bernhard
2014-03-01
During the curing process of light curing dental composites the mobility of molecules and molecule segments is reduced leading to a significant increase of the viscosity as well as the ion viscosity. Thus, the kinetics of the curing behavior of 6 different composites was derived from dielectric analysis (DEA) using especially redesigned flat sensors with interdigit comb electrodes allowing for irradiation at the top side and measuring the ion viscosity at the bottom side. As the ion viscosities of dental composites change 1-3 orders of magnitude during the curing process, DEA provides a sensitive approach to evaluate their curing behavior, especially in the phase of undisturbed chain growth. In order to determine quantitative kinetic parameters a kinetic model is presented and examined for the evaluation of the ion viscosity curves. From the obtained results it is seen that DEA might be employed in the investigation of the primary curing process, the quality assurance of ingredients as well as the control of processing stability of the light curing dental composites. Copyright © 2014 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
NASA Astrophysics Data System (ADS)
Li, Dongna; Li, Xudong; Dai, Jianfeng
2018-06-01
In this paper, two kinds of transient models, the viscoelastic model and the linear elastic model, are established to analyze the curing deformation of the thermosetting resin composites, and are calculated by COMSOL Multiphysics software. The two models consider the complicated coupling between physical and chemical changes during curing process of the composites and the time-variant characteristic of material performance parameters. Subsequently, the two proposed models are implemented respectively in a three-dimensional composite laminate structure, and a simple and convenient method of local coordinate system is used to calculate the development of residual stresses, curing shrinkage and curing deformation for the composite laminate. Researches show that the temperature, degree of curing (DOC) and residual stresses during curing process are consistent with the study in literature, so the curing shrinkage and curing deformation obtained on these basis have a certain referential value. Compared the differences between the two numerical results, it indicates that the residual stress and deformation calculated by the viscoelastic model are more close to the reference value than the linear elastic model.
NASA Technical Reports Server (NTRS)
Kumar, Devendra (Inventor); Fohlen, George M. (Inventor); Parker, John A. (Inventor)
1977-01-01
Aminophenoxy cyclotriphosphazenes such as hexakis (4-aminophenoxy) cyclotriphosphazene and tris (4-aminophenoxy)-tris phenoxy cyclotriphosphazene are used as curing agents for epoxy resins. These 1,2-epoxy resins are selected from di- or polyepoxide containing organic moieties of the formula (CH2-CHO-CH2) m-W-R-W- (CH2CH-CH2O)m where R is diphenyl dimethylmethane, diphenylmethane; W is a nitrogen or oxygen atom; and m is 1 when W is oxygen and 2 when W is nitrogen. The resins are cured thermally in stages at between about 110 to 135 C for between about 1 and 10 min, then at between about 175 to 185 C for between 0.5 to 10 hr and post cured at between about 215 and 235 C for between 0.1 and 2 hr. These resins are useful for making fire resistant elevated temperature stable composites, laminates, molded parts, and adhesives and structures, usually for aircraft secondary structures and for spacecraft construction.
Lopes, Lawrence Gonzaga; Franco, Eduardo Batista; Pereira, José Carlos; Mondelli, Rafael Francisco Lia
2008-01-01
The aim of this study was to evaluate the polymerization shrinkage and shrinkage stress of composites polymerized with a LED and a quartz tungsten halogen (QTH) light sources. The LED was used in a conventional mode (CM) and the QTH was used in both conventional and pulse-delay modes (PD). The composite resins used were Z100, A110, SureFil and Bisfil 2B (chemical-cured). Composite deformation upon polymerization was measured by the strain gauge method. The shrinkage stress was measured by photoelastic analysis. The polymerization shrinkage data were analyzed statistically using two-way ANOVA and Tukey test (p≤0.05), and the stress data were analyzed by one-way ANOVA and Tukey's test (p≤0.05). Shrinkage and stress means of Bisfil 2B were statistically significant lower than those of Z100, A110 and SureFil. In general, the PD mode reduced the contraction and the stress values when compared to CM. LED generated the same stress as QTH in conventional mode. Regardless of the activation mode, SureFil produced lower contraction and stress values than the other light-cured resins. Conversely, Z100 and A110 produced the greatest contraction and stress values. As expected, the chemically cured resin generated lower shrinkage and stress than the light-cured resins. In conclusion, The PD mode effectively decreased contraction stress for Z100 and A110. Development of stress in light-cured resins depended on the shrinkage value. PMID:19089287
Double Vacuum Bag Process for Resin Matrix Composite Manufacturing
NASA Technical Reports Server (NTRS)
Hou, Tan-Hung (Inventor); Jensen, Brian J. (Inventor)
2007-01-01
A double vacuum bag molding assembly with improved void management and laminate net shape control which provides a double vacuum enviromnent for use in fabricating composites from prepregs containing air and/or volatiles such as reactive resin matrix composites or composites from solvent containing prepregs with non-reactive resins matrices. By using two vacuum environments during the curing process, a vacuum can be drawn during a B-stage of a two-step cycle without placing the composite under significant relative pressure. During the final cure stage, a significant pressure can be applied by releasing the vacuum in one of the two environments. Inner and outer bags are useful for creating the two vacuum environments with a perforated tool intermediate the two. The composite is placed intermediate a tool plate and a caul plate in the first environment with the inner bag and tool plate defining the first environment. The second environment is characterized by the outer bag which is placed over the inner bag and the tool plate.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Keeratitham, Waralee, E-mail: waralee.ke@student.chula.ac.th; Somwangthanaroj, Anongnat, E-mail: anongnat.s@chula.ac.th
Herein, our main objective is to prepare the fast curing epoxy system with high glass transition temperature (T{sub g}) by incorporating the multifunctional epoxy resin into the mixture of diglycidyl ether of bisphenol A (DGEBA) as a major epoxy component and aromatic diamine as a hardener. Furthermore, the curing behavior as well as thermal and thermomechanical properties were investigated by differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA) and thermomechanical analysis (TMA). It was found that T{sub g} obtained from tan δ of DGEBA/aromatic diamine system increased from 100 °C to 205 °C with the presence of 30 percentage bymore » weight of multifunctional epoxy resin. Additionally, the isothermal DSC results showed that the multifunctional epoxy resin can accelerate the curing reaction of DGEBA/aromatic diamine system. Namely, a high degree of curing (∼90%) was achieved after a few minutes of curing at low temperature of 130 °C, owing to a large number of epoxy ring of multifunctional epoxy resin towards the active hydrogen atoms of aromatic diamine.« less
Tulunoglu, O; Uçtaşh, M; Alaçam, A; Omürlü, H
2000-01-01
This in vitro study evaluated the effect of dentin bonding agents in reducing microleakage after three months in Class V restorations restored with Z100 resin composite. Materials tested were three types of resin-based dentin bonding agents: a multi-step (Scotchbond Multi-Purpose); a one-step (Scotchbond One-Step); a self-etching, self-priming (Clearfil Liner Bond) and a resin-modified glass ionomer (GC Fuji Bond LC). Class V cavity preparations with occlusal margins in enamel and gingival margins in cementum were prepared both on labial and lingual surfaces of extracted premolar teeth. Restorations (two per tooth) were distributed randomly into nine test groups (n = 10) consisting of the various DBAs applied with co-cure and pre-cure techniques, and no dentin bonding as a negative control group. Samples were stored in saline for three months, thermocycled, stained with silver nitrate, then sectioned through the middle of the preparation to facilitate the removal of the composite resin restoration. For groups treated with the pre-cure technique, the differences between the enamel leakage values of SBMP-control, CFLB-control and SB1S-control subgroups were significant (p < 0.05). For enamel leakage values of groups treated with the co-cure technique, the differences between the SBMP-control, SB1S-control, CFLB-control and Fuji LC-control subgroups were significant (p < 0.05). For cementum leakage values of groups treated with pre-cure technique, the difference between the CFLB-control and the Fuji, SBMP and SB1S groups was significant (p < 0.05). No significant differences could be detected between the cementum leakage values of groups treated with the co-cure technique (p > 0.05). The differences between the values obtained with application of CFLB with the pre-cure and co-cure techniques at the cementum margins were found to be statistically significant (p = 0.02). No statistically significant differences could be detected between the pre-cure and co-cure values of the other test materials. Generally for every group, cementum microleakage values were greater than enamel microleakage values (p < 0.05). The use of Scotchbond Multi-Purpose, Scotchbond One-Step and Fuji Bond LC with the co-cure technique to decrease the application time did not cause any significant increase in microleakage. Only pre-curing using Clearfil Liner Bond provided better microleakage properties than the other pre-cured adhesives.
Cytotoxicity of four categories of dental cements.
Schmid-Schwap, Martina; Franz, Alexander; König, Franz; Bristela, Margit; Lucas, Trevor; Piehslinger, Eva; Watts, David C; Schedle, Andreas
2009-03-01
Assessment of dental material biocompatibility is gaining increasing importance for both patients and dentists. Dental cements may be in contact with oral soft tissues for prolonged periods of time and play an important role in prosthetic rehabilitation. The aim of the present study was to evaluate eight dental cements using a standardized L929-fibroblast cell culture test. For each material, fresh specimens (added to the cultures immediately after preparation) and specimens preincubated for 7 days in cell culture medium were prepared according to the manufacturers' recommendations. After exposure to test specimens, cell numbers were compared to glass controls. The main outcome was a two-sided 95% confidence interval for the mean value of the standardized cell number for each substance investigated. Fresh specimens of all tested cements showed significant cytotoxicity, which diminished after 7 days preincubation. Cytotoxicity of fresh adhesive and self-adhesive resin cements was lower when specimens were dual-cured compared to self-cured. A rank order of cytotoxicity was established based on mean values: Nexus 2 (dual-cured) showed least cytotoxicity, followed by Variolink II (dual-cured), Nexus 2 (self-cured), Harvard, RelyxUnicem (dual-cured), Panavia 21, Fujicem, Durelon, Variolink II (self-cured), RelyxUnicem (self-cured), Maxcem (dual-cured) and Maxcem (self-cured). When bondings were added to Nexus 2 or Variolink II specimens, a slight increase in cytotoxicity was observed. Adhesive resin cements showed less cytotoxicity than self-adhesive and chemically setting cements. Bonding only slightly influenced cytotoxicity of the adhesive resin cements. Dual-cured specimens of adhesive and self-adhesive resin cements showed significantly less toxicity than self-cured specimens.
Exploratory Development of Corrosion Inhibiting Primers
1977-07-01
Phenolic Hardener From previous studies, phenol formaldehyde resins of the novolac (two-step) type have given superior properties when used to cure epoxy...novolacs and three resole (one-step) type phenol- formaldehyde resins which also perform as epoxide curing agents. First, Model #1, as de;crihed in Section...results. Varcum 4326 resin was chosen at this stage for further use with the model systems. It is a low molecular weight phenol- formaldehyde resin used
[Preparation of carbon fiber reinforced fluid type resin denture (author's transl)].
Kasuga, H; Sato, H; Nakabayashi, N
1980-01-01
Transverse strength of cured fluid resins is weaker than that of the heat cured. We have studied to improve the mechanical strength of self-cured acrylic resin by application of carbon fibers as reinforcement and simple methods which must be acceptable for technicians are proposed. A cloth type carbon fiber was the best reinforcement among studied carbon fibers such as chopped or mat. The chopped fibers were difficult to mix homogeneously with fluid resins and effectiveness of the reinforcement was low. Breaking often occurred at the interface between the reinforcement and resin in the cases of mat which gave defects to the test specimens. To prepare reinforced denture, the cloth was trimmed on the master cast after removal of wax and the prepreg was formed with the alginate impression on the cast by Palapress and the cloth. Other steps were same as the usual fluid resin.
Gad, Mohammed M; Al-Thobity, Ahmad M; Shahin, Suliman Y; Alsaqer, Badar T; Ali, Aiman A
2017-01-01
Background Despite drawbacks, cold-cured acrylic resin is still the most common material used in denture repair. Zirconia nanoparticles were among the reinforcements added to increase the strength of the resin. The effect on Candida due to the addition of zirconia nanoparticles to the resin has not been investigated. Purpose The aim of this study was to evaluate the effect of zirconia nanoparticles added to cold-cured acrylic resin on Candida albicans adhesion. Materials and methods A total of 120 acrylic resin specimens with dimensions measuring 22×10×2.5 mm3 were prepared and divided into two equal groups. One group (repair) comprised heat-polymerized specimens that were sectioned at the center and prepared to create a 2 mm repair area that was repaired with cold-cured resin reinforced with 0% wt, 2.5% wt, 5% wt, and 7.5% wt zirconia nanoparticles. The second group contained intact cold-cured acrylic resin specimens reinforced with 0% wt, 2.5% wt, 5% wt, and 7.5% wt zirconia nanoparticles. Specimens were incubated at 37°C in artificial saliva containing C. albicans, and the effect of zirconia nanoparticles on C. albicans was assessed using two methods: 1) a slide count method and 2) a direct culture test. Variations in the number of living Candida were observed in relation to the different concentrations of zirconia nanoparticles. Analysis of variance (ANOVA) and post hoc Tukey’s tests were performed for data analysis. If the P-value was ≤0.05, then the difference was considered as statistically significant. Results It was found that C. albicans adhesion to repaired specimens was significantly decreased by the addition of zirconia nanoparticles (P<0.00001) in comparison with the control group. Intact cold-cured groups and groups repaired with cold-cured resin reinforced with 7.5% wt zirconia nanoparticles showed the lowest Candida count. Tukey’s test showed a significant difference between the repaired group and the intact cold-cured group, while the later demonstrated a lower Candida count. Conclusion The addition of zirconia nanoparticles to cold-cured acrylic resin is an effective method for reducing Candida adhesion to repaired polymethyl methacrylate (PMMA) denture bases and cold-cured removable prosthesis. Clinical significance Based on the results of the current study, zirconia nanoparticles have an antifungal effect, which could be incorporated in the repair material for repairing denture bases and in PMMA removable prostheses as a possible approach for denture stomatitis prevention. PMID:28814859
Gad, Mohammed M; Al-Thobity, Ahmad M; Shahin, Suliman Y; Alsaqer, Badar T; Ali, Aiman A
2017-01-01
Despite drawbacks, cold-cured acrylic resin is still the most common material used in denture repair. Zirconia nanoparticles were among the reinforcements added to increase the strength of the resin. The effect on Candida due to the addition of zirconia nanoparticles to the resin has not been investigated. The aim of this study was to evaluate the effect of zirconia nanoparticles added to cold-cured acrylic resin on Candida albicans adhesion. A total of 120 acrylic resin specimens with dimensions measuring 22×10×2.5 mm 3 were prepared and divided into two equal groups. One group (repair) comprised heat-polymerized specimens that were sectioned at the center and prepared to create a 2 mm repair area that was repaired with cold-cured resin reinforced with 0% wt, 2.5% wt, 5% wt, and 7.5% wt zirconia nanoparticles. The second group contained intact cold-cured acrylic resin specimens reinforced with 0% wt, 2.5% wt, 5% wt, and 7.5% wt zirconia nanoparticles. Specimens were incubated at 37°C in artificial saliva containing C. albicans , and the effect of zirconia nanoparticles on C. albicans was assessed using two methods: 1) a slide count method and 2) a direct culture test. Variations in the number of living Candida were observed in relation to the different concentrations of zirconia nanoparticles. Analysis of variance (ANOVA) and post hoc Tukey's tests were performed for data analysis. If the P -value was ≤0.05, then the difference was considered as statistically significant. It was found that C. albicans adhesion to repaired specimens was significantly decreased by the addition of zirconia nanoparticles ( P <0.00001) in comparison with the control group. Intact cold-cured groups and groups repaired with cold-cured resin reinforced with 7.5% wt zirconia nanoparticles showed the lowest Candida count. Tukey's test showed a significant difference between the repaired group and the intact cold-cured group, while the later demonstrated a lower Candida count. The addition of zirconia nanoparticles to cold-cured acrylic resin is an effective method for reducing Candida adhesion to repaired polymethyl methacrylate (PMMA) denture bases and cold-cured removable prosthesis. Based on the results of the current study, zirconia nanoparticles have an antifungal effect, which could be incorporated in the repair material for repairing denture bases and in PMMA removable prostheses as a possible approach for denture stomatitis prevention.
Out-Life Characteristics of IM7/977-3 Composites
NASA Technical Reports Server (NTRS)
Miller, Sandi G.; Sutter, James K.; Hou, Tan-Hung; Scheiman, Daniel A.; Martin, Richard E.; Maryanski, Michael; Schlea, Michelle; Gardner, John M.; Schiferl, Zack R.
2010-01-01
The capability to manufacture large structures leads to weight savings and reduced risk relative to joining smaller components. However, manufacture of increasingly large composite components is pushing the out-time limits of epoxy/ carbon fiber prepreg. IM7/977-3 is an autoclave processable prepreg material, commonly used in aerospace structures. The out-time limit is reported as 30 days by the manufacturer. The purpose of this work was to evaluate the material processability and composite properties of 977-3 resin and IM7/977-3 prepreg that had been aged at room temperature for up to 60 days. The effects of room temperature aging on the thermal and visco-elastic properties of the materials were investigated. Neat resin was evaluated by differential scanning calorimetry to characterize thermal properties and change in activation energy of cure. Neat resin was also evaluated by rheometry to characterize its processability in composite fabrication. IM7/977-3 prepreg was evaluated by dynamic mechanical analysis to characterize the curing behavior. Prepreg tack was also evaluated over 60 days. The overall test results suggested that IM7/977-3 was a robust material that offered quality laminates throughout this aging process when processed by autoclave.
Egilmez, Ferhan; Ergun, Gulfem; Kaya, Bekir M.
2013-01-01
Objective: The objective of this study was to compare microhardness of resin cements under different thicknesses of zirconia and the light transmittance of zirconia as a function of thickness. Study design: A total of 126 disc-shaped specimens (2 mm in height and 5 mm in diameter) were prepared from dual-cured resin cements (RelyX Unicem, Panavia F and Clearfil SA cement). Photoactivation was performed by using quartz tungsten halogen and light emitting diode light curing units under different thicknesses of zirconia. Then the specimens (n=7/per group) were stored in dry conditions in total dark at 37°C for 24 h. The Vicker’s hardness test was performed on the resin cement layer with a microhardness tester. Statistical significance was determined using multifactorial analysis of variance (ANOVA) (alpha=.05). Light transmittance of different thicknesses of zirconia (0.3, 0.5 and 0.8 mm) was measured using a hand-held radiometer (Demetron, Kerr). Data were analyzed using one-way ANOVA test (alpha=.05). Results: ANOVA revealed that resin cement and light curing unit had significant effects on microhardness (p < 0.001). Additionally, greater zirconia thickness resulted in lower transmittance. There was no correlation between the amount of light transmitted and microhardness of dual-cured resin cements (r = 0.073, p = 0.295). Conclusion: Although different zirconia thicknesses might result in insufficient light transmission, dual-cured resin cements under zirconia restorations could have adequate microhardness. Key words:Zirconia, microhardness, light transmittance, resin cement. PMID:23385497
NASA Astrophysics Data System (ADS)
Park, Sang Yoon; Choi, Chi Hoon; Choi, Won Jong; Hwang, Seong Soon
2018-05-01
The non-autoclave curing technique with vacuum bag only (VBO) prepreg has been conceived as a cost-effective manufacturing method for producing high-quality composite part. This study demonstrated the feasibility of improving composite part's performances and established the effective mitigation strategies for manufacturing induced defects, such as internal voids and surface porosity. The experimental results highlighted the fact that voids and surface porosity were clearly dependent on the resin viscosity state at an intermediate dwell stage of the curing process. Thereafter, the enhancement of resin flow could lead to achieving high quality parts with minimal void content (1.3%) and high fiber fraction (53 vol.%). The mechanical testing showed comparable in-plane shear and compressive strength to conventional autoclave. The microscopic observations also supported the evidence of improved interfacial bonding in terms of excellent fiber wet-out and minimal void content for the optimized cure cycle condition.
Byung-Dae Park; Charles R. Frihart; Yan Yu; Adya P. Singh
2013-01-01
To understand the influence of formaldehyde/urea (F/U) mole ratio on the properties of ureaâformaldehyde (UF) resins, this study investigated hardness of cured UF resins with different F/U mole ratios using a nanoindentation method. The traditional Brinell hardness (HB) method was also used...
Formaldehyde emission and high-temperature stability of cured urea-formaldehyde resins
Shin-ichiro Tohmura; Chung-Yun Hse; Mitsuo Higuchi
2000-01-01
A test method for measuring formaldehyde from urea-formaldehyde (UF) resins at high temperature was developed and used to assess the influence of the reaction pH on the formaldehyde emission and heat stability of the cured resins. Additionally, solid-state 13C CP/MAS nuclear magnetic resonance (NMR) techniques were used to investigate the...
Preparation and characterization of a siloxane containing bismaleimide
NASA Technical Reports Server (NTRS)
Maudgal, S.; St. Clair, T. L.
1984-01-01
A novel siloxane containing bismaleimide has been prepared by reacting maleic anhydride, benzophenonetetracarboxylic dianhydride and bis(gamma-aminopropyl)tetramethyldisiloxane. Characterization of this monomer was done by comparing its nuclear magnetic resonance spectrum (NMR) to those of model compounds. Solubility of the prepolymer was tested in amide, chlorinated and ether solvents. Films were cast from solution as well as by melt processing and a cure cycle was determined. Infrared spectrum (IR) of the resulting film was obtained. Thermal polymerization was investigated by differential scanning calorimetry (DSC). Thermal properties of the cured resin were followed by means of thermogravimetric analysis (TGA), torsional braid analysis (TBA) and dynamic mechanical analysis (DMA). Thermomechanical analysis (TMA) was used to study the effect of postcure on the glass transition temperature (Tg) of the resin. Adhesive strength of the resin was obtained at ambient temperature.
NASA Technical Reports Server (NTRS)
Serafini, T. T.
1982-01-01
The basic chemistry, cure processes, properties, and applications of high temperature resins known as polyimides are surveyed. Condensation aromatic polymides are prepared by reacting aromatic diamines with aromatic dianhydrides, aromatic tetracarboxylic acids, or with dialkyl esters of aromatic tetracarboxylic acids, depending on the intended end use. The first is for coatings or films while the latter two are more suitable for polyimide matrix resins. Prepreg solutions are made by dissolving reactants in an aprotic solvent, and advances in the addition of a diamine on the double bond and radical polymerization of the double bond are noted to have yielded a final cure product with void-free characteristics. Attention is given to properties of the Skybond, Pyralin, and NR-150B polyimide prepreg materials and characteristics of aging in the NP-150 polyimides. Finally, features of the NASA-developed PMR polyimides are reviewed.
Takubo, Chikako; Yasuda, Genta; Murayama, Ryosuke; Ogura, Yukari; Tonegawa, Motoka; Kurokawa, Hiroyasu; Miyazaki, Masashi
2010-08-01
We used ultrasonic measurements to monitor the influence of power density and primer application on the polymerization reaction of dual-cured resin cements. The ultrasonic equipment comprised a pulser-receiver, transducers, and an oscilloscope. Resin cements were mixed and inserted into a transparent mould, and specimens were placed on the sample stage, onto which the primer, if used, was also applied. Power densities of 0 (no irradiation), 200, or 600 mW cm(-2) were used for curing. The transit time through the cement disk was divided by the specimen thickness to obtain the longitudinal sound velocity. When resin cements were light-irradiated, each curve displayed an initial plateau of approximately 1,500 m s(-1), which rapidly increased to a second plateau of 2,300-2,900 m s(-1). The rate of sound velocity increase was retarded when the cements were light-irradiated at lower power densities, and increased when the primer was applied. The polymerization behaviour of dual-cured resin cements was therefore shown to be affected by the power density of the curing unit and the application of self-etching primer. (c) 2010 The Authors. Journal compilation (c) 2010 Eur J Oral Sci.
The Evaluation of Water Sorption/Solubility on Various Acrylic Resins
Tuna, Suleyman Hakan; Keyf, Filiz; Gumus, Hasan Onder; Uzun, Cengiz
2008-01-01
Objectives The absorption of water by acrylic resins is a phenomenon of considerable importance since it is accompanied by dimensional changes, a further undesirable effect of absorbed water in acrylic resins to reduce the tensile strength of the material. Solubility is also an important property because it represents the mass of soluble materials from the polymers. Methods Ten acrylic resin-based materials were evaluated: two heat cure acrylic resins (De Trey QC-20, Meliodent Heat Cure) and eight self cure acrylic resins (Meliodent Cold, Akrileks, Akribel, Akribel Transparent, Vertex Trayplast, Formatray, Dentalon Plus, Palavit G). To evaluate water sorption and water solubility, thirty square-shaped specimens (20×20×1.5 mm) were fabricated from the wax specimens. One way ANOVA test, Tukey test and Pearson correlation coefficient performed for data. Results Water sorption mean values varied from 11.33±0.33 to 30.46±0.55 μg/mm3. Water solubility mean values varied from −0.05±0.23 to 3.69±0.12 μg/mm3. There was statistically significant difference between mean values of the materials (P<.05). There was no linear correlation between sorption and solubility values. Conclusions The results of the water sorption and water solubility values of both self-cured and heat-cured acrylic resins were in accordance with the ISO specification. No correlation found between water sorption and water solubility values. PMID:19212546
Prepreg cure monitoring using diffuse reflectance-FTIR. [Fourier Transform Infrared Technique
NASA Technical Reports Server (NTRS)
Young, P. R.; Chang, A. C.
1984-01-01
An in situ diffuse reflectance-Fourier transform infrared technique was developed to determine infrared spectra of graphite fiber prepregs as they were being cured. A bismaleimide, an epoxy, and addition polyimide matrix resin prepregs were studied. An experimental polyimide adhesive was also examined. Samples were positioned on a small heater at the focal point of diffuse reflectance optics and programmed at 15 F/min while FTIR spectra were being scanned, averaged, and stored. An analysis of the resulting spectra provided basic insights into changes in matrix resin molecular structure which accompanied reactions such as imidization and crosslinking. An endo-exothermal isomerization involving reactive end-caps was confirmed for the addition polyimide prepregs. The results of this study contribute to a fundamental understanding of the processing of composites and adhesives. Such understanding will promote the development of more efficient cure cycles.
Depth of cure of bulk-fill flowable composite resins.
Pedalino, Inaam; Hartup, Grant R; Vandewalle, Kraig S
2015-01-01
In recent years, manufacturers have introduced flowable composite resins that reportedly can be placed in increments of 4 mm or greater. The purpose of this study was to evaluate the depth of cure of bulk-fill flowable composite resins (SureFil SDR Flow, Grandio Flow, and Venus Bulk Fill) and a conventional flowable composite resin (Revolution Formula 2). Depth of cure was measured in terms of bottom-maximum Knoop hardness number (KHN) ratios and the International Organization for Standardization (ISO) 4049 scrape technique. Shades A2 and A3 of SureFil SDR Flow, Grandio Flow, and Revolution Formula 2 were tested. Venus Bulk Fill was tested in its only available shade (universal). Specimens in thicknesses of 2, 3, 4, 5, and 6 mm were polymerized for 20 or 40 seconds, and a hardness tester was used to determine the hardness ratios for each shade at each thickness. For the scraping technique, after specimens were exposed to the curing light, unpolymerized composite resin was removed with a plastic instrument, the polymerized composite was measured, and the length was divided by 2 per ISO guidelines. According to the KHN ratios and the scrape test, Venus Bulk Fill predictably exceeded the manufacturer's claim of a 4-mm depth of cure at both 20 and 40 seconds of curing time. The overall results for depth of cure showed that Venus Bulk Fill ≥ SureFil SDR Flow ≥ Grandio Flow ≥ Revolution Formula 2.
Optimisation des proprietes physiques d'un composite carbone epoxy fabrique par le procede RFI
NASA Astrophysics Data System (ADS)
Koanda, Mahamat Mamadou Lamine
The RFI (Resin Film Infusion) process is a composite materials manufacturing process. Especially known for the small investment it requires, RFI processes are more and more widely used in the aeronautical industry. However a number of aspects of this process are still not well controlled. The quality of the final part depends on which process is used. In the case of RFI, controlling physical characteristics such as thickness, fiber volume fraction or void content remains a major challenge. This dissertation deals with the optimization of the physical properties of a carbon composite manufactured with RFI processes. The ASTMD3171 and ASTMD792 standards were used to measure the void content and fiber volume fraction. First, we introduced different layup sequences in the RFI process and evaluate their impact on the physical properties of the final product. The experiments show the primary mode A, with the resin film at the bottom, resulting in much better quality with controlled fiber volume fraction and void content. Mode B (film in the symmetrical plane) yields results identical to mode A except more irregular thicknesses. Mode C (symmetrical film in the laminate) produces locally unacceptable void contents. Mode D (resin film on the top of the laminate) yields much better results than mode A with the exception of the more irregular thicknesses. Making gaps and overlaps with the resin film has negative effects beyond 2.54
Imide Oligomers Containing Pendent and Terminal Phenylethynyl Groups-2
NASA Technical Reports Server (NTRS)
Connell, J. W.; Smith, J. G., Jr.; Hergenrother, P. M.
1998-01-01
As part of a program to develop high-performance/high-temperature structural resins for aeronautical applications, imide oligomers containing pendent and terminal phenylethynyl groups were prepared, characterized and the cured resins evaluated as composite matrices. The oligomers were prepared at a calculated number-average molecular weight of 5000 g/mol and contained 15-20 mol% pendent phenylethynyl groups. In previous work, an oligomer containing pendent and terminal phenylethynyl groups exhibited a high glass transition temperature (approximately 313 C), and laminates therefrom exhibited high compressive properties, but processability, fracture toughness, microcrack resistance and damage tolerance were less than desired. In an attempt to improve these deficiencies, modifications in the oligomeric backbone involving the incorporation of 1,3-bis(3-aminophenoxy)benzene were investigated as a means of improving processability and toughness without detracting from the high glass transition temperature and high compressive properties. The amide acid oligomeric solutions were prepared in N-methyl-2-pyrrolidinone and were subsequently processed into imide powder, thin films, adhesive tape and carbon fiber prepreg. Neat resin plaques were fabricated from imide powder by compression moulding. The maximum processing pressure was 1.4 MPa and the cure temperature ranged from 350 to 371 C for 1 h for the mouldings, adhesives, films and composites. The properties of the 1,3-bis(3-aniinophenoxy)benzene modified cured imide oligomers containing pendent and terminal phenylethynyl groups are compared with those of previously prepared oligomers containing pendent and terminal phenylethynyl groups of similar composition and molecular weight.
Zhu, Lin-Lin; Qiu, Li-Hong; Liu, Li-Yang; Li, Xiao-Lin
2017-10-01
To determine the effect of the thickness of reinforced glass ceramics on the degree of conversion (DC) of three dual-cure resin cements (Multilink N, RelyX Ultimate and NX3-Nexus). Upcera reinforced glass ceramics and IPS e.max CAD test specimen were processed, with different thickness, transmittance was tested by ultraviolet and visible spectrometer. The DC was evaluated using Fourier transform infrared (FT-IR) spectrometer, then the degree of conversion of polymerization before and after curing was calculated. SPSS 21.0 software package was used for data analysis. Transmittance decreased along with the thickness of reinforced glass ceramics increased. At 2 mm -thickness transmittance of upcera lithium disilicate glass ceramics was superior to IPS e.max CAD. The DC of dual-cured resin cement was decreased with the increase of thickness. At the same 2 mm group, the DC of Multilink N and RelyX Ultimate under upcera lithium disilicate glass ceramics were superior to that under IPS e.max CAD groups. At 2 mm-thickness transmittance of upcera lithium disilicate glass ceramics was superior to IPS e.max CAD. At the same 2 mm group, the DC of Multilink N and RelyX Ultimate under upcera lithium disilicate glass ceramics were superior to that under IPS e.max CAD groups.
Temperature rise in pulpal chamber during fabrication of provisional resinous crowns.
Castelnuovo, J; Tjan, A H
1997-11-01
The heat generated during the exothermic polymerization reaction of autopolymerizing resinous materials and the heat generated by ultraviolet lamps during irradiation of photopolymerizing resinous materials could cause pulpal damage when a direct technique is used to fabricate provisional restorations. This could occur if temperature elevations overcome the physiological heat dissipating mechanisms of the dental-periodontal system. This in vitro study compared the rise in temperatures in the pulpal chamber during fabrication of provisional complete veneer crowns by direct method with different autopolymerizing and photopolymerizing resins. The effect of curing resinous crowns in different matrices, such as a polyvinyl siloxane impression and a vaccuum-formed polypropylene sheet, was also evaluated. The results demonstrated that the amount of heat generated during resin polymerization and transmitted to the pulpal chamber could be damaging to pulpal tissues including odontoblasts. When curing of provisional resinous crowns was performed in the polyvinyl siloxane impression, significantly lower temperatures were recorded compared with curing in the vacuum-formed polypropylene sheet. To prevent pulpal damage, effective cooling procedures are strongly recommended when directly fabricating resinous provisional crowns.
Process Optimization of Bismaleimide (BMI) Resin Infused Carbon Fiber Composite
NASA Technical Reports Server (NTRS)
Ehrlich, Joshua W.; Tate, LaNetra C.; Cox, Sarah B.; Taylor, Brian J.; Wright, M. Clara; Caraccio, Anne J.; Sampson, Jeffery W.
2013-01-01
Bismaleimide (BMI) resins are an attractive new addition to world-wide composite applications. This type of thermosetting polyimide provides several unique characteristics such as excellent physical property retention at elevated temperatures and in wet environments, constant electrical properties over a vast array of temperature settings, and nonflammability properties as well. This makes BMI a popular choice in advance composites and electronics applications [I]. Bismaleimide-2 (BMI-2) resin was used to infuse intermediate modulus 7 (IM7) based carbon fiber. Two panel configurations consisting of 4 plies with [+45deg, 90deg]2 and [0deg]4 orientations were fabricated. For tensile testing, a [90deg]4 configuration was tested by rotating the [0deg]4 configirration to lie orthogonal with the load direction of the test fixture. Curing of the BMI-2/IM7 system utilized an optimal infusion process which focused on the integration of the manufacturer-recommended ramp rates,. hold times, and cure temperatures. Completion of the cure cycle for the BMI-2/IM7 composite yielded a product with multiple surface voids determined through visual and metallographic observation. Although the curing cycle was the same for the three panellayups, the surface voids that remained within the material post-cure were different in abundance, shape, and size. For tensile testing, the [0deg]4 layup had a 19.9% and 21.7% greater average tensile strain performance compared to the [90deg]4 and [+45deg, 90deg, 90deg,-45degg] layups, respectively, at failure. For tensile stress performance, the [0deg]4 layup had a 5.8% and 34.0% greater average performance% than the [90deg]4 and [+45deg, 90deg, 90deg,-45deg] layups.
Changes in degree of conversion and microhardness of dental resin cements.
Yan, Yong Li; Kim, Young Kyung; Kim, Kyo-Han; Kwon, Tae-Yub
2010-01-01
There are few studies available on the post-light activation or post-mix polymerization of dental resin cements as a function of time. This in vitro study evaluated the successive changes in the degree of conversion (DC) and microhardness during polymerization of six commercial resin cements (light-cured [Choice 2, RelyX Veneer], chemical-cured [Multilink, C&B Cement] and dual-cured [Calibra, RelyX ARC]) within the first 24 hours and up to seven days. Resin specimens were prepared for Fourier transform infrared (FTIR) spectroscopy and microhardness testing to determine the DC and Vickers hardness (VH), respectively. The light-cured materials or mixed pastes of the dual-cured materials were irradiated with a light-curing unit (Elipar TriLight) through a precured composite overlay for 40 seconds. The FTIR spectra and microhardness readings were taken at specified times: 1, 2, 5, 10, 15, 30 and 60 minutes; 24 hours and after two days and seven days. According to the FTIR study, most of the curing reaction of Choice 2 and RelyX Veneer occurred within 10 and 30 minutes, respectively. Multilink, C&B Cement and Calibra exhibited gradual increases in the DC up to 24 hours, with no further statistically significant increase (p > 0.05). RelyX ARC attained a DC value within five minutes, similar to that at seven days (p > 0.05). Choice 2 and RelyXARC showed gradual increases in the VH, up to 15 minutes, with no further significant change over the remaining observation time (p > 0.05). For RelyX Veneer, Multilink, C&B Cement and Calibra, there were no significant increases in the VH value after 24 hours (p > 0.05). The light-cured materials produced significantly higher DC values than the chemical-cured materials (p < 0.05). The DC values of the two dual-cured resin cements were significantly different from each other (p < 0.001). The results suggest that the significant polymerization reaction was finished within 24 hours post-mix or post-light activation for all resin cements tested.
Insitu measurement and control of processing properties of composite resins in a production tool
NASA Technical Reports Server (NTRS)
Kranbuehl, D.; Hoff, M.; Haverty, P.; Loos, A.; Freeman, T.
1988-01-01
An in situ measuring technique for use in automated composite processing and quality control is discussed. Frequency dependent electromagnetic sensors are used to measure processing parameters at four ply positions inside a thick section 192-ply graphite-epoxy composite during cure in an 8 x 4 in. autoclave. Viscosity measurements obtained using the sensors are compared with the viscosities calculated using the Loos-Springer cure process model. Good overall agreement is obtained. In a subsequent autoclave run, the output from the four sensors was used to control the autoclave temperature. Using the 'closed loop' sensor controlled autoclave temperature resulted in a more uniform and more rapid cure cycle.
High energy electron beam curing of epoxy resin systems incorporating cationic photoinitiators
Janke, C.J.; Lopata, V.J.; Havens, S.J.; Dorsey, G.F.; Moulton, R.J.
