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1.
Vinyl-containing poly(acrylic acid-co-itaconic acid) copolymers were synthesized and used to formulate light-curable cements containing reactive glass fillers (Fuji II LC). The conditions for light curing were studied and optimized. Effects of molecular weight (MW), grafting ratio, comonomer, liquid composition, powder/liquid (P/L) ratio, glass powder and aging were evaluated. The results show that the vinyl-containing glass-ionomer cements (GICs) prepared in this study exhibit higher compressive strength (CS, 225.6 MPa), diametral tensile strength (DTS, 28.4 MPa) and much higher flexural strength (FS, 116.4 MPa), as compared to commercial Fuji II LC GIC (186.6 in CS, 19.1 in DTS and 57.1 in FS). The optimal light-exposure time was found to be around 10 min, and concentrations of CQ and DC were 0.5% (by weight) and 1.0%, respectively. Effects of MW, grafting ratio, P/L ratio and content of polymer in the liquid formulation were significant. The highest strengths were found for the optimal formulations where the MW was 15,000 (weight average), grafting ratio 25 mol%, P/L ratio 2.7 and liquid composition 50:20:30. During aging, the cement showed an increase of strength over the first week and then no change for a month. SEM analysis suggests that more integrated microstructures and smaller glass particles can lead to higher FS and higher polymer content in GICs leads to tough fracture surface and plastic deformation.  相似文献   

2.
Poly(acrylic acid-co-itaconic acid) copolymers containing pendent methacrylates were synthesized and used to formulate redox-initiated in situ cured glass-ionomer cements (GICs) by mixing with reactive glass fillers (Fuji II LC). Various formulations for the redox initiator were studied, and flexural strength (FS) was used as a screening tool for optimization. Effects of molecular weight (MW), grafting ratio, comonomer, polymer content in the liquid composition, powder/liquid (P/L) ratio, and aging on FS were investigated. The results show that the in situ cured GICs demonstrated higher FS (89.6-123.2 MPa), as compared to commercial Fuji II LC GIC (57.1 MPa). The optimal concentrations for redox initiators were found to be 0.15% (by weight) for K2S2O8 and 0.2% for ascorbic acid (or 0.6% for microencapsulated ascorbic acid), respectively. Effects of MW, grafting ratio, P/L ratio and polymer content in the liquid formulation were significant. During aging, the cement showed an increase in strength over 24 h and then no change for time periods up to six months. SEM analysis supports the strength data associated with the formulations. The exotherm and setting time suggest that novel redox-initiated resin-modified GICs hold promise as biocompatible and workable cement for orthopedic applications.  相似文献   

3.
A series of copolymers containing various molar ratios of acrylic acid, itaconic acid and N-methacryloylglutamic acid were prepared in aqueous solution, using standard free-radical polymerization conditions. Specimens for mechanical property studies were prepared by mixing water solutions of the copolymers (50:50, wt:wt) with a commercial, calcium-fluoroaluminosilicate glass powder, with curing or hardening achieved by salt-bridge formation. The glass powder used in the formulation(s) was the same as that used in Fuji II (GC America) glass-ionomer. The working and setting times of the various formulations were evaluated. The compressive strength was used as the basic screening property to find the optimum molar ratio of the three monomers. The diametral tensile strength, flexural strength and Knoop surface hardness of the cured materials were also determined. All mechanical properties were measured after the specimens were conditioned in distilled water for 7 days at 37°C. Based on the compressive strength (CS), poly (AA-co-IA-co-MGA) with a monomers ratio of 8:1:1, respectively, showed the highest CS (269.9 MPa). The 8:1:1 copolymer with different molecular weights were also prepared to evaluate the effect of MW on the compressive strength. The optimum MW copolymer gave a glass-ionomer having the compressive strength improved by 30%, compared to Fuji II (293.9 MPa vs. 224.9 MPa). The same polymer solution was also mixed with glass powders used in other commercial glass-ionomers, i. e., Ketac-Molar (ESPE, Seefeld, Germany), α-Fil and α-Silver (DMG, Hamburg, Germany) to produce conventional glass-ionomers test specimens. The mechanical properties of these materials were also obtained and compared to the Fuji II, Ketac-Molar, α-Fil and α-Silver controls.  相似文献   