1999-03-02
A mixture of epoxy resins such as a semi-solid triglycidyl ether of tris (hydroxyphenyl) methane and a low viscosity bisphenol A glycidyl ether and a cationic photoinitiator such as a diaryliodonium salt is cured by irradiating with a dosage of electron beams from about 50 to about 150 kGy, forming a cross-linked epoxy resin polymer.
High energy electron beam curing of epoxy resin systems incorporating cationic photoinitiators
Janke, Christopher J.; Lopata, Vincent J.; Havens, Stephen J.; Dorsey, George F.; Moulton, Richard J.
1999-01-01
A mixture of epoxy resins such as a semi-solid triglycidyl ether of tris (hydroxyphenyl) methane and a low viscosity bisphenol A glycidyl ether and a cationic photoinitiator such as a diaryliodonium salt is cured by irradiating with a dosage of electron beams from about 50 to about 150 kGy, forming a cross-linked epoxy resin polymer.
Ognibene, Giulia; Mannino, Salvatore
2018-01-01
Electrospun veils from copolyethersulfones (coPES) were prepared as soluble interlaminar veils for carbon fiber/epoxy composites. Neat, resin samples were impregnated into coPES veils with unmodified resin, while dry carbon fabrics were covered with electrospun veils and then infused with the unmodified epoxy resin to prepare reinforced laminates. The thermoplastic content varied from 10 wt% to 20 wt%. TGAP epoxy monomer showed improved and fast dissolution for all the temperatures tested. The unreinforced samples were cured first at 180 °C for 2 h and then were post-cured at 220 °C for 3 h. These sample showed a high dependence on the curing cycle. Carbon reinforced samples showed significant differences compared to the neat resin samples in terms of both viscoelastic and morphological properties. PMID:29522444
Epoxy hydantoins as matrix resins
NASA Technical Reports Server (NTRS)
Weiss, J.
1983-01-01
Tensile strength and fracture toughness of castings of the hydantoin resins cured with methylenedianiline are significantly higher than MY 720 control castings. Water absorption of an ethyl, amyl hydantoin formulation is 2.1 percent at equilibrium and Tg's are about 160 C, approximately 15 deg below the final cure temperature. Two series of urethane and ester-extended hydantoin epoxy resins were synthesized to determine the effect of crosslink density and functional groups on properties. Castings cured with methylenedianiline or with hexahydrophthalic anhydride were made from these compounds and evaluated. The glass transition temperatures, tensile strengths and moduli, and fracture toughness values were all much lower than that of the simple hydantoin epoxy resins. Using a methylene bishydantoin epoxy with a more rigid structure gave brittle, low-energy fractures, while a more flexible, ethoxy-extended hydantoin epoxy resin gave a very low Tg.
Positioning and aligning CNTs by external magnetic field to assist localised epoxy cure
NASA Astrophysics Data System (ADS)
Ariu, G.; Hamerton, I.; Ivanov, D.
2016-01-01
This work focuses on the generation of conductive networks through the localised alignment of nano fillers, such as multi-walled carbon nanotubes (MWCNTs). The feasibility of alignment and positioning of functionalised MWCNTs by external DC magnetic fields was investigated. The aim of this manipulation is to enhance resin curing through AC induction heating due to hysteresis losses from the nanotubes. Experimental analyses focused on in-depth assessment of the nanotube functionalisation, processing and characterisation of magnetic, rheological and cure kinetics properties of the MWCNT solution. The study has shown that an external magnetic field has great potential for positioning and alignment of CNTs. The study demonstrated potential for creating well-ordered architectures with an unprecedented level of control of network geometry. Magnetic characterisation indicated cobalt-plated nanotubes to be the most suitable candidate for magnetic alignment due to their high magnetic sensitivity. Epoxy/metal-plated CNT nanocomposite systems were validated by thermal analysis as induction heating mediums. The curing process could therefore be optimised by the use of dielectric resins. This study offers a first step towards the proof of concept of this technique as a novel repair technology.
Bunichiro Tomita; Hideaki Osawa; Chung-Yun Hse; George E. Myers
1989-01-01
A nonconventional curing system was developed using a simple mixing of urea-formaldehyde (UF) resins with polyfunctional hydrazide compounds under neutral contition. Several kinds of low molecular-weight dihydrazide compounds were investigated as hardners of the UF resins. Results were as follows: 1) As the minimum gelation times were observed in the range of molar...
Kanie, Takahito; Arikawa, Hiroyuki; Fujii, Koichi; Ban, Seiji
2004-10-01
A newly designed light-cured reinforcement made from urethanemethacrylate oligomer and woven glass cloth has orthotropic anisotropy. This is produced for incorporation into the outermost position under the greatest tension in denture base resins. In this study, the flexural properties of self-, heat-, and light-curing reinforced resins were determined. The silanized glass cloth was soaked in urethanemethacrylate oligomer containing camphorquinone and 2-(dimethylamino)ethylmethacrylate. It was sandwiched between two pieces of polyethylene film and pressed to form a reinforcement sheet 0.3 mm in thickness, which was light-cured and prepared using four different surface conditions: with or without the polyethylene film and with or without a bonding agent. The reinforcement sheet was fixed in a fluorocarbon resin mold 3 mm in thickness, which was filled with self-, heat-, or light-curing resin and cured. The cured laminated plate was cut for flexural testing (40 x 7 x 3 mm3). A three-point flexural test was carried out at a crosshead speed of 2 mm/min and a span length of 30 mm. In this study, the glass fiber content was measured at percentages by weight because it was not possible to determine accurately the volume of the various polymers. The baseline flexural strengths of the self-, heat-, and light-curing resins were 76.2, 68.6, and 55.6 MPa, respectively, and these values were increased to 271.7, 216.4, and 266.5 MPa by the reinforcement sheet. The baseline flexural moduli of self-, heat-, and light-curing resins were 2.0, 2.4, and 2.1 GPa, respectively. These values were increased to 7.2, 5.1, and 6.6 GPa by the reinforcement sheet. SEM photographs revealed good impregnation of the glass fiber within the polymer matrix. The differences in the flexural strengths and flexural moduli of the control and reinforced specimens were significant (p < 0.01).
Performance Properties of Graphite Reinforced Composites with Advanced Resin Matrices
NASA Technical Reports Server (NTRS)
Kourtides, Demetrius A.
1980-01-01
This article looks at the effect of different resin matrices on thermal and mechanical properties of graphite composites, and relates the thermal and flammability properties to the anaerobic char yield of the resins. The processing parameters of graphite composites utilizing graphite fabric and epoxy or other advanced resins as matrices are presented. Thermoset resin matrices studied were: aminecured polyfunctional glycidyl aminetype epoxy (baseline), phenolicnovolac resin based on condensation of dihydroxymethyl-xylene and phenol cured with hexamine, two types of polydismaleimide resins, phenolic resin, and benzyl resin. The thermoplastic matrices studied were polyethersulfone and polyphenylenesulfone. Properties evaluated in the study included anaerobic char yield, limiting oxygen index, smoke evolution, moisture absorption, and mechanical properties at elevated temperatures including tensile, compressive, and short-beam shear strengths. Generally, it was determined that graphite composites with the highest char yield exhibited optimum fire-resistant properties.
40 CFR 63.1179 - For curing ovens, what standards must I meet?
Code of Federal Regulations, 2010 CFR
2010-07-01
... operating limits for each curing oven: (1) Maintain the free-formaldehyde content of each resin lot and the formaldehyde content of each binder formulation at or below the specification ranges of the resin and binder...
40 CFR 63.1179 - For curing ovens, what standards must I meet?
Code of Federal Regulations, 2014 CFR
2014-07-01
... operating limits for each curing oven: (1) Maintain the free-formaldehyde content of each resin lot and the formaldehyde content of each binder formulation at or below the specification ranges of the resin and binder...
2.45 GHz Microwave Processing and Its Influence on Glass Fiber Reinforced Plastics.
Teufl, Daniel; Zaremba, Swen
2018-05-18
During the production of fiber-reinforced composite materials, liquid resin is introduced into the fiber material and cured, i.e., hardened. An elevated temperature is needed for this curing. Microwave curing of composites has been investigated for some time, but it has mostly been done using small domestic or laboratory equipment. However, no investigation has been carried out using an industrial-sized chamber-microwave for glass fiber-reinforced plastic (GFRP). Here, we show that microwave curing produces laminates of the same quality as oven-cured ones. The study shows that, if the process is done right, GFRP samples can be produced with an industrial scale microwave. Even if not fully cured, microwave samples show a glass transition temperature measured with DMA ( T g-DMA ) that is comparable to the T g-DMA according to the proposed cure cycle on the data sheet. Specific microwave-cured configurations show better inter-laminar shear strength than oven specimens. The results show that microwave-based heat introduction can be a beneficial curing method for GFRP laminates. A microwave-optimized process is faster and leads to better mechanical properties.
2.45 GHz Microwave Processing and Its Influence on Glass Fiber Reinforced Plastics
Zaremba, Swen
2018-01-01
During the production of fiber-reinforced composite materials, liquid resin is introduced into the fiber material and cured, i.e., hardened. An elevated temperature is needed for this curing. Microwave curing of composites has been investigated for some time, but it has mostly been done using small domestic or laboratory equipment. However, no investigation has been carried out using an industrial-sized chamber-microwave for glass fiber-reinforced plastic (GFRP). Here, we show that microwave curing produces laminates of the same quality as oven-cured ones. The study shows that, if the process is done right, GFRP samples can be produced with an industrial scale microwave. Even if not fully cured, microwave samples show a glass transition temperature measured with DMA (Tg-DMA) that is comparable to the Tg-DMA according to the proposed cure cycle on the data sheet. Specific microwave-cured configurations show better inter-laminar shear strength than oven specimens. The results show that microwave-based heat introduction can be a beneficial curing method for GFRP laminates. A microwave-optimized process is faster and leads to better mechanical properties. PMID:29783684
Modeling the curing process of thick-section autoclave cured composites
NASA Technical Reports Server (NTRS)
Loos, A. C.; Dara, P. H.
1985-01-01
Temperature gradients are significant during cure of large area, thick-section composites. Such temperature gradients result in nonuniformly cured parts with high void contents, poor ply compaction, and variations in the fiber/resin distribution. A model was developed to determine the temperature distribution in thick-section autoclave cured composites. Using the model, long with temperature measurements obtained from the thick-section composites, the effects of various processing parameters on the thermal response of the composites were examined. A one-dimensional heat transfer model was constructed for the composite-tool assembly. The governing differential equations and associated boundary conditions describing one-dimensional unsteady heat-conduction in the composite, tool plate, and pressure plate are given. Solution of the thermal model was obtained using an implicit finite difference technique.
França, Flávio Álvares; Oliveira, Michele de; Rodrigues, José Augusto; Arrais, César Augusto Galvão
2011-01-01
This study evaluated the degree of conversion (DC) and ultimate tensile strength (UTS) of dual-cured resin cements heated to 50º C prior to and during polymerization. Disc- and hourglass-shaped specimens of Rely X ARC (RX) and Variolink II (VII) were obtained using addition silicon molds. The products were manipulated at 25º C or 50º C and were subjected to 3 curing conditions: light-activation through a glass slide or through a pre-cured 2-mm thick resin composite disc, or they were allowed to self-cure (SC). All specimens were dark-stored dry for 15 days. For DC analysis, the resin cements were placed into the mold located on the center of a horizontal diamond on the attenuated total reflectance element in the optical bench of a Fourier Transformed Infrared spectrometer. Infrared spectra (n = 6) were collected between 1680 and 1500 cm-1, and DC was calculated by standard methods using changes in ratios of aliphatic-to-aromatic C=C absorption peaks from uncured and cured states. For UTS test, specimens (n = 10) were tested in tension in a universal testing machine (crosshead speed of 1 mm/min) until failure. DC and UTS data were submitted to 2-way ANOVA, followed by Tukey's test (α= 5%). Both products showed higher DC at 50º C than at 25º C in all curing conditions. No significant difference in UTS was noted between most light-activated groups at 25º C and those at 50º C. VII SC groups showed higher UTS at 50º C than at 25º C (p < 0.05). Increased temperature led to higher DC, but its effects on resin cement UTS depended on the curing condition.
Simulation Based Low-Cost Composite Process Development at the US Air Force Research Laboratory
NASA Technical Reports Server (NTRS)
Rice, Brian P.; Lee, C. William; Curliss, David B.
2003-01-01
Low-cost composite research in the US Air Force Research Laboratory, Materials and Manufacturing Directorate, Organic Matrix Composites Branch has focused on the theme of affordable performance. Practically, this means that we use a very broad view when considering the affordability of composites. Factors such as material costs, labor costs, recurring and nonrecurring manufacturing costs are balanced against performance to arrive at the relative affordability vs. performance measure of merit. The research efforts discussed here are two projects focused on affordable processing of composites. The first topic is the use of a neural network scheme to model cure reaction kinetics, then utilize the kinetics coupled with simple heat transport models to predict, in real-time, future exotherms and control them. The neural network scheme is demonstrated to be very robust and a much more efficient method that mechanistic cure modeling approach. This enables very practical low-cost processing of thick composite parts. The second project is liquid composite molding (LCM) process simulation. LCM processing of large 3D integrated composite parts has been demonstrated to be a very cost effective way to produce large integrated aerospace components specific examples of LCM processes are resin transfer molding (RTM), vacuum assisted resin transfer molding (VARTM), and other similar approaches. LCM process simulation is a critical part of developing an LCM process approach. Flow simulation enables the development of the most robust approach to introducing resin into complex preforms. Furthermore, LCM simulation can be used in conjunction with flow front sensors to control the LCM process in real-time to account for preform or resin variability.
Exploration Of `Click' Chemistry For Microelectronic Applications
NASA Astrophysics Data System (ADS)
Musa, Osama M.; Sridhar, Laxmisha M.
The ‘Click’ chemistry was explored for low temperature snap cure and for possible use as an adhesion promoter in electronic applications. Several azide and alkyne resins were synthesized and their curing potential was evaluated with a special emphasis on exploring Cu(I) catalyst effect. The preliminary curing study in the absence of catalysts showed a strong dependence of cure temperatures on the electronic nature of alkynes. The cure temperatures showed a tendency to increase with decreasing electronegativity of the substituent on alkynes. The capability of Cu(I) catalysts to accelerate the ‘Click’ chemistry was demonstrated for the first time in bulk phase. Using several Cu(I) catalysts, the cure temperatures could be lowered by as much as 40-100°C compared to the control, depending on the nature of catalyst and the catalyst loading. We discovered a novel synergistic effect between Cu(I) and silver filler in lowering the cure temperatures. Using this combination, lower cure temperatures could be obtained than using either alone. Among several resins screened, one resin system has shown promise for 80°C snap-cure in which the aforementioned synergistic effect is operative. Solution phase ‘Click’ chemistry was employed for the synthesis of a hybrid triazole-epoxy resin system. This system was found to cure without added amine curative. The triazole group here serves as a linker as well as an internal adhesion promoter. To address the incompatibility and volatility issues, which arose during evaluation, a controlled oligomerization method has been developed using controlled heating of azides and alkynes in solution phase.
Low cost tooling material and process for graphite and Kevlar composites
NASA Technical Reports Server (NTRS)
Childs, William I.
1987-01-01
An Extruded Sheet Tooling Compound (ESTC) was developed for use in quickly building low cost molds for fabricating composites. The ESTC is a very highly mineral-filled resin system formed into a 6 mm thick sheet. The sheet is laid on the pattern, vacuum (bag) is applied to remove air from the pattern surface, and the assembly is heat cured. The formed ESTC is then backed and/or framed and ready for use. The cured ESTC exhibits low coefficient of thermal expansion and maintains strength at temperatures of 180 to 200 C. Tools were made and used successfully for: Compression molding of high strength epoxy sheet molding compound, stamping of aluminum, resin transfer molding of polyester, and liquid resin molding of polyester. Several variations of ESTC can be made for specific requirements. Higher thermal conductivity can be achieved by using an aluminum particle filler. Room temperature gel is possible to allow use of foam patterns.
Heat resistant composite structure for shuttle applications (Ryton-B)
NASA Technical Reports Server (NTRS)
1972-01-01
A program was undertaken to characterize Ryton-B resin, develop graphite filament prepregs, undirectional laminates and determine the strength and heat resistance of the composite system. Through the use of a water soluble resin binder, high quality prepreg tape, three inches wide with 4 tows of HM-S were produced. The tape laminated to 0.00175 inch per ply. A wide range of properties in the cured resin and laminate were found using different curing conditions. The thermal stability and strength of molded laminates appears to be very dependent upon the cure cycle used for polymerization.
Use of 2,5-dimethyl-2,5-hexane diamine as a curing agent for epoxy resins
Rinde, J.A.; Newey, H.A.
1981-02-24
Primary diamines are disclosed of the formula shown in a diagram wherein R is a straight chain saturated hydrocarbon of 2 to 4 carbons, a disubstituted benzene ring, or disubstituted dibenzomethane for use as a curing agent for epoxy resins. These curing agents can be used to form epoxy resin mixtures useful in filament winding and pre-impregnated fiber molding and in formulating film adhesives, powder coatings and molding powders. The epoxy mixtures form for such uses as room temperature non-reacting, intermediate stable state which has a latent cross-linking capability.
Use of 2,5-dimethyl-2,5-hexane diamine as a curing agent for epoxy resins
Rinde, James A. [Livermore, CA; Newey, Herbert A. [Lafayette, CA
1981-02-24
Primary diamines of the formula ##STR1## wherein R is a straight chain saturated hydrocarbon of 2 to 4 carbons, a disubstituted benzene ring, or disubstituted dibenzo methane for use as a curing agent for epoxy resins. These curing agents can be used to form epoxy resin mixtures useful in filament winding and pre-impregnated fiber molding and in formulating film adhesives, powder coatings and molding powders. The epoxy mixtures form for such uses as room temperature non-reacting, intermediate stable state which has a latent cross-linking capability.
Effect of light-curing units, post-cured time and shade of resin cement on knoop hardness.
Reges, Rogério Vieira; Costa, Ana Rosa; Correr, Américo Bortolazzo; Piva, Evandro; Puppin-Rontani, Regina Maria; Sinhoreti, Mário Alexandre Coelho; Correr-Sobrinho, Lourenço
2009-01-01
The aim of this study was to evaluate the Knoop hardness after 15 min and 24 h of different shades of a dual-cured resin-based cement after indirect photoactivation (ceramic restoration) with 2 light-curing units (LCUs). The resin cement Variolink II (Ivoclar Vivadent) shade XL, A2, A3 and opaque were mixed with the catalyst paste and inserted into a black Teflon mold (5 mm diameter x 1 mm high). A transparent strip was placed over the mold and a ceramic disc (Duceram Plus, shade A3) was positioned over the resin cement. Light-activation was performed through the ceramic for 40 s using quartz-tungsten-halogen (QTH) (XL 2500; 3M ESPE) or light-emitting diode (LED) (Ultrablue Is, DMC) LCUs with power density of 615 and 610 mW/cm(2), respectively. The Koop hardness was measured using a microhardness tester HMV 2 (Shimadzu) after 15 min or 24 h. Four indentations were made in each specimen. Data were subjected to ANOVA and Tukey's test (alpha=0.05). The QTH LCU provided significantly higher (p<0.05) KHN values than the LED LCU. When the post-cure times were compared for the same shade, QTH and LED at 24 h provided significantly higher (p<0.05) KHN values than at 15 min. It may be concluded that the Knoop hardness was generally dependent on the LCU and post-cure time. The opaque shade of the resin cement showed lower Knoop hardness than the other shades for both LCUs and post-cure times.
Thermoplastic composite matrices with improved solvent resistance
NASA Technical Reports Server (NTRS)
Hergenrother, P. M.; Jensen, B. J.; Havens, S. J.
1984-01-01
In order to improve solvent resistance of aromatic thermoplastic polymers, ethynyl-terminated aromatic sulfone polymers (ETS), sulfone/ester polymers (SEPE) containing pendent ethynyl groups, and phenoxy resin containing pendent ethynyl groups are synthesized. Cured polysulfones and phenoxy resins containing ethynyl groups on the ends or pendent on the molecules exhibited systematic behavior in solvent resistance, film flexibility, and toughness as a function of crosslink density. The film and composite properties of a cured solvent-resistant ETS were better than those of a commercially available solvent sensitive polysulfone. The study was part of a NASA program to better understand the trade-offs between solvent resistance, processability and mechanical properties which may be useful in designing composite structures for aerospace vehicles.
Validation of the filament winding process model
NASA Technical Reports Server (NTRS)
Calius, Emilo P.; Springer, George S.; Wilson, Brian A.; Hanson, R. Scott
1987-01-01
Tests were performed toward validating the WIND model developed previously for simulating the filament winding of composite cylinders. In these tests two 24 in. long, 8 in. diam and 0.285 in. thick cylinders, made of IM-6G fibers and HBRF-55 resin, were wound at + or - 45 deg angle on steel mandrels. The temperatures on the inner and outer surfaces and inside the composite cylinders were recorded during oven cure. The temperatures inside the cylinders were also calculated by the WIND model. The measured and calculated temperatures were then compared. In addition, the degree of cure and resin viscosity distributions inside the cylinders were calculated for the conditions which existed in the tests.
Effect of light dispersion of LED curing lights on resin composite polymerization.
Vandewalle, Kraig S; Roberts, Howard W; Andrus, Jeffrey L; Dunn, William J
2005-01-01
This study evaluated the effect of light dispersion of halogen and LED curing lights on resin composite polymerization. One halogen (Optilux 501, SDS/Kerr, Orange, CA, USA) and five light-emitting diode (LED) curing lights (SmartLite iQ, Dentsply Caulk, Milford, DE, USA; LEDemetron 1, SDS/Kerr; FLASHlite 1001, Discus Dental, Culver City, CA, USA; UltraLume LED 5, Ultradent Products, South Jordan, UT, USA; Allegro, Den-Mat, Santa Maria, CA, USA) were used in this study. Specimens (8 mm diameter by 2 mm thick) were made in polytetrafluoroethylene molds using hybrid (Z100, 3M ESPE, St. Paul, MN, USA) and microfill (A110, 3M ESPE) composite resins. The top surface was polymerized for 5 seconds with the curing light guide tip positioned at a distance of 1 and 5 mm. Degree of conversion (DC) of the composite specimens was analyzed on the bottom surface using micro-Fourier Transform Infrared (FTIR) spectroscopy (Perkin-Elmer FTIR Spectrometer, Wellesley, PA, USA) 10 minutes after light activation. DC at the bottom of the 2 mm specimen was expressed as a percentage of the mean maximum DC. Five specimens were created per curing light and composite type (n=5). Percent mean DC ratios and SDs were calculated for each light under each testing condition. Data were analyzed by analysis of variance (ANOVA)/Tukey's test (alpha = .05). A beam analyzer (LBA-700, Spiricon, Logan, UT, USA) was used to record the emitted light from the curing lights at 0 and 5 mm distances (n=5). A Top Hat factor was used to compare the quality of the emitted beam profile (LBA/PC, Spiricon). The divergence angle from vertical was also determined in the x- and y-axes (LBA/PC). Mean values and SDs were calculated for each light under each testing condition (0 and 5 mm, x- and y-axes) and analyzed by a two-way ANOVA/Tukey's test (alpha = .05). For DC ratios, significant differences were found based on curing light and curing distance (p < .05). At 1 mm, Optilux 501 and FLASHlite 1001 produced significantly higher DC ratios with the hybrid resin composite. No differences were found among lights with the microfill at 1 mm. At 5 mm, SmartLite iQ, FLASHlite 1001, LEDemetron 1, and UltraLume LED 5 produced significantly higher DC ratios with the hybrid resin composite, whereas LEDemetron 1 and SmartLite iQ produced significantly higher DC ratios with the microfill resin composite. The UltraLume LED 5, Allegro, and Optilux 501 had significant reductions in mean DC ratios at curing distances of 1 and 5 mm with both resin composite types. For dispersion of light, significant differences were found in Top Hat factor and divergence angle (p < .001). SmartLite iQ had overall the highest Top Hat factor and lowest divergence angle of tested lights. A linear regression analysis relating pooled DC with pooled Top Hat factors and divergence angles found a very good correlation (r2 = .86) between dispersion of light over distance and the ability to polymerize resin composite. The latest generation of LED curing lights provides DC ratios similar to or better than the halogen curing light at a curing distance of 5 mm. Dispersion of light plays a significant role in the DC of resin composite. To maximize curing effectiveness, light guides should be maintained in close proximity to the surface of the light-activated restorative material.
Nezu, Takashi; Nagano-Takebe, Futami; Endo, Kazuhiko
2017-09-26
Antimicrobial cetylpyridinium chloride (CPC) has low miscibility with acrylic resin monomer but can be homogeneously mixed using ethanol as a cosolvent. This study investigated the effects of ethanol addition on the properties of a cold-cure acrylic resin. Ethanol was an excellent cosolvent for CPC and methyl methacrylate monomer (MMA), but the cured resin exhibited a strong change in coloration to yellow (ΔE* ab >8) and a drastically reduced bending strength (from 97 to 25 MPa) and elastic modulus (from 2.7 to 0.6 GPa) when equal volumes of ethanol and monomer were used together, possibly due to the solvation and deactivation of radicals by ethanol. However, these unfavorable effects diminished when the ethanol/MMA ratio was reduced to 0.25, and became smaller when each specimen was depressurized and excess ethanol was removed. Thus, it may be possible to develop a molecularly uniform antibacterial acrylic resin with acceptable color and strength using this simple technique.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Li, Yang; Zhao, Qiangsheng; Mirdamadi, Mansour
Woven fabric carbon fiber/epoxy composites made through compression molding are one of the promising choices of material for the vehicle light-weighting strategy. Previous studies have shown that the processing conditions can have substantial influence on the performance of this type of the material. Therefore the optimization of the compression molding process is of great importance to the manufacturing practice. An efficient way to achieve the optimized design of this process would be through conducting finite element (FE) simulations of compression molding for woven fabric carbon fiber/epoxy composites. However, performing such simulation remains a challenging task for FE as multiple typesmore » of physics are involved during the compression molding process, including the epoxy resin curing and the complex mechanical behavior of woven fabric structure. In the present study, the FE simulation of the compression molding process of resin based woven fabric composites at continuum level is conducted, which is enabled by the implementation of an integrated material modeling methodology in LS-Dyna. Specifically, the chemo-thermo-mechanical problem of compression molding is solved through the coupling of three material models, i.e., one thermal model for temperature history in the resin, one mechanical model to update the curing-dependent properties of the resin and another mechanical model to simulate the behavior of the woven fabric composites. Preliminary simulations of the carbon fiber/epoxy woven fabric composites in LS-Dyna are presented as a demonstration, while validations and models with real part geometry are planned in the future work.« less
Graphite polystyryl pyridine (PSP) structural composites
NASA Technical Reports Server (NTRS)
Malassine, B.
1981-01-01
PSP6022 M resin, PSP 6024 M resin and W 133 Thormel T 300 graphite fabric reinforced panels were fabricated and provided to NASA Ames Research Center. PSP6022 and PSP6024 characteristics, process specifications for the fabriation of prepregs and of laminates are detailed. Mechanical properties, thermomechanical properties and moisture resistance were evaluated. PSP6022 and PSP6024 appear as high performance thermostable systems, very easy to process, being soluble in MEK for prepregging and being cured at no more than 250C, and even 200C.
Health Problems of Epoxy Resins and Amine-curing Agents
Bourne, L. B.; Milner, F. J. M.; Alberman, K. B.
1959-01-01
Epoxy resins were first introduced about 10 years ago. Toxic effects, particularly dermatitis, have been frequently described. An investigation into the possible causes of pathological sequelae following the use of epoxy resin/amine mixtures has been undertaken. The cause of most cases of dermatitis and sensitization appears to be uncombined amine which is present in recent mixtures and persists in hardened resin for long periods. The results of experiments with two of the most commonly used resin/amine mixtures confirm this. Cold-cured resins are more dangerous and remain so even when hardened. A simple theory is suggested for the mechanism of the reaction between epoxy resins, amines, and biological systems. This theory leads logically to the handling precautions outlined. Images PMID:13651551
NASA Technical Reports Server (NTRS)
Kranbuehl, D. E.; Delos, S. E.; Hoff, M. S.; Weller, L. W.; Haverty, P. D.
1987-01-01
An in situ NDE dielectric impedance measurement method has been developed for ascertaining the cure processing properties of high temperature advanced thermoplastic and thermosetting resins, using continuous frequency-dependent measurements and analyses of complex permittivity over 9 orders of magnitude and 6 decades of frequency at temperatures up to 400 C. Both ionic and Debye-like dipolar relaxation processes are monitored. Attention is given to LARC-TPI, PEEK, and poly(arylene ether) resins' viscosity, glass transition temperature, recrystallization, and residual solvent content and evolution properties.
Characterization-curing-property studies of HBRF 55A resin formulations
NASA Technical Reports Server (NTRS)
Pearce, E. M.; Mijovic, J.
1985-01-01
Characterization curing property investigations on HBRF 55A resin formulations are reported. The initial studies on as received cured samples cut from a full-size FWC are reviewed. Inadequacies of as-received and aged samples are pointed out and additional electron microscopic evidence is offered. Characterization of as-received ingredients of HBRF 55A formulation is described. Specifically, Epon 826, Epon 828, EpiRez 5022, RD-2 and various amines, including Tonox and Tonox 60.40, were characterized. Cure kinetics of various formulations are investigated. Changes in physical/thermal properties (viscosity, specific heat, thermal conductivity and density) during cure are described.
Lombardini, Marco; Chiesa, Marco; Scribante, Andrea; Colombo, Marco; Poggio, Claudio
2012-11-01
Adequate polymerization of resin composites could be considered as a crucial factor in obtaining good clinical performance, particularly in stress-bearing areas. An insufficient curing degree affects the resin composite's chemical properties The current in vitro study evaluated the influence of polymerization time and depth of cure of six commercial resin composites by Vickers microhardness (VK). SIX RESIN COMPOSITES WERE SELECTED: Three microhybrid (Esthet.X HD, Amaris, Filtek Silorane), two nanohybrid (Grandio, Ceram.X mono), and one nanofilled (Filtek Supreme XT). The VK of the surface was determined by a microhardness tester using a Vickers diamond indenter and a 200 g load applied for 15 s. The bottom to top mean VK ratio was calculated using the formula: Hardness ratio = VK of bottom surface/VK of top surface. Vickers hardness values of test materials during exposure time of 20 and 40 s and depths of cure of 2 and 3 mm were determined and compared. Data were analyzed using analysis of variance (ANOVA) test. For all the tested materials and with all the exposure time periods, hardness ratio was higher than the minimum value indicated in literature (0.8). Exposure time and depth of cure did not affect hardness ratio values for Filtek Silorane, Grandio, and Filtek Supreme XT. Among the materials tested, the nanofilled and the nanohybrid resin composites were rather insensible to thickness variations. Miicrohybrid composites, instead, had features different from one another.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Paulauskas, F.L.; Meek, T.T.
Studies of microwave-assisted curing of neat resins (epoxy) and unidirectional glass and carbon fiber laminates have shown that a substantial reduction in the curing time was obtained. This may be explained by the penetration of microwave energy directly and throughout the laminate with enhancement of the kinetics of the chemical reaction. Results of this work indicate that the microwave assisted curing of glass fiber laminates also shows a substantial reduction of the required curing time. Microwave radiation of 2.45 GHz has been demonstrated to be an acceptable method to cure unidirectional carbon fiber laminates. Also, effective curing of crossply (0/90)more » laminates through this method was observed when proper rotation of the parts accompanied the curing process. This is in accordance with previous work. Multidirectional carbon fiber/epoxy laminates demonstrate a lack of coupling during the curing process. A direct curing of these laminates was not possible by microwave radiation with the experimental approach used, in agreement with previous work. Nevertheless, a moderate reduction in the curing time of these thin laminates was observed due to hybrid curing.« less
Wang, Lijun; Zhang, Chun; Gong, Wei; Ji, Yubi; Qin, Shuhao; He, Li
2018-01-01
3D cross-linking networks are generated through chemical reactions between thermosetting epoxy resin and hardener during curing. The curing degree of epoxy material can be increased by increasing curing temperature and/or time. The epoxy material must then be fully cured through a postcuring process to optimize its material characteristics. Here, a limited-foaming method is introduced for the preparation of microcellular epoxy foams (Lim-foams) with improved cell morphology, high thermal expansion coefficient, and good compressive properties. Lim-foams exhibit a lower glass transition temperature (T g ) and curing degree than epoxy foams fabricated through free-foaming process (Fre-foams). Surprisingly, however, the T g of Lim-foams is unaffected by postcuring temperature and time. This phenomenon, which is related to high gas pressure in the bubbles, contradicts that indicated by the time-temperature-transformation cure diagram. High bubble pressure promotes the movement of molecular chains under heating at low temperature and simultaneously suppresses the etherification cross-linking reaction during post-curing. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
Process for the manufacture of low density bis-maleimide-carbon microballoon composites
NASA Technical Reports Server (NTRS)
Kourtides, Demetrius A. (Inventor); Parker, John A. (Inventor)
1980-01-01
A process for the preparation of composite laminate structures of glass cloth preimpregnated with polybismaleimide resin and adhered to a polybismaleimide-glass or aromatic polyamide paper honeycomb cell structure filled or partially filled with a syntactic foam consisting of a mixture of bismaleimide resin and carbon microballoons. The carbon microballoons are prepared by pyrolyzing phenolic microballoons and subsequently bonded using a 2% bismaleimide solution. The laminate structures are cured for two hours at 477.degree. K. and are adhered to the honeycomb bismaleimide adhesive using a pressure of 700 kN/m.sup.2 pressure at 450.degree. K. The laminate composite is then post-cured for two hours at 527.degree. K. to produce a composite laminate having a density in the range from about 95 kilograms per cubic meter to 130 kilograms per cubic meter.
Studies on Hot-Melt Prepregging on PRM-II-50 Polyimide Resin with Graphite Fibers
NASA Technical Reports Server (NTRS)
Shin, E. Eugene; Sutter, James K.; Juhas, John; Veverka, Adrienne; Klans, Ojars; Inghram, Linda; Scheiman, Dan; Papadopoulos, Demetrios; Zoha, John; Bubnick, Jim
2004-01-01
A second generation PMR (in situ Polymerization of Monomer Reactants) polyimide resin PMR-II-50, has been considered for high temperature and high stiffness space propulsion composites applications for its improved high temperature performance. As part of composite processing optimization, two commercial prepregging methods: solution vs. hot-melt processes were investigated with M40J fabrics from Toray. In a previous study a systematic chemical, physical, thermal and mechanical characterization of these composites indicated the poor resin-fiber interfacial wetting, especially for the hot-melt process, resulted in poor composite quality. In order to improve the interfacial wetting, optimization of the resin viscosity and process variables were attempted in a commercial hot-melt prepregging line. In addition to presenting the results from the prepreg quality optimization trials, the combined effects of the prepregging method and two different composite cure methods, i.e. hot press vs. autoclave on composite quality and properties are discussed.
Studies on Hot-Melt Prepregging of PMR-II-50 Polyimide Resin with Graphite Fibers
NASA Technical Reports Server (NTRS)
Shin, E. Eugene; Sutter, James K.; Juhas, John; Veverka, Adrienne; Klans, Ojars; Inghram, Linda; Scheiman, Dan; Papadopoulos, Demetrios; Zoha, John; Bubnick, Jim
2003-01-01
A Second generation PMR (in situ Polymerization of Monomer Reactants) polyimide resin, PMR-II-50, has been considered for high temperature and high stiffness space propulsion composites applications for its improved high temperature performance. As part of composite processing optimization, two commercial prepregging methods: solution vs. hot-melt processes were investigated with M40J fabrics from Toray. In a previous study a systematic chemical, physical, thermal and mechanical characterization of these composites indicated that poor resin-fiber interfacial wetting, especially for the hot-melt process, resulted in poor composite quality. In order to improve the interfacial wetting, optimization of the resin viscosity and process variables were attempted in a commercial hot-melt prepregging line. In addition to presenting the results from the prepreg quality optimization trials, the combined effects of the prepregging method and two different composite cure methods, i.e., hot press vs. autoclave on composite quality and properties are discussed.
NASA Technical Reports Server (NTRS)
Alston, William B.
1992-01-01
Relationships are identified between the thermo-oxidative stability (TOS) at 316 C of a wide variety of PMR (polymerization of monomeric reactants) addition cured polyimide resins and their corresponding graphite fiber composites. Weight loss results at 316 C confirmed the expected relationship of increasing aliphatic endcap content with decreasing TOS. Moreover, the resin TOS study also showed an unexpected linear correlation of decreasing weight loss to increasing ratio of benzylic diamine to aliphatic endcap in the range of the stoichiometries studied. Only after long term 316 C aging does the dianhydride used with the benzylic diamines become an additional factor in influencing the amount of PMR resin and composite weight losses. Also, the benzylic systems consistently showed much lower resin and composite weight losses at 316 C than the corresponding nonbenzylic norbornenyl resins and composites, except when the nonbenzylic diamine monomer does not contain a connecting group. Instead, this diamine resulted in a 316 C resin and composite weight loss that was only competitive with benzylic type diamines. Results show excellent correlation between TOS of all graphite fiber PMR composites and resins.
Control and reduction of peak temperature in self-curing resins.
Schiavetti, R; DE Vico, G; Casucci, A; Covello, F; Ottria, L; Sannino, G; Barlattani, A
2009-07-01
INTRODUCTION.: The aim of this experimental study was to reduce the exothermic reaction during curing of the resins to cold. The significant exotherm generated by the reaction of polymerization of the resin curing involves many clinical complications including the high risk of necrosis against tooth. MATERIAL AND METHODS.: They were used four different types of self curing resins all based on methyl methacrylate, Jet Kit, Major Dentin, Dura Lay, Temporary Cold. The reaction of polymerization of the resins was done in Teflon pans and was monitored by a thermocouple which recorded the highest level reached by each temperature resin with and without additive. The polymerization reaction took place for each resin in the presence of an essential oil, the terpinolene, which acted as a "chain transfer" and different temperatures were recorded. RESULTS.: Resins Dura Lay and Jet kit showed a reduction of very high temperature in the presence of terpinolene, with a statistically significant difference compared to the same reaction without terpinolene Major resin dentin in the presence of the additive has reduced by 8.4°C peak temperature. Resin Temporary Cold has showed benefits with respect to peak temperature, but the reaction was much more 'consistent presence of the additive. DISCUSSION.: The system through which the chain transfer acts to lower the temperature of the reaction is that of chain transfer. Namely that interfere with the reaction of the polymer chains, by transferring these acrylic radicals are no longer active, ie, no longer able to bind to other monomer units, thus avoiding the excessive growth of macromolecules which are those that determine the temperature rise. This leads to the formation of more polymer chains with lower molecular weight.
Cure Chemistry of Phenylethynyl Terminated Oligomers
NASA Technical Reports Server (NTRS)
Wood, Karen H.; Orwoll, Robert A.; Young, Philip R.; Jensen, Brian J.; McNair, Harold M.
1997-01-01
The ability to process high performance polymers into quality, void-free composites has been significantly advanced using oligomers terminated with reactive groups which cure or crosslink at elevated temperature without the evolution of volatile byproducts. Several matrix resin systems of considerable interest to the aerospace community utilize phenylethynyl-terminated imide (PETI) technology to achieve this advantage. The present paper addresses the cure chemistry of PETI oligomers. The thermal cure of a low molecular weight model compound was studied using a variety of analytical techniques including differential scanning calorimetry, Fourier transform infrared spectroscopy, and liquid chromatography-mass spectroscopy. The studies indicate an extremely complex cure process. Many stable products were isolated and this paper reports current work on identification of those products. The intent of this research is to provide fundamental insight into the molecular structure of the cured PETI engineering materials so that performance and durability can be more fully assessed.
Watanabe, H; Kazama, Re; Asai, T; Kanaya, F; Ishizaki, H; Fukushima, M; Okiji, T
2015-01-01
This study aimed to evaluate the ability of high-intensity light-emitting diode (LED) and other curing units to cure dual-cured resin cement through ceramic material. A halogen curing unit (Jetlite 3000, Morita), a second-generation LED curing unit (Demi, Kerr), and two high-intensity LED curing units (PenCure 2000, Morita; Valo, Ultradent) were tested. Feldspathic ceramic plates (VITABLOCS Mark II, A3; Vita Zahnfabrik) with thicknesses of 1.0, 2.0, and 3.0 mm were prepared. Dual-cured resin cement samples (Clearfil Esthetic Cement, Kuraray Noritake Dental) were irradiated directly or through one of the ceramic plates for different periods (5, 10, 15, or 20 seconds for the high-intensity LED units and 20, 40, 60, or 80 seconds for the others). The Knoop hardness test was used to determine the level of photopolymerization that had been induced in the resin cement. Data were analyzed by one-way analysis of variance and Dunnett's post-hoc test to identify test-control (maximum irradiation without a ceramic plate) differences for each curing unit (p<0.05). For all curing units, the curing conditions had a statistically significant effect on the Knoop hardness numbers (KHNs) of the irradiated cement samples (p<0.001). In general, the KHN decreased with increasing plate thickness and increased as the irradiation period was extended. Jetlite 3000 achieved control-level KHN values only when the plate thickness was 1.0 mm. At a plate thickness ≥2.0 mm, the LED units (except for PenCure 2000 at 3.0 mm) were able to achieve control-level KHN values when the irradiation time was extended. At a plate thickness of 3.0 mm, irradiation for 20 seconds with the Valo or for 80 seconds with the Demi were the only methods that produced KHN values equivalent to those produced by direct irradiation. Regardless of the type of curing unit used, indirect irradiation of dual-cured resin cement through a ceramic plate resulted in decreased KHN values compared with direct irradiation. When the irradiation period was extended, only the LED units were able to achieve similar KHN values to those observed under direct irradiation in the presence of plates ≥2.0-mm thick. High-intensity LED units require a shorter irradiation period than halogen and second-generation LED curing units to obtain KHN values similar to those observed during direct irradiation.
PMR polyimides: Processable high temperature composite matrix resins
NASA Technical Reports Server (NTRS)
Winters, W. E.; Serafini, T. T.
1975-01-01
Processing reproducibility and versatility were demonstrated for producing addition-cured polyimide/graphite fiber composites using an in situ polymerization of monomeric reactants directly on the fiber surface. The polymers so derived, designated PMR polyimides, can be fabricated into composite structures by laminating, random fiber molding or autoclave curing. Composites were determined to be thermally stable and retain useful properties after extended exposures at 550 F to 650 F. The material and fabrication capability were demonstrated by the fabrication and evaluation of prototype complex fan blades.
PMR polyimides - Processable high temperature composite matrix resins
NASA Technical Reports Server (NTRS)
Winters, W. E.; Serafini, T. T.
1975-01-01
Processing reproducibility and versatility were demonstrated for producing addition-cured polyimide/graphite fiber composites using a unique in situ polymerization of monomeric reactants directly on the fiber surface. The polymers so derived, designated PMR polyimides, can be fabricated into composite structures by laminating, random fiber molding or autoclave curing. Composites were determined to be thermally stable and retain useful properties after extended exposures at 550 to 650 F. The material and fabrication capability were demonstrated by the fabrication and evaluation of prototype complex fan blades.-
Ceramic electrical insulation for electrical coils, transformers, and magnets
Rice, John A.; Hazelton, Craig S.; Fabian, Paul E.
2002-01-01
A high temperature electrical insulation is described, which is suitable for electrical windings for any number of applications. The inventive insulation comprises a cured preceramic polymer resin, which is preferably a polysiloxane resin. A method for insulating electrical windings, which are intended for use in high temperature environments, such as superconductors and the like, advantageously comprises the steps of, first, applying a preceramic polymer layer to a conductor core, to function as an insulation layer, and second, curing the preceramic polymer layer. The conductor core preferably comprises a metallic wire, which may be wound into a coil. In the preferred method, the applying step comprises a step of wrapping the conductor core with a sleeve or tape of glass or ceramic fabric which has been impregnated by a preceramic polymer resin. The inventive insulation system allows conducting coils and magnets to be fabricated using existing processing equipment, and maximizes the mechanical and thermal performance at both elevated and cryogenic temperatures. It also permits co-processing of the wire and the insulation to increase production efficiencies and reduce overall costs, while still remarkably enhancing performance.
Tassery, H; de Donato, P; Barrès, O; Déjou, J
2001-01-01
This study was undertaken to evaluate several polymerization and filling procedures (incremental, bulk, light-tip, soft-cured, plasma devices) in Class II restorations through (1) a sealing evaluation of restorations filled with Tetric Ceram (TC) and Bisfil 2B (B2B, self-cured composite used as a control), (2) a FTIR analysis measuring the variations of the degree of conversion in terms of area unit ratio of the relevant resin composites and (3) a microhardness test to corroborate the FTIR analysis. The length of the tracer penetration was measured from the gingival margin up to the cavity wall with an episcope on sectioned teeth. A ceramic mould, simulating a Class II, was filled according to the different groups and the samples were analyzed with a Bruker IFS 55 spectrometer on ultrathin sections (3 mu). The results were analyzed in terms of area unit ratio and total exposed energy. Under the same conditions, a microhardness test was run with a Frank Weihem machine. The results of the sealing evaluation for light-tip, incremental and self-cured techniques did not differ. The plasma procedure failed in this evaluation as the bottom increment was not polymerized. The smallest area unit ratio (the best degree of conversion) was observed in 2 groups: one, the combination of the light-tip and soft process, and two, the self-cured resin composite (B2B). The distance at which the plasma procedure failed to cure the resin composite was between 3.5 and 4.5 mm. The microhardness test confirmed the FTIR analysis except for the group G2 (TC + light-tip). As also shown by FTIR analysis, no difference between the two relevant levels was observed with the hardness test. The dentin marginal sealing efficiency of Tetric Ceram restorations was increased with the light-tip technique, but was not better than the self-cured resin composite (B2B). For Tetric Ceram, the combination of the light-tip and soft process leads to a higher degree of conversion than the other groups. There is no linear relationship between the degree of conversion, the microhardness and the total exposed energy. The combination of the soft polymerization and the light-tip device might be an alternative restorative technique to the current incremental technique.
Effects of hydrothermal exposure on a low-temperature cured epoxy
NASA Technical Reports Server (NTRS)
Lauver, R. W.
1978-01-01
Thermal mechanical analysis was employed to monitor the penetration temperature of a low-temperature epoxy resin. Both neat resin and E-glass composite samples were examined. The effects of cure temperature variation and moisture content on the apparent glass transition temperature were determined.
Toughening reinforced epoxy composites with brominated polymeric additives
NASA Technical Reports Server (NTRS)
Nir, Z. (Inventor); Gilwee, W. J., Jr. (Inventor)
1985-01-01
Cured polyfunctional epoxy resins including tris(hydroxyphenyl)methane triglycidyl ether are toughened by addition of polybrominated polymeric additives having an EE below 1500 to the pre-cure composition. Carboxy-terminated butadiene-acrylonitrile rubber is optionally present in the pre-cure mixture as such or as a pre-formed copolymer with other reactants. Reinforced composites, particularly carbon-reinforced composites, of these resins are disclosed and shown to have improved toughness.
Depth of Cure of New Flowable Composite Resins
2012-03-30
Flowable composites were introduced to the dental community in the late 1990’s (Ikeda, 2009; Bayne, 1998). The advantage of flowable composite-based...Depth of Cure of New Flowable Composite Resins A THESIS Presented to the Faculty of The Air Force Postgraduate Dental School...SCIENCE In Oral Biology By Inaam A. Pedalino, BS, DDS Dunn Dental Clinic Lackland AFB, TX 30 March 2012 Depth of Cure of New
1974-12-01
Polymerization 13 9. Polymers with Bridged Ring Systems 14 10. Spiro Polymers 14 11. Polyphenylene s 16 12. Phenol - Formaldehyde Resins 17 13. Polyphenylene... Formaldehyde Resins A wide variety of phenol- formaldehyde resins , cured with various curing agents, has been evaluated. The Tdec’s (N 2 ), which...415 0 570 415 540C 2- 410 0 -CHI - 0- c-Ci.f-CCH = 1-eC.- 390 540 0 (Phenol- Formaldehyde Resins ) -CVH- (aliph.) 390 / F_ 535 0 - CHL" (epoxy
Strain and temperature measurement in pultrusion processes by fiber Bragg grating sensors
NASA Astrophysics Data System (ADS)
Tucci, Fausto; Rubino, Felice; Carlone, Pierpaolo
2018-05-01
Injection Pultrusion (IP) is one of the most effective processes, in terms of productivity and costs, to manufacture fiber reinforced polymers. In IP roving of fiber are driven through an injection chamber in which they are impregnated by the resin and then formed in a shaped die. The die is heated in order to cure the resin. Pultruded products are in most cases characterized by constant cross-section profile, whereas unidirectional long fibers are mainly used as reinforcing material. Two relevant phenomena occur within the injection chamber and the heated die, namely the impregnation of the fibers and the polymerization of the resin. Furthermore, thermal expansion, resin chemical shrinkage and the interaction between the die and the impregnated fibers strongly influence the process [1]. Clearly, thermal and mechanical fields significantly impact on these strictly chained behaviours. The use of thermocouples to evaluate temperature within pultrusion die is already widespread, but they are not capable to acquire any information concerning stress-strain levels. In the present work Fibers Bragg Gratings (FBG) sensors were used to measure thermal and strain profiles in selected material location within the injection chamber and the curing die. Being the differences among the spectres transmitted and received are related to the variations in both temperature and strain, commercial FBG sensors were opportunely modified and calibrated. The optical fibers were hooked to the fibers entering into the injection pultrusion die. Taking the pulling speed into account, each waveform acquired was correlated to a position within the die. Obtained data highlight the effect of the heat generation due to resin reaction as well as longitudinal strains related to the pulling force, the thermal expansion and the chemical shrinkage of the resin system.
ATR technique, an appropriate method for determining the degree of conversion in dental giomers
NASA Astrophysics Data System (ADS)
Prejmerean, Cristina; Prodan, Doina; Vlassa, Mihaela; Streza, Mihaela; Buruiana, Tinca; Colceriu, Loredana; Prejmerean, Vasile; Cuc, Stanca; Moldovan, Marioara
2016-12-01
Dental light-curing giomers were developed to combine the favourable properties of diacrylic resin composites (DRCs) and glass-ionomer cements (GICs) in a single material and to eliminate their inherent drawbacks. Giomers are characterized by their aesthetic appearance, high mechanical properties, adhesion to dental tissues as well as fluoride release and recharge abilities. The qualities of the giomers are greatly influenced by the level of conversion of the component resins. Infrared spectroscopy is one of the most largely used techniques for the determination of the degree of conversion in resin-based dental materials. However different results were obtained due to the performances of the used methods. The present work presents the determination of conversion degree in a series of dental copolymers and their corresponding giomers using transmission Fourier transform infrared spectroscopy (FTIR) and an attenuated total reflection technique (ATR) technique, respectively, the main aim being the study of the influence of the materials composition and of the light curing modes upon the achieved conversion in the cured giomers. Beautifil II commercial giomer was used as a control. A halogen lamp and a diode-blue LED lamp were used for the curing of the materials. The results showed that the composition of the resins greatly influenced the conversion. The highest conversions (up to 79%) were obtained in the case of the experimental giomers which contained the experimental Bis-GMA urethane analogue, followed by the Beautifil II giomer (61%) and experimental giomers based on commercial Bis-GMA (up to 50%), respectively. The resins light-cured by using the diode-blue LED lamp presented slightly higher conversions than the resins cured by halogen lamp. The study demonstrates the possibility to evaluate easily and reproducibly the conversion in light-curing composite materials with complex chemical composition and structure, particularly in the case of giomers by using the ATR technique.
Solubilization and spore recovery from silicone polymers. Ph.D. Thesis
NASA Technical Reports Server (NTRS)
Hsiao, Y. C.
1974-01-01
A non-sporicidal technique for solvent degradation of cured silicone polymers was developed which involves chemical degradation of cured silicone polymers by amine solvents at room temperature. Substantial improvements were obtained in the recovery of seeded spores from room temperature cured polymers as compared to the standard recovery procedures, which indicates that the curing process is not sufficiently exothermic to reduce spore viability. The dissolution reaction of cured silicone polymers whith amine solvents is proposed to occur by bimolecular nucleophilic displacement. The chemical structure of silicone polymers was determined by spectroscopic methods. The phenyl to methyl ratio, R/Si ratio, molecular weight, and hydroxyl content of the silicone resins were determined.
Moon, H-J; Lee, Y-K; Lim, B-S; Kim, C-W
2004-03-01
The purpose of this study was to evaluate the effect of the various light curing units (plasma arc, halogen and light-emitting diodes) and irradiation methods (one-step, two-step and pulse) using different light energy densities on the leachability of unreacted monomers (Bis-GMA and UDMA) and the surface hardness of a composite resin (Z250, 3M). Leachability of the specimens immersed for 7 days in ethanol was analysed by HPLC. Vicker's hardness number (VHN) was measured immediately after curing (IC) and after immersion in ethanol for 7 days. Various irradiation methods with three curing units resulted in differences in the amount of leached monomers and VHN of IC when light energy density was lower than 17.0 J cm(-2) (P = 0.05). However, regardless of curing units and irradiation methods, these results were not different when the time or light energy density increased. When similar light energy density was irradiated (15.6-17.7 J cm(-2)), the efficiency of irradiation methods was different by the following order: one-step > or = two-step > pulse. These results suggest that the amount of leached monomers and VHN were influenced by forming polymer structure in activation and initiation stages of polymerization process with different light source energies and curing times.
NASA Astrophysics Data System (ADS)
Kosaka, Tatsuro; Osaka, Katsuhiko; Nakakita, Satoru; Fukuda, Takehito
2003-08-01
This paper describes cure and health monitoring of glass fiber reinforced plastics (GFRP) textile composites both during a resin transfer molding (RTM) process and in loading tests. Carbon fiber reinforced plastics (CFRP) textile composites also were used for a comparative study. Fiber Bragg grating (FBG) fiber optic sensors were embedded in FRP to monitor internal strain. From the results of cure monitoring, it was found that the embedded FBG sensors were useful to know when cured resin constrained fibers. It also appeared that specimens were subjected to friction stress resulted from difference of coefficient of thermal expansion between FRP and a stainless steel mold in cooling process of RTM molding. After the molding, tensile and fatigue tests were conducted. The results of tensile tests showed that output of the embedded FBG sensors agreed well that of surface-bonded strain gauges despite deterioration of reflected spectra form the sensors. From the results of fatigue tests, the FBG sensors showed good status until 100,000 cycles when specimens had no damage. From these results, it can be concluded that embedded FBG sensors have good capability of monitoring internal strain in textile FRP both during RTM process and in service.
Processing Science of Epoxy Resin Composites
1984-01-15
3 2.2 LAMINATE FABRICATION 30 2.2.1 Baseline Laminate Fabrication 30 2.2.2 Large Laminate Fabrication 36 2.3 DIFFUSIVITY AND SOLUBILITY...Thick Laminate 42 28 Baseline Cure Cycle With Specimen Advancement Levels 45 29 Composite Panel Fabrication 47 30 Composite Panel Fabrication 48 31...first change was the elimination of the different 1 resin formulations and concentration on the normal or baseline 5208/T300 prepreg as produced by
NASA Technical Reports Server (NTRS)
Alston, W. B.
1980-01-01
The contributions of individual resin components to total resin weight loss in 600 F air aged Celion 6000/PMR-15 polyimide composites were determined from the overall resin weight loss in the composite by chemically separating the PMR-15 matrix resin into its monomeric components. The individual resin components were also analyzed by spectroscopic techniques in order to elucidate curing and degradation mechanisms of the PMR-15 matrix resin. The isothermal weight loss of the individual resin components during prolonged 600 F thermo-oxidative aging of the composite was correlated to the changes observed in the Fourier Transform infrared spectra and Fourier Transform nuclear magnetic resonance spectra of the individual resin components. The correlation was used to identify the molecular site of the thermo-oxidative changes in PMR-15 polyimide matrix resin during 600 F curing the prolonged 600 F thermo-oxidative aging.
Quantitation of buried contamination by use of solvents
NASA Technical Reports Server (NTRS)
Pappas, S. P.; Hsiao, P.; Hill, L. W.
1972-01-01
Solubilization studies were carried out on various cured silicone resins. A solvent spectrum was prepared. It was found that complete dissolution of cured silicone resins could be achieved without extensive physical degradation of samples. Based on the solubilization results, amine solvents were selected for spore viability studies.
Method for epoxy foam production using a liquid anhydride
Celina, Mathias [Albuquerque, NM
2012-06-05
An epoxy resin mixture with at least one epoxy resin of between approximately 50 wt % and 100 wt %, an anhydride cure agent of between approximately 0 wt % and approximately 50 wt %, a tert-butoxycarbonyl anhydride foaming agent of between proximately 0.1-20 wt %, a surfactant and an imidazole or similar catalyst of less than approximately 2 wt %, where the resin mixture is formed from at least one epoxy resin with a 1-10 wt % tert-butoxycarbonyl anhydride compound and an imidazole catalyst at a temperature sufficient to keep the resin in a suitable viscosity range, the resin mixture reacting to form a foaming resin which in the presence of an epoxy curative can then be cured at a temperature greater than 50.degree. C. to form an epoxy foam.
All-fiber optoelectronic sensor with Bragg gratings for in-situ cure monitoring
NASA Astrophysics Data System (ADS)
Cusano, Andrea; Breglio, Giovanni; Cutolo, Antonello; Calabro, Antonio M.; Giordano, Michele; Nicolais, Luigi, II
2000-08-01
Real-time, in situ monitoring for quality control of the polymer cure process is of high interest, since thermoset polymer-matrix composite are widely used in large industrial areas: aeronautical, aerospace, automotive and civil due to their low cost/low weight features. However, their final properties are strongly dependence on the processing parameters, such as temperature and pressure sequence. The key-point for advanced composite materials is the possibility to have distributed and simultaneous monitoring of chemoreological and physical properties during the cure process. To this aim, we have developed and tested an optoelectronic fiber optic sensor based on the Fresnel principle able to monitor the variations of the refractive index due to the cure process of an epoxy based resin. Experimental results have been obtained on sensor capability to monitor the cure kinetics by assuming the refractive index as reaction co-ordinate. The integration with in-fiber Bragg grating in order to measure the local temperature has been discussed and tested.
Development of tough, moisture resistant laminating resins
NASA Technical Reports Server (NTRS)
Brand, R. A.; Harrison, E. S.
1982-01-01
Tough, moisture resistant laminating resins for employment with graphite fibers were developed. The new laminating resins exhibited cost, handleability and processing characteristics equivalent to 394K (250 F) curing epoxies. The laminating resins were based on bisphenol A dicyanate and monofunctional cyanates with hydrophobic substituents. These resins sorb only small quantities of moisture at equilibrium (0.5% or less) with minimal glass transition temperature depression and represent an improvement over epoxies which sorb around 2% moisture at equilibrium. Toughening was accomplished by the precipitation of small diameter particles of butadiene nitrile rubber throughout the resin matrix. The rubber domains act as microcrack termini and energy dissipation sites, allowing increased stress accommodation prior to catastrophic failure. A unique blend of amine terminated butadiene nitrile elastomer (MW 2,000) and a high nitrile content butadiene nitrile rubber yielded the desired resin morphology.
Advantages and drawbacks of Thiol-ene based resins for 3D-printing
NASA Astrophysics Data System (ADS)
Leonards, Holger; Engelhardt, Sascha; Hoffmann, Andreas; Pongratz, Ludwig; Schriever, Sascha; Bläsius, Jana; Wehner, Martin; Gillner, Arnold
2015-03-01
The technology of 3D printing is conquering the world and awakens the interest of many users in the most varying of applications. New formulation approaches for photo-sensitive thiol-ene resins in combination with various printing technologies, like stereolithography (SLA), projection based printing/digital light processing (DLP) or two-photon polymerization (TPP) are presented. Thiol-ene polymerizations are known for its fast and quantitative reaction and to form highly homogeneous polymer networks. As the resins are locally and temporally photo-curable the polymerization type is very promising for 3D-printing. By using suitable wavelengths, photoinitiator-free fabrication is feasible for single- and two photon induced polymerization. In this paper divinyl ethers of polyethylene glycols in combination with star-shaped tetrathiols were used to design a simple test-system for photo-curable thiol-ene resins. In order to control and improve curing depth and lateral resolution in 3D-polymerization processes, either additives in chemical formulation or process parameters can be changed. The achieved curing depth and resolution limits depend on the applied fabrication method. While two-/multiphoton induced lithography offers the possibility of micron- to sub-micron resolution it lacks in built-up speed. Hence single-photon polymerization is a fast alternative with optimization potential in sub-10-micron resolution. Absorber- and initiator free compositions were developed in order to avoid aging, yellowing and toxicity of resulting products. They can be cured with UV-laser radiation below 300 nm. The development at Fraunhofer ILT is focusing on new applications in the field of medical products and implants, technical products with respect to mechanical properties or optical properties of 3D-printed objects. Recent process results with model system (polyethylene glycol divinylether/ Pentaerithrytol tetrakis (3-mercaptopropionat), Raman measurements of polymer conversion and surface modifications using bifunctional crosslinkers are presented with advantages, drawbacks and a general outlook.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Dirmyer, Matthew R.
This report serves as a follow up to our initial development lot 1 chemical analysis report (LA-UR-16-21970). The purpose of that report was to determine whether or not certain combinations of resin lots and curing agent lots resulted in chemical differences in the final material. One finding of that report suggested that pad P053389 was different from the three other pads analyzed. This report consists of chemical analysis of P053387, P053388, and a reinvestigation of P053389 all of which came from the potentially suspect combination of resin and curing agents lot. The goal of this report is to determine whethermore » the observations relating to P053389 were isolated to that particular pad or systemic to that combination of resin and curing agent lot. The following suite of analyses were performed on the pads: Differential Scanning Calorimetry (DSC), Thermogravimetric Analysis (TGA), Fourier Transform Infrared Spectroscopy (FT-IR), and Solid State Nuclear Magnetic Resonance (NMR). The overall conclusions of the study are that pads P053387 and P053388 behave more consistently with the pads of other resin lot and curing agent lot combinations and that the chemical observations made regarding pad P053389 are isolated to that pad and not representative of an issue with that resin lot and curing agent lot combination.« less
Monitoring in situ in real time of resin infusion for thermoset composite structures
NASA Astrophysics Data System (ADS)
Faci, A.; Wang, P.; Cochrane, C.; Koncar, V.
2017-10-01
The presented work investigates changes in electrical resistance of embedded sensory yarns as a method to monitor the resin flow front position and curing degree of resin during manufacturing of composite structures by vacuum infusion technology. The sensor concept is based on Piezo-resistive sensors integrated to the flax fabric, having almost identical propriety and dimensions as the flax threads used for the production of reinforcements. In the first time sensors have been characterized and first measures of the resin infusion have been realized in order to demonstrate the feasibility of the proposed approach. Then, the measures in real time were realized with fibrous sensors added to the flax fabric (green composites) to monitor the flow front of resin. A large amount of data recorded, filtered, examined, analysed and processed in order to understand and to optimize the infusion and polymerization process.
LED Curing Lights and Temperature Changes in Different Tooth Sites
Armellin, E.; Bovesecchi, G.; Coppa, P.; Pasquantonio, G.; Cerroni, L.
2016-01-01
Objectives. The aim of this in vitro study was to assess thermal changes on tooth tissues during light exposure using two different LED curing units. The hypothesis was that no temperature increase could be detected within the dental pulp during polymerization irrespective of the use of a composite resin or a light-curing unit. Methods. Caries-free human first molars were selected, pulp residues were removed after root resection, and four calibrated type-J thermocouples were positioned. Two LED lamps were tested; temperature measurements were made on intact teeth and on the same tooth during curing of composite restorations. The data was analyzed by one-way analysis of variance (ANOVA), Wilcoxon test, Kruskal-Wallis test, and Pearson's χ 2. After ANOVA, the Bonferroni multiple comparison test was performed. Results. Polymerization data analysis showed that in the pulp chamber temperature increase was higher than that without resin. Starlight PRO, in the same condition of Valo lamp, showed a lower temperature increase in pre- and intrapolymerization. A control group (without composite resin) was evaluated. Significance. Temperature increase during resin curing is a function of the rate of polymerization, due to the exothermic polymerization reaction, the energy from the light unit, and time of exposure. PMID:27195282
LED Curing Lights and Temperature Changes in Different Tooth Sites.
Armellin, E; Bovesecchi, G; Coppa, P; Pasquantonio, G; Cerroni, L
2016-01-01
Objectives. The aim of this in vitro study was to assess thermal changes on tooth tissues during light exposure using two different LED curing units. The hypothesis was that no temperature increase could be detected within the dental pulp during polymerization irrespective of the use of a composite resin or a light-curing unit. Methods. Caries-free human first molars were selected, pulp residues were removed after root resection, and four calibrated type-J thermocouples were positioned. Two LED lamps were tested; temperature measurements were made on intact teeth and on the same tooth during curing of composite restorations. The data was analyzed by one-way analysis of variance (ANOVA), Wilcoxon test, Kruskal-Wallis test, and Pearson's χ (2). After ANOVA, the Bonferroni multiple comparison test was performed. Results. Polymerization data analysis showed that in the pulp chamber temperature increase was higher than that without resin. Starlight PRO, in the same condition of Valo lamp, showed a lower temperature increase in pre- and intrapolymerization. A control group (without composite resin) was evaluated. Significance. Temperature increase during resin curing is a function of the rate of polymerization, due to the exothermic polymerization reaction, the energy from the light unit, and time of exposure.
Qualitative Beam Profiling of Light Curing Units for Resin Based Composites.
Haenel, Thomas; Hausnerová, Berenika; Steinhaus, Johannes; Moeginger, Ing Bernhard
2016-12-01
This study investigates two technically simple methods to determine the irradiance distribution of light curing units that governs the performance of a visible-light curing resin-based composites. Insufficient light irradiation leads to under-cured composites with poor mechanical properties and elution of residual monomers. The unknown irradiance distribution and its effect on the final restoration are the main critical issues requiring highly sophisticated experimental equipment. The study shows that irradiance distributions of LCUs can easily be determined qualitatively with generally available equipment. This significantly helps dentists in practices to be informed about the homogeneity of the curing lights. Copyright© 2016 Dennis Barber Ltd.
Zhang, Lei; Luo, Xiao Ping; Tan, Ren Xiang
2018-05-31
To evaluate the effect of light-cured resin cement application based on etching and silanization on the translucent property of ceramic veneers in different thicknesses, testing the hypothesis that the surface treatment and subsequent resin cement application could influence the translucency of ceramic veneers. The relationship between translucency of ceramic veneers and light transmission irradiated by LED polymerization units was also determined. 40 specimens (10 mm diameter) were fabricated from IPS e.max Press HT A2 ceramic ingots, and polished to 0.3 ± 0.01 mm, 0.5 ± 0.01 mm, 0.7 ± 0.01 mm, 1.0 ± 0.01 mm, and 1.5 ± 0.01 mm thick (n = 8/group). One surface of each disc was etched with HF acid, silanized with Monobond-S, and applied with a light-cured resin cement (Variolink N Transparent Base). Before and after the above procedure, the total luminous transmittance (τ) of all specimens was assessed by a spectrophotometer in a wavelength range of 380-780 nm. A handheld radiometer was used to measure the light intensity irradiated by three LED polymerization units. Light transmission (LT) through ceramic specimens after resin cement application was calculated. Data were statistically analyzed using two-way ANOVA (p = 0.05) and Tukey's test. The correlation between translucency (τ) of ceramic veneers after resin cement application and light transmission (LT) of curing units was statistically evaluated using Spearman correlation test (p = 0.05). With the increase of ceramic thickness, the transmittance decreased significantly (p < 0.05). For the 0.3-mm, 0.5-mm, and 0.7-mm-thick groups, the transmittance of ceramic specimens was statistically significantly lower after resin cement application (p < 0.05). The r value of Bluephase C8 was 0.988, 0.977 for Bluphase, and 0.883 for Bluephase 20i, indicating that the light transmission (LT%) was positively correlated to the translucency of ceramic veneers, regardless of the type of curing units. After the light-cured resin cement application based on etching and silanization, the ceramic veneers (less than 0.7-mm thick) were less translucent, and the translucency decreased when the thickness increased. Because of the lower translucency of ceramic veneers, the light intensity of LED units transmitted to resin layer would decrease when curing. © 2018 by the American College of Prosthodontists.
Manufacturing a 9-Meter Thermoplastic Composite Wind Turbine Blade: Preprint
DOE Office of Scientific and Technical Information (OSTI.GOV)
Murray, Robynne; Snowberg, David R; Berry, Derek S
Currently, wind turbine blades are manufactured from a combination of glass and/or carbon fiber composite materials with a thermoset resin such as epoxy, which requires energy-intensive and expensive heating processes to cure. Newly developed in-situ polymerizing thermoplastic resin systems for composite wind turbine blades polymerize at room temperature, eliminating the heating process and significantly reducing the blade manufacturing cycle time and embodied energy, which in turn reduces costs. Thermoplastic materials can also be thermally welded, eliminating the need for adhesive bonds between blade components and increasing the overall strength and reliability of the blades. As well, thermoplastic materials enable end-of-lifemore » blade recycling by reheating and decomposing the materials, which is a limitation of existing blade technology. This paper presents a manufacturing demonstration for a 9-m-long thermoplastic composite wind turbine blade. This blade was constructed in the Composites Manufacturing Education and Technology facility at the National Wind Technology Center at the National Renewable Energy Laboratory (NREL) using a vacuum-assisted resin transfer molding process. Johns Manville fiberglass and an Arkema thermoplastic resin called Elium were used. Additional materials included Armacell-recycled polyethylene terephthalate foam from Creative Foam and low-cost carbon- fiber pultruded spar caps (manufactured in collaboration with NREL, Oak Ridge National Laboratory, Huntsman, Strongwell, and Chomarat). This paper highlights the development of the thermoplastic resin formulations, including an additive designed to control the peak exothermic temperatures. Infusion and cure times of less than 3 hours are also demonstrated, highlighting the efficiency and energy savings associated with manufacturing thermoplastic composite blades.« less
Optimal cure cycle design of a resin-fiber composite laminate
NASA Technical Reports Server (NTRS)
Hou, Jean W.; Sheen, Jeenson
1987-01-01
A unified computed aided design method was studied for the cure cycle design that incorporates an optimal design technique with the analytical model of a composite cure process. The preliminary results of using this proposed method for optimal cure cycle design are reported and discussed. The cure process of interest is the compression molding of a polyester which is described by a diffusion reaction system. The finite element method is employed to convert the initial boundary value problem into a set of first order differential equations which are solved simultaneously by the DE program. The equations for thermal design sensitivities are derived by using the direct differentiation method and are solved by the DE program. A recursive quadratic programming algorithm with an active set strategy called a linearization method is used to optimally design the cure cycle, subjected to the given design performance requirements. The difficulty of casting the cure cycle design process into a proper mathematical form is recognized. Various optimal design problems are formulated to address theses aspects. The optimal solutions of these formulations are compared and discussed.
Optimizing Polymer Infusion Process for Thin Ply Textile Composites with Novel Matrix System
Bhudolia, Somen K.; Perrotey, Pavel; Joshi, Sunil C.
2017-01-01
For mass production of structural composites, use of different textile patterns, custom preforming, room temperature cure high performance polymers and simplistic manufacturing approaches are desired. Woven fabrics are widely used for infusion processes owing to their high permeability but their localised mechanical performance is affected due to inherent associated crimps. The current investigation deals with manufacturing low-weight textile carbon non-crimp fabrics (NCFs) composites with a room temperature cure epoxy and a novel liquid Methyl methacrylate (MMA) thermoplastic matrix, Elium®. Vacuum assisted resin infusion (VARI) process is chosen as a cost effective manufacturing technique. Process parameters optimisation is required for thin NCFs due to intrinsic resistance it offers to the polymer flow. Cycles of repetitive manufacturing studies were carried out to optimise the NCF-thermoset (TS) and NCF with novel reactive thermoplastic (TP) resin. It was noticed that the controlled and optimised usage of flow mesh, vacuum level and flow speed during the resin infusion plays a significant part in deciding the final quality of the fabricated composites. The material selections, the challenges met during the manufacturing and the methods to overcome these are deliberated in this paper. An optimal three stage vacuum technique developed to manufacture the TP and TS composites with high fibre volume and lower void content is established and presented. PMID:28772654
Optimizing Polymer Infusion Process for Thin Ply Textile Composites with Novel Matrix System.
Bhudolia, Somen K; Perrotey, Pavel; Joshi, Sunil C
2017-03-15
For mass production of structural composites, use of different textile patterns, custom preforming, room temperature cure high performance polymers and simplistic manufacturing approaches are desired. Woven fabrics are widely used for infusion processes owing to their high permeability but their localised mechanical performance is affected due to inherent associated crimps. The current investigation deals with manufacturing low-weight textile carbon non-crimp fabrics (NCFs) composites with a room temperature cure epoxy and a novel liquid Methyl methacrylate (MMA) thermoplastic matrix, Elium ® . Vacuum assisted resin infusion (VARI) process is chosen as a cost effective manufacturing technique. Process parameters optimisation is required for thin NCFs due to intrinsic resistance it offers to the polymer flow. Cycles of repetitive manufacturing studies were carried out to optimise the NCF-thermoset (TS) and NCF with novel reactive thermoplastic (TP) resin. It was noticed that the controlled and optimised usage of flow mesh, vacuum level and flow speed during the resin infusion plays a significant part in deciding the final quality of the fabricated composites. The material selections, the challenges met during the manufacturing and the methods to overcome these are deliberated in this paper. An optimal three stage vacuum technique developed to manufacture the TP and TS composites with high fibre volume and lower void content is established and presented.
Monitoring cure properties of out-of-autoclave BMI composites using IFPI sensor
NASA Astrophysics Data System (ADS)
Kaur, Amardeep; Anandan, Sudharshan; Yuan, Lei; Watkins, Steve E.; Chandrashekhara, K.; Xiao, Hai; Phan, Nam
2016-04-01
A non-destructive technique for inspection of a Bismaleimide (BMI) composite is presented using an optical fiber sensor. High performance BMI composites are used for Aerospace application for their mechanical strength. They are also used as an alternative to toughened epoxy resins. A femtosecond-laser-inscribed Intrinsic Fabry-Perot Interferometer (IFPI) sensor is used to perform real time cure monitoring of a BMI composite. The composite is cured using the out-of-autoclave (OOA) process. The IFPI sensor was used for in-situ monitoring; different curing stages are analyzed throughout the curing process. Temperature-induced-strain was measured to analyze the cure properties. The IFPI structure comprises of two reflecting mirrors inscribed on the core of the fiber using a femtosecond-laser manufacturing process. The manufacturing process makes the sensor thermally stable and robust for embedded applications. The sensor can withstand very high temperatures of up to 850 °C. The temperature and strain sensitivities of embedded IFPI sensor were measured to be 1.4 pm/μepsilon and 0.6 pm/μepsilon respectively.