4.
The monomers N-acryloyl (AGA) and N-methacryloylglutamic acid (MGA) have been prepared and copolymerized with acrylic acid (AA) and itaconic acid (IA) to make polyelectrolytes for evaluation in glass polyalkenoates or glass-ionomers. It was shown that poly(AA-co-IA-co-AGA) and poly(AA-co-IA-co-MGA), having a monomers ratio, respectively, of 7:3:3 could be formulated with glass powders used in Fuji II (GC America), α-Silver (DMG-Hamburg), α-Fil (DMG-Hamburg) and Ketac-Molar (ESPE, Seefeld, Germany) to produce conventional glass-ionomers with improved compressive strength (CS), flexural strength (FS) and fracture toughness (FT), compared to Fuji II, α-Silver, α-Fil and Ketac-Molar controls. Since MGA is much easier to produce in high yields than AGA, it was important to show that MGA could be used as well as AGA to produce new matrix resins for glass-ionomers. Furthermore, we demonstrated that both the 7:3:3 AGA and MGA copolymers could be reacted with 2-isocyanatoethyl methacrylate (IEM) to produce intermediates useful for formulating visible light-curable (VLC) glass-ionomers with improved CS, FS and FT, compared to two com-mercial VLC materials Fuji IITM LC and VitremerTM Tricure. Here again, it was found that MGA could be used as well as AGA to prepare improved materials. We also demonstrated that poly(AA-co-MGA) could be used to formulate glass-ionomers with improved properties. Further, we demonstrated that small amounts of MGA could be used as a reactive diluent in VLC formulations such as Fuji IITM LC, VitremerTM Tricure, and an experimental VLC formulation to improve their mechanical properties, adhesion to tooth structure, and fluoride release.  相似文献   

5.
Abstract

The flexural strengths of N-vinylpyrrolidone modified glass-ionomer cements were investigated. The optimal molar ratio of the monomers in copolymers, composed of the three components acrylic acid, itaconic acid and N-vinylpyrrolidone, was determined using a SAS statistical program. The copolymers were prepared using a free-radical polymerization process. The viscosities of aqueous solutions of these polymers were determined. Cements were formed by the reaction of these solutions with glass particles. Flexural strength (FS) was used as the basic screening property to find the optimum molar ratio. Statistical models were applied to predict the optimum molar ratios. All strength values were recorded on the specimens conditioned in distilled water at 37°C for 7 days. The optimal molar ratio for these copolymers was 7:1:3 for poly(acrylic acid-co-itaconic acid-co-N-vinylpyrrolidone), based on flexural strength and viscosity. The effect of molecular weight (MW) on FS was also evaluated. Copolymer with a MW of 10, 800 (Mn) showed 85% higher FS than the Ketac-Molar (KM) system, along with a reasonable working viscosity.  相似文献   

6.
ABSTRACT

High fluidity solvents, such as supercritical fluids, have several advantages over traditional solvents as polymerization media, such as offering a more environmentally-friendly reaction media, providing increased reaction rates, and simplifying the separation and purification of polymers. In this study, a traditional glass-ionomer polymer, poly(acrylic acid-co-itaconic acid) (PAA/IA) was synthesized by using mixtures of CO2 and methanol as the reaction solvent and was characterized by 1H-NMR, FT-IR, GPC, and viscometry. The mechanical and working properties of the glass-ionomer cements, prepared by mixing aqueous solutions of the polymers with Fuji II glass powder, were evaluated for compressive strength (CS), diametral tensile strength (DTS) and flexural strength (FS), as well as setting time and working time. The results showed that the polymerization reaction in CO2/methanol mixtures was faster and had higher conversion than the polymerization reaction in water. The glass-ionomer formulations made from the copolymer prepared under SC conditions showed higher CS, comparable FS and DTS compared with those made from the same polymer prepared in water. Both of the synthesized copolymers had significantly higher CS and FS than Fuji II. The working properties of PAA/IA made in CO2/methanol met the requirement of ANSI/ADA No. 96.  相似文献   