Effects of hydrothermal exposure on a low-temperature cured epoxy
NASA Technical Reports Server (NTRS)
Lauver, R. W.
1978-01-01
Thermal mechanical analysis was employed to monitor the penetration temperature of a low-temperature epoxy resin (EPON 826/D230). Both neat resin and E-glass composite samples were examined. The effects of cure temperature variation and moisture content on the apparent glass transition temperature were determined.
Cytotoxicity and cytokine expression induced by silorane and methacrylate-based composite resins
LONGO, Daniele Lucca; PAULA-SILVA, Francisco Wanderley Garcia; FACCIOLI, Lucia Helena; GATÓN-HERNÁNDEZ, Patrícia Maria; de QUEIROZ, Alexandra Mussolino; da SILVA, Léa Assed Bezerra
2016-01-01
ABSTRACT The successful use of composite resins in Dentistry depends on physicochemical properties, but also on the biological compatibility of resins, because of the close association between pulp and dentin. Objective The aim of this study was to evaluate cytotoxicity and cytokine production induced by light-cured or non-light-cured methacrylate-based and silorane composite resins in RAW 264.7 macrophages. Material and Methods Cells were stimulated with the extracts from light-cured or non-light-cured composite resins. After incubation for 24 h, cytotoxicity was assessed with the lactate dehydrogenase (LDH) and methyl thiazolyl tetrazolium (MTT) assays, and total protein was quantified using the Lowry method. TNF-α detection was examined with an enzyme-linked immunosorbent assay (ELISA) conducted with cell supernatants after cell stimulation for 6, 12, and 24 h. Data were analyzed using one-way analysis of variance (ANOVA) and Tukey’s post hoc test (α=0.05). Results KaloreTM and FiltekTM Silorane were cytotoxic with or without light curing (p<0.05) after 24 h of incubation. KaloreTM stimulated the early production of TNF-α in comparison with control (p<0.05), whereas FiltekTM Silorane did not affect TNF-α levels after 6 and 12 h (p>0.05). However, after 24 h FiltekTM Silorane inhibited the production of TNF-α (p<0.05). Conclusions KaloreTM and FiltekTM Silorane were cytotoxic regardless of light curing. The extract obtained from KaloreTM after 15 days of incubation stimulated the production of TNF-α, unlike that obtained from FiltekTM Silorane. PMID:27556204
Interpenetrating polymer networks from acetylene terminated materials
NASA Technical Reports Server (NTRS)
Connell, J. W.; Hergenrother, P. M.
1989-01-01
As part of a program to develop high temperature/high performance structural resins for aerospace applications, the chemistry and properties of a novel class of interpenetrating polymer networks (IPNs) were investigated. These IPNs consist of a simple diacetylenic compound (aspartimide) blended with an acetylene terminated arylene ether oligomer. Various compositional blends were prepared and thermally cured to evaluate the effect of crosslink density on resin properties. The cured IPNs exhibited glass transition temperatures ranging from 197 to 254 C depending upon the composition and cure temperature. The solvent resistance, fracture toughness and coefficient of thermal expansion of the cured blends were related to the crosslink density. Isothermal aging of neat resin moldings, adhesive and composite specimens showed a postcure effect which resulted in improved elevated temperature properties. The chemistry, physical and mechanical properties of these materials will be discussed.
A review of devices used for photocuring resin-based composites.
Small, B W
2001-01-01
Composite resin shrinks up to 5% by volume upon curing. This shrinkage and the associated contraction stress remain the two most significant clinical problems with curing resin composite restorations. Many patients continue to experience sensitivity following placement of direct composites and seating of indirect restorations utilizing resin cements. Unfortunately, some claims made by manufacturers or certain clinicians that promise to alleviate these problems are made from a marketing standpoint, with no refereed literature to support those claims. Even within the literature, contradictory results have been reported, perpetuating the confusion. It is of utmost importance that all practicing dentists be aware of the various types of curing systems available and the advantages and disadvantages of each system. It is the opinion of the author that no existing system will alleviate every problem. Until new composite systems are perfected, such as the cyclopolymerizable resins and expanding polymers, we will continue to have shrinkage and stress. Be aware of false claims, read and interpret the literature, and, most importantly, do what is best for your patients.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Oakdale, James S.; Ye, Jianchao; Smith, William L.
Here, two photon polymerization (TPP) is a precise, reliable, and increasingly popular technique for rapid prototyping of micro-scale parts with sub-micron resolution. The materials of choice underlying this process are predominately acrylic resins cross-linked via free-radical polymerization. Due to the nature of the printing process, the derived parts are only partially cured and the corresponding mechanical properties, i.e. modulus and ultimate strength, are lower than if the material were cross-linked to the maximum extent. Herein, post-print curing via UV-driven radical generation, is demonstrated to increase the overall degree of cross-linking of low density, TPP-derived structures.
Oakdale, James S.; Ye, Jianchao; Smith, William L.; ...
2016-11-28
Here, two photon polymerization (TPP) is a precise, reliable, and increasingly popular technique for rapid prototyping of micro-scale parts with sub-micron resolution. The materials of choice underlying this process are predominately acrylic resins cross-linked via free-radical polymerization. Due to the nature of the printing process, the derived parts are only partially cured and the corresponding mechanical properties, i.e. modulus and ultimate strength, are lower than if the material were cross-linked to the maximum extent. Herein, post-print curing via UV-driven radical generation, is demonstrated to increase the overall degree of cross-linking of low density, TPP-derived structures.
RTM: Cost-effective processing of composite structures
NASA Technical Reports Server (NTRS)
Hasko, Greg; Dexter, H. Benson
1991-01-01
Resin transfer molding (RTM) is a promising method for cost effective fabrication of high strength, low weight composite structures from textile preforms. In this process, dry fibers are placed in a mold, resin is introduced either by vacuum infusion or pressure, and the part is cured. RTM has been used in many industries, including automotive, recreation, and aerospace. Each of the industries has different requirements of material strength, weight, reliability, environmental resistance, cost, and production rate. These requirements drive the selection of fibers and resins, fiber volume fractions, fiber orientations, mold design, and processing equipment. Research is made into applying RTM to primary aircraft structures which require high strength and stiffness at low density. The material requirements are discussed of various industries, along with methods of orienting and distributing fibers, mold configurations, and processing parameters. Processing and material parameters such as resin viscosity, perform compaction and permeability, and tool design concepts are discussed. Experimental methods to measure preform compaction and permeability are presented.
Li, Yang; Zhao, Qiangsheng; Mirdamadi, Mansour; ...
2016-01-06
Woven fabric carbon fiber/epoxy composites made through compression molding are one of the promising choices of material for the vehicle light-weighting strategy. Previous studies have shown that the processing conditions can have substantial influence on the performance of this type of the material. Therefore the optimization of the compression molding process is of great importance to the manufacturing practice. An efficient way to achieve the optimized design of this process would be through conducting finite element (FE) simulations of compression molding for woven fabric carbon fiber/epoxy composites. However, performing such simulation remains a challenging task for FE as multiple typesmore » of physics are involved during the compression molding process, including the epoxy resin curing and the complex mechanical behavior of woven fabric structure. In the present study, the FE simulation of the compression molding process of resin based woven fabric composites at continuum level is conducted, which is enabled by the implementation of an integrated material modeling methodology in LS-Dyna. Specifically, the chemo-thermo-mechanical problem of compression molding is solved through the coupling of three material models, i.e., one thermal model for temperature history in the resin, one mechanical model to update the curing-dependent properties of the resin and another mechanical model to simulate the behavior of the woven fabric composites. Preliminary simulations of the carbon fiber/epoxy woven fabric composites in LS-Dyna are presented as a demonstration, while validations and models with real part geometry are planned in the future work.« less
DOE Office of Scientific and Technical Information (OSTI.GOV)
Janke, C.J.
Electron beam (EB) curing is a technology that promises, in certain applications, to deliver lower cost and higher performance polymer matrix composite (PMC) structures compared to conventional thermal curing processes. PMCs enhance performance by making products lighter, stronger, more durable, and less energy demanding. They are essential in weight- and performance-dominated applications. Affordable PMCs can enhance US economic prosperity and national security. US industry expects rapid implementation of electron beam cured composites in aircraft and aerospace applications as satisfactory properties are demonstrated, and implementation in lower performance applications will likely follow thereafter. In fact, at this time and partly becausemore » of discoveries made in this project, field demonstrations are underway that may result in the first fielded applications of electron beam cured composites. Serious obstacles preventing the widespread use of electron beam cured PMCs in many applications are their relatively poor interfacial properties and resin toughness. The composite shear strength and resin toughness of electron beam cured carbon fiber reinforced epoxy composites were about 25% and 50% lower, respectively, than those of thermally cured composites of similar formulations. The essential purpose of this project was to improve the mechanical properties of electron beam cured, carbon fiber reinforced epoxy composites, with a specific focus on composite shear properties for high performance aerospace applications. Many partners, sponsors, and subcontractors participated in this project. There were four government sponsors from three federal agencies, with the US Department of Energy (DOE) being the principal sponsor. The project was executed by Oak Ridge National Laboratory (ORNL), NASA and Department of Defense (DOD) participants, eleven private CRADA partners, and two subcontractors. A list of key project contacts is provided in Appendix A. In order to properly manage the large project team and properly address the various technical tasks, the CRADA team was organized into integrated project teams (IPT's) with each team focused on specific research areas. Early in the project, the end user partners developed ''exit criteria'', recorded in Appendix B, against which the project's success was to be judged. The project team made several important discoveries. A number of fiber coatings or treatments were developed that improved fiber-matrix adhesion by 40% or more, according to microdebond testing. The effects of dose-time and temperature-time profiles during the cure were investigated, and it was determined that fiber-matrix adhesion is relatively insensitive to the irradiation procedure, but can be elevated appreciably by thermal postcuring. Electron beam curable resin properties were improved substantially, with 80% increase in electron beam 798 resin toughness, and {approx}25% and 50% improvement, respectively, in ultimate tensile strength and ultimate tensile strain vs. earlier generation electron beam curable resins. Additionally, a new resin electron beam 800E was developed with generally good properties, and a very notable 120% improvement in transverse composite tensile strength vs. earlier generation electron beam cured carbon fiber reinforced epoxies. Chemical kinetics studies showed that reaction pathways can be affected by the irradiation parameters, although no consequential effects on material properties have been noted to date. Preliminary thermal kinetics models were developed to predict degree of cure vs. irradiation and thermal parameters. These models are continually being refined and validated. Despite the aforementioned impressive accomplishments, the project team did not fully realize the project objectives. The best methods for improving adhesion were combined with the improved electron beam 3K resin to make prepreg and uni-directional test laminates from which composite properties could be determined. Nevertheless, only minor improvements in the composite shear strength, and moderate improvements in the transverse tensile strength, were achieved. The project team was not satisfied with the laminate quality achieved, and low quality (specifically, high void fraction) laminates will compromise the composite properties. There were several problems with the prepregging and fabrication, many of them related to the use of new fiber treatments.« less
NASA Astrophysics Data System (ADS)
Amran, Umar Adli; Zakaria, Sarani; Chia, Chin Hua
2013-11-01
A preliminary study on the reaction between aqueous resole type resinified liquefied palm oil empty fruit bunches fibres (RLEFB) with epoxidized natural rubber (ENR). Liquefaction of empty fruit bunches (EFB) is carried out at different ratio of phenol to EFB (P:EFB). Resole type phenolic resin is prepared using sodium hydroxide (NaOH) as the catalyst with the ratio of liquefied EFB (LEFB) to formaldehyde (LEFB:F) of 1:1.8. 50% epoxidation of epoxidized natural rubber (ENR-50) is used to react with resole resin by mixing with ENR with aqueous resole resin. The cured resin is characterized with FT-IR and SEM. Aqueous system have been found to be unsuitable medium in the reaction between resin and ENR. This system produced a highly porous product when RLEFB/ENR resin is cured.
Fiber-Reinforced Epoxy Composites and Methods of Making Same Without the Use of Oven or Autoclave
NASA Technical Reports Server (NTRS)
Barnell, Thomas J. (Inventor); Rauscher, Michael D. (Inventor); Stienecker, Rick D. (Inventor); Nickerson, David M. (Inventor); Tong, Tat H. (Inventor)
2016-01-01
Method embodiments for producing a fiber-reinforced epoxy composite comprise providing a mold defining a shape for a composite, applying a fiber reinforcement over the mold, covering the mold and fiber reinforcement thereon in a vacuum enclosure, performing a vacuum on the vacuum enclosure to produce a pressure gradient, insulating at least a portion of the vacuum enclosure with thermal insulation, infusing the fiber reinforcement with a reactive mixture of uncured epoxy resin and curing agent under vacuum conditions, wherein the reactive mixture of uncured epoxy resin and curing agent generates exothermic heat, and producing the fiber-reinforced epoxy composite having a glass transition temperature of at least about 100.degree. C. by curing the fiber reinforcement infused with the reactive mixture of uncured epoxy resin and curing agent by utilizing the exothermically generated heat, wherein the curing is conducted inside the thermally insulated vacuum enclosure without utilization of an external heat source or an external radiation source.
Effect of inhomogeneity of light from light curing units on the surface hardness of composite resin.
Arikawa, Hiroyuki; Kanie, Takahito; Fujii, Koichi; Takahashi, Hideo; Ban, Seiji
2008-01-01
This study investigated the characteristics of output light from different types of light curing units, and their effects on polymerization of light-activated composite resin. Three quartz-tungsten-halogen lamps, one plasma arc lamp, and one LED light curing unit were used. Intensity distribution of light emitted from the light guide tip was measured at 1.0-mm intervals across the guide tip. Distribution of Knoop hardness number on the surface of resin irradiated with the light curing units was also measured. For all units, inhomogeneous distribution of light intensity across the guide tip was observed. Minimum light intensity values were 19-80% of the maximum values. In terms of surface hardness, inhomogeneous distribution was also observed for the materials irradiated with the tested units. Minimum values were 53-92% of the maximum values. Our results indicated that markedly inhomogeneous light emitted from light curing unit could result in inhomogeneous polymerization in some areas of the restoration below the light guide tip.
NASA Technical Reports Server (NTRS)
Thompson, C. M.; Smith, J. G., Jr.; Connell, J. W.; Hergenrother, P. M.; Lyon, R. E.
2004-01-01
As part of a program to develop fire resistant exterior composite structures for future subsonic commercial aircraft, flame retardant epoxy resins are under investigation. Epoxies and their curing agents (aromatic diamines) containing phosphorus were synthesized and used to prepare epoxy formulations. Phosphorus was incorporated within the backbone of the epoxy resin and not used as an additive. The resulting cured epoxies were characterized by thermogravimetric analysis, propane torch test, elemental analysis and microscale combustion calorimetry. Several formulations showed excellent flame retardation with phosphorous contents as low as 1.5% by weight. The fracture toughness of plaques of several cured formulations was determined on single-edge notched bend specimens. The chemistry and properties of these new epoxy formulations are discussed.
Development of phosphorylated adhesives
NASA Technical Reports Server (NTRS)
Bilow, N.; Giants, T. W.; Jenkins, R. K.; Campbell, P. L.
1983-01-01
The synthesis of epoxy prepolymers containing phosphorus was carried out in such a manner as to provide adhesives containing at least 5 percent of this element. The purpose of this was to impart fire retardant properties to the adhesive. The two epoxy derivatives, bis(4-glycidyl-oxyphenyl)phenylphosphine oxide and bis(4-glycidyl-2-methoxyphenyl)phenylphosphonate, and a curing agent, bis(3-aminophenyl)methylphosphine oxide, were used in conjunction with one another and along with conventional epoxy resins and curing agents to bond Tedlar and Polyphenylethersulfone films to Kerimid-glass syntactic foam-filled honeycomb structures. Elevated temperatures are required to cure the epoxy resins with the phosphorus-contaning diamine; however, when Tedlar is being bonded, lower curing temperatures must be used to avoid shrinkage and the concomitant formation of surface defects. Thus, the phosphorus-containing aromatic amine curing agent cannot be used alone, although it is possible to use it in conjunction with an aliphatic amine which would allow lower cure temperatures to be used. The experimental epoxy resins have not provided adhesive bonds quite as strong as those provided by Epon 828 when compared in peel tests, but the differences are not very significant. It should be noted, if optimum properties are to be realized. In any case the fire retardant characteristics of the neat resin systems obtained are quite pronounced, since in most cases the self-extinguishing properties are evident almost instantly when specimens are removed from a flame.
Feasibility study on the development of tough, moisture-resistant laminating resins
NASA Technical Reports Server (NTRS)
Brand, R. A.; Harrison, E. S.
1979-01-01
The potential of cyanate resins as replacement for epoxy resins in composites with graphite fiber reinforcement was investigated in an effort to provide improved moisture resistance and toughness in laminating systems at a projected cost, handleability, and processing requirements equivalent to 400 K (260 F) curing epoxies. Monomer synthesis, formulation, blending, resin preparation, catalysis studies, prepreg preparation, laminate fabrication, and testing are discussed. A graphite fiber reinforced laminate was developed with 95 percent retention of the original 363 K (180 F) flexural strength and 70 percent retention of the 363 K (180 F) short beam shear strength after 500 hour exposure to 95 + 7 relative humidity at 324 K (120 F).
NASA Technical Reports Server (NTRS)
Benzie, M. A.
1998-01-01
The objective of this research project was to examine processing and design parameters in the fabrication of composite components to obtain a better understanding and attempt to minimize springback associated with composite materials. To accomplish this, both processing and design parameters were included in a Taguchi-designed experiment. Composite angled panels were fabricated, by hand layup techniques, and the fabricated panels were inspected for springback effects. This experiment yielded several significant results. The confirmation experiment validated the reproducibility of the factorial effects, error recognized, and experiment as reliable. The material used in the design of tooling needs to be a major consideration when fabricating composite components, as expected. The factors dealing with resin flow, however, raise several potentially serious material and design questions. These questions must be dealt with up front in order to minimize springback: viscosity of the resin, vacuum bagging of the part for cure, and the curing method selected. These factors directly affect design, material selection, and processing methods.
NASA Astrophysics Data System (ADS)
Souza, Christiane S. R.; Cândido, Geraldo M.; Alves, Wellington; Marlet, José Maria F.; Rezende, Mirabel C.
2017-10-01
This study aims to contribute to sustainability by proposing the reuse of composite prepreg scrap as an added value from discards. The research evaluates the microstructure and mechanical properties of laminates processed by the reuse of uncured carbon fibre/F155-epoxy resin prepreg scraps, waste from the ply cutting area of an aeronautical industry. The composite scraps were used as collected and were randomly positioned to produce laminates to be cured at an autoclave. The mechanical characterization shows a decrease of 39% for the compression property due to the discontinuous fibres in the laminate and an increase of 34% for the interlaminar shear strength, when compared to continuous fibre laminates. This increase is attributed to the higher crosslink density of the epoxy resin, as a result of the cure temperature used in autoclave (60 °C higher than suggested by supplier) and also to the randomly positioned scraps. Microscopic analyses confirm the consolidation of laminates, although show resin rich areas with different sizes and shapes attributed to the overlapping of the scraps with different sizes and shapes. These resin rich areas may contribute to decrease the mechanical properties of laminates. The correlation between mechanical and morphological results shows potential to be used on non-critical structural application, as composite jigs, contributing to sustainability.
Measurement of the degree of cure in epoxies with ultrasonic velocity
NASA Technical Reports Server (NTRS)
Winfree, W. P.; Parker, F. R.
1986-01-01
The use of ultrasonic longitudinal velocity values to measure the degree of cure (defined for an epoxide system as the concentration of epoxide/amine bonds divided by the initial epoxide concentration) in epoxy resins is investigated. The experimental setup used to measure the changes in longitudinal velocity with time is described, together with the technique used to calculate the degree of cure from the acoustic data, using the principle of additive module. Measurements were done with diglycidyl ether of bisphenol A epoxy resin cured with an amine adduct agent. Good qualitative agreement was shown between the time dependence of the acoustically measured degree of cure and the predicted rate of reaction.
Chen, Yi; Lin, Liang-Kai; Chiang, Shu-Jen; Liu, Ying-Ling
2017-02-01
In this work, a cocatalytic effect between Meldrum's acid (MA) and benzoxazine (Bz) compounds has been explored to build up a self-promoting curing system. Consequently, the MA/Bz reactive blend exhibits a relatively low reaction temperature compared to the required temperatures for the cross-linking reactions of the pure MA and Bz components. This feature is attractive for energy-saving processing issues. Moreover, the thermosetting resins based on the MA/Bz reactive blends have been prepared. The MA component can generate additional free volume in the resulting resins, so as to trap air in the resin matrix and consequently to bring low dielectric constants to the resins. The MA-containing agent is an effective modifier for benzoxazine resins to reduce their dielectric constants. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
The influence of polishing techniques on pre-polymerized CAD\\CAM acrylic resin denture bases
Alammari, Manal Rahma
2017-01-01
Background Lately, computer-aided design and computer-aided manufacturing (CAD/CAM) has broadly been successfully employed in dentistry. The CAD/CAM systems have recently become commercially available for fabrication of complete dentures, and are considered as an alternative technique to conventionally processed acrylic resin bases. However, they have not yet been fully investigated. Objective The purpose of this study was to inspect the effects of mechanical polishing and chemical polishing on the surface roughness (Ra) and contact angle (wettability) of heat-cured, auto-cured and CAD/CAM denture base acrylic resins. Methods This study was conducted at the Advanced Dental Research Laboratory Center of King Abdulaziz University from March to June 2017. Three denture base materials were selected: heat cure poly-methylmethacrylate resin, thermoplastic (polyamide resin) and (CAD\\CAM) denture base resin. Sixty specimens were prepared and divided into three groups, twenty in each. Each group was divided according to the polishing techniques into (Mech P) and (Chem P), ten specimens in each; surface roughness and wettability were investigated. Data were analyzed by SPSS version 22, using one-way ANOVA and Pearson coefficient. Results One-way analysis of variance (ANOVA) and post hoc tests were used for comparing the surface roughness values between three groups which revealed a statistical significant difference between them (p1<0.001). Heat-cured denture base material of (Group I) in both methods, showed the highest mean surface roughness value (2.44±0.07, 2.72±0.09, Mech P and Chem P respectively); while CAD\\CAM denture base material (group III) showed the least mean values (1.08±0.23, 1.39±0.31, Mech P and Chem P respectively). CAD/CAM showed the least contact angle in both polishing methods, which were statistically significant at 5% level (p=0.034 and p<0.001). Conclusion Mechanical polishing produced lower surface roughness of CAD\\CAM denture base resin with superior smooth surface compared to chemical polishing. Mechanical polishing is considered the best effective polishing technique. CAD/CAM denture base material should be considered as the material of choice for complete denture construction in the near future, especially for older dental patients with changed salivary functions, because of its wettability. PMID:29238483
The influence of polishing techniques on pre-polymerized CAD\\CAM acrylic resin denture bases.
Alammari, Manal Rahma
2017-10-01
Lately, computer-aided design and computer-aided manufacturing (CAD/CAM) has broadly been successfully employed in dentistry. The CAD/CAM systems have recently become commercially available for fabrication of complete dentures, and are considered as an alternative technique to conventionally processed acrylic resin bases. However, they have not yet been fully investigated. The purpose of this study was to inspect the effects of mechanical polishing and chemical polishing on the surface roughness (Ra) and contact angle (wettability) of heat-cured, auto-cured and CAD/CAM denture base acrylic resins. This study was conducted at the Advanced Dental Research Laboratory Center of King Abdulaziz University from March to June 2017. Three denture base materials were selected: heat cure poly-methylmethacrylate resin, thermoplastic (polyamide resin) and (CAD\\CAM) denture base resin. Sixty specimens were prepared and divided into three groups, twenty in each. Each group was divided according to the polishing techniques into (Mech P) and (Chem P), ten specimens in each; surface roughness and wettability were investigated. Data were analyzed by SPSS version 22, using one-way ANOVA and Pearson coefficient. One-way analysis of variance (ANOVA) and post hoc tests were used for comparing the surface roughness values between three groups which revealed a statistical significant difference between them (p 1 <0.001). Heat-cured denture base material of (Group I) in both methods, showed the highest mean surface roughness value (2.44±0.07, 2.72±0.09, Mech P and Chem P respectively); while CAD\\CAM denture base material (group III) showed the least mean values (1.08±0.23, 1.39±0.31, Mech P and Chem P respectively). CAD/CAM showed the least contact angle in both polishing methods, which were statistically significant at 5% level (p=0.034 and p<0.001). Mechanical polishing produced lower surface roughness of CAD\\CAM denture base resin with superior smooth surface compared to chemical polishing. Mechanical polishing is considered the best effective polishing technique. CAD/CAM denture base material should be considered as the material of choice for complete denture construction in the near future, especially for older dental patients with changed salivary functions, because of its wettability.
Ruan, Jian-Yong; Gong, Zheng-Lin; Zhang, Rui-Zhi; Zhang, Zhe; Xu, Ran; Li, Da-Xu; Ren, Le; Tao, Hong
2017-09-16
BACKGROUND This study aimed to conduct a clinical evaluation of four restorative materials for restoration of dental wedge-shaped defect (WSD) and their impacts on periodontal tissues. MATERIAL AND METHODS A total of 280 maxillary premolars with dental WSD were selected from 106 patients; the patient cases were divided into eight groups according to different combinations of restorative materials (flowable resin composites, Dyract compomers, glass ionomer cement (GIC), light-curing composite resin), and WSD positions (approaching gingival and subgingival positions). Gingival crevicular fluid (GCF) volume, levels of aspartate aminotransferase (AST), alkaline phosphatase (ALP), and interleukin-1β (IL-1β) in GCF were analyzed, while probing depth (PD), plaque index (PLI), and sulcus bleeding index (SBI) were also measured. The periodontal conditions of all patients were followed prior to restoration, as well as six months and 12 months after restoration. RESULTS After six months of restoration, the overall clinical success rates of flowable resin composites, Dyract compomers, and light-curing composite resin were greater than those of GIC. GCF volume, GCF-AST, IL-1β levels, PD, PLI, and SBI of cases restored by GIC were higher than those restored by the other three materials. After 12 months of restoration, the overall clinical success rates of flowable resin composites and Dyract compomers were greater than those of light-curing composite resin and GIC. GCF volume, GCF-AST, GCF-ALP, IL-1β levels, PD, PLI, and SBI of cases restored by GIC were higher than those restored by the other three materials. CONCLUSIONS Our study provided evidence that the clinical efficacy of flowable resin composites, Dyract compomers, and light-curing composite resin was greater than that of GIC for restoration of dental WSD.
Ruan, Jian-Yong; Gong, Zheng-Lin; Zhang, Rui-Zhi; Zhang, Zhe; Xu, Ran; Li, Da-Xu; Ren, Le; Tao, Hong
2017-01-01
Background This study aimed to conduct a clinical evaluation of four restorative materials for restoration of dental wedge-shaped defect (WSD) and their impacts on periodontal tissues. Material/Methods A total of 280 maxillary premolars with dental WSD were selected from 106 patients; the patient cases were divided into eight groups according to different combinations of restorative materials (flowable resin composites, Dyract compomers, glass ionomer cement (GIC), light-curing composite resin), and WSD positions (approaching gingival and subgingival positions). Gingival crevicular fluid (GCF) volume, levels of aspartate aminotransferase (AST), alkaline phosphatase (ALP), and interleukin-1β (IL-1β) in GCF were analyzed, while probing depth (PD), plaque index (PLI), and sulcus bleeding index (SBI) were also measured. The periodontal conditions of all patients were followed prior to restoration, as well as six months and 12 months after restoration. Results After six months of restoration, the overall clinical success rates of flowable resin composites, Dyract compomers, and light-curing composite resin were greater than those of GIC. GCF volume, GCF-AST, IL-1β levels, PD, PLI, and SBI of cases restored by GIC were higher than those restored by the other three materials. After 12 months of restoration, the overall clinical success rates of flowable resin composites and Dyract compomers were greater than those of light-curing composite resin and GIC. GCF volume, GCF-AST, GCF-ALP, IL-1β levels, PD, PLI, and SBI of cases restored by GIC were higher than those restored by the other three materials. Conclusions Our study provided evidence that the clinical efficacy of flowable resin composites, Dyract compomers, and light-curing composite resin was greater than that of GIC for restoration of dental WSD. PMID:28917087
Botsali, Murat Selim; Kuşgöz, Adem; Altintaş, Subutay Han; Ülker, Hayriye Esra; Kiliç, Serdar; Başak, Feridun; Ülker, Mustafa
2014-01-01
The purpose of this study was first to evaluate the elution of 2-hydroxyethyl methacrylate (HEMA) and triethylene glycol dimethacrylate (TEGDMA) monomers from resin-modified glass ionomer cement (RMGIC) and compomers cured with halogen and light-emitting diode (LED) light-curing units (LCUs). The effect of cured materials on the viability of L929 fibroblast cells was also evaluated. One RMGIC (Ketac N100) and two compomers (Dyract Extra and Twinkystar) were tested. Materials were prepared in teflon disks and light-cured with LED or halogen LCUs. The residual monomers of resin materials in solution were identified using high-performance liquid chromatography. The fibroblast cells' viability was analyzed using MTT assay. The type of LCU did not have a significant effect on the elution of HEMA and TEGDMA. A greater amount of HEMA than TEGMDA was eluted. The amount of TEGDMA eluted from Twinkystar was greater than Dyract Extra (P < 0.05) when cured with a halogen LCU. All material-LCU combinations decreased the fibroblast cells' viability more than the control group (P < 0.01), except for Dyract Extra cured with a halogen LCU (P > 0.05). Curing with the LED LCU decreased the cells' viability more than curing with the halogen LCU for compomers. For Ketac N100, the halogen LCU decreased the cells' viability more than the LED LCU. PMID:24592149
Effect of mold diameter on the depth of cure of a resin-based composite material.
Erickson, Robert L; Barkmeier, Wayne W
2017-02-01
The purpose of this study was to examine the effect of mold diameter on depth of cure of a resin-based composite material for varying amounts of irradiation. A resin-based composite was light-cured for 10-80 s in stainless-steel molds of either 6 mm or 4 mm in diameter and then dark-stored for 24 h. Specimens were then scraped back and the length of the cured specimens was measured to provide depth of cure (D SB ). Radiant exposure to each of the mold diameters was determined by measuring the power. The D SB values using the 4-mm molds were lower than those of the 6-mm molds. The average difference between the two groups for each irradiation time was 0.45 ± 0.02 mm. A fixed depth of cure required about 39% more irradiation time for the 4-mm mold than for the 6-mm mold but 75% more radiant exposure. The difference in cure depth for a fixed radiant exposure was 0.79 mm. A better comparison of depth of cure is obtained by using identical radiant exposures for different mold diameters. It is believed that greater loss of light by absorption at the stainless-steel cylinder walls for the 4-mm-diameter cylinders accounts for the lower depth of cure when compared with the 6-mm molds. © 2017 Eur J Oral Sci.
Okumura, Tetsu; Okanoya, Kazuo; Tani, Jun
2007-01-01
In chronic recording experiments, self-curing dental acrylic resins have been used as a mounting base of electrodes or microdialysis-probes. Since these acrylics do not bond to the bone, screws have been used as anchors. However, in small experimental animals like finches or mouse, their craniums are very fragile and can not successfully hold the anchors. In this report, we propose a new application of light-curing dental resins for mounting base of electrodes or microdialysis probes in chronic experiments. This material allows direct bonding to the cranium. Therefore, anchor screws are not required and surgical field can be reduced considerably. Past experiences show that the bonding effect maintains more than 2 months. Conventional resin's window of time when the materials are pliable and workable is a few minutes. However, the window of working time for these dental adhesives is significantly wider and adjustable. PMID:18997897
Designing of cardanol based polyol and its curing kinetics with melamine formaldehyde resin
Balgude, Dinesh Bapurao; Sabnis, Anagha Shyamsunder; Ghosh, Swapan Kumar
2017-01-01
Abstract Commercially used industrial baking enamels consist of alkyd or polyester resin with melamine formaldehyde. These resins are mainly derived from fossil resources. Considering growing environmental legislation regarding use of petroleum based raw materials, utilization of renewable resources to synthesize various chemistries can be the only obvious option as far as academia and industries are concerns. The present work deals with exploration of one of the natural resources (Cardanol) for polyol synthesis, its characterization (FTIR and NMR) and its curing behavior with melamine formaldehyde resin by differential scanning calorimetry (DSC). The optimized formulations from DSC study were further evaluated for general coating properties to study the suitability of developed polyol for industrial coating application. The experimental studies revealed that melamine content in the curing mixtures and thereby developed crosslinking density played an important role in deciding the coatings properties. PMID:29491791
Yang, Y W; Yu, F; Zhang, H C; Dong, Y; Qiu, Y N; Jiao, Y; Xing, X D; Tian, M; Huang, L; Chen, J H
2018-01-01
To evaluate in vitro the physicochemical properties, cytotoxicity and calcium phosphate nucleation of an experimental light-curable pulp capping material composed of a resin with antibacterial monomer (MAE-DB) and Portland cement (PC). The experimental material was prepared by mixing PC with a resin containing MAE-DB at a 2 : 1 ratio. Cured pure resin containing MAE-DB served as control resin. ProRoot MTA and Dycal served as commercial controls. The depth of cure, degree of monomer conversion, water absorption and solubility of dry samples, calcium release, alkalinizing activity, calcium phosphate nucleation and the cytotoxicity of materials were evaluated. Statistical analysis was carried out using anova followed by Tukey's HSD test (equal variance assumed) or Tamhane test (equal variance not assumed) and independent-samples t-tests. The experimental material had a cure depth of 1.19 mm, and the mean degree of monomer conversion was 70.93% immediately post-cure and 88.75% at 24 h post-cure. The water absorption of the experimental material was between those of MTA and Dycal, and its solubility was significantly less (P < 0.05) than that of Dycal and higher than that of MTA. The experimental material exhibited continuous calcium release and an alkalinizing power between those of MTA and Dycal throughout the test period. Freshly set experimental material, control resin and all 24-h set materials had acceptable cytotoxicity. The experimental material, MTA and Dycal all exhibited the formation of apatite precipitates after immersion in phosphate-buffered saline. The experimental material possessed adequate physicochemical properties, low cytotoxicity and good calcium phosphate nucleation. © 2017 International Endodontic Journal. Published by John Wiley & Sons Ltd.
Grande da Cruz, Fernanda Zander; Grande, Christiana Zander; Roderjan, Douglas Augusto; Galvão Arrais, César Augusto; Bührer Samra, Adriana Postiglione; Calixto, Abraham Lincoln
2012-01-01
Objective To evaluate the effects of etch-and-rinse and self-etching adhesive systems on Vickers hardness (VHN) uniformity of dual-cured resin cements after fiber post cementation. Methods: Fifty glass fiber posts were cemented into bovine roots using the following cementing systems: Prime&Bond 2.1 Dual Cure and Enforce with light-activation (PBDC-LCEN); Prime&Bond 2.1 and Enforce with light-activation (PB-CLEN); Prime&Bond 2.1 Dual Cure and Enforce without light exposure (PBDC-SCEN); ED Primer and Panavia 21 (ED-SCPN); and Clearfil SE Bond and Panavia 21 (CF-SCPN). The roots were stored in distilled water for 72 h and transversely sectioned into thirds (coronal, medium, and apical). The VHN values of the resin cement layers were measured close to the post and to the dentin wall on the transversely sectioned flat surfaces. The results were analyzed by three-way repeated measures analysis of variance (ANOVA) and Tukey’s post-hoc test (pre-set alpha of 5%). Results: Most resin cements presented higher VHN values near the post than near the dentin wall. The ED-SCPN group showed the highest VHN values regardless of the root third, while the self-cured group PBDC-SCEN exhibited the lowest values. The resin cements from the light-activated groups PBDC-LCEN and PB-LCEN showed lower VHN values at the apical third than at the coronal third. The VHN values were not influenced by the root third in self-cured groups PBDC-SCEN, ED-SCPN, and ED-SCPN. Conclusion: Depending on the product, bonding agents might promote changes in hardness uniformity of resin cements after post cementation. PMID:22904652
NASA Astrophysics Data System (ADS)
Gholipour-Mahmoudalilou, Meysam; Roghani-Mamaqani, Hossein; Azimi, Reza; Abdollahi, Amin
2018-01-01
Thermal properties of epoxy resin were improved by preparation of a curing agent of poly (amidoamine) (PAMAM) dendrimer-grafted graphene oxide (GO). Hyperbranched PAMAM-modified GO (GD) was prepared by a divergent dendrimer synthesis methodology. Modification of GO with (3-Aminopropyl)triethoxysilane (APTES), Michael addition of methacrylic acid, and amidation reaction with ethylenediamine results in the curing agent of GD. Then, epoxy resin was cured in the presence of different amounts of GD and the final products were compared with ethylenediamine-cured epoxy resin (E) in their thermal degradation temperature and char contents. Functionalization of GO with APTES and hyperbranched dendrimer formation at the surface of GO were evaluated by Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, X-ray diffraction, and thermogravimetric analysis (TGA) results. TGA results showed that the weight loss associated with chemical moieties in GONH2, GOMA, and GD is estimated to be 10.1, 12.2, and 14.1%, respectively. Covalent attachment of dendrimer at the surface of GO increases its thermal stability. TGA also showed that decomposition temperature and char content are higher for composites compared with E. Scanning and transmission electron microscopies show that flat and smooth graphene nanolayers are wrinkled in GO and re-stacking and flattening of nanolayers is observed in GD.
Photosensitive filler minimizes internal stresses in epoxy resins
NASA Technical Reports Server (NTRS)
Dillon, J. N.
1967-01-01
Photosensitive filler is added to curable epoxy resins to minimize stress from internal shrinkage during curing or polymerization. Cinnamic acid resins and cinnamal ketones may be added in the amount of 1 to 3 percent by weight of the resin mixture.
Bond strength of orthodontic light-cured resin-modified glass ionomer cement.
Cheng, Hsiang Yu; Chen, Chien Hsiu; Li, Chuan Li; Tsai, Hung Huey; Chou, Ta Hsiung; Wang, Wei Nan
2011-04-01
The purpose of this study was to compare the bond strengths and debonded interfaces achieved with light-cured resin-modified glass ionomer cement (RMGIC) and conventional light-cured composite resin. In addition, the effects of acid etching and water contamination were examined. One hundred human premolars were randomly divided into five equal groups. The mini Dyna-lock upper premolar bracket was selected for testing. The first four groups were treated with light-cured RMGIC with or without 15 per cent phosphoric acid-etching treatment and with or without water contamination preceding bracket bonding. The control samples were treated with the conventional light-cured Transbond composite resin under acid etching and without water contamination. Subsequently, the brackets were debonded by tensile force using an Instron machine. The modified adhesive remnant index (ARI) scores were assigned to the bracket base of the debonded interfaces using a scanning electron microscope. The bond strength and modified ARI scores were determined and analysed statistically by one-way analysis of variance and chi-square test. Under all four conditions, the bond strength of the light-cure RMGIC was equal to or higher than that of the conventional composite resin. The highest bond strength was achieved when using RMGIC with acid etching but without water contamination. The modified ARI scores were 2 for Fuji Ortho LC and 3 for Transbond. No enamel detachment was found in any group. Fifteen per cent phosphoric acid etching without moistening the enamel of Fuji Ortho LC provided the more favourable bond strength. Enamel surfaces, with or without water contamination and with or without acid etching, had the same or a greater bond strength than Transbond.
Shimizu, Y; Tsujimoto, A; Furuichi, T; Suzuki, T; Tsubota, K; Miyazaki, M; Platt, J A
2015-01-01
We examined the influence of light intensity on surface free energy characteristics and dentin bond strength of dual-cure direct core build-up resin systems. Two commercially available dual-cure direct core build-up resin systems, Clearfil DC Core Automix with Clearfil Bond SE One and UniFil Core EM with Self-Etching Bond, were studied. Bovine mandibular incisors were mounted in acrylic resin and the facial dentin surfaces were wet ground on 600-grit silicon carbide paper. Adhesives were applied to dentin surfaces and cured with light intensities of 0 (no irradiation), 200, 400, and 600 mW/cm(2). The surface free energy of the adhesives (five samples per group) was determined by measuring the contact angles of three test liquids placed on the cured adhesives. To determine the strength of the dentin bond, the core build-up resin pastes were condensed into the mold on the adhesive-treated dentin surfaces according to the methods described for the surface free energy measurement. The resin pastes were cured with the same light intensities as those used for the adhesives. Ten specimens per group were stored in water maintained at 37°C for 24 hours, after which they were shear tested at a crosshead speed of 1.0 mm/minute in a universal testing machine. Two-way analysis of variance (ANOVA) and a Tukey-Kramer test were performed, with the significance level set at 0.05. The surface free energies of the adhesive-treated dentin surfaces decreased with an increase in the light intensity of the curing unit. Two-way ANOVA revealed that the type of core build-up system and the light intensity significantly influence the bond strength, although there was no significant interaction between the two factors. The highest bond strengths were achieved when the resin pastes were cured with the strongest light intensity for all the core build-up systems. When polymerized with a light intensity of 200 mW/cm(2) or less, significantly lower bond strengths were observed. CONClUSIONS: The data suggest that the dentin bond strength of core build-up systems are still affected by the light intensity of the curing unit, which is based on the surface free energy of the adhesives. On the basis of the results and limitations of the test conditions used in this study, it appears that a light intensity of >400 mW/cm(2) may be required for achieving the optimal dentin bond strength.
Influence of post pattern and resin cement curing mode on the retention of glass fibre posts.
Poskus, L T; Sgura, R; Paragó, F E M; Silva, E M; Guimarães, J G A
2010-04-01
To evaluate the influence of post design and roughness and cement system (dual- or self-cured) on the retention of glass fibre posts. Two tapered and smooth posts (Exacto Cônico No. 2 and White Post No. 1) and two parallel-sided and serrated posts (Fibrekor 1.25 mm and Reforpost No. 2) were adhesively luted with two different resin cements--a dual-cured (Rely-X ARC) and a self-cured (Cement Post)--in 40 single-rooted teeth. The teeth were divided into eight experimental groups (n = 5): PFD--Parallel-serrated-Fibrekor/dual-cured; PRD--Parallel-serrated-Reforpost/dual-cured; TED--Tapered-smooth-Exacto Cônico/dual-cured; TWD--Tapered-smooth-White Post/dual-cured; PFS--Parallel-serrated-Fibrekor/self-cured; PRS--Parallel-serrated-Reforpost/self-cured; TES--Tapered-smooth-Exacto Cônico/self-cured; TWS--Tapered-smooth-White Post/self-cured. The specimens were submitted to a pull-out test at a crosshead speed of 0.5 mm min(-1). Data were analysed using analysis of variance and Bonferroni's multiple comparison test (alpha = 0.05). Pull-out results (MPa) were: PFD = 8.13 (+/-1.71); PRD = 8.30 (+/-0.46); TED = 8.68 (+/-1.71); TWD = 9.35 (+/-1.99); PFS = 8.54 (+/-2.23); PRS = 7.09 (+/-1.96); TES = 8.27 (+/-3.92); TWS = 7.57 (+/-2.35). No statistical significant difference was detected for posts and cement factors and their interaction. The retention of glass fibre posts was not affected by post design or surface roughness nor by resin cement-curing mode. These results imply that the choice for serrated posts and self-cured cements is not related to an improvement in retention.
Development and evaluation of epoxidized soybean oil-based polymers
NASA Astrophysics Data System (ADS)
Juangvanich, Nuanpen
Epoxidized Soybean Oil (ESO) based polymers were developed using diamine curing agents and BF3:NH2C2H5 as catalyst. Reactions involved the curing process were explored and monitored by DSC and IR analysis. Amine-epoxy addition reactions governed the main curing reaction at the temperature range of 60--235°C, and the supplementary reactions at higher temperatures were either homopolymerization or etherification reaction. In the aliphatic curing reactions, the epoxy-rich system favored the supplementary reactions at high temperature, however, ESO cured with 1,6 hexanediamine (HDA) always produced the high temperature reaction products, due to some side reactions and the high volatile nature. The curing reaction with aromatic diamines produced inherent rigidity to the cured ESO network, which decreased the high temperature reactions. The system cured with a short aromatic diamine, 1,4-phenyldiamine (PDA), produced a small extent of high temperature reaction, as well. It was believed that the long length diamine with wide separation of the two amines underwent an intermolecular cross-linking reaction, and derived better properties than the shorter diamine. A post-cure process was used to improve the final polymer properties by increasing the temperature after the initial curing reaction was quenched due to gelation. Extending the time of post-curing did not significantly improve properties of the final ESO polymers. Exposing the cured samples at 180°C for longer than 12 hours decreased the properties of the cured material, due to thermal strain generating in the network structure. To increase time efficiency, short heat cycles were performed by post-curing right after gelation, and the cured ESO polymer had tensile strength of 32 MPa, modulus 750 MPa and toughness 1.3 MPa. With the introduction of EPON 828, the mechanical properties of a new ESO polymer improved; having strength above 40 MPa, modulus great than 1,000 MPa, and Tg higher than 40°C. Finally, a rice hull particleboard was developed using the cured ESO resin as adhesive, and the board had strength comparable to the National Bureau of Standards minimum requirement for particleboard. A 35 wt % of ESO resin imparted the highest strength for the rice hull board, with a value of 15.5 MPa.
Efficiency of polymerization of bulk-fill composite resins: a systematic review.
Reis, André Figueiredo; Vestphal, Mariana; Amaral, Roberto Cesar do; Rodrigues, José Augusto; Roulet, Jean-François; Roscoe, Marina Guimarães
2017-08-28
This systematic review assessed the literature to evaluate the efficiency of polymerization of bulk-fill composite resins at 4 mm restoration depth. PubMed, Cochrane, Scopus and Web of Science databases were searched with no restrictions on year, publication status, or article's language. Selection criteria included studies that evaluated bulk-fill composite resin when inserted in a minimum thickness of 4 mm, followed by curing according to the manufacturers' instructions; presented sound statistical data; and comparison with a control group and/or a reference measurement of quality of polymerization. The evidence level was evaluated by qualitative scoring system and classified as high-, moderate- and low- evidence level. A total of 534 articles were retrieved in the initial search. After the review process, only 10 full-text articles met the inclusion criteria. Most articles included (80%) were classified as high evidence level. Among several techniques, microhardness was the most frequently method performed by the studies included in this systematic review. Irrespective to the "in vitro" method performed, bulk fill RBCs were partially likely to fulfill the important requirement regarding properly curing in 4 mm of cavity depth measured by depth of cure and / or degree of conversion. In general, low viscosities BFCs performed better regarding polymerization efficiency compared to the high viscosities BFCs.
NASA Astrophysics Data System (ADS)
Kim, Ye Chan; Min, Hyunsung; Hong, Sungyong; Wang, Mei; Sun, Hanna; Park, In-Kyung; Choi, Hyouk Ryeol; Koo, Ja Choon; Moon, Hyungpil; Kim, Kwang J.; Suhr, Jonghwan; Nam, Jae-Do
2017-08-01
As packaging technologies are demanded that reduce the assembly area of substrate, thin composite laminate substrates require the utmost high performance in such material properties as the coefficient of thermal expansion (CTE), and stiffness. Accordingly, thermosetting resin systems, which consist of multiple fillers, monomers and/or catalysts in thermoset-based glass fiber prepregs, are extremely complicated and closely associated with rheological properties, which depend on the temperature cycles for cure. For the process control of these complex systems, it is usually required to obtain a reliable kinetic model that could be used for the complex thermal cycles, which usually includes both the isothermal and dynamic-heating segments. In this study, an ultra-thin prepreg with highly loaded silica beads and glass fibers in the epoxy/amine resin system was investigated as a model system by isothermal/dynamic heating experiments. The maximum degree of cure was obtained as a function of temperature. The curing kinetics of the model prepreg system exhibited a multi-step reaction and a limited conversion as a function of isothermal curing temperatures, which are often observed in epoxy cure system because of the rate-determining diffusion of polymer chain growth. The modified kinetic equation accurately described the isothermal behavior and the beginning of the dynamic-heating behavior by integrating the obtained maximum degree of cure into the kinetic model development.
2014-01-01
Background The aim of this study is to compare the microleakage of Class II dental composite resin restorations which have been cured by three different LED (light emitting diode) light curing modes compared to control samples cured by QTH (quartz tungsten halogen) light curing units (LCUs), to determine the most effective light curing unit and mode of curing. Results In this experimental study, class II cavities were prepared on 100 sound human premolars which have been extracted for orthodontic treatment. The teeth were randomly divided into four groups; three experimental and one control group of 25 teeth each. Experimental groups were cured by either conventional, pulse-delay, or ramped curing modes of LED. The control group was cured for 20 seconds by QTH. The restorations were thermocycled (1000 times, between 5 and 55°C, for 5 seconds dwell time), dyed, sectioned mesio-distally and viewed under stereo-microscope (40×) magnification. Teeth were then scored on a 0 to 4 scale based on the amount of microleakage. The data were analyzed by Chi-square test. No significant difference was demonstrated between the different LCUs (light curing units), or modes of curing, at the enamel side (p > 0.05). At the dentin side, all modes of LED curing could significantly reduce microleakage (p < 0.05). The results suggest that slow start curing improves marginal integrity and seal. High intense curing endangers those aims. Conclusions Comparison between the three LED mode cured composite resin restorations and QTH curing showed LED curing in all modes is more effective than QTH for reducing microleakage. Both LED and QTH almost completely eliminate the microleakage on the enamel side, however none of them absolutely eliminated microleakage on the dentin side. PMID:24990296
Adhesive and composite evaluation of acetylene-terminated phenylquinoxaline resins
NASA Technical Reports Server (NTRS)
Hergenrother, P. M.
1981-01-01
A series of acetylene-terminated phenylquinoxaline (ATPQ) oligomers of various molecular weights were prepared and subsequently chain extended by the thermally induced reaction of the ethynyl groups. The processability and thermal properties of these oligomers and their cured resins were compared with that of a relatively high molecular weight linear polyphenylquinoxaline (PPQ) with the same chemical backbone. The ATPQ oligomers exhibited significantly better processability than the linear PPQ but the PPQ displayed substantially better thermooxidative stability. Adhesive (Ti/Ti) and composite (graphite filament reinforcement) work was performed to evaluate the potential of these materials for structural applications. The PPQ exhibited better retention of adhesive and laminate properties than the ATPQ resins at 260 C after aging for 500 hr at 260 C in circulating air.
Development of lightweight graphite/polyimide sandwich panels, phases 3, 4 and 5
NASA Technical Reports Server (NTRS)
Merlette, J. B.
1972-01-01
Work performed in the last three phases of the program included: (1) face sheet processing; (2) honeycomb core manufacture; (3) face sheet-to-core bonding development; and (4) sandwich panel fabrication and testing. Resin cure studies were a major portion of this effort since processing problems traced to the polyimide matrix resin had to be resolved before quality core and face sheets could be fabricated. Honeycomb core fabrication and testing were conducted by Hexcel Corporation. A total of four graphite/polyimide resin composite cores were fabricated, tested, and reported. Two sandwich panels weighing .48 and .58 lb/sq ft, respectively were designed and fabricated which meet the support structure loads for the shuttle orbiter thermal protection system.
Properties of Two Carbon Composite Materials Using LTM25 Epoxy Resin
NASA Technical Reports Server (NTRS)
Cruz, Juan R.; Shah, C. H.; Postyn, A. S.
1996-01-01
In this report, the properties of two carbon-epoxy prepreg materials are presented. The epoxy resin used in these two materials can yield lower manufacturing costs due to its low initial cure temperature, and the capability of being cured using vacuum pressure only. The two materials selected for this study are MR50/LTM25, and CFS003/LTM25 with Amoco T300 fiber; both prepregs are manufactured by The Advanced Composites Group. MR50/LTM25 is a unidirectional prepreg tape using Mitsubishi MR50 carbon fiber impregnated with LTM25 epoxy resin. CRS003/LTM25 is a 2 by 2 twill fabric using Amoco T300 fiber and impregnated with LTM25 epoxy resin. Among the properties presented in this report are strength, stiffness, bolt bearing, and damage tolerance. Many of these properties were obtained at three environmental conditions: cold temperature/dry (CTD), room temperature/dry (RTD), and elevated temperature/wet (ETW). A few properties were obtained at room temperature/wet (RTW), and elevated temperature/dry (ETD). The cold and elevated temperatures used for testing were -125 F and 180 F, respectively. In addition, several properties related to processing are presented.
Release of Self-Healing Agents in a Material: What Happens Next?
Lee, Min Wook; Yoon, Sam S; Yarin, Alexander L
2017-05-24
A microfluidic chip-like setup consisting of a vascular system of microchannels alternatingly filled with either a resin monomer or a curing agent is used to study the intrinsic physical healing mechanism in self-healing materials. It is observed that, as a prenotched crack propagates across the chip, the resin and curing agent are released from the damaged channels. Subsequently, both the resin and the curing agent wet the surrounding polydimethylsiloxane (PDMS) matrix and spread over the crack banks until the two blobs come in contact, mix, and polymerize through an organometallic cross-linking reaction. Moreover, the polymerized domains form a system of pillars, which span the crack banks on the opposite side. This "stitching" phenomenon prevents further propagation of the crack.
Flammability of Epoxy Resins Containing Phosphorus
NASA Technical Reports Server (NTRS)
Hergenrother, P. M.; Thompson, C. M.; Smith, J. G.; Connell, J. W.; Hinkley, J. A.
2005-01-01
As part of a program to develop fire-resistant exterior composite structures for future subsonic commercial and general aviation aircraft, flame-retardant epoxy resins are under investigation. Epoxies and their curing agents (aromatic diamines) containing phosphorus were synthesized and used to prepare epoxy formulations. Phosphorus was incorporated within the backbone of the epoxy resin and not used as an additive. The resulting cured neat epoxy formulations were characterized by thermogravimetric analysis, propane torch test, elemental analysis, microscale combustion calorimetry, and fire calorimetry. Several formulations showed excellent flame retardation with phosphorous contents as low as 1.5% by weight. The fracture toughness and compressive strength of several cured formulations showed no detrimental effect due to phosphorus content. The chemistry and properties of these new epoxy formulations are discussed.
Linear and volumetric dimensional changes of injection-molded PMMA denture base resins.
El Bahra, Shadi; Ludwig, Klaus; Samran, Abdulaziz; Freitag-Wolf, Sandra; Kern, Matthias
2013-11-01
The aim of this study was to evaluate the linear and volumetric dimensional changes of six denture base resins processed by their corresponding injection-molding systems at 3 time intervals of water storage. Two heat-curing (SR Ivocap Hi Impact and Lucitone 199) and four auto-curing (IvoBase Hybrid, IvoBase Hi Impact, PalaXpress, and Futura Gen) acrylic resins were used with their specific injection-molding technique to fabricate 6 specimens of each material. Linear and volumetric dimensional changes were determined by means of a digital caliper and an electronic hydrostatic balance, respectively, after water storage of 1, 30, or 90 days. Means and standard deviations of linear and volumetric dimensional changes were calculated in percentage (%). Statistical analysis was done using Student's and Welch's t tests with Bonferroni-Holm correction for multiple comparisons (α=0.05). Statistically significant differences in linear dimensional changes between resins were demonstrated at all three time intervals of water immersion (p≤0.05), with exception of the following comparisons which showed no significant difference: IvoBase Hi Impact/SR Ivocap Hi Impact and PalaXpress/Lucitone 199 after 1 day, Futura Gen/PalaXpress and PalaXpress/Lucitone 199 after 30 days, and IvoBase Hybrid/IvoBase Hi Impact after 90 days. Also, statistically significant differences in volumetric dimensional changes between resins were found at all three time intervals of water immersion (p≤0.05), with exception of the comparison between PalaXpress and Futura Gen. Denture base resins (IvoBase Hybrid and IvoBase Hi Impact) processed by the new injection-molding system (IvoBase), revealed superior dimensional precision. Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
Studies on the structural changes during curing of epoxy and its blend with CTBN
NASA Astrophysics Data System (ADS)
Srivastava, Kavita; Rathore, Ashwani Kumar; Srivastava, Deepak
2018-01-01
Cashew nut shell liquid (CNSL), an agricultural renewable resource material, produces natural phenolic distillates such as cardanol. Cardanol condenses with formaldehyde at the ortho- and para-position of the phenolic ring under acidic or alkaline condition to yield a series of polymers of novolac- or resol-type phenolic resins. These phenolic resins may further be modified by epoxidation with epichlorohydrin to duplicate the performance of such phenolic-type novolacs (CFN). The structural changes during curing of blend samples of epoxy and carboxyl terminated poly (butadiene-co-acrylonitrile) (CTBN) were studies by Fourier-transform infrared (FTIR) spectrophotometer. The epoxy samples were synthesized by biomass material, cardanol. Blend sample was prepared by physical mixing of CTBN ranging between 0 and 20 weight percent CTBN liquid rubber into cardanol-based epoxidized novolac (CEN) resin. The FTIR spectrum of uncured blend sample clearly indicated that there appeared a band in the region of 3200-3500 cm- 1 which might be due to the presence of phenolic hydroxyl group and sbnd OH group of the opened epoxide. Pure epoxy resin showed peaks near 856 cm- 1 which might be due to oxirane functionality of the epoxidized novolac resin. Both epoxy and its blend sample was cured with polyamine. The cure temperature of CEN resin was found to be decreased by the incorporation of CTBN. The decomposition behavior was also studied by thermogravimetric analyzer (TGA). Two-step decomposition behavior was observed in both epoxy and its blend samples.
Studies on the structural changes during curing of epoxy and its blend with CTBN.
Srivastava, Kavita; Rathore, Ashwani Kumar; Srivastava, Deepak
2018-01-05
Cashew nut shell liquid (CNSL), an agricultural renewable resource material, produces natural phenolic distillates such as cardanol. Cardanol condenses with formaldehyde at the ortho- and para-position of the phenolic ring under acidic or alkaline condition to yield a series of polymers of novolac- or resol-type phenolic resins. These phenolic resins may further be modified by epoxidation with epichlorohydrin to duplicate the performance of such phenolic-type novolacs (CFN). The structural changes during curing of blend samples of epoxy and carboxyl terminated poly (butadiene-co-acrylonitrile) (CTBN) were studies by Fourier-transform infrared (FTIR) spectrophotometer. The epoxy samples were synthesized by biomass material, cardanol. Blend sample was prepared by physical mixing of CTBN ranging between 0 and 20weightpercent CTBN liquid rubber into cardanol-based epoxidized novolac (CEN) resin. The FTIR spectrum of uncured blend sample clearly indicated that there appeared a band in the region of 3200-3500cm -1 which might be due to the presence of phenolic hydroxyl group and OH group of the opened epoxide. Pure epoxy resin showed peaks near 856cm -1 which might be due to oxirane functionality of the epoxidized novolac resin. Both epoxy and its blend sample was cured with polyamine. The cure temperature of CEN resin was found to be decreased by the incorporation of CTBN. The decomposition behavior was also studied by thermogravimetric analyzer (TGA). Two-step decomposition behavior was observed in both epoxy and its blend samples. Copyright © 2017 Elsevier B.V. All rights reserved.
NASA Technical Reports Server (NTRS)
1981-01-01
Progress in the development of processes for production of Celion/LARC-160 graphite-polyimide materials, quality control methods, and the fabrication of Space Shuttle composite structure components is reported. The formulation and processing limits for three batches of resin are presented. Process improvements for simplification of the imidizing and autoclave cure cycles are described. Imidized and autoclave cured test panels were prepared. Celion/LARC-160 cure process verification and the fabrication of honeycomb sandwich panel elements and skin/stringer panels are described. C-scans of laminates imidized at 163 C to 218 C for periods from 30 to 180 minutes, and of process verification laminates made from different batches of prepreg are presented. Failure modes and load/strain characteristics of sandwich elements and C-scans of stringer to skin bond joints are also given.
Ultrasonic mixing of epoxy curing agents
NASA Technical Reports Server (NTRS)
Hodges, W. T.; St.clair, T. L.
1983-01-01
A new technique for mixing solid curing agents into liquid epoxy resins using ultrasonic energy was developed. This procedure allows standard curing agents such as 4,4 prime-diaminodiphenyl sulfone (4,4 prime-DDS) and its 3,3 prime-isomer, (3,3 prime-DDS) to be mixed without prior melting of the curing agent. It also allows curing agents such as 4,4 prime-diaminodiphenyl sulfone (4,4 prime-DDS) and its 3,3 prime-isomer, (3,3 prime-DDS) to be mixed without prior melting of the curing agent. It also allows curing agents with very high melt temperatures such as 4,4 prime-diaminobenzophenone (4,4 prime-DABP) (242 C) to be mixed without premature curing. Four aromatic diamines were ultrasonically blended into MY-720 epoxy resin. These were 4,4 prime-DDS; 3,3 prime-DDA; 4,4 prime-DABP and 3,3 prime-DABP. Unfilled moldings were cast and cured for each system and their physical and mechanical properties compared.
Poggio, C; Lombardini, M; Gaviati, S; Chiesa, M
2012-07-01
The current in vitro study evaluated Vickers hardness (VK) and depth of cure (hardness ratio) of six resin composites, polymerized with a light-emitting diode (LED) curing unit by different polymerization modes: Standard 20 s, Standard 40 s, Soft-start 40 s. SIX RESIN COMPOSITES WERE SELECTED FOR THE PRESENT STUDY: three microhybrid (Esthet.X HD, Amaris, Filtek Silorane), two nanohybrid (Grandio, Ceram.X mono) and one nanofilled (Filtek Supreme XT). The VK of the surface was determined with a microhardness tester using a Vickers diamond indenter and a 200 g load applied for 15 seconds. The mean VK and hardness ratio of the specimens were calculated using the formula: hardness ratio = VK of bottom surface / VK of top surface. For all the materials tested and with all the polymerization modes, hardness ratio was higher than the minimum value indicated in literature in order to consider the bottom surface as adequately cured (0.80). Curing time did not affect hardness ratio values for Filtek Silorane, Grandio and Filtek Supreme XT. The effectiveness of cure at the top and bottom surface was not affected by Soft-start polymerization mode.
Thermal Expansion Measurements of Polymer Matrix Composites and Syntactics
1992-04-01
828 (Shell Chemical) epoxy combined with 50.0 PBW EPON® V-40 polyamide curing agent (Shell Chemical) and Owens Corning (E-780) polyester combined 1...with 24 oz. woven roving with an Owens Corning 463 finish. " A 3 x 1, S-2 glass with 27 oz. woven roving with an Owens Corning 933 finish, nominally...wet polyester resin ( Owens Corning E-780) and subsequently processing the composites using the standard vacuum bag cure cycle for this polyester
NASA Technical Reports Server (NTRS)
Long, E. R., Jr.
1979-01-01
The Bethe-Bloch stopping power relations for inelastic collisions were used to determine the absorption of electron and proton energy in cured neat epoxy resin and the absorption of electron energy in a graphite/epoxy composite. Absorption of electron energy due to bremsstrahlung was determined. Electron energies from 0.2 to 4.0 MeV and proton energies from 0.3 to 1.75 MeV were used. Monoenergetic electron energy absorption profiles for models of pure graphite, cured neat epoxy resin, and graphite/epoxy composites are reported. A relation is determined for depth of uniform energy absorption in a composite as a function of fiber volume fraction and initial electron energy. Monoenergetic proton energy absorption profiles are reported for the neat resin model. A relation for total proton penetration in the epoxy resin as a function of initial proton energy is determined. Electron energy absorption in the composite due to bremsstrahlung is reported. Electron and proton energy absorption profiles in cured neat epoxy resin are reported for environments approximating geosynchronous earth orbit.
Imaging resin infiltration into non-cavitated carious lesions by optical coherence tomography.
Schneider, Hartmut; Park, Kyung-Jin; Rueger, Claudia; Ziebolz, Dirk; Krause, Felix; Haak, Rainer
2017-05-01
Visualisation of the etching process and resin penetration at white spot carious lesions by spectral domain optical coherence tomography (SD-OCT). The non-cavitated carious lesions (ICDAS code 2) of four visually preselected extracted human molars and premolars were verified as enamel lesions by micro computed tomography (μCT). One region of interest (ROI) per tooth was marked by two drill-holes in occlusal-cervical direction. The lesions were imaged by SD-OCT. Lesions were infiltrated (Icon, DMG) according to the manufacturer's instructions. During each treatment step and after light curing of the infiltrant, the ROIs were imaged again by SD-OCT. Teeth were sectioned through the ROIs and section layers were imaged by scanning electron microscopy in order to compare with the OCT images. The image sequences for etching and infiltration were viewed in time lapse. During the etching process, numerous bubbles formed on the lesion surface. Using OCT, the process of resin penetration into the carious lesion body became visible. The early enamel carious lesion was completely infiltrated by the resin whereas infiltration of the advanced enamel carious lesion was incomplete and inhomogeneous. Resin infiltration can be increased by optimizing the etching process. Optical coherence tomography provides information about the process and degree of resin infiltration. Active acid application before resin infiltration is recommendable. Copyright © 2017 Elsevier Ltd. All rights reserved.
700 F properties of autoclave cured PMR-II composites
NASA Technical Reports Server (NTRS)
Cifani, Diane
1988-01-01
Studies were conducted to develop autoclave processing parameters for graphite reinforced PMR-2 resin composite materials intended for use in applications at temperatures up to 371 degrees (700 F). The effect of resin composition on autoclaveability was investigated. The effect of various graphite fibers and resin composition on 343 C (650 F) and 371 C (700 F) thermo-oxidative stability and mechanical properties was also investigated. The results of the processing studies show that PMR-2 resin composites can be easily fabricated under autoclave conditions. Autoclaved laminates exposed to 1 atm of air at 343 C (650 F) and 371 C (700 F) exhibited less than 5 percent weight loss after 750 hr exposure to 650 F air and 8 percent weight loss during exposure to 700 F air for 500 hr. After 500 hr exposure, autoclaved laminates exhibited greater than 90 percent retention of initial 650 and 700 F flexural and interlaminar shear strengths. The effect of resin formulated molecular weight and postcure conditions on laminate glass transition temperature is also discussed.
The 700 F properties of autoclave cured PMR-2 composites
NASA Technical Reports Server (NTRS)
Vannucci, Raymond D.; Cifani, Diane
1988-01-01
Studies were conducted to develop autoclave processing parameters for graphite reinforced PMR-2 resin composite materials intended for use in applications at temperatures up to 371 degrees (700 F). The effect of resin composition on autoclaveability was investigated. The effect of various graphite fibers and resin composition on 343 C (650 F) and 371 C (700 F) thermo-oxidative stability and mechanical properties was also investigated. The results of the processing studies show that PMR-2 resin composites can be easily fabricated under autoclave conditions. Autoclaved laminates exposed to 1 atm of air at 343 C (650 F) and 371 C (700 F) exhibited less than 5 percent weight loss after 750 hr exposure to 650 F air and 8 percent weight loss during exposure to 700 F air for 500 hr. After 500 hr exposure, autoclaved laminates exhibited greater than 90 percent retention of initial 650 and 700 F flexural and interlaminar shear strengths. The effect of resin formulated molecular weight and postcure conditions on laminate glass transition temperature is also discussed.
Potting procedure for electronic components
NASA Technical Reports Server (NTRS)
Rubino, A. G.; Zimmerman, J.
1977-01-01
Potting process is modified to effect a match more closely between embedded electronic components, potting mediums, and thermal environment. Application of room-temperature vulcanizing silicone rubber band cured in modified thermal cycle minimizes coil-to-resin adhesion and thus lowers stresses between transformer and potting compound.
Adhesion of resin composite core materials to dentin.
O'Keefe, K L; Powers, J M
2001-01-01
This study determined (1) the effect of polymerization mode of resin composite core materials and dental adhesives on the bond strength to dentin, and (2) if dental adhesives perform as well to dentin etched with phosphoric acid as to dentin etched with self-etching primer. Human third molars were sectioned 2 mm from the highest pulp horn and polished. Three core materials (Fluorocore [dual cured], Core Paste [self-cured], and Clearfil Photo Core [light cured]) and two adhesives (Prime & Bond NT Dual Cure and Clearfil SE Bond [light cured]) were bonded to dentin using two dentin etching conditions. After storage, specimens were debonded in microtension and bond strengths were calculated. Scanning electron micrographs of representative bonding interfaces were analyzed. Analysis showed differences among core materials, adhesives, and etching conditions. Among core materials, dual-cured Fluorocore had the highest bond strengths. There were incompatibilities between self-cured Core Paste and Prime & Bond NT in both etched (0 MPa) and nonetched (3.0 MPa) dentin. Among adhesives, in most cases Clearfil SE Bond had higher bond strengths than Prime & Bond NT and bond strengths were higher to self-etched than to phosphoric acid-etched dentin. Scanning electron micrographs did not show a relationship between resin tags and bond strengths. There were incompatibilities between a self-cured core material and a dual-cured adhesive. All other combinations of core materials and adhesives produced strong in vitro bond strengths both in the self-etched and phosphoric acid-etched conditions.
Electron Beam-Cure Polymer Matrix Composites: Processing and Properties
NASA Technical Reports Server (NTRS)
Wrenn, G.; Frame, B.; Jensen, B.; Nettles, A.
2001-01-01
Researchers from NASA and Oak Ridge National Laboratory are evaluating a series of electron beam curable composites for application in reusable launch vehicle airframe and propulsion systems. Objectives are to develop electron beam curable composites that are useful at cryogenic to elevated temperatures (-217 C to 200 C), validate key mechanical properties of these composites, and demonstrate cost-saving fabrication methods at the subcomponent level. Electron beam curing of polymer matrix composites is an enabling capability for production of aerospace structures in a non-autoclave process. Payoffs of this technology will be fabrication of composite structures at room temperature, reduced tooling cost and cure time, and improvements in component durability. This presentation covers the results of material property evaluations for electron beam-cured composites made with either unidirectional tape or woven fabric architectures. Resin systems have been evaluated for performance in ambient, cryogenic, and elevated temperature conditions. Results for electron beam composites and similar composites cured in conventional processes are reviewed for comparison. Fabrication demonstrations were also performed for electron beam-cured composite airframe and propulsion piping subcomponents. These parts have been built to validate manufacturing methods with electron beam composite materials, to evaluate electron beam curing processing parameters, and to demonstrate lightweight, low-cost tooling options.
Characterization of the relationship of the cure cycle chemistry to cure cycle processing properties
NASA Technical Reports Server (NTRS)
Kranbuehl, D. E.
1986-01-01
Dynamic Dielectric measurements made over a wide range of frequency provide a sensitive and convenient means for monitoring the cure process in thermosets and thermoplastics. The measurement of dielectric relaxation is one of only a few instrumental techniques available for studying molecular properties in both the liquid and solid states. Furthermore, it is probably the only convenient experimental technique for studying the polymerization process of going from a monomeric liquid of varying viscosity to a crosslinked, insoluble, high temperature solid. The objective of the research is to develop on-line dielectric instrumentation for quantitative nondestructive material evaluation and closed loop smart cure cycle control. The key is to relate the chemistry of the cure cycle process to the dielectric properties of the polymer system by correlating the time, temperature, and frequency dependent dielectric measurements with chemical characterization measurements. Measurement of the wide variation in magnitude of the complex permittivity with both frequency and state of cure, coupled with chemical characterization work, have been shown in the laboratory to have the potential to determine: resin quality, composition and age; cure cycle window boundaries; onset of flow and point of maximum flow; extent of and completion of reaction; evolution of volatiles; T sub g; and, crosslinking and molecular weight buildup.
Leitch, B J; Worth, A J
2018-05-01
To provide veterinarians with confidence when using a commercially available epoxy resin in external skeletal fixators (ESF), testing was conducted to determine exothermia during curing of the epoxy resin compared to polymethylmethacrylate (PMMA), the hardness of the epoxy resin as a bar over 16 weeks, and the strength of the epoxy resin bar compared with metal clamps in similarly constructed Type 1a ESF constructs simulating the repair of feline long bone fractures. Exothermia of the epoxy resin during curing was tested against PMMA with surface temperatures recorded over the first 15 minutes of curing, using four samples of each product. The hardness of 90 identical epoxy resin bars was tested by subjecting them to cyclic loads (1,000 cycles of 20.5 N, every 7 days) over a 16-week period and impact testing 10 bars every 2 weeks. Ten bars that were not subjected to cyclic loads were impact tested at 0 weeks and another 10 at 16 weeks. Strength of the epoxy resin product, as a bar and clamp composite, was tested against metal SK and Kirschner-Ehmer (KE) clamps and bars in Type 1a, tied-in intramedullary pin, ESF constructs with either 90° or 75° pin placement, subjected to compressive and bending loads to 75 N. The maximum temperature during curing of the epoxy resin (min 39.8, max 43.0)°C was less than the PMMA (min 85.2, max 98.5)°C (p<0.001). There was no change in hardness of the epoxy resin bars over the 16 weeks of cyclic loading (p=0.58). There were no differences between the median strength of the epoxy resin, SK or KE ESF constructs in compression or bending when tested to 75 N (p>0.05). Stiffness of constructs with 75° pin placement was greater for SK than epoxy resin constructs in compression (p=0.046), and was greater for KE than epoxy resin constructs in bending (p=0.033). The epoxy resin tested was found to be less exothermic than PMMA; bars made from the epoxy resin showed durability over an expected fracture healing timeframe and had mechanical strength characteristics comparable to metal bar and clamp ESF constructs. The epoxy resin ESF construct tested in this study can be considered a suitable replacement for SK or KE ESF constructs in the treatment of feline long-bone fractures, in terms of mechanical strength.
Self-contained exothermic applicator and process
Koehmstedt, Paul L.
1984-01-01
An adhesive resin application system which requires no external heating apparatus, and which is operative in the absence of a reactive atmosphere, is disclosed. The system provides its own heat by employing an adhesive material containing reactants which react exothermally when electrically ignited. After ignition of the reactants, sufficient heat energy is liberated by the exothermic reaction either to plasticize a thermoplastic resin or to cure a thermosetting resin and therby bond together two closely spaced objects. This application is a continuation-in-part of application Ser. No. 489,006, filed Apr. 27, 1983, which is a continuation-in-part of application, Ser. No. 929,120, filed July 28, 1978, both now abandoned.
Rheological characterization of addition polyimide matrix resins and prepregs
NASA Technical Reports Server (NTRS)
Maximovich, M. G.; Galeos, R. M.
1984-01-01
Although graphite-reinforced polyimide matrix composites offer outstanding specific strength and stiffness, together with high thermal oxidative stability, processing problems connected with their rheological behavior remain to be addressed. The present rheological studies on neat polyimide resin systems encountered outgassing during cure. A staging technique has been developed which can successfully handle polyimide samples, and novel methods were applied to generate rheological curves for graphite-reinforced prepregs. The commercial graphite/polyimide systems studied were PRM 15, LARC 160, and V378A.
NASA Astrophysics Data System (ADS)
Tomlins, Peter H.; Rahman, Mohammed Wahidur; Donnan, Robert S.