7.
A novel synthetic biodegradable oligomer based upon methacrylated aminocaproyl maleamic acid (MACMA), was synthesized and characterized. Injectable and in situ crosslinkable polymer networks were formulated by copolymerization of MACMA with triethyleneglycol dimethacrylate (TEGDMA). In addition, composites composed of MACMA, TEGDMA and beta-tricalcium phosphate (β-TCP) were prepared. The networks and composites were initiated by photo- and redox-polymerization, respectively. The initial compressive (CS) and diametral tensile strengths (DTS) of these materials were determined and used to evaluate the effects of MACMA/TEGDMA ratios on the degradation behavior of the materials. The neat resin networks exhibited initial CS values ranging from 6.7 to 284.2 MPa and the composites demonstrated initial DTS values ranging from 2.8 to 20.8 MPa and CS values ranging from 19.1 to 119.5 MPa. During the course of degradation the polymer neat resins lost 51%, 69% and 61% of their initial CS after 3 weeks for the MACMA/TEGDMA ratios at 25/75, 50/50 and 75/25, respectively. The resin with the MACMA/TEGDMA ratio of 75/25 completely degraded after 6 months. The composite with the MACMA/TEGDMA ratio of 25/75 exhibited a significant increase in CS after an initial decrease for 7 days and then lost 57% of its initial CS after 3 months. The composite composed of poly(MACMA) homopolymer showed a complete degradation after 21 days.  相似文献   

8.
Three novel adhesive oligomers having carboxylic acid and methacrylate groups were synthesized, characterized and used to formulate composite bone cements with newly synthesized zinc-calcium-silicate phosphate. The optimal formulation was determined based on types of oligomer, oligomer/diluent ratio, initiator concentration, and filler level using compressive strength (CS) and curing time (CT) as screening tools. Shrinkage, exotherm and aging of the formed composite cements were also evaluated. Results show that the experimental cement was 186% higher in CS, 16% higher in diametral tensile strength, similar in flexural strength, 56% less in exotherm and 64% less in shrinkage, as compared to conventional polymethylmethacrylate cement. The optimal concentrations for initiators were found to be 1.5% (by weight) for both benzoyl peroxide and N,N-dimethyl-p-toluidine. With increasing initiator concentration, diluent content and zinc oxide content in the cement formulation, CS of the cement increased but curing time decreased. Shrinkage and exotherm of the cement decreased with increasing filler level. CS was not proportional to an increase of filler level and CT increased with an increase of filler level. During aging, the cement showed an increase of strength over 24 h and then no change for over nine months. It appears that this novel cement may be a potential candidate for orthopedic restoration if its biological performance is good and the formulation is optimized.  相似文献   

9.
Starting with the L-and D,L-lactide copolymer (L:DL = 9: 1) [P(L-DL)LA] of M_w = 32.1×10~4, rods were obtainedthrough a two stage process: (1) melt-extrusion at 155℃, and (2) hot-drawing at 90℃ to various drawing ratios. Themolecular weight of P(L-DL)LA fell to 9.3×10~4 as a consequence of the production process. The crystallization andmolecular orientation of P(L-DL)LA developed as a result of the hot-drawing. The mechanical strengths of the rods increasewith the drawing ratio. The maximum for tensile strength, bending strength, bending modulus, and shear strength are329 MPa, 237 MPa, 8.8 GPa, and 157 MPa, respectively.  相似文献   

10.
The fracture behavior of acrylic bone cements modified with comonomers containing amine groups was studied using the essential work of fracture approach. The cements were prepared with either 2-(diethylamino)ethyl-acrylate (DEAEA), 2-(dimethylamino)ethyl-methacrylate (DMAEM) or 2-(diethylamino)ethyl-methacrylate (DEAEM) as comonomer in the liquid phase. Double-Edge-Notched Tensión (DENT) specimens were tested in a universal testing machine at 5 mm/min. The results showed that the essential work (we) and nonspecific value of fracture (βwp) of bone cements modified with all percentages of comonomer were notably increased compared with unmodified bone cement. From Scanning Electron Microscopy (SEM) micrographs, ductile behavior was observed for modified bone cements, i.e. the crack propagation is stable, whereas the unmodified cement exhibited brittle behavior indicating unstable crack propagation. The use of the essential work of fracture approach is suggested to determine the fracture behavior of cements that do not exhibit a linear stress-strain relationship.  相似文献   