2016-04-01
This study aimed to determine the feasibility of using optical coherence elastography to measure internal displacements during the curing phase of a light-activated, resin-based composite material. Displacement vectors were spatially mapped over time within a commercial dental composite. Measurements revealed that the orientation of cure-induced displacement vectors varied spatially in a complex manner; however, each vector showed a systematic evolution with time. Precision of individual displacements was estimated to be ˜1 to 2 μm, enabling submicrometer time-varying displacements to be detected.
Cure width potential for MOD resin composite molar restorations.
Palin, William M; Senyilmaz, Dilek P; Marquis, Peter M; Shortall, Adrian C
2008-08-01
To investigate the capability of modern light-curing units exhibiting differences in emission spectra and light source exit window dimensions, for "one-shot" full-width curing of extensive (molar MOD) resin composite restorations. Specimens of Tetric (TT), Tetric Ceram HB (TC), Tetric Evoceram (TE) and Tetric Ceram Bleach (TB) resin composites containing varying ratios of Lucirin (TPO) and/or camphorquinone (CQ) photoinitiators were packed into a bar-shaped mould (12 mm length x 2 mm width x 2 mm thickness). Each product was irradiated using a halogen (Optilux 401; QTH), a conventional LED (LEDemetron; LED) and two so-called "third generation" oval-footprint LED light-curing units (LCUs) of the same model. The latter featured bimodal emission spectra (blue and ultraviolet diodes) with either high (unmodified output) and approximately 50% (modified output) blue light intensity (UltraLume-5; ULs, ULm, respectively). Vickers hardness number was obtained across the lateral extent of the bar at 1mm increments from the centre point on both upper and lower surfaces of the specimens. Significant linear relationships (R(2)=0.71-0.98) for each distance from the central position of all LCUs were identified between measured light intensity and corresponding upper and lower surface hardness values for each product (P<0.05). No significant differences (P>0.05) were recorded in total upper surface hardness of TC or TE cured with LED (68.7+/-3.2 and 70.5+/-2.5) or ULm (56.8+/-2.0 and 57.7+/-2.0). However, upper surface hardness of TT (CQ only) cured with ULm was significantly decreased (P<0.05) compared with other LCUs. When the ratio of hardness at the edge to central positions of the bar-shaped specimens for either surface was calculated, no significant difference (P>0.05) was identified for TB (containing TPO and decreased CQ) cured with either ULs or ULm (P>0.05) and was significantly increased (P<0.05) when cured with ULs compared with LED and QTH. Variability in light intensity across the curing-tip face, spectral output of dental light-curing units and differences in product photoinitiator chemistry all influence curing efficiency significantly across the width of extensive resin composite geometries.
Mainardi, Maria do Carmo A J; Giorgi, Maria Cecília C; Lima, Débora A N L; Marchi, Giselle M; Ambrosano, Gláucia M; Paulillo, Luiz A M S; Aguiar, Flávio H B
2015-02-01
In the present study, we evaluated the influence of the photo-curing delay time and energy density on the degree of conversion and the Knoop microhardness of a resin cement. Seventy-eight samples were assigned to 13 groups (n = 6), one of which received no light curing (control). The samples were made of a dual-cured resin cement (RelyX ARC) with the aid of a Teflon matrix, submitted to one of the following energy densities (J/cm²): 7, 14, 20, and 28. Delay times were immediate (0), 1 min, or 2 min. After 24 h, the degree of conversion and microhardness were measured at three segments: cervical, medium, and apical. Data were submitted to three-way anova and Tukey's and Dunnett's tests, the latest of which was used to compare the control to the experimental groups. No interaction was observed between delay time and energy density regarding the degree of conversion. The cervical segment showed the highest values, while the apical showed the lowest. Microhardness values concerning the cervical segment in all groups were statistically different from that obtained for the control. A high-irradiance light-curing unit allows for a reduced irradiation exposure time with a short delay time, aimed at tooth restorations using a dual-cured resin cement. © 2014 Wiley Publishing Asia Pty Ltd.
NASA Astrophysics Data System (ADS)
Mosca, Rodrigo C.; Young, Nicholas; Zeituni, Carlos A.; Arany, Praveen R.
2018-02-01
The use of nanoparticle on dental light cure resin is not new, currently several compounds (nanoadditives) are used to promote better communication between the restorative material and biological tissues. The interest for this application is growing up to enhance mechanical proprieties to dental tissue cells regeneration. Bioactive nanoparticles and complex compounds with multiple functions are the major target for optimizing the restorative materials. In this work, we incorporate [Ru(bipy)3]2+ nanoparticles, that absorbs energy at 450 nm (blue-light) and emits strongly at 620 nm (red-light), in PLGA Microspheres and insert it in Dental Light Cure Resin to promote the Photobiomodulation Therapy (PBM) effects to accelerate dental pulp repair by in vitro using cytotoxicity and proliferation assay.
RAMOS, Marcelo Barbosa; PEGORARO, Thiago Amadei; PEGORARO, Luiz Fernando; CARVALHO, Ricardo Marins
2012-01-01
Objectives To determine the micro-hardness profile of two dual cure resin cements (RelyX - U100®, 3M-ESPE and Panavia F 2.0®, Kuraray) used for cementing fiber-reinforced resin posts (Fibrekor® - Jeneric Pentron) under three different curing protocols and two water storage times. Material and methods Sixty 16mm long bovine incisor roots were endodontically treated and prepared for cementation of the Fibrekor posts. The cements were mixed as instructed, dispensed in the canal, the posts were seated and the curing performed as follows: a) no light activation; b) light-activation immediately after seating the post, and; c) light-activation delayed 5 minutes after seating the post. The teeth were stored in water and retrieved for analysis after 7 days and 3 months. The roots were longitudinally sectioned and the microhardness was determined at the cervical, middle and apical regions along the cement line. The data was analyzed by the three-way ANOVA test (curing mode, storage time and thirds) for each cement. The Tukey test was used for the post-hoc analysis. Results Light-activation resulted in a significant increase in the microhardness. This was more evident for the cervical region and for the Panavia cement. Storage in water for 3 months caused a reduction of the micro-hardness for both cements. The U100 cement showed less variation in the micro-hardness regardless of the curing protocol and storage time. Conclusions The micro-hardness of the cements was affected by the curing and storage variables and were material-dependent. PMID:23138743
NASA Technical Reports Server (NTRS)
Kranbuehl, D. E.
1982-01-01
The polyimide resin, LARC-160, was prepared from diethyl-3, 3', 4,4'-benzophenone tetracarboxylate, ethyl-5-norbornene-2,3-dicarboxylate and Jeffamine AP-22. The imidization reactions of NE and BTDE were studied by HPLC, C-13-NMR and IR. NE imidizes slowly at 12 C; BTDE imidizes when the resin is heated above 100 C. Both imidization reactions proceed directly to the imide. Neither amic acid is present in significant quantities at any stage of the imidization reactions. The monomer mixture was stored at 12 C for periods up to 14 months. The effects of resin aging at this temperature on the chemical composition of the resin monomer mixture and the imidized polymer formed on curing were investigated. Aging the resin monomer mixture has the effect of partially advancing the imidization reaction. The average size of the cured polymer increases slightly with resin age.
Effect of incremental filling technique on adhesion of light-cured resin composite to cavity floor.
Chikawa, Hirokazu; Inai, Norimichi; Cho, Eitetsu; Kishikawa, Ryuzo; Otsuki, Masayuki; Foxton, Richard M; Tagami, Junji
2006-09-01
The purpose of this study was to evaluate the effect of various incremental filling techniques on adhesion between composite and cavity floor using light-cured resin composite. Black ABS resin and hybrid resin composite were used as mold materials--instead of dentin--for the preparation of cavities, and standardized to 5x5x5 mm. Each cavity was then treated with a bonding system (Clearfil SE bond). Resin composite (Clearfil Photo Core) was placed on the bonding resin using different incremental filling techniques or in bulk and irradiated for a total of 80 seconds using a halogen light unit. Specimens were subjected to the micro-tensile bond test at a crosshead speed of 1 mm/min. Data were analyzed by two-way ANOVA. The results indicated that an incremental filling technique was more effective in improving adhesion to the cavity floor than a bulk filling technique.
D'Arcangelo, Camillo; De Angelis, Francesco; Vadini, Mirco; Carluccio, Fabio; Vitalone, Laura Merla; D'Amario, Maurizio
2012-08-01
To assess the microhardness of three resin composites employed in the adhesive luting of indirect composite restorations and examine the influence of the overlay material and thickness as well as the curing time on polymerization rate. Three commercially available resin composites were selected: Enamel Plus HRI (Micerium) (ENA), Saremco ELS (Saremco Dental) (SAR), Esthet-X HD (Dentsply/DeTrey) (EST-X). Post-polymerized cylinders of 6 different thicknesses were produced and used as overlays: 2 mm, 3 mm, 3.5 mm, 4 mm, 5 mm, and 6 mm. Two-mm-thick disks were produced and employed as underlays. A standardized amount of composite paste was placed between the underlay and the overlay surfaces which were maintained at a fixed distance of 0.5 mm. Light curing of the luting composite layer was performed through the overlays for 40, 80, or 120 s. For each specimen, the composite to be cured, the cured overlay, and the underlay were made out of the same batch of resin composite. All specimens were assigned to three experimental groups on the basis of the resin composite used, and to subgroups on the basis of the overlay thickness and the curing time, resulting in 54 experimental subgroups (n = 5). Forty-five additional specimens, 15 for each material under investigation, were produced and subjected to 40, 80, or 120 s of light curing using a microscope glass as an overlay; they were assigned to 9 control subgroups (n = 5). Three Vicker's hardness (VH) indentations were performed on each specimen. Means and standard deviations were calculated. Data were statistically analyzed using 3-way ANOVA. Within the same material, VH values lower than 55% of control were not considered acceptable. The used material, the overlay thickness, and the curing time significantly influenced VH values. In the ENA group, acceptable hardness values were achieved with 3.5-mm or thinner overlays after 120 or 80 s curing time (VH 41.75 and 39.32, respectively), and with 2-mm overlays after 40 s (VH 54.13). In the SAR group, acceptable hardness values were only achieved with 2-mm-thick overlays after 120 or 80 s curing time (VH 39.81 and 29.78, respectively). In the EST-X group, acceptable hardness values were only achieved with 3-mm or thinner overlays, after 120 or 80 s curing time (VH 36.20 and 36.03, respectively). Curing time, restoration thickness, and overlay material significantly influenced the microhardness of the tested resin composites employed as luting agents. The clinician should carefully keep these factors under control.
NASA Technical Reports Server (NTRS)
Wilkes, G. L.
1982-01-01
The effects of physical aging on the material properties of some linear and network macromolecular glasses are discussed. The free volume concept is used to describe this behavior. The effect of physical aging on properties of some uniaxial graphite/fiber epoxy resin composites is investigated using stress relaxation in both tensile and flexural modes. The matrix polymers used were resins both of which are based on a 4,4-methylenedianiline derivative of epichlorohydrin with diamino diphenyl sulfone (DDS) as the curing agent. The matrix resin, as used in the practical application in composites, not fully cured and the glass transition of the network was dependent on the curing schedule. The physical aging of the bulk crosslinked epoxy was found to depend on the annealing temperature, and the T sub g of the resin. The physical aging of the composite, monitored by the stress relaxation method, was found to be dependent on the testing direction.
Yang, Yang; Gong, Hai-Huan; Song, Ai-Yang; Feng, Dan; Jin, Jie; Zhu, Song
2015-02-01
To determine the influence of denture base resins coated with antibacterial coating on water sorption, solubility and monomer elution. The values of water sorption and solubility were measured according to YY 0270-2003 and gas chromatography was used to examine the leachability of 4 commercially available heat-cured acrylic resins between experimental group and control group. Degree of crosslinking of the experimental heat-cured acrylic denture bases we remeasured by soxhlet extraction method. The data was analyzed by 17.0 software package. The values of water sorption, solubility and monomer elution of experimental group were lower compared to the control group. Degree of crosslinking of Heraeus reins was the highest among the experimental heat-cured acrylic denture bases. There is a same trend among water sorption, degree of crosslinking and the monomer elution. When the degree of crosslinking increases, the values of water sorption and monomer elution decrease. Antibacterial coating can improve the comprehensive properties of the denture base resins.
Lohitha, K; Prakash, M; Gopinadh, A; Sai Sankar, A J; Sandeep, C H; Sreedevi, B
2016-01-01
Regular usage of denture cleansers is recommended in complete denture wearers for effective plaque control, and these cleansers alter the physical properties of acrylic resin over a period of time. Thus, an in vitro study was carried out to assess the effect of denture cleansers on the color stability of heat-cure denture base resin. The aim of the present study was to evaluate the effect of commercially available fast-acting denture cleansers on the color stability of heat-cure denture base resin at different time intervals. Thirty-six heat-cure acrylic resin (Ivoclar Triplex Hot-V) specimens are randomly allocated into four groups - Group A (distilled water as control); Group B (polident - 3 min); Group C (fixodent scope plus); and Group D (stain away plus) comprising of nine samples each. After recording the baseline values, the specimens were immersed in their respective cleansing solutions for a prescribed time interval. This procedure was repeated daily, and the color change (ΔE) was evaluated after 90 and 180 days interval using a colorimeter in a standard "Commission International de l'Eclairage" color system. Paired t -test and Dunnett's T3 test. All the groups exhibited a variable color change (ΔE) for an immersion period of 90 days. However, significant color differences ( P = 0.001) were noticed among the test groups after 180 days. The color change of denture base resin was greater for Group D followed by Groups B, C, and A respectively after 180 days of immersion. The ΔE values of all test groups increased with time.
Bond performance of "Touch and Cure" adhesives on resin core systems.
Kadowaki, Yoshitaka; Kakuda, Shinichi; Kawano, Shimpei; Katsumata, Aiichiro; Ting, Shihchun; Hoshika, Shuhei; Ikeda, Takatsumi; Tanaka, Toru; Carvalho, Ricardo Marinsde; Sano, Hidehiko
2016-01-01
The purpose of this study was to compare the micro-tensile bond strength (µTBS) of three resin core composites to dentin and to examine the bonded interface of the composites. One experimental TDK-03(TD) and, two commercial, DC core Automix One (DC) and Unifil core EM(UN) were used. Flat dentin surfaces of human molars were exposed using #600 SiC paper and bonded with the respective adhesive of each system. After bonding, the composites were built up on the surfaces and cured under two conditions: "light condition" or "dark condition". µTBSs (MPa) in the light condition were: TD; 60.02±17.08, DC; 38.21±13.70, and UN; 29.50±9.71; in the dark condition: TD; 54.62±17.11, DC; 8.40±4.81, and UN; 9.47±6.56. Dark curing negatively affected the bond strength of the two commercial resin-core materials. The experimental material was not affected by the curing conditions.
Study on epoxy resin modified by polyether ionic liquid
NASA Astrophysics Data System (ADS)
Jin, X. C.; Guo, L. Y.; Deng, L. L.; Wu, H.
2017-06-01
Chloride 1-carboxyl polyether-3-methyl imidazole ionic liquid (PIIL) was synthesized. Then blended with epoxy resin(EP) to prepare the composite materials of PIIL/EP, which cured with aniline curing agent. The structure and curing performance of PIIL/EP were determined by FT-IR and DSC. The effects of the content of PIIL on strength of EP were studied. The results show that the PIIL was the target product. The strength was improved significantly with increase of the PIIL content. The obvious rubber elasticity of PIIL/EP after cured was showed when the content of PIIL accounts for 40% and the impact strength was up to 15.95kJ/m2.
Depth of cure of proximal composite resin restorations using a new perforated metal matrix.
Nguyen, Duke P; Motyka, Nancy C; Meyers, Erik J; Vandewalle, Kraig S
2018-01-01
The purpose of this study was to compare the depths of cure of a proximal box preparation filled in bulk with various approaches: filled with a bulk-fill or conventional composite; placed with a new perforated metal matrix, a traditional metal matrix, or a clear matrix; and polymerized with either occlusal-only or tri-sited light curing. After tri-sited curing, the use of the new perforated metal matrix band resulted in a depth of cure that was not significantly different from that achieved with the use of metal bands (removed during curing) or transparent matrix bands. Adequate polymerization was obtained at depths of more than 5.0 mm for the bulk-fill composite and more than 4.0 mm for the conventional composite when tri-sited light curing was used. Tri-sited light curing resulted in a significantly greater depth of cure than occlusal-only curing. The perforated metal band may be used as an alternative to the use of solid metal bands or transparent matrix bands to provide similar depths of cure for composite resins, with the possible benefits of malleability and the ability to leave the band in place during tri-sited light curing.
A cure-rate model for the Shuttle filament-wound case
NASA Technical Reports Server (NTRS)
Cagliostro, D. E.; Islas, A.; Hsu, Ming-Ta
1987-01-01
An epoxy and carbon fiber composite has been used to produce a light-weight rocket case for the Space Shuttle. A kinetic model is developed which can predict the extent of epoxy conversion during the winding and curing of the case. The model accounts for both chemical and physical kinetics. In the model, chemical kinetics occur exclusively up to the time the transition temperature equals the reaction temperature. At this point the resin begins to solidify and the rate of this process limits the rate of epoxy conversion. A comparison of predicted and actual epoxy conversion is presented for isothermal and temperature programmed cure schedules.
Bond Potential of Lithium Disilicate to Heat-Cured Polymethylmethacrylate (PMMA)
2016-06-07
Restitution of maxillary anterior esthetics with all-ceramic components. International Dental Journal , 52(1): 47-56. Albarky M, Guazzato M, Swain MV...2004). An introduction to silanes and their clinical applications in dentistry. The International Journal of Prosthodontics, 17(2): 155-164...autopolymerizing denture resin and light cured composite resin to denture teeth. International Dental Journal , 52(1): 20-24. Zarb GA and Bolender
Effects of panel density and mat moisture content on processing medium density fiberboard
Zhiyong Cai; James H. Muehl; Jerrold E. Winandy
2006-01-01
Development of a fundamental understanding of heat transfer and resin curing during hot- pressing will help to optimize the manufacturing process of medium density fiberboard (MDF) allowing increased productivity, improved product quality, and enhanced durability. Effect of mat moisture content (MC) and panel density on performance of MDF panels, heat transfer,...
Advanced manufacturing development of a composite empennage component for L-1011 aircraft
NASA Technical Reports Server (NTRS)
1978-01-01
Work continued toward the development of tooling and processing concepts required for a cocured hat/skin cover assembly. A plan was developed and implemented to develop the process for using preimpregnated T300/5208 with a resin content of 34 + or - 2 percent by weight. Use of this material results in a simplified laminating process because removal by bleeding or prebleeding is no longer required. The approach to this task basically consists of fabricating and testing flat laminated panels and simulated structural panels to verify known processing techniques relative to end-laminate quality. The flat panels were used to determine air bleeding arrangement and required cure cycle. Single and multihat-stiffened panels were fabricated using the established air bleeding arrangement and cure cycle with the resulting cured parts yielding excellent correlation of ply thickness with all surfaces clear of porosity and voids.
Modelling and simulation of cure in pultrusion processes
NASA Astrophysics Data System (ADS)
Tucci, F.; Rubino, F.; Paradiso, V.; Carlone, P.; Valente, R.
2017-10-01
Trial and error approach is not a suitable method to optimize the pultrusion process because of the high times required for the start up and the wide range of possible combinations of matrix and reinforcement. On the other hand, numerical approaches can be a suitable solution to test different parameter configuration. One of the main tasks in pultrusion processes is to obtain a complete and homogeneous resin polymerization. The formation of cross-links between polymeric chains is thermally induced but it leads to a strong exothermic heat generation, hence the thermal and the chemical phenomena are mutually affected. It requires that the two problems have to be modelled in coupled way. The mathematical model used in this work considers the composite as a lumped material, whose thermal and mechanical properties are evaluated as function of resin and fibers properties. The numerical pattern is based on a quasi-static approach in a three-dimensional Eulerian domain, which describes both thermal and chemical phenomena. The data obtained are used in a simplified C.H.I.L.E. (Cure Hardening Instantaneous Linear Elastic) model to compute the mechanical properties of the resin fraction in the pultruded. The two combined approaches allow to formulate a numerical model which takes into account the normal (no-penetration) and tangential (viscosity/friction) interactions between die and profile, the pulling force and the hydrostatic pressure of the liquid resin to evaluate the stress and strain fields induced by the process within the pultruded. The implementation of the numerical models has been carried out using the ABAQUS finite element suite, by means of several user subroutines (in Fortran language) which improve the basic software potentialities.
High performance UV and thermal cure hybrid epoxy adhesive
NASA Astrophysics Data System (ADS)
Chen, C. F.; Iwasaki, S.; Kanari, M.; Li, B.; Wang, C.; Lu, D. Q.
2017-06-01
New type one component UV and thermal curable hybrid epoxy adhesive was successfully developed. The hybrid epoxy adhesive is complete initiator free composition. Neither photo-initiator nor thermal initiator is contained. The hybrid adhesive is mainly composed of special designed liquid bismaleimide, partially acrylated epoxy resin, acrylic monomer, epoxy resin and latent curing agent. Its UV light and thermal cure behavior was studied by FT-IR spectroscopy and FT-Raman spectroscopy. Adhesive samples cured at UV only, thermal only and UV + thermal cure conditions were investigated. By calculated conversion rate of double bond in both acrylic component and maleimide compound, satisfactory light curability of the hybrid epoxy adhesive was confirmed quantitatively. The investigation results also showed that its UV cure components, acrylic and bismalimide, possess good thermal curability too. The initiator free hybrid epoxy adhesive showed satisfactory UV curability, good thermal curability and high adhesion performance.
Zhang, Hongkun; Xu, Miaojun; Li, Bin
2016-03-01
A novel phosphorus-containing compound diphenyl-(2,5-dihydroxyphenyl)-phosphine oxide defined as DPDHPPO was synthesized and used as flame retardant and curing agent for epoxy resins (EP). The chemical structure was well characterized by Fourier transform infrared (FTIR) spectroscopy, 1H, 13C and 31P nuclear magnetic resonance. The flame retardant properties, combusting performances and thermal degradation behaviors of the cured epoxy resins were investigated by limiting oxygen index (LOI), vertical burning tests (UL-94), cone calorimeter and thermogravimetric analysis (TGA) tests. The morphologies and chemical compositions of char residues for cured epoxy resins were investigated by scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS), respectively. The water resistant properties were evaluated by putting the samples into distilled water at 70 degrees C for 168 h. The results revealed that the EP/40 wt% DPDHPPO/60 wt% PDA thermosets successfully passed UL-94 V-0 flammability rating and the LOI value was as high as 31.9%. The cone tests results revealed that the incorporation of DPDHPPO efficiently reduced the combustion parameters of epoxy resins thermosets, such as heat release rate (HRR), total heat release (THR) and so on. The TGA results indicated that the introduction of DPDHPPO promoted epoxy resins matrix decomposed ahead of time compared with that of pure EP and led to a higher char yield and thermal stability at high temperature. The morphological structures and analysis of XPS of char residues revealed that DPDHPPO benefited to the formation of a sufficient, compact and homogeneous char layer with rich flame retardant elements on the epoxy resins materials surface during combustion. After water resistance tests, EP/40 wt% DPDHPPO/60 wt% PDA thermosets still remained excellent flame retardancy, the moisture absorption of epoxy resins thermosets decreased with the increase of DPDHPPO contents in the thermosets due to the existing of P-C bonds and the rigid aromatic hydrophobic structure.
Schroeder, Walter F; Cook, Wayne D; Vallo, Claudia I
2008-05-01
The present study was carried out in order to assess the suitability of N,N-dimethylaminobenzyl alcohol (DMOH) as co-initiator of camphorquinone (CQ) and 1-phenyl-1,2-propanedione (PPD) in light-cured dental resins. DMOH was synthesized and used as co-initiator for the photopolymerization of a model resin based on {2,2-bis[4-(2-hydroxy-3-methacryloxyprop-1-oxy)phenyl]propane} (Bis-GMA)/triethylene glycol dimethacrylate (TEGDMA). Experimental formulations containing CQ or PPD in combination with DMOH at different concentrations were studied. The photopolymerization was carried out by means of a commercial light-emitting diode (LED) curing unit. The evolution of double bonds consumption versus irradiation time was followed by near-infrared spectroscopy (NIR). The photon absorption efficiency (PAE) of the photopolymerization process was calculated from the spectral distribution of the LED unit and the molar absorption coefficient distributions of PPD and CQ. DMOH is an efficient photoreducer of CQ and PPD resulting in higher polymerization rate and higher double bond conversion compared with dimethylaminoethylmethacrylate. The PAE for PPD was higher than that for CQ. However, the polymerization initiated by PPD progressed at a lower rate and exhibited lower values of final conversion compared with the resins containing CQ. This observation indicates that the lower polymerization rate of the PPD/amine system should be explained in terms of the mechanism of generating primary radicals by PPD, which is less efficient compared with CQ. The DMOH/benzoyl peroxide redox system, has recently been proposed as a more biocompatible accelerator for the polymerization of bone cements based on poly(methyl methacrylate), because cytotoxity tests have demonstrated that DMOH possesses better biocompatibility properties compared with traditional tertiary amines. The results obtained in the present study reveal the suitability of the CQ/DMOH initiator system for the polymerization of light-cured dental composites.
Epoxy matrix with triaromatic mesogenic unit in dielectric spectroscopy observation
NASA Astrophysics Data System (ADS)
Włodarska, Magdalena; Mossety-Leszczak, Beata; Bąk, Grzegorz W.; Kisiel, Maciej; Dłużniewski, Maciej; Okrasa, Lidia
2018-04-01
This paper describes the dielectric response of a selected liquid crystal epoxy monomer (plain and in curing systems) in a wide range of frequency and temperature. The dielectric spectroscopy, thanks to its sensitivity, is a very good tool for studying phase transitions, reaction progress, or material properties. This sensitivity is important in the case of liquid crystal epoxy resins, where properties of the final network depend on the choice of monomers, curing agents, curing conditions and post-curing treatment, or applying an external electric or magnetic field during the reaction. In most of the obtained cured products, the collected dielectric data show two relaxation processes. The α-process is related to a structural reorientation; it can usually be linked with the glass transition and the mechanical properties of the material. The β-process can be identified as a molecular motion process, probably associated with the carboxyl groups in the mesogen. A transient Maxwell-Wagner relaxation observed in one of the compositions after the initial curing is removed by post-curing treatment at elevated temperatures. Post-curing is therefore necessary for obtaining uniformly cured products in those cases. In the investigated systems, the choice of a curing agent can change the glass transition temperature by at least 70 °C. The obtained results are in a good agreement with an earlier study employing other techniques. Finally, we assess the influence of the direction of mesogen alignment on the dielectric properties of one selected system, where a global order was induced by applying an external magnetic field in the course of curing.
Caul and method for bonding and curing intricate composite structures
NASA Technical Reports Server (NTRS)
Willden, Kurtis S. (Inventor); Goodno, Kenneth N. (Inventor)
1993-01-01
The invention disclosed here is a method for forming and curing an intricate structure of criss-crossing composite stringers and frames that are bonded to a skin panel. A structure constructed in accordance with the invention would be well-suited for use as a portion of an aircraft fuselage, a boat hull, or the like. The method is preferably practiced by applying uncured composite stringers to an uncured composite sheet panel. This is followed by placing cured frames crosswise over the stringers. The frames have openings at the locations where they intersect with the stringers which enables the frames to come into direct contact with the skin along most of their length. During the forming and curing process, the stringers are covered with a plurality of cauls, and the entire assembly of skin panel, stringers, frames and cauls is subjected to a vacuum bagging and curing process. The cauls serve to maintain both part shape and to control the flow of resin within the stringers as they are cured. Further, they probably eliminate the need for intermediate protective materials between the vacuum bag and the stringers.
Assessing the irradiance delivered from light-curing units in private dental offices in Jordan.
Maghaireh, Ghada A; Alzraikat, Hanan; Taha, Nessrin A
2013-08-01
The authors conducted a study to examine the irradiance from light-curing units (LCUs) used in dental offices in Jordan. Two of the authors visited 295 private dental offices (15 percent) in Jordan and collected the following information about the LCUs: age, type (quartz-tungsten-halogen or light-emitting diode), date of last maintenance, type of maintenance, last date of use, number of times used during the day, availability of a radiometer, exposure time for each resin-based composite increment, size of light-curing tips and presence of resin-based composite on the tips. The authors used a radiometer to measure the irradiance from the LCUs. They used linear regression with stepwise correlation for the statistical analysis. The authors set the minimum acceptable irradiance at 300 milliwatts/square centimeter. The mean irradiance of the 295 LCUs examined was 361 mW/cm(2), and 136 LCUs (46.1 percent) delivered an irradiance of less than 300 mW/cm(2). The unit's age, type and presence of resin-based composite on the light-curing tips had a significant effect on the irradiance (P ≤ .001). Only 37 of the 141 quartz-tungsten-halogen units (26.2 percent) and 122 of the 154 light-emitting diode units (79.2 percent) delivered at least 300 mW/cm(2). Resin contamination on the light-curing tips had a significant effect on the irradiance delivered. The irradiance from the LCUs decreased with use. Practical Implications. The irradiance from many of the units in this study was less than 300 mW/cm(2), which may affect the quality of resin-based composite restorations. Dentists should monitor the performance of the LCUs in their offices weekly.
Changes on degree of conversion of dual-cure luting light-cured with blue LED
NASA Astrophysics Data System (ADS)
Bandéca, M. C.; El-Mowafy, O.; Saade, E. G.; Rastelli, A. N. S.; Bagnato, V. S.; Porto-Neto, S. T.
2009-05-01
The indirect adhesive procedures constitute recently a substantial portion of contemporary esthetic restorative treatments. The resin cements have been used to bond tooth substrate and restorative materials. Due to recently introduction of the self-bonding resin luting cement based on a new monomer, filler and initiation technology has become important to study the degree of conversion of these new materials. In the present work the polymerization reaction and the filler content of dual-cured dental resin cements were studied by means of infra-red spectroscopy (FT-IR) and thermogravimetry (TG). Twenty specimens were made in a metallic mold (8 mm diameter × 1 mm thick) from each of 2 cements, Panavia® F2.0 (Kuraray) and RelyX™ Unicem Applicap (3M/ESPE). Each specimen was cured with blue LED with power density of 500 mW/cm2 for 30 s. Immediately after curing, 24 and 48 h, and 7 days DC was determined. For each time interval 5 specimens were pulverized, pressed with KBr and analyzed with FT-IR. The TG measurements were performed in Netzsch TG 209 under oxygen atmosphere and heating rate of 10°C/min from 25 to 700°C. A two-way ANOVA showed DC (%) mean values statistically significance differences between two cements ( p < 0.05). The Tukey’s test showed no significant difference only for the 24 and 48 h after light irradiation for both resin cements ( p > 0.05). The Relx-Y™ Unicem mean values were significantly higher than Panavia® F 2.0. The degree of conversion means values increasing with the storage time and the filler content showed similar for both resin cements.
Correlating cytotoxicity to elution behaviors of composite resins in term of curing kinetic.
Meng, Junquan; Yang, Huichuan; Cao, Man; Li, Lei; Cai, Qing
2017-09-01
Cytotoxicity of photocurable composite resins is a key issue for their safe use in dental restoration. Curing kinetic and elution behaviors of the composite resin would have decisive effects on its cytotoxicity. In this study, composite resins composed of bisphenol-glycidyl dimethacrylate (Bis-GMA), triethyleneglycol dimethacrylate (TEGDMA), camphorquinone (CQ), N,N-dimethylaminoethyl methacrylate (DMAEMA) and barium glass powders were prepared by setting the photoinitiators CQ/DMAEMA at 0.5wt%, 1wt% or 3wt% of the total weight of Bis-GMA/TEGDMA. The ratio of Bis-GMA/TEGDMA was 6:4, the ratio of CQ/DMAEMA was 1:1, and the incorporated inorganic powder was 75wt%. Then, curing kinetics were studied by using real-time Fourier transform infrared spectroscopy (FTIR) and photo-DSC (differential scanning calorimeter). Elution behaviors in both ethanol solution and deionized water were monitored by using liquid chromatogram/mass spectrometry (LC/MS). Cytotoxicity was evaluated by in vitro culture of L929 fibroblasts. Finally, they were all analyzed and correlated in terms of initiator contents. It was found that the commonly used 0.5wt% of photoinitiators was somewhat insufficient in obtaining composite resin with low cytotoxicity. Copyright © 2017. Published by Elsevier B.V.
NASA Technical Reports Server (NTRS)
Crivello, James V.
2000-01-01
Several new series of novel, high reactivity epoxy resins are described which are designed specifically for the fabrication of high performance carbon fiber reinforced composites for commercial aircraft structural applications using cationic UV and e-beam curing. The objective of this investigation is to provide resin matrices which rapidly and efficiently cure under low e-beam doses which are suitable to high speed automated composite fabrication techniques such as automated tape and tow placement. It was further the objective of this work to provide resins with superior thermal, oxidative and atomic oxygen resistance.
Mechanical and Thermal Properties of Dental Composites Cured with CAD/CAM Assisted Solid-State Laser
De Santis, Roberto; Gloria, Antonio; Maietta, Saverio; Martorelli, Massimo; De Luca, Alessandro; Spagnuolo, Gianrico; Riccitiello, Francesco; Rengo, Sandro
2018-01-01
Over the last three decades, it has been frequently reported that the properties of dental restorative composites cured with argon laser are similar or superior to those achieved with conventional halogen and light emitting diode (LED) curing units. Whereas laser curing is not dependent on the distance between the curing unit and the material, such distance represents a drawback for conventional curing units. However, a widespread clinical application of this kind of laser remains difficult due to cost, heavy weight, and bulky size. Recently, with regard to the radiation in the blue region of the spectrum, powerful solid-state lasers have been commercialized. In the current research, CAD (computer-aided design)/CAM (computer-aided manufacturing) assisted solid-state lasers were employed for curing of different dental restorative composites consisting of micro- and nanoparticle-reinforced materials based on acrylic resins. Commercial LED curing units were used as a control. Temperature rise during the photopolymerisation process and bending properties were measured. By providing similar light energy dose, no significant difference in temperature rise was observed when the two light sources provided similar intensity. In addition, after 7 days since curing, bending properties of composites cured with laser and LED were similar. The results suggested that this kind of laser would be suitable for curing dental composites, and the curing process does not suffer from the tip-to-tooth distance. PMID:29584683
Nejatian, Touraj; Sefat, Farshid; Johnson, Tony
2015-01-01
The fracture resistance of polymethylmethacrylate (PMMA) as the most popular denture base material is not satisfactory. Different factors can be involved in denture fracture. Among them, flexural fatigue and impact are the most common failure mechanisms of an acrylic denture base. It has been shown that there is a correlation between the static strength and fatigue life of composite resins. Therefore, the transverse strength of the denture base materials can be an important indicator of their service life. In order to improve the fracture resistance of PMMA, extensive studies have been carried out; however, only a few promising results were achieved, which are limited to some mechanical properties of PMMA at the cost of other properties. This study aimed at optimizing the packing and processing condition of heat-cured PMMA as a denture base resin in order to improve its biaxial flexural strength (BFS). The results showed that the plain type of resin with a powder/monomer ratio of 2.5:1 or less, packed conventionally and cured in a water bath for 2 h at 95 °C provides the highest BFS. Also, it was found that the performance of the dry heat processor is inconsistent with the number of flasks being loaded.
Ultra-low Temperature Curable Conductive Silver Adhesive with different Resin Matrix
NASA Astrophysics Data System (ADS)
Zhou, Xingli; Wang, Likun; Liao, Qingwei; Yan, Chao; Li, Xing; Qin, Lei
2018-03-01
The ultra-low temperature curable conductive silver adhesive with curing temperature less than 100 °C needed urgently for the surface conductive treatment of piezoelectric composite material due to the low thermal resistance of composite material and low adhesion strength of adhesive. An ultra-low temperature curable conductive adhesive with high adhesion strength was obtained for the applications of piezoelectric composite material. The microstructure, conductive properties and adhesive properties with different resin matrix were investigated. The conductive adhesive with AG-80 as the resin matrix has the shorter curing time (20min), lower curing temperature (90°C) and higher adhesion strength (7.6MPa). The resistivity of AG-80 sample has the lower value (2.13 × 10-4Ω·cm) than the 618 sample (4.44 × 10-4Ω·cm).
Mitigation and control of the overcuring effect in mask projection micro-stereolithography
NASA Astrophysics Data System (ADS)
O'Neill, Paul F.; Kent, Nigel; Brabazon, Dermot
2017-10-01
Mask Projection micro-Stereolithography (MPμSL) is an additive manufacturing technique capable of producing solid parts with micron-scale resolution from a vat of photocurable liquid polymer resin. Although the physical mechanism remains the same, the process differs from traditional laser-galvanometer based stereolithography (SL) in its use of a dynamic mask UV projector, or digital light processor (DLP), which cures each location within each 3D layer at the same time. One area where MPµSL has garnered considerable attention is in the field of microfluidics and Lab-on-a-Chip, where complex multistep microfabrication techniques adopted from the semiconductor industry are still widely used, and where MPµSL offers the ability to fabricate completely encapsulated fluidic channels in a single step and at low cost [1-3]. However, a significant obstacle exists in the prevention of channel blockage due to overcuring of the polymer resin [4, 5]. Overcuring can be attributed to the so-called `back side effect' [2] which occurs during the build process as light from successive layers penetrates into the resin to a depth greater than the layer thickness. This effect is most prevalent in channels or features oriented horizontally (in a parallel plane to that of the build platform). Currently there are two main approaches in controlling the cure depth; 1. the chemical approach, which involves doping the resin material with a chemical light absorber [6-8]; and 2. by improving the system's hardware and optical elements to improve the homogeneity of the light dosage and control the cure depth [9]. Here we investigate a third approach through modification of the 3D CAD file prior to printing to mitigate for UV light leakage from successive build layers. Although used here in conjunction with the MPμSL technique, this approach can be applied to a range of SL techniques to improve printer resolution and enable production of internal features with higher dimensional accuracy.
Interlaminar Toughening of Fiber Reinforced Polymers
NASA Astrophysics Data System (ADS)
Bian, Dakai
Modification in the resin-rich region between plies, also known as the interlaminar region, was investigated to increase the toughness of laminate composites structures. To achieve suitable modifications, the complexities of the physical and chemical processes during the resin curing procedure must be studied. This includes analyses of the interactions among the co-dependent microstructure, process parameters, and material responses. This dissertation seeks to investigate these interactions via a series of experimental and numerical analyses of the geometric- and temperature-based effects on locally interleaving toughening methods and further interlaminar synergistic toughening without interleaf. Two major weaknesses in composite materials are the brittle resin-rich interlaminar region which forms between the fiber plies after resin infusion, and the ply dropoff region which introduces stress concentration under loads. To address these weaknesses and increase the delamination resistance of the composite specimens, a dual bonding process was explored to alleviate the dropoff effect and toughen the interlaminar region. Hot melt bonding was investigated by applying clamping pressure to ductile thermoplastic interleaf and fiber fabric at an elevated temperature, while diffusion bonding between thermoplastic interleaf and thermoset resin is performed during the resin infusion. This method increased the fracture energy level and thus delamination resistance in the interlaminar region because of deep interleaf penetration into fiber bundles which helped confining crack propagation in the toughened area. The diffusion and precipitation between thermosets and thermoplastics also improved the delamination resistance by forming a semi-interpenetration networks. This phenomenon was investigated in concoctions of low-concentration polystyrene additive modified epoxy system, which facilitates diffusion and precipitation without increasing the viscosity of the system. Additionally, chemical reaction induced phase separation, concentration of polystyrene, and various curing temperatures are used to evaluate their effects on diffusion and precipitation. These effects were directly investigated by performing attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR). The diffusivity and curing kinetics experiments are performed to quantify the diffusivity coefficient of epoxy, hardener and thermoplastics, as well as the reaction rate constant of curing epoxy at various temperatures. Finally, mechanical testing and fracture surface imaging were used to quantify the improvements and characterize the toughening mechanism. Further improvement on delamination resistance was studied through the synergistic effect of combining different modification methods without the interleaf. Polysulfone molecules are end-capped with epoxide groups. Fiber surface is functionalized with amino groups to generate micro-mechanical interlocks. The interaction between two individual modifications chemically links the modified semi-interpenetration networks to the improved interfacial strength between fiber and epoxy to. The impact of the additive on the crosslinking density was examined through glass transition temperatures, and the chemical modification was characterized by Raman spectroscopy. Mode I and II fracture tests were performed to quantify the improvement of delamination resistance under pure opening and shear loads. The mechanism of synergistic effect was explained based on the fracture surface morphology and the interactions between the modification methods.
Glass Reinforcement of Various Epoxy Resins-Polyurea Systems
NASA Astrophysics Data System (ADS)
Joshi, Medha; Jauhari, Smita
2012-07-01
Polyureas (PUs) were prepared by the polycondensation reaction of disperse dyes containing -NH2 group and toluene 2, 4-diisocyanate. The disperse dyes have been prepared by coupling of various 2-diazobenzothiazoles with 1,3-benzenediamine. All the PUs were characterized by elemental analysis, spectral studies, number average molecular weight ( {overline{{Mn}} } ), and thermogravimetry. Further reaction of PUs was carried out with an epoxy resin (i.e., DGEBA). The curing study of prepared resins was monitored by differential scanning calorimeter (DSC). Based on DSC, thermograms glass fiber-reinforced composites have been laminated and characterized by chemical, mechanical, and electrical properties. The unreinforced cured resins were subjected to thermogravimetric analysis (TGA). The laminated composites showed excellent resistance properties against chemicals and good mechanical and electrical properties.
Development of new addition-type composite resins
NASA Technical Reports Server (NTRS)
Kray, R. J.
1981-01-01
The most promising of a number of new addition type polyimides and polyaromatic melamine (NCNS) resins for use in high performance composite materials. Three different cure temperature ranges were of interest: 530-560 K (500-550 F), 475-530 K (400-500 F), and 450 K (350 F). Examined were a wide variety of polyimide precursors terminated with 5 norbornene groups and addition polymerized at 560 K similar to PMR-15 and LARC-160 polyimides. In addition, a number of lower curing cinnamal end capped polyimides and a bismaleimide were investigated but were not found promising. A group of NCNS resins were investigated and some were found to be superior to current epoxy resins in moisture resistance, oxidative aging and flame and smoke properties.
Phosphorus-containing imide resins
NASA Technical Reports Server (NTRS)
Varma, I. K.; Fohlen, G. M.; Parker, J. A. (Inventor)
1985-01-01
Cured polymers of bis and tris-imides derived from tris(m-aminophenyl) phosphine oxides by reaction with maleic anhydride or its derivatives, and addition polymers of such imides, including a variant in which a monoimide is condensed with a dianhydride and the product is treated with a further quantity of maleic anhydride prior to curing are disclosed and claimed. Such polymers are flame resistant. Also disclosed are an improved method of producing tris(m-aminophenyl) phosphine oxides from the nitro analogues by reduction with hydrazine hydrate using palladized charcoal or Raney nickel as the catalyst and fiber reinforced cured resin composites.
Radiation cured polyester compositions containing metal-properties
NASA Astrophysics Data System (ADS)
Szalińska, H.; Pietrzak, M.; Gonerski, A.
The subject of the studies was unsaturated polyester resin, Polimal-109 and its compositions containing acrylates of: sodium, potassium, calcium, magnesium, barium, manganese, iron, cobalt, copper and acrylic acid. Polyester resin modified with acrylic acid salts was cured with 60Co gamma radiation. Measurements of Vicat softening temperature, water absorption, creep current resistance, volume and surface resistivity, the tangent of dielectric loss angle and permittivity of radiation cured compositions were carried out. The results of the studies presented testify to the fact that the properties of cross-linked polymers alter after ionogenic compounds have been introduced into them.
Tack, Jeremy L; Ford, David M
2008-06-01
Fully atomistic molecular dynamics (MD) simulations were used to predict the properties of diglycidyl ether of bisphenol F (DGEBF) crosslinked with curing agent diethyltoluenediamine (DETDA). This polymer is a commercially important epoxy resin and a candidate for applications in nanocomposites. The calculated properties were density and bulk modulus (at near-ambient pressure and temperature) and glass transition temperature (at near-ambient pressure). The molecular topology, degree of curing, and MD force-field were investigated as variables. The models were created by densely packing pre-constructed oligomers of different composition and connectivity into a periodic simulation box. For high degrees of curing (greater than 90%), the density was found to be insensitive to the molecular topology and precise value of degree of curing. Of the two force-fields that were investigated, cff91 and COMPASS, the latter clearly gave more accurate values for the density as compared to experiment. In fact, the density predicted by COMPASS was within 6% of reported experimental values for the highly crosslinked polymer. The predictions of both force-fields for glass transition temperature were within the range of reported experimental values, with the predictions of cff91 being more consistent with a highly cured resin.
Effect of cavity preparation on the flexural strengths of acrylic resin repairs
ELHADIRY, Safa Salim; YUNUS, Norsiah; ARIFFIN, Yusnidar Tajul
2010-01-01
Objective To investigate the effect of cavity preparation on the flexural strength of heat-curing denture resin when repaired with an auto-curing resin. Material and methods Ninety-six rectangular specimens (64x10x2.5 mm) prepared from heat-curing denture base resin (Meliodent) were randomly divided into four groups before repair. One group was left intact as control. Each repair specimen was sectioned into two; one group was repaired using the conventional repair method (Group 1). Two groups had an additional transverse cavity (2x3.5x21.5 mm) prepared prior to the repair; one repaired with (Group 2) and one without glass-fiber reinforcement (Group 3). A three-point flexural bending test according to the ISO 1567:1999 specification8 for denture base polymers was carried out on all groups after 1, 7 and 30 days of water immersion. Statistical analysis was carried out using two-way ANOVA, Kruskal Wallis and post-hoc Mann Whitney tests. Results The highest flexural strength was observed in the control group. Control and conventional repairs group (Group 1) showed reduction in the flexural strength 30 days after water immersion. No significant change in the strength was observed for Groups 2 and 3 where the repair joints were similarly prepared with additional transverse cavity. Conclusion Repaired specimens showed lower flexural strength values than intact heat-curing resin. Cavity preparation had no significant effect on the flexural strength of repair with water immersion. PMID:21308283
[A light-cured acrylic adhesive for fixing resin retention devices to the wax pattern].
Matsumura, H; Tanaka, T; Atsuta, M
1990-04-01
A light-cured acrylic adhesive for fixing resin retention devices to the wax pattern was prepared. The adhesive consisted of trimethylolpropane triacrylate, 2-ethylhexyl acrylate, benzoin methyl ether, p dimethylaminobenzaldehyde and p-methoxyphenol. The adhesive could be cured within 20 sec not only by an UV photo curing unit but by a visible-light source with a xenon lamp. The adhesive and retention beads burned out after about an hour in the electric furnace at 400 c. The metal specimens with retention devices were cast in Ag-Pd-Cu-Au alloy with the use of two types of retention beads adhesive. The light-cured adhesive was superior to the conventional one in handling and some other properties. This adhesive may be used to fabricate composite veneered prostheses with minimum errors in laboratory procedure.
Toughening reinforced epoxy composites with brominated polymeric additives
NASA Technical Reports Server (NTRS)
Nir, Z.; Gilwee, W. J., Jr. (Inventor)
1985-01-01
Cured polyfunctional epoxy resins including tris (hydroxyphenyl) methane triglycidyl ether are toughened by addition of polybrominated polymeric additives having an EE below 1500 to the pre-cure composition. Carboxy terminated butadiene acrylonitrile rubber is optionally present in the precure mixture as such or as a pre-formed copolymer with other reactants. Reinforced composites, particularly carbon reinforced composites, of these resins are disclosed and shown to have improved toughness.
Ultrasonic Mixing of Epoxy Curing Agents.
1983-05-01
Li~fl , • 4 Future generation aircraft need higher performance polymer matrices to fully achieve the weight savings possible with composite materials...ref. 1). New resins are being formulated in an effort to understand basic polymer behav- ior and to develop improved resins (refs. 2, 3 and 4). Some... polymer /curing agent combinations that could be useful, cannot be mixed properly using conven- tional methods because of the high melting temperature
Alpöz, A. Riza; Ertuḡrul, Fahinur; Cogulu, Dilsah; Ak, Asli Topaloḡlu; Tanoḡlu, Metin; Kaya, Elçin
2008-01-01
Objectives The aim of this study was to investigate microhardness and compressive strength of composite resin (Tetric-Ceram, Ivoclar Vivadent), compomer (Compoglass, Ivoclar, Vivadent), and resin modified glass ionomer cement (Fuji II LC, GC Corp) polymerized using halogen light (Optilux 501, Demetron, Kerr) and LED (Bluephase C5, Ivoclar Vivadent) for different curing times. Methods Samples were placed in disc shaped plastic molds with uniform size of 5 mm diameter and 2 mm in thickness for surface microhardness test and placed in a diameter of 4 mm and a length of 2 mm teflon cylinders for compressive strength test. For each subgroup, 20 samples for microhardness (n=180) and 5 samples for compressive strength were prepared (n=45). In group 1, samples were polymerized using halogen light source for 40 seconds; in group 2 and 3 samples were polymerized using LED light source for 20 seconds and 40 seconds respectively. All data were analyzed by two way analysis of ANOVA and Tukey’s post-hoc tests. Results Same exposure time of 40 seconds with a low intensity LED was found similar or more efficient than a high intensity halogen light unit (P>.05), however application of LED for 20 seconds was found less efficient than 40 seconds curing time (P=.03). Conclusions It is important to increase the light curing time and use appropriate light curing devices to polymerize resin composite in deep cavities to maximize the hardness and compressive strength of restorative materials. PMID:19212507
Composite structural materials
NASA Technical Reports Server (NTRS)
Ansell, G. S.; Loewy, R. G.; Wiberley, S. E.
1984-01-01
Progress is reported in studies of constituent materials composite materials, generic structural elements, processing science technology, and maintaining long-term structural integrity. Topics discussed include: mechanical properties of high performance carbon fibers; fatigue in composite materials; experimental and theoretical studies of moisture and temperature effects on the mechanical properties of graphite-epoxy laminates and neat resins; numerical investigations of the micromechanics of composite fracture; delamination failures of composite laminates; effect of notch size on composite laminates; improved beam theory for anisotropic materials; variation of resin properties through the thickness of cured samples; numerical analysis composite processing; heat treatment of metal matrix composites, and the RP-1 and RP2 gliders of the sailplane project.
Measurement of solubility and water sorption of dental nanocomposites light cured by argon laser.
Mirsasaani, Seyed Shahabeddin; Ghomi, Farhad; Hemati, Mehran; Tavasoli, Tina
2013-03-01
Different parameters used for photoactivation process and also composition provide changes in the properties of dental composites. In the present work the effect of different power density of argon laser and filler loading on solubility (SL) and water sorption (WS) of light-cure dental nanocomposites was studied. The resin of nanocomposites was prepared by mixing bisphenol A glycol dimethacrylate (Bis-GMA) and triethylene glycol dimethacrylate (TEGDMA) with a mass ratio of 65/35. 20 wt.% and 25 wt.% of nanosilica fillers with a primary particle size of 10 nm were added to the resin. Camphorquinone (CQ) and DMAEMA were added as photoinitiator system. The nanocomposites were cured by applying the laser beam at the wavelength of 472 nm and power densities of 260 and 340 mW/cm(2) for 40 sec. Solubility and water sorption were then measured according to ISO 4049, which in our case, the maximums were 2.2% and 4.3% at 260 mW/cm(2) and 20% filler, respectively. The minimum solubility (1.2%) and water sorption (3.8%) were achieved for the composite containing 25% filler cured at 340 mW/cm(2). The results confirmed that higher power density and filler loading decreased solubility of unreacted monomers and water sorption and improved physico-mechanical properties of nanocomposites.
UV-cured adhesives for carbon fiber composite applications
NASA Astrophysics Data System (ADS)
Lu, Hsiao-Chun
Carbon fiber composite materials are increasingly used in automobile, marine, and aerospace industries due to their unique properties, including high strength, high stiffness and low weight. However, due to their brittle characteristic, these structures are prone to physical damage, such as a bird strike or impact damage. Once the structure is damaged, it is important to have fast and reliable temporary repair until the permanent repair or replacement can take place. In this dissertation, UV-based adhesives were used to provide a bonding strength for temporary repair. Adhesively bonded patch repair is an efficient and effective method for temporary repair. In this study, precured patches (hard patches) and dry fabric patches with laminating resins (soft patches) were performed. UV-based epoxy adhesives were applied to both patch repair systems. For precured patch repair, the bonding strengths were investigated under different surface treatments for bonding area and different adhesives thicknesses. The shear stresses of different UV exposure times and curing times were tested. Besides, the large patch repair was investigated as well. For soft patch repair, the hand wet lay-up was applied due to high viscosity of UV resins. A modified single lap shear testing (ASTM D5868) was applied to determine the shear stress. The large patches used fiber glass instead of carbon fiber to prove the possibility of repair with UV epoxy resin by hand wet lay-up process. The hand lay-up procedure was applied and assisted by vacuum pressure to eliminate the air bubbles and consolidate the patches. To enhance the bonding strength and effective soft patch repair, vacuum assisted resin transferring molding (VaRTM) is the better option. However, only low viscosity resins can be operated by VaRTM. Hence, new UV-based adhesives were formulated. The new UV-based adhesives included photoinitiator (PI), epoxy and different solvents. Solvents were used to compound the photoinitiator into epoxy monomer. Acetone, tetrahydrofuran (THF) and chloroform were used as well as their anhydrous solvents. The UV exposure times and curing times of new UV-based resins were tested. FT-IR, DSC and DMA were used to investigate structure, glass transition temperatures(Tg) and properties of polymer. In summary, the UV-based adhesive was applied to adhesively bonded hard patch and soft patch repair. In addition, new UV-based resins were formulated for the VaRTM process. The in-field repair can be effective and efficient by using UV adhesives.
Silanated Surface Treatment: Effects on the Bond Strength to Lithium Disilicate Glass-Ceramic.
Baratto, Samantha Schaffer Pugsley; Spina, Denis Roberto Falcão; Gonzaga, Carla Castiglia; Cunha, Leonardo Fernandes da; Furuse, Adilson Yoshio; Baratto Filho, Flares; Correr, Gisele Maria
2015-10-01
The aim of this study was to evaluate the effect of silanization protocols on the bond strength of two resin cements to a lithium disilicate glass-ceramic. Thirty-two ceramic discs were assigned to 2 groups (n=16): G1 - dual-cured resin cement and G2 - light-cured resin cement. Four subgroups were evaluated according to the used silanization protocol. The glass-ceramic was etched with 10% hydrofluoric acid for 20 s and silane was applied for 1 min, as follows: CTL - according to the manufacturer's instructions; HA - dried with hot air; NWA - washed and dried with water and air at room temperature; HWA - washed and dried with hot water and hot air. Thereafter, adhesive was applied and light-cured for 20 s. Silicon molds were used to prepare resin cement cylinders (1x1 mm) on the ceramic surface. The specimens were stored in deionized water at 37 °C for 48 h and subjected to a micro-shear test. The data were submitted to statistical analysis (?#61537;=0.05). Group G1 showed higher bond strengths than G2, except for the CTL and NWA subgroups. Differences as function of the silanization protocol were only observed in G1: HWA (25.13±6.83)≥HA (22.95±7.78)≥CTL(17.44±7.24) ≥NWA(14.63±8.76). For G2 there was no difference among the subgroups. In conclusion, the silanization protocol affected the resin cement/ceramic bond strengths, depending on the material. Washing/drying with hot water and/or hot air increased only the bond strength of the dual-cured resin cement.
Auvinen, T; Tiihonen, R; Soini, M; Wangel, M; Sipponen, A; Jokinen, J J
2015-10-01
Norway spruce (Picea abies) produces resin to protect against decomposition by microbial pathogens. In vitro tests have shown that spruce resin has antifungal properties against dermatophytes known to cause nearly 90% of onychomycosis in humans. To confirm previous in vivo observations that a topical resin lacquer provides mycological and clinical efficacy, and to compare this lacquer with topical amorolfine hydrochloride lacquer and systemic terbinafine for treating dermatophyte toenail onychomycosis. In this prospective, randomized, controlled, investigator-blinded study, 73 patients with onychomycosis were randomized to receive topical 30% resin lacquer once daily for 9 months, topical 5% amorolfine lacquer once weekly for 9 months, or 250 mg oral terbinafine once daily for 3 months. The primary outcome measure was complete mycological cure at 10 months. Secondary outcomes were clinical efficacy, cost-effectiveness and patient compliance. At 10 months, complete mycological cure rates with the resin, amorolfine and terbinafine treatments were 13% [95% confidence interval (CI) 0-28], 8% (95% CI 0-19) and 56% (95% CI 35-77), respectively (P ≤ 0·002). At 10 months, clinical responses were complete in four patients (16%) treated with terbinafine, and partial in seven (30%), seven (28%) and nine (36%) patients treated with resin, amorolfine and terbinafine, respectively (P < 0·05). Resin, amorolfine and terbinafine treatments cost €41·6, €56·3 and €52·1, respectively, per patient (P < 0·001). Topical 30% resin lacquer and topical 5% amorolfine lacquer provided similar efficacy for treating dermatophyte toenail onychomycosis. However, orally administered terbinafine was significantly more effective in terms of mycological cure and clinical outcome than either topical therapy at the 10-month follow-up. © 2015 British Association of Dermatologists.
Aesthetic guidelines for second-generation indirect inlay and onlay composite restorations.
Miara, P
1998-05-01
Recent innovations in indirect composite technology and adhesive bonding procedures have resulted in the development of advanced materials particularly suited for inlay and onlay restorations. Microhybrid composite resins are characterized by a filler/matrix ratio that is significantly greater than that of earlier materials. This article reviews the physical properties and clinical application of these "second-generation" composite resins, with emphasis on a system that utilizes a heat-curing process in conjunction with nitrogen pressure to fabricate a material with improved mechanical and aesthetic properties.
Material Property Characterization of AS4/VRM-34 Textile Laminates
NASA Technical Reports Server (NTRS)
Grenoble, Ray W.; Johnston, William M
2013-01-01
Several material properties (modulus, strengths, and fracture toughness) of a textile composite have been evaluated to provide input data to analytical models of Pultruded Rod Stiffened Efficient Unitized Structure (PRSEUS). The material system is based on warp-knitted preforms of AS4 carbon fibers and VRM-34 epoxy resin, which have been processed via resin infusion and oven curing. Tensile, compressive, shear, and fracture toughness properties have been measured at ambient and elevated temperatures. All specimens were tested in as-fabricated (dry) condition. Specimens were tested with and without through-thickness stitching.
Bismaleimide resins for flame resistant honeycomb sandwich panels
NASA Technical Reports Server (NTRS)
1978-01-01
A 60 kg batch of Resin M751 was produced in pilot plant scale. The resin was delivered to the prepreg company as an NMP solution. 100 kg of glass-fabric prepregs were fabricated. Prepreg characteristics and curing cycles for laminate fabrication were provided. A new batch of Resin M756 (Code M756 - 2) was synthesized.
Creep of experimental short fiber-reinforced composite resin.
Garoushi, Sufyan; Kaleem, Muhammad; Shinya, Akikazu; Vallittu, Pekka K; Satterthwaite, Julian D; Watts, David C; Lassila, Lippo V J
2012-01-01
The purpose of this study was to investigate the reinforcing effect of short E-glass fiber fillers oriented in different directions on composite resin under static and dynamic loading. Experimental short fiber-reinforced composite resin (FC) was prepared by mixing 22.5 wt% of short E-glass fibers, 22.5 wt% of resin, and 55 wt% of silane-treated silica fillers. Three groups of specimens (n=5) were tested: FC with isotropic fiber orientation, FC with anisotropic fiber orientation, and particulate-filled composite resin (PFC) as a control. Time-dependent creep and recovery were recorded. ANOVA revealed that after secondary curing in a vacuum oven and after storage in dry condition for 30 days, FC with isotropic fiber orientation (1.73%) exhibited significantly lower static creep value (p<0.05) than PFC (2.54%). For the different curing methods and storage conditions evaluated in this study, FC achieved acceptable static and dynamic creep values when compared to PFC.
Light-attenuating effect of dentin on the polymerization of light-activated restorative resins.
Arikawa, Hiroyuki; Kanie, Takahito; Fujii, Koichi; Ban, Seiji; Takahashi, Hideo
2004-12-01
The light-attenuating effect of dentin on the mechanical properties of light-activated composite resins was evaluated using a simple experimental filter. The filter was designed to simulate the light transmittance and light diffusion characteristics of 1.0-mm thick dentin. The depth of cure, surface hardness, and flexural strength for 13 shades of three light-activated restorative resins were examined. These resins were cured either using direct irradiation with a light source, or indirect irradiation through the filter. The attenuation of light intensity by 1.0-mm thick dentin reached 85-90% in the 400-550 nm wavelength region. For all materials, the values of depth of cure, surface hardness on the top and bottom surfaces, and flexural strength of specimens irradiated indirectly through the simulated 1.0-mm thick dentin filter decreased by 37-60%, 16-55%, 50-83%, and 44-82% in comparison with those by direct irradiation, respectively. Recovery from mechanical properties' reduction was achieved when materials were irradiated 1.5-4 times longer than the standard irradiation time.
da Silva, Gisele Rodrigues; Simamoto-Júnior, Paulo Cezar; da Mota, Adérito Soares; Soares, Carlos José
2007-03-01
This study aimed to analyze the microhardness (KHN) and diametral tensile strength (DTS) of two hybrid resin composites (TPH Spectrum and Filtek Z250). To this end, the composites were polymerized with six laboratory photo-curing units (LPUs) and the results compared with an alternative polymerization method using conventional halogen light source in conjunction with additional polymerization in an autoclave (15 minutes/100 degrees C). LPUs were used following the manufacturers' instructions. Diametral tensile strength and Knoop hardness tests were conducted for all groups (n=5). Data were statistically compared using ANOVA and Tukey's test (alpha = 0.05). Among the LPUs, the one that provided light curing in conjunction with heat and nitrogen pressure resulted in a significant increase in KHN and DTS of resin composites. Between the resin composites, Filtek Z250 showed higher hardness values than TPH Spectrum. It was concluded that the use of alternative polymerization with conventional light polymerization and autoclave was feasible with a wide implication for the general public in terms of reduced dental treatment cost.
Arikawa, Hiroyuki; Takahashi, Hideo; Kanie, Takahito; Ban, Seiji
2009-07-01
The purpose of this study was to investigate effects of various visible light photoinitiators on the polymerization efficiency and color of the light-activated resins. Four photoinitiators, including camphorquinone, phenylpropanedione, monoacrylphosphine oxide (TPO), and bisacrylphosphine oxide (Ir819), were used. Each photoinitiator was dissolved in a Bis-GMA and TEGDMA monomer mixture. Materials were polymerized using dental quartz-tungsten halogen lamp (QTH), plasma-ark lamp and blue LED light-curing units, and a custom-made violet LED light unit. The degree of monomer conversion and CIE L*a*b* color values of the resins were measured using a FTIR and spectral transmittance meter. The degree of monomer conversions of TPO- and Ir819-containing resins polymerized with the violet-LED unit were higher than camphorquinone-containing resin polymerized with the QTH light-curing unit. The lowest color values were observed for the TPO-containing resin. Our results indicate that the TPO photoinitiator and the violet-LED light unit may provide a useful and improved photopolymerization system for dental light-activated resins.
Chu, Wei-Cheng; Chiang, Shih-Fan; Li, Jheng-Guang; Kuo, Shiao-Wei
2013-01-01
After blending the triblock copolymer, poly(ethylene oxide-b-propylene oxide-b-ethylene oxide) (PEO-b-PPO-b-PEO) with novolac-type phenolic resin, Fourier transform infrared spectroscopy revealed that the ether groups of the PEO block were stronger hydrogen bond acceptors for the OH groups of phenolic resin than were the ether groups of the PPO block. Thermal curing with hexamethylenetetramine as the curing agent resulted in the triblock copolymer being incorporated into the phenolic resin, forming a nanostructure through a mechanism involving reaction-induced microphase separation. Mild pyrolysis conditions led to the removal of the PEO-b-PPO-b-PEO triblock copolymer and formation of mesoporous phenolic resin. This approach provided a variety of composition-dependent nanostructures, including disordered wormlike, body-centered-cubic spherical and disorder micelles. The regular mesoporous novolac-type phenolic resin was formed only at a phenolic content of 40–60 wt %, the result of an intriguing balance of hydrogen bonding interactions among the phenolic resin and the PEO and PPO segments of the triblock copolymer. PMID:28788378
Keogh, Pauraic; Ray, Noel J; Lynch, Christopher D; Burke, Francis M; Hannigan, Ailish
2004-12-01
This investigation determined the minimum exposure times consistent with optimised surface microhardness parameters for a commercial resin composite cured using a "first-generation" light-emitting diode activation lamp. Disk specimens were exposed and surface microhardness numbers measured at the top and bottom surfaces for elapsed times of 1 hour and 24 hours. Bottom/top microhardness number ratios were also calculated. Most microhardness data increased significantly over the elapsed time interval but microhardness ratios (bottom/top) were dependent on exposure time only. A minimum exposure of 40 secs is appropriate to optimise microhardness parameters for the combination of resin composite and lamp investigated.
NASA Technical Reports Server (NTRS)
Roberts, Gary D.; Malarik, Diane C.; Robaidek, Jerrold O.
1991-01-01
The viscoelastic properties of an addition-cured polyimide, PMR-15, were evaluated through dynamic mechanical and stress relaxation testing. Below the glass transition temperature, the dynamic mechanical properties of the composites are strongly affected by the absorbed moisture in the resin. At temperature 20 C and more above the glass transition temperature, the storage modulus increases continuously with time, indicating that additional crosslinking is occurring in the resin. For resin moisture contents less than 2 percent, stress relaxation curves measured at different temperatures can be superimposed using horizontal shifts along the log(time) axis with only small shifts along the vertical axis.
Souza-Junior, Eduardo José; Borges, Boniek Castillo Dutra; Montes, Marcos Antônio Japiassú Resende; Alonso, Roberta Caroline Bruschi; Ambrosano, Glaucia Maria Bovi; Sinhoreti, Mário Alexandre Coelho
2012-01-01
This study evaluated the impact of extended etching and bonding strategies on the microshear bond strength of three sealant materials. Two pit-and-fissure sealants [FluroShield, Dentsply (light-cured) and AlphaSeal, DFL (self-cured)] and one light-cured flowable composite resin (Permaflo, Ultradent) were evaluated according to different enamel etching times (15 s or 30 s) and bonding procedures (no adhesive application, application of primer/hydrophobic resin or hydrophobic resin only). Intact enamel blocks were obtained from bovine teeth and sealed via the tested protocols. After 24 h, the microshear bond strength test was performed in a universal testing machine at a crosshead speed of 0.5 mm/min. Failure modes were classified by stereomicroscopy. Data were submitted to a three-way ANOVA and to Tukey's test (α=0.05). There was no statistically significant difference (p>0.05) among the materials. Permaflo showed higher bond strength when etched for 30 s alone. Enamel overetching decreased the bond strength of the light-cured sealant. Primer/bond previous treatment improved bond performance for AlphaSeal. In conclusion, from the tested conditions, all sealant materials presented similar bond strength values in relation to bonding protocol and etching time. The flowable composite can be used as a pit-and-fissure sealant. The use of a three-step adhesive system was essential for the self-cured sealant application.
Cytotoxicity and cytokine expression induced by silorane and methacrylate-based composite resins.
Longo, Daniele Lucca; Paula-Silva, Francisco Wanderley Garcia; Faccioli, Lucia Helena; Gatón-Hernández, Patrícia Maria; Queiroz, Alexandra Mussolino de; Silva, Léa Assed Bezerra da
2016-01-01
The aim of this study was to evaluate cytotoxicity and cytokine production induced by light-cured or non-light-cured methacrylate-based and silorane composite resins in RAW 264.7 macrophages. Cells were stimulated with the extracts from light-cured or non-light-cured composite resins. After incubation for 24 h, cytotoxicity was assessed with the lactate dehydrogenase (LDH) and methyl thiazolyl tetrazolium (MTT) assays, and total protein was quantified using the Lowry method. TNF-α detection was examined with an enzyme-linked immunosorbent assay (ELISA) conducted with cell supernatants after cell stimulation for 6, 12, and 24 h. Data were analyzed using one-way analysis of variance (ANOVA) and Tukey's post hoc test (α=0.05). KaloreTM and FiltekTM Silorane were cytotoxic with or without light curing (p<0.05) after 24 h of incubation. KaloreTM stimulated the early production of TNF-α in comparison with control (p<0.05), whereas FiltekTM Silorane did not affect TNF-α levels after 6 and 12 h (p>0.05). However, after 24 h FiltekTM Silorane inhibited the production of TNF-α (p<0.05). KaloreTM and FiltekTM Silorane were cytotoxic regardless of light curing. The extract obtained from KaloreTM after 15 days of incubation stimulated the production of TNF-α, unlike that obtained from FiltekTM Silorane.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Paulauskas, F.L.
The objective of this work was to investigate the beneficial effect of the variable frequency microwave (VFM) technology to cure thermosetting prepreg laminates. Further, it was to investigate the interrelationship and effect on the curing process of frequency, band width, and curing time with different types of laminates. Previous studies of microwave-assisted curing of neat resins (epoxy) and unidirectional glass and carbon fiber laminates with a fixed frequency of 2.45 GHz, have shown that a substantial reduction in the curing time was obtained. Results of this earlier work indicate that the microwave-assisted curing of multidirectional glass fiber laminates also showmore » a substantial reduction of the required curing time. This may be explained by the penetration of microwave energy directly and throughout the laminate with enhancement of the kinetics of the chemical reaction. The fixed frequency microwave radiation of 2.45 GHz has been demonstrated to be a partially acceptable method to cure unidirectional carbon fiber laminates. Multidirectional carbon fiber/epoxy laminates demonstrate a lack of coupling during the curing process. A direct curing of these laminates was not possible by microwave radiation with the experimental approach used in agreement with previous work. In addition to this short coming, the unidirectional laminate samples cured with the fixed frequency are visually nonuniform. Localized areas of darker colors (burn, hot spots, overheating) are attributed to the formation of standing waves within the microwave cavity. For this reason, the laminates are subject to proper rotation while curing through fixed frequency. The present research indicates that variable frequency microwave technology is a sound and acceptable processing method to effectively cure uni-, bi- or multi-directional thermosetting glass fiber laminates. Also, this methodology will effectively cure unidirectional thermosetting carbon fiber laminates. For all these cases, this technology yielded a substantial reduction in the required cure time of these laminates. Multidirectional carbon fiber laminates demonstrated a lack of coupling of VFM energy during the curing process.« less
Phenylethynyl Terminated Imide (PETI) Composites Made by High Temperature Vartm
NASA Technical Reports Server (NTRS)
Ghose, Sayata; Watson, Kent A.; Cano, Roberto J.; Britton, Sean M.; Jensen, Brian J.; Connell, John W.; Herring, Helen M.; Lineberry, Quentin J.
2010-01-01
The use of composites as primary structures on aerospace vehicles has increased dramatically over the past decade. As these advanced structures increase in size and complexity, their production costs have grown significantly. A major contributor to these manufacturing costs is the requirement of elevated pressures, during high temperature processing, to create fully consolidated composite parts. Recently, NASA Langley has licensed a series of low viscosity Phenyl Ethynyl Terminated Imide, PETI, oligomers that possess a wide processing window to allow for Resin Transfer Molding, RTM, processing. These resins, PETI-8 and PETI-330, demonstrate void fractions of approx.1% under elevated pressure consolidation. However, when used with a standardized thermal curing cycle in a High Temperature Vacuum Assisted RTM (HT-VARTM) process, they display undesirable void contents in excess of 7%. It was determined previously that under the thermal cycles used for laminate fabrication, the phenylethynyl endcap underwent degradation leading to volatile evolution. Modifications to the processing cycle used in the laminate fabrication have reduced the void content significantly (typically less than 3%) for carbon fiber biaxially woven fabric. For carbon fiber uniaxial fabric, void contents of less than 2% have been obtained using both PETI-8 and PETI-330. The resins were infused into carbon fiber preforms at 260 C and cured between 316 C and 371 C. Photomicrographs of the panels were taken and void contents were determined by acid digestion. Mechanical properties of the panels were determined at both room and elevated temperatures. These include short beam shear and flexure tests. The results of this work are presented herein.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Jones, Brad H.; Wheeler, David R.; Black, Hayden T.
Physical stress relaxation in rubbery, thermoset polymers is limited by cross-links, which impede segmental motion and restrict relaxation to network defects, such as chain ends. In parallel, the cure shrinkage associated with thermoset polymerizations leads to the development of internal residual stress that cannot be effectively relaxed. Recent strategies have reduced or eliminated such cure stress in thermoset polymers largely by exploiting chemical relaxation processes, wherein temporary cross-links or otherwise transient bonds are incorporated into the polymer network. In this paper, we explore an alternative approach, wherein physical relaxation is enhanced by the incorporation of organometallic sandwich moieties into themore » backbone of the polymer network. A standard epoxy resin is cured with a diamine derivative of ferrocene and compared to conventional diamine curing agents. The ferrocene-based thermoset is clearly distinguished from the conventional materials by reduced cure stress with increasing cure temperature as well as unique stress relaxation behavior above its glass transition in the fully cured state. The relaxation experiments exhibit features characteristic of a physical relaxation process. Furthermore, the cure stress is observed to vanish precipitously upon deliberate introduction of network defects through an increasing imbalance of epoxy and amine functional groups. Finally, we postulate that these beneficial properties arise from fluxional motion of the cyclopentadienyl ligands on the polymer backbone.« less
Difference in the color stability of direct and indirect resin composites
LEE, Yong-Keun; YU, Bin; LIM, Ho-Nam; LIM, Jin Ik
2011-01-01
Indirect resin composites are generally regarded to have better color stability than direct resin composites since they possess higher conversion degree Objective The present study aimed at comparing the changes in color (∆E) and color coordinates (∆L, ∆a and ∆b) of one direct (Estelite Sigma: 16 shades) and 2 indirect resin composites (BelleGlass NG: 16 shades; Sinfony: 26 shades) after thermocycling. Material and Methods Resins were packed into a mold and light cured; post-curing was performed on indirect resins. Changes in color and color coordinates of 1-mm-thick specimens were determined after 5,000 cycles of thermocycling on a spectrophotometer. Results ∆E values were in the range of 0.3 to 1.2 units for direct resins, and 0.3 to 1.5 units for indirect resins, which were clinically acceptable (∆E<3.3). Based on t-test, ∆E values were not significantly different by the type of resins (p>0.05), while ∆L, ∆a and ∆b values were significantly different by the type of resins (p<0.05). For indirect resins, ∆E values were influenced by the brand, shade group and shade designation based on three-way ANOVA (p<0.05). Conclusion Direct and indirect resin composites showed similar color stability after 5,000 cycles of thermocycling; however, their changes in the color coordinates were different. PMID:21552717
Mechanical properties of resin cements with different activation modes.