11.
Although several natural plants and mixtures have been known and used over the centuries for their antibacterial activity, few have been thoroughly explored in the field of dentistry. Thus, the aim of this study was to enhance the antimicrobial activity of a conventional glass ionomer cement (GIC) with natural plant extracts. The effect of this alteration on the bond strength and film thickness of glass ionomer cement was evaluated and related to an 0.5% chlorohexidine modified GIC. Olive leaves (Olea europaea), Fig tree (Ficus carica), and the leaves and roots of Miswak (Salvadora persica) were used to prepare an alcoholic extract mixture. The prepared extract mixture after the evaporation of the solvent was used to modify a freeze-dried glass ionomer cement at three different extracts: water mass ratios 1:2, 1:1, and 2:1. An 0.5% chlorhexidine diacetate powder was added to a conventional GIC for the preparation of a positive control group (CHX-GIC) for comparison. The bond strength to dentine was assessed using a material-testing machine at a cross head speed of 0.5 mm/min. Failure mode was analyzed using a stereomicroscope at 12× magnification. The cement film thickness was evaluated in accordance with ISO standard 9917-1. The minimum number of samples in each group was n = 10. Statistical analysis was performed using a Kruskal–Wallis test followed by Dunn’s post hoc test for pairwise comparison. There was a statistically insignificant difference between the median shear bond strength (p = 0.046) of the control group (M = 3.4 MPa), and each of the CHX-GIC (M = 1.7 MPa), and the three plant modified groups of 1:2, 1:1, 2:1 (M = 5.1, 3.2, and 4.3 MPa, respectively). The CHX-GIC group showed statistically significant lower median values compared to the three plant-modified groups. Mixed and cohesive failure modes were predominant among all the tested groups. All the tested groups (p < 0.001) met the ISO standard of having less than 25 µm film thickness, with the 2:1 group (M = 24 µm) being statistically the highest among all the other groups. The plant extracts did not alter either the shear bond strength or the film thickness of the GIC and thus might represent a promising additive to GICs.  相似文献   

12.
The influence of quiescent molten-state annealing process on the phase structure and morphology of poly(propylene)/poly(ethylene-co-octene) blends with co-continuous morphology was studied using scanning electron microscopy (SEM). The structure parameter called characteristic length (L) was calculated by the pattern analysis of SEM micrographs to describe morphological variation with annealing time during molten-state annealing process under quiescent condition. Moreover, the potential fractal behavior of the phase structure and morphology of PP/PEOc?=?50/50 blend during the process were discussed. The histograms of P(L/L m ) obtained at various annealing time fell on a master curve, demonstrating the self-similar growth of the phase structure of the blends during quiescent molten-state annealing process.  相似文献   

13.

For this study, ion-eroded cement was prepared from the cement required for construction of middle- and low-level radioactive waste repositories in caves. The properties for adsorption of 137Cs on cement before and after ion erosion were investigated. XRF, XRD, SEM–EDS and BET were used to analyse various cement materials. The effects of reaction time, solid–liquid ratio, initial radioactivity and different ions on adsorption were studied by static batch experiments. When the initial radioactivity was 1114.5 Bq L?1 and the solid–liquid ratio was 5 g L?1, the adsorption equilibrium time was 12 h. Adsorption of 137Cs on ion-eroded cement was more effective than that on untreated cement. The adsorption process was consistent with the pseudosecond-order kinetic model and the Freundlich isotherm model, and the process involved multilayer chemisorption. This study provides basic research data for construction of a disposal repository.

  相似文献   

14.
The electrochemical quartz crystal microbalance (EQCM) technique was used to investigate the electrodeposition of the charge-transfer complex (CTC) generated during electrooxidation of o-tolidine (o-TD) in Britton-Robinson buffers and the effects of coexisting chondroitin sulfate (CS). A V-shaped frequency response to the cyclic voltammetric switching of o-TD indicated the precipitation and dissolution of the poorly soluble CTC, an oxidation intermediate, formed at the Au electrode during the redox switching of o-TD in a neutral or a weakly acidic medium (pH=4.07-6.50). The effects of potential scan rate, solution pH, and several supporting electrolytes were examined. The depth of the V-shaped frequency curves (-Δf0V) was related to the supporting electrolyte used, with a decreasing sequence