Braga, R R; Cesar, P F; Gonzaga, C C
2002-03-01
Dual-cured cements have been studied in terms of the hardness or degree of conversion achieved with different curing modes. However, little emphasis is given to the influence of the curing method on other mechanical properties. This study investigated the flexural strength, flexural modulus and hardness of four proprietary resin cements. Materials tested were: Enforce and Variolink II (light-, self- and dual-cured), RelyX ARC (self- and dual-cured) and C & B (self-cured). Specimens were fractured using a three-point bending test. Pre-failure loads corresponding to specific displacements of the cross-head were used for flexural modulus calculation. Knoop hardness (KHN) was measured on fragments obtained after the flexural test. Tests were performed after 24 h storage at 37 degrees C. RelyX ARC dual-cured showed higher flexural strength than the other groups. RelyX ARC and Variolink II depended upon photo-activation to achieve higher hardness values. Enforce showed similar hardness for dual- and self-curing modes. No correlation was found between flexural strength and hardness, indicating that other factors besides the degree of cure (e.g. filler content and monomer type) affect the flexural strength of composites. No statistical difference was detected in the flexural modulus among the different groups.
Almaroof, A; Rojo, L; Mannocci, F; Deb, S
2016-02-01
To formulate and evaluate new dual cured resin composite based on the inclusion of eugenyl methacrylate monomer (EgMA) with Bis-GMA/TEGDMA resin systems for intracanal post cementation and core build-up restoration of endodontically treated teeth. EgMA was synthesized and incorporated at 5% (BTEg5) or 10% (BTEg10) into dual-cure formulations. Curing properties, viscosity, Tg, radiopacity, static and dynamic mechanical properties of the composites were determined and compared with Clearfil™DC Core-Plus, a commercial dual-cure, two-component composite. Statistical analysis of the data was performed with ANOVA and the Tukey's post-hoc test. The experimental composites were successfully prepared, which exhibited excellent curing depths of 4.9, 4.7 and 4.2 mm for BTEg0, BTEg5 and BTEg10 respectively, which were significantly higher than Clearfil™DC. However, the inclusion of EgMA initially led to a lower degree of cure, which increased when measured at 24 h with values comparable to formulations without EgMA, indicating post-curing. The inclusion of EgMA also lowered the polymerization exotherm thereby reducing the potential of thermal damage to host tissue. Both thermal and viscoelastic analyses confirmed the ability of the monomer to reduce the stiffness of the composites by forming a branched network. The compressive strength of BTEg5 was significantly higher than the control whilst flexural strength increased significantly from 95.9 to 114.8 MPa (BTEg5) and 121.9 MPa (BTEg10). Radiopacity of the composites was equivalent to ∼3 mm Al allowing efficient diagnosis. The incorporation of EgMA within polymerizable formulations provides a novel approach to prepare reinforced resin composite material for intracanal post cementation and core build-up and the potential to impart antibacterial properties of eugenol to endodontic restorations. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
Tetraglycidyl epoxy resins and graphite fiber composites cured with flexibilized aromatic diamines
NASA Technical Reports Server (NTRS)
Delvigs, P.
1986-01-01
Studies were performed to synthesize new ether modified, flexibilized aromatic diamine hardeners for curing epoxy resins. The effect of moisture absorption on the glass transition temperatures of a tetraglycidyl epoxy, MY 720, cured with flexibilized hardeners and a conventional aromatic diamine was studied. Unidirectional composites, using epoxy-sized Celion 6000 graphite fiber as the reinforcement, were fabricated. The room temperature and 300 F mechanical properties of the composites, before and after moisture exposure, were determined. The Mode I interlaminar fracture toughness of the composites was characterized using a double cantilever beam technique to calculate the critical strain energy release rate.
Molecular Mobility in Hyperbranched Polymers and Their Interaction with an Epoxy Matrix
Román, Frida; Colomer, Pere; Calventus, Yolanda; Hutchinson, John M.
2016-01-01
The molecular mobility related to the glass transition and secondary relaxations in a hyperbranched polyethyleneimine, HBPEI, and its relaxation behaviour when incorporated into an epoxy resin matrix are investigated by dielectric relaxation spectroscopy (DRS) and dynamic mechanical analysis (DMA). Three systems are analysed: HBPEI, epoxy and an epoxy/HBPEI mixture, denoted ELP. The DRS behaviour is monitored in the ELP system in three stages: prior to curing, during curing, and in the fully cured system. In the stage prior to curing, DRS measurements show three dipolar relaxations: γ, β and α, for all systems (HBPEI, epoxy and ELP). The α-relaxation for the ELP system deviates significantly from that for HBPEI, but superposes on that for the epoxy resin. The fully cured thermoset displays both β- and α-relaxations. In DMA measurements, both α- and β-relaxations are observed in all systems and in both the uncured and fully cured systems, similar to the behaviour identified by DRS. PMID:28773319
Tanaka, T; Nakabayashi, N; Masuhara, E
1978-07-01
The whitish translucent shade of a thermosetting resin cured from a mixture of a 2,2-Bis (p-methacryloxy (ethoxy)1-2 phenyl)-propane monomer and PMMA pearls makes it difficult to reconstruct a shade of the natural tooth. The attempt to improve the transparency of the mixed polymer was made in this study. Varying the molecular weight of BisMEPP monomer, PMMA polymer and curing temperature, cured specimens were prepared and their transparency was measured with a spectrophotometer. The results obtained are as follows. 1) In any molecular weight of PMMA, BisMEPP with 2.3 to 3.3 average number of ethylene oxide linkage showed the highest transpalency on the specimen. 2) With increasing the curing temperature, transpalency of the specimens made from BisME4.0 PP increased. With another molecular of BisMEPP, transpalency of the cured specimens showed the highest transpalency at the curing temperature of 120 degrees C. 3) With increasing the molecular weight of PMMA, the transpalency increased.
Hybrid Composite Cryogenic Tank Structure
NASA Technical Reports Server (NTRS)
DeLay, Thomas
2011-01-01
A hybrid lightweight composite tank has been created using specially designed materials and manufacturing processes. The tank is produced by using a hybrid structure consisting of at least two reinforced composite material systems. The inner composite layer comprises a distinct fiber and resin matrix suitable for cryogenic use that is a braided-sleeve (and/or a filamentwound layer) aramid fiber preform that is placed on a removable mandrel (outfitted with metallic end fittings) and is infused (vacuum-assisted resin transfer molded) with a polyurethane resin matrix with a high ductility at low temperatures. This inner layer is allowed to cure and is encapsulated with a filamentwound outer composite layer of a distinct fiber resin system. Both inner and outer layer are in intimate contact, and can also be cured at the same time. The outer layer is a material that performs well for low temperature pressure vessels, and it can rely on the inner layer to act as a liner to contain the fluids. The outer layer can be a variety of materials, but the best embodiment may be the use of a continuous tow of carbon fiber (T-1000 carbon, or others), or other high-strength fibers combined with a high ductility epoxy resin matrix, or a polyurethane matrix, which performs well at low temperatures. After curing, the mandrel can be removed from the outer layer. While the hybrid structure is not limited to two particular materials, a preferred version of the tank has been demonstrated on an actual test tank article cycled at high pressures with liquid nitrogen and liquid hydrogen, and the best version is an inner layer of PBO (poly-pphenylenebenzobisoxazole) fibers with a polyurethane matrix and an outer layer of T-1000 carbon with a high elongation epoxy matrix suitable for cryogenic temperatures. A polyurethane matrix has also been used for the outer layer. The construction method is ideal because the fiber and resin of the inner layer has a high strain to failure at cryogenic temperatures, and will not crack or produce leaks. The outer layer serves as more of a high-performance structural unit for the inner layer, and can handle external environments.
Adhesion of Candida albicans to Vanillin Incorporated Self-Curing Orthodontic PMMA Resin.
NASA Astrophysics Data System (ADS)
Zam, K.; Sawaengkit, P.; Thaweboon, S.; Thaweboon, B.
2018-02-01
It has been observed that there is an increase in Candida carriers during the treatment with orthodontic removable appliance. Vanillin is flavouring agent, which is known to have antioxidant and antimicrobial properties. The aim of this study was to evaluate the effect of vanillin incorporated PMMA on adhesion of Candida albicans. A total of 36 orthodontic self-curing PMMA resin samples were fabricated. The samples were divided into 3 groups depending on percentage of vanillin incorporated (0.1%, 0.5% and PMMA without vanillin as control). PMMA samples were coated with saliva. The adhesion assay was performed with C. albicans (ATCC 10231). The adherent yeast cells were stained with crystal violet and counted under microscope by random selection of 3 fields at 10X magnification. The statistical analyses performed by Kruskal Wallis and Mann Whitney non-parametric test. It was found that the PMMA resin samples with vanillin incorporation significantly reduced the adhesion of C. albicans as compared to the control group. This study indicates that vanillin incorporated resin can impede the adhesion of C. albicans to about 45 - 56 %. With further testing and development, vanillin can be employed as an antifungal agent to prevent adhesion of C. albicans to orthodontic self-curing PMMA resin.
Translucency changes of direct esthetic restorative materials after curing, aging and treatment
2016-01-01
The purpose of this article was to review the changes in translucency of direct esthetic restorative materials after curing, aging and treatment. As a criterion for the evaluation of clinical translucency changes, visual perceptibility threshold in translucency parameter difference (ΔTP) of 2 was used. Translucency changes after curing were perceivable depending on experimental methods and products (largest ΔTP in resin composites = 15.9). Translucency changes after aging were reported as either relatively stable or showed perceivable changes by aging protocols (largest ΔTP in resin composites = -3.8). Translucency changes after curing, aging and treatment were perceivable in several products and experimental methods. Therefore, shade matching of direct esthetic materials should be performed considering these instabilities of translucency in direct esthetic materials. PMID:27847744
Design, Development, and Testing of Advanced Bridge Structures
1993-12-23
experiment used a reduced EEW resin (215) with Hycar CTBN 1872 being added with the curing agent, rather than the resin . The result was a very... resins are mainly phenolics , carbon monoxide and water. Thermal decomposition products should therefore be treated as potentially hazardous substances...26 2.3.5 Chemical Surface Modification ............................................. 26 2.3.5.1 Resin Impregnation of a Swelled
Kim, Tae-Wan; Lee, Jang-Hoon; Jeong, Seung-Hwa; Ko, Ching-Chang; Kim, Hyung-Il; Kwon, Yong Hoon
2015-04-01
The purpose of the present study was to investigate the usefulness of 457 and 473 nm lasers for the curing of composite resins during the restoration of damaged tooth cavity. Monochromaticity and coherence are attractive features of laser compared with most other light sources. Better polymerization of composite resins can be expected. Eight composite resins were light cured using these two lasers and a light-emitting diode (LED) light-curing unit (LCU). To evaluate the degrees of polymerization achieved, polymerization shrinkage and flexural and compressive properties were measured and compared. Polymerization shrinkage values by 457 and 473 nm laser, and LED ranged from 10.9 to 26.8, from 13.2 to 26.1, and from 11.5 to 26.3 μm, respectively. The values by 457 nm laser was significantly different from those by 473 and LED LCU (p<0.05). However, there was no statistical difference between values by 473 and LED LCU. Before immersion in distilled water, flexural strength (FS) and compressive modulus (CM) of the specimens were inconsistently influenced by LCUs. On the other hand, flexural modulus (FM) and compressive strength (CS) were not significantly different for the three LCUs (p>0.05). For the tested LCUs, no specific LCU could consistently achieve highest strength and modulus from the specimens tested. Two lasers (457 and 473 nm) can polymerize composite resins to the level that LED LCU can achieve despite inconsistent trends of polymerization shrinkage and flexural and compressive properties of the tested specimens.
Polymerization contraction stress in thin resin composite layers as a function of layer thickness.
Alster, D; Feilzer, A J; de Gee, A J; Davidson, C L
1997-05-01
In the present study, the effect of layer thickness on the curing stress in thin resin composite layers was investigated. Since the value of the contraction stress is dependent on the compliance of the measuring equipment (especially for thin films), a method to determine the compliance of the test apparatus was tested. A chemically initiated resin composite (Clearfil F2, Kuraray) was inserted between two sandblasted and silane-coated stainless steel discs in a tensilometer. The curing contraction of the cylindrical samples was continuously counteracted by feedback displacement of the tensilometer crosshead, and the curing stress development was registered. After 20 min, the samples were loaded in tension until fracture. The curing stress was determined for layer thicknesses of 50, 100, 200, 300, 400, 500, 600, 700 microns, 1.4 mm and 2.7 mm. The compliance of the apparatus was calculated with the aid of a non-linear regression analysis, using an equation derived from Hooke's Law as the model. None of the samples fractured due to contraction stress prior to tensile loading. The contraction stress after 20 min decreased from 23.3 +/- 5.3 MPa for the 50 microns layer to 5.5 +/- 0.6 MPa for the 2.7 mm layer. The compliance on the apparatus was 0.029 mm/MPa. A measuring method was developed which was found to be suitable for the determination of axial polymerization contraction stress in this films of chemically initiated resin composites. The method makes it possible to estimate the stress levels that occur in resin composite films in the clinical situation.
Delayed cure bismaleimide resins
Not Available
1982-08-12
Prior art polybismaleimides begin to polymerize at or just above the melting point of the monomer. This patent describes new bismaleimide resins which have an increased pot life and provide longer time periods in which the monomer remains fluid. The resins can be polymerized into molded articles with a high uniformity of properties. (DLC)
Bortolotto, Tissiana; Betancourt, Francisco; Krejci, Ivo
2016-12-01
This study evaluated the influence of curing devices on marginal adaptation of cavities restored with self-etching adhesive containing CQ and PPD initiators and hybrid composite. Twenty-four class V (3 groups, n=8) with margins located on enamel and dentin were restored with Clearfil S3 Bond and Clearfil APX PLT, light-cured with a monowave LED, multiwave LED and halogen light-curing unit (LCU). Marginal adaptation was evaluated with SEM before/after thermo-mechanical loading (TML). On enamel, significantly lower % continuous margins (74.5±12.6) were found in group cured by multiwave LED when compared to monowave LED (87.6±9.5) and halogen LCU (94.4±9.1). The presence of enamel and composite fractures was significantly higher in the group light-cured with multiwave LED, probably due to an increased materials' friability resulted from an improved degree of cure. The clinician should aware that due to a distinct activation of both initiators, marginal quality may be influenced on the long-term.
Tongtaksin, A; Leevailoj, C
This study investigated the influence of battery charge levels on the stability of light-emitting diode (LED) curing-light intensity by measuring the intensity from fully charged through fully discharged batteries. The microhardness of resin composites polymerized by the light-curing units at various battery charge levels was measured. The light intensities of seven fully charged battery LED light-curing units-1) LY-A180, 2) Bluephase, 3) Woodpecker, 4) Demi Plus, 5) Saab II, 6) Elipar S10, and 7) MiniLED-were measured with a radiometer (Kerr) after every 10 uses (20 seconds per use) until the battery was discharged. Ten 2-mm-thick cylindrical specimens of A3 shade nanofilled resin composite (PREMISE, Kerr) were prepared per LED light-curing unit group. Each specimen was irradiated by the fully charged light-curing unit for 20 seconds. The LED light-curing units were then used until the battery charge fell to 50%. Specimens were prepared again as described above. This was repeated again when the light-curing units' battery charge fell to 25% and when the light intensity had decreased to 400 mW/cm 2 . The top/bottom surface Knoop hardness ratios of the specimens were determined. The microhardness data were analyzed by one-way analysis of variance with Tukey test at a significance level of 0.05. The Pearson correlation coefficient was used to determine significant correlations between surface hardness and light intensity. We found that the light intensities of the Bluephase, Demi Plus, and Elipar S10 units were stable. The intensity of the MiniLED unit decreased slightly; however, it remained above 400 mW/cm 2 . In contrast, the intensities of the LY-A180, Woodpecker, and Saab II units decreased below 400 mW/cm 2 . There was also a significant decrease in the surface microhardnesses of the resin composite specimens treated with MiniLED, LY-A180, Woodpecker, and Saab II. In conclusion, the light intensity of several LED light-curing units decreased as the battery was discharged, with a coincident reduction in the units' ability to polymerize resin composite. Therefore, the intensity of an LED light-curing unit should be evaluated during the life of its battery charge to ensure that sufficient light intensity is being generated.
A Durable Airfield Marking System.
1985-06-01
Resin is Mixed with the Black Curing Agent to Form the Epoxy Adhesive ..... ........... 17 14 The Gray Adhesive (White Resin Mixed with Black Curing...rubber 100 0 Polyester (peroxide-catalyzed) 100 0 Urethane 100 0 Epoxy polyamide 100 0 Acrylic latex (TT-P-1952) 100 0 Thermoplastic Tapes Type 1 100 0...suzmarrizes cost data co1parisons for traffic marking tapes, CAS tiles, fluorocarbon composites (Teflon ),and acrylic latex paint TT-P-1952. 8 -p °’. TABLE 2
Rapidly curable electrically conductive clear coatings
DOE Office of Scientific and Technical Information (OSTI.GOV)
Bowman, Mark P.; Anderson, Lawrence G.; Post, Gordon L.
2018-01-16
Rapidly curable electrically conductive clear coatings are applied to substrates. The electrically conductive clear coating includes to clear layer having a resinous binder with ultrafine non-stoichiometric tungsten oxide particles dispersed therein. The clear coating may be rapidly cured by subjecting the coating to infrared radiation that heats the tungsten oxide particles and surrounding resinous binder. Localized heating increases the temperature of the coating to thereby thermally cure the coating, while avoiding unwanted heating of the underlying substrate.
Surface roughness of denture bases after immersion in fishcake vinegar solution
NASA Astrophysics Data System (ADS)
Kodir, K.; Tanti, I.; Odang, R. W.
2017-08-01
Fishcake is a common food in Palembang city and is usually eaten with fishcake vinegar sauce. Fishcake vinegar solution contains acetic acid and chloride and fluoride ions, all of which cause surface roughness on the denture base material. The objective of this study was to analyze the effect of fishcake vinegar solution on the surface roughness of heat-cured acrylic resin, thermoplastic nylon, and cobalt-chromium alloy denture bases. This laboratory-based experimental study was performed on heat-cured acrylic resins, thermoplastic nylon specimen plates formed in 15 × 10 × 1 mm shapes, and cobalt-chromium alloy specimens in cylinder forms with a 7.7 mm diameter and 17.5-mm height. Each group consisted of 10 pieces. Each specimen was immersed in a fishcake vinegar solution at 37 °C for 4 days. The surface roughness was measured using a profilometer before and after immersion. Statistical analyses showed significant (p < 0.05) changes in heat-cured acrylic resin, thermoplastic nylon, and the cobalt chromium alloy plates after immersion in a fishcake vinegar solution for 4 days. Fishcake vinegar solution affects the surface roughness of heat-cured acrylic resin, thermoplastic nylon, and cobalt-chromium alloy plates after a 4-day immersion period. The greatest surface roughness change occurred in the thermoplastic nylon plate, while the lowest change occurred in the cobalt-chromium alloy.
Influence of light curing and sample thickness on microhardness of a composite resin
Aguiar, Flávio HB; Andrade, Kelly RM; Leite Lima, Débora AN; Ambrosano, Gláucia MB; Lovadino, José R
2009-01-01
The aim of this in vitro study was to evaluate the influence of light-curing units and different sample thicknesses on the microhardness of a composite resin. Composite resin specimens were randomly prepared and assigned to nine experimental groups (n = 5): considering three light-curing units (conventional quartz tungsten halogen [QTH]: 550 mW/cm2 – 20 s; high irradiance QTH: 1160 mW/cm2 – 10 s; and light-emitting diode [LED]: 360 mW/cm2 – 40 s) and three sample thicknesses (0.5 mm, 1 mm, and 2 mm). All samples were polymerized with the light tip 8 mm away from the specimen. Knoop microhardness was then measured on the top and bottom surfaces of each sample. The top surfaces, with some exceptions, were almost similar; however, in relation to the bottom surfaces, statistical differences were found between curing units and thicknesses. In all experimental groups, the 0.5-mm-thick increments showed microhardness values statistically higher than those observed for 1- and -2-mm increments. The conventional and LED units showed higher hardness mean values and were statistically different from the high irradiance unit. In all experimental groups, microhardness mean values obtained for the top surface were higher than those observed for the bottom surface. In conclusion, higher levels of irradiance or thinner increments would help improve hybrid composite resin polymerization. PMID:23674901
Fatigue crack propagation in self-assembling nanocomposites
NASA Astrophysics Data System (ADS)
Klingler, Andreas; Wetzel, Bernd
2016-05-01
Self-assembling block-copolymers allow the easy manufacturing of nanocomposites due to the thermodynamically driven in situ formation of nanosized phases in thermosetting resins during the curing process. Complex mechanical dispersion processes can be avoided. The current study investigates the effect of a block-copolymer on the fatigue crack propagation resistance of a cycloaliphatic amine cured epoxy resin. It was found that a small amount of MAM triblock-copolymer significantly increases the resistance to fatigue crack propagation of epoxy. Crack growth rate and the Paris law exponent for fatigue-crack growth were considerably reduced from m=15.5 of the neat epoxy to m=8.1 of the nanocomposite. To identify the related reinforcing and fracture mechanisms structural analyses of the fractured surfaces were performed by scanning electron microscope. Characteristic features were identified to be deformation, debonding and fracture of the nano-phases as well as crack pinning. However, the highest resistance against fatigue crack propagation was achieved in a bi-continuous microstructure that consisted of an epoxy-rich phase with embedded submicron sized MAM inclusions, and which was surrounded by a block-copolymer-rich phase that showed rupture and plastic deformation.
Yu, Bin; Lee, Young-Keun
2013-01-01
To evaluate translucency, fluorescence and opalescence stabilities of direct and indirect composite resins after aging. One direct (16 shades) and two indirect composite resins (16 and 26 shades) were investigated. Resins were filled in a mold (1 mm thick) and light cured; post-curings were performed for indirect resins. Color was measured before and after 5,000 cycles of thermocycling on a reflection spectrophotometer in reflectance and transmittance modes to calculate parameters for translucency (TP), fluorescence (FL) and opalescence (OP). Differences in the changes of TP, FL and OP after aging by the type of resin were determined by t test, and those were also determined by one-way ANOVA with the factor of the brand or the shade group (P < 0.05). Changes in TP, FL and OP were -1.2 to 0.7, -0.2 to 0.4 and -0.6 to 1.3, respectively, for direct resins; and were -2.0 to 1.8, -0.9 to 0.4 and -2.9 to 3.7, respectively, for indirect resins. Changes in TP were not significantly different by the type of resin, but those in FL and OP were different (P = 0.05). Changes in optical parameters were influenced by the brand or the shade group of the resins (P < 0.05). Stabilities in optical properties of resins varied depending on type, brand or shade group. Aging significantly affected fluorescence and opalescence, but not translucency, of indirect resins compared to those of direct resins.
Fiber Optic Sensors for Cure/Health Monitoring of Composite Materials
NASA Technical Reports Server (NTRS)
Wood, K. H.; Brown, T. L.; Wu, M. C.; Gause, C. B.
2004-01-01
The objective of the current program is to develop techniques for using optical fibers to monitor the cure of composite materials in real time during manufacture and to monitor the in-service structural health of composite structures. Single and multimode optical fibers containing Bragg gratings have been used to perform Near Infrared (NIR) spectroscopy on high refractive index resins and show promise as embedded sensors. In order for chemical spectroscopy to be possible, intimate contact must be achieved between the fiber core and the composite resin. This contact is often achieved by stripping the cladding off of a portion of the fiber, thus making it brittle and easily broken in the composite processing environment. To avoid weakening the fiber to this extent, high refractive index fibers have been fabricated that use a low refractive index acrylate coating which serves as the cladding. This is ideal, as the coating is easily solvent stripped and intimate contact with the glass core can be achieved. Real time resin and composite chemical spectra have been obtained, with possible multifunctional capability using Bragg gratings to assess physical properties such as strain, modulus and other parameters of interest.
Shining a light on high volume photocurable materials.
Palin, William M; Leprince, Julian G; Hadis, Mohammed A
2018-05-01
Spatial and temporal control is a key advantage for placement and rapid setting of light-activated resin composites. Conventionally, placement of multiple thin layers (<2mm) reduces the effect of light attenuation through highly filled and pigmented materials to increase polymerisation at the base of the restoration. However, and although light curing greater than 2mm thick layers is not an entirely new phenomenon, the desire amongst dental practitioners for even more rapid processing in deep cavities has led to the growing acceptance of so-called "bulk fill" (4-6mm thick) resin composites that are irradiated for 10-20s in daily clinical practice. The change in light transmission and attenuation during photopolymerisation are complex and related to path length, absorption properties of the photoinitiator and pigment, optical properties of the resin and filler and filler morphology. Understanding how light is transmitted through depth is therefore critical for ensuring optimal material properties at the base of thick increments. This article will briefly highlight the advent of current commercial materials that rationalise bulk filling techniques in dentistry, the relationship between light transmission and polymerisation and how optimal curing depths might be achieved. Copyright © 2018 The Academy of Dental Materials. Published by Elsevier Inc. All rights reserved.
Stress Relaxation in Epoxy Thermosets via a Ferrocene-Based Amine Curing Agent
Jones, Brad H.; Wheeler, David R.; Black, Hayden T.; ...
2017-06-29
Physical stress relaxation in rubbery, thermoset polymers is limited by cross-links, which impede segmental motion and restrict relaxation to network defects, such as chain ends. In parallel, the cure shrinkage associated with thermoset polymerizations leads to the development of internal residual stress that cannot be effectively relaxed. Recent strategies have reduced or eliminated such cure stress in thermoset polymers largely by exploiting chemical relaxation processes, wherein temporary cross-links or otherwise transient bonds are incorporated into the polymer network. In this paper, we explore an alternative approach, wherein physical relaxation is enhanced by the incorporation of organometallic sandwich moieties into themore » backbone of the polymer network. A standard epoxy resin is cured with a diamine derivative of ferrocene and compared to conventional diamine curing agents. The ferrocene-based thermoset is clearly distinguished from the conventional materials by reduced cure stress with increasing cure temperature as well as unique stress relaxation behavior above its glass transition in the fully cured state. The relaxation experiments exhibit features characteristic of a physical relaxation process. Furthermore, the cure stress is observed to vanish precipitously upon deliberate introduction of network defects through an increasing imbalance of epoxy and amine functional groups. Finally, we postulate that these beneficial properties arise from fluxional motion of the cyclopentadienyl ligands on the polymer backbone.« less
NASA Astrophysics Data System (ADS)
Schumann, M.; Geiß, P. L.
2015-05-01
Faultless processing of thermoset polymers in demanding applications requires a profound mastering of the curing kinetics considering both the physico-chemical changes in the transition from the liquid to the solid state and the consolidation of the polymers network in the diffusion controlled curing regime past the gel point. Especially in adhesive joints shrinkage stress occurring at an early state of the curing process under confined conditions is likely to cause defects due to local debonding and thus reduce their strength and durability1. Rheometry is considered the method of choice to investigate the change of elastic and viscous properties in the progress of curing. Drawbacks however relate to experimental challenges in accessing the full range of kinetic parameters of thermoset resins with low initial viscosity from the very beginning of the curing reaction to the post-cure consolidation of the polymer due to the formation of secondary chemical bonds. Therefore the scope of this study was to interrelate rheological data with results from in-situ measurements of the shrinkage stress formation in adhesive joints and with the change of refractive index in the progress of curing. This combination of different methods has shown to be valuable in gaining advanced insight into the kinetics of the curing reaction. The experimental results are based on a multi component thermoset epoxy-amine adhesive.
Stress Relaxation in Epoxy Thermosets via a Ferrocene-Based Amine Curing Agent
DOE Office of Scientific and Technical Information (OSTI.GOV)
Jones, Brad H.; Wheeler, David R.; Black, Hayden T.
Physical stress relaxation in rubbery, thermoset polymers is limited by cross-links, which impede segmental motion and restrict relaxation to network defects, such as chain ends. In parallel, the cure shrinkage associated with thermoset polymerizations leads to the development of internal residual stress that cannot be effectively relaxed. Recent strategies have reduced or eliminated such cure stress in thermoset polymers largely by exploiting chemical relaxation processes, wherein temporary cross-links or otherwise transient bonds are incorporated into the polymer network. In this paper, we explore an alternative approach, wherein physical relaxation is enhanced by the incorporation of organometallic sandwich moieties into themore » backbone of the polymer network. A standard epoxy resin is cured with a diamine derivative of ferrocene and compared to conventional diamine curing agents. The ferrocene-based thermoset is clearly distinguished from the conventional materials by reduced cure stress with increasing cure temperature as well as unique stress relaxation behavior above its glass transition in the fully cured state. The relaxation experiments exhibit features characteristic of a physical relaxation process. Furthermore, the cure stress is observed to vanish precipitously upon deliberate introduction of network defects through an increasing imbalance of epoxy and amine functional groups. Finally, we postulate that these beneficial properties arise from fluxional motion of the cyclopentadienyl ligands on the polymer backbone.« less
DOE Office of Scientific and Technical Information (OSTI.GOV)
John J. Gangloff Jr; Shatil Sinha; Suresh G. Advani
The formation and transport of voids in composite materials remains a key research area in composite manufacturing science. Knowledge of how voids, resin, and fiber reinforcement propagate throughout a composite material continuum from green state to cured state during an automated tape layup process is key to minimizing defects induced by void-initiated stress concentrations under applied loads for a wide variety of composite applications. This paper focuses on modeling resin flow in a deforming fiber tow during an automated process of partially impregnated thermoset prepreg composite material tapes. In this work, a tow unit cell based model has been presentedmore » that determines the consolidation and impregnation of a thermoset prepreg tape under an input pressure profile. A parametric study has been performed to characterize the behavior of varying tow speed and compaction forces on the degree of consolidation. Results indicate that increased tow consolidation is achieved with slower tow speeds and higher compaction forces although the relationship is not linear. The overall modeling of this project is motivated to address optimization of the 'green state' composite properties and processing parameters to reduce or eliminate 'cured state' defects, such as porosity and de-lamination. This work is partially funded by the Department of Energy under Award number DE-EE0001367.« less
Simultaneous acoustic and dielectric real time curing monitoring of epoxy systems
NASA Astrophysics Data System (ADS)
Gkikas, G.; Saganas, Ch.; Grammatikos, S. A.; Aggelis, D. G.; Paipetis, A. S.
2012-04-01
The attainment of structural integrity of the reinforcing matrix in composite materials is of primary importance for the final properties of the composite structure. The detailed monitoring of the curing process on the other hand is paramount (i) in defining the optimal conditions for the impregnation of the reinforcement by the matrix (ii) in limiting the effects of the exotherm produced by the polymerization reaction which create unwanted thermal stresses and (iii) in securing optimal behavior in matrix controlled properties, such as off axis or shear properties and in general the durability of the composite. Dielectric curing monitoring is a well known technique for distinguishing between the different stages of the polymerization of a typical epoxy system. The technique successfully predicts the gelation and the vitrification of the epoxy and has been extended for the monitoring of prepregs. Recent work has shown that distinct changes in the properties of the propagated sound in the epoxy which undergoes polymerization is as well directly related to the gelation and vitrification of the resin, as well as to the attainment of the final properties of the resin system. In this work, a typical epoxy is simultaneously monitored using acoustic and dielectric methods. The system is isothermally cured in an oven to avoid effects from the polymerization exotherm. Typical broadband sensors are employed for the acoustic monitoring, while flat interdigital sensors are employed for the dielectric scans. All stages of the polymerization process were successfully monitored and the validity of both methods was cross checked and verified.
Rahal, Juliana Saab; Mesquita, Marcelo Ferraz; Henriques, Guilherme Elias Pessanha; Nóbilo, Mauro Antonio Arruda
2004-01-01
Influence of polishing methods on water sorption and solubility of denture base acrylic resins was studied. Eighty samples were divided into groups: Classico (CL), and QC 20 (QC) - hot water bath cured; Acron MC (AC), and Onda Cryl (ON) - microwave cured; and submitted to mechanical polishing (MP) - pumice slurry, chalk powder, soft brush and felt cone in a bench vise; or chemical polishing (CP) - heated monomer fluid in a chemical polisher. The first desiccation process was followed by storage in distilled water at 37 +/- 1 degrees C for 1 h, 1 day, 1, 2, 3 and 4 weeks. Concluding each period, water sorption was measured. After the fourth week, a second desiccation process was done to calculate solubility. Data were submitted to analysis of variance, followed by Tukey test (p
High Temperature Transfer Molding Resins
NASA Technical Reports Server (NTRS)
Connell, John W. (Inventor); Smith, Joseph G., Jr. (Inventor); Hergenrother, Paul M. (Inventor)
2000-01-01
High temperature resins containing phenylethynyl groups that are processable by transfer molding have been prepared. These phenylethynyl containing oligomers were prepared from aromatic diamines containing phenylethynyl groups and various ratios of phthalic anhydride and 4-phenylethynlphthalic anhydride in glacial acetic acid to form a mixture of imide compounds in one step. This synthetic approach is advantageous since the products are a mixture of compounds and consequently exhibit a relatively low melting temperature. In addition, these materials exhibit low melt viscosities which are stable for several hours at 210-275 C, and since the thermal reaction of the phenylethynyl group does not occur to any appreciable extent at temperatures below 300 C, these materials have a broad processing window. Upon thermal cure at approximately 300-350 C, the phenylethynyl groups react to provide a crosslinked resin system. These new materials exhibit excellent properties and are potentially useful as adhesives, coatings, films, moldings and composite matrices.
Epoxy Resins in Electron Microscopy
Finck, Henry
1960-01-01
A method of embedding biological specimens in araldite 502 (Ciba) has been developed for materials available in the United States. Araldite-embedded tissues are suitable for electron microscopy, but the cutting qualities of the resin necessitates more than routine attention during microtomy. The rather high viscosity of araldite 502 also seems to be an unnecessary handicap. The less viscous epoxy epon 812 (Shell) produces specimens with improved cutting qualities, and has several features—low shrinkage and absence of specimen damage during cure, minimal compression of sections, relative absence of electron beam-induced section damage, etc.—which recommends it as a routine embedding material. The hardness of the cured resin can be easily adjusted by several methods to suit the materials embedded in it. Several problems and advantages of working with sections of epoxy resins are also discussed. PMID:13822825
Effect of light-curing units on microleakage under dental composite resins
NASA Astrophysics Data System (ADS)
Queiroz, R. S.; Bandéca, M. C.; Calixto, L. R.; Saade, E. G.; Nadalin, M. R.; Andrade, M. F.; Porto-Neto, S. T.
2009-09-01
The aim of this study was to determine the effect of two light-curing units (QTH and LED) on microleakage of Class II composite resin restorations with dentin cavosurface margins. Twenty extracted mandibular first premolars, free of caries and fractures were prepared two vertical “slot” cavities in the occluso-mesial and -destal surfaces (2 mm buccal-lingually, 2 mm proximal-axially and cervical limit in enamel) and divided into 4 equal groups ( n = 8): GI and GII: packable posterior composite light-activated with LED and QTH, respectively; GIII and GIV: micro-hybrid composite resin light-activated with LED and QTH, respectively. The composite resins were applied following the manufacturer’s instructions. After 24 h of water storage specimens were subjected to thermocycling for a total of 500 cycles at 5 and 55°C and the teeth were then sealed with impermeable material. Teeth were immersed in 0.5% Basic fuchsin during 24 h at room temperature, and zero to three levels of penetration score were attributed. The Mann-Whitney and Kruskal-Wallis tests showed significant statistically similar ( P > 0.05) from GI to GII and GIII to GIV, which the GII (2.750) had the highest mean scores and the GIII and GIV (0.875) had lowest mean scores. The use of different light-curing units has no influence on marginal integrity of Class II composite resin restorations and the proprieties of composite resins are important to reduce the microleakage.
Effect of ceramic thickness and shade on mechanical properties of a resin luting agent.
Passos, Sheila Pestana; Kimpara, Estevão Tomomitsu; Bottino, Marco Antonio; Rizkalla, Amin S; Santos, Gildo Coelho
2014-08-01
This study aimed to investigate the influence of ceramic thickness and shade on the Knoop hardness and dynamic elastic modulus of a dual-cured resin cement. Six ceramic shades (Bleaching, A1, A2, A3, A3.5, B3) and two ceramic thicknesses (1 mm, 3 mm) were evaluated. Disk specimens (diameter: 7 mm; thickness: 2 mm) of the resin cement were light cured under a ceramic block. Light-cured specimens without the ceramic block at distances of 1 and 3 mm were also produced. The Knoop hardness number (KHN), density, and dynamic Young's moduli were determined. Statistical analysis was conducted using ANOVA and a Tukey B rank order test (p = 0.05). The bleaching 1-mm-thick group exhibited significantly higher dynamic Young's modulus. Lower dynamic Young's moduli were observed for the 3-mm-thick ceramic groups compared to bleaching 3-mm-thick group, and no difference was found among the other 3-mm groups. For the KHN, when A3.5 3-mm-thick was used, the KHN was significantly lower than bleaching and A1 1-mm-thick ceramic; however, no difference was exhibited between the thicknesses of the same shade. The dual-cured resin cement studied irradiated through the 1-mm-thick ceramic with the lightest shade (bleaching ceramic) exhibited a better elastic modulus, and there was no effect in KHN of the resin cement when light cured under different ceramic shades and thicknesses (1 and 3 mm), except when the A3.5 3-mm-thick ceramic was used. Variolink II irradiated through ceramic with the lowest chroma exhibited the highest elastic modulus; therefore, the light activation method might not be the same for all clinical situations. © 2014 by the American College of Prosthodontists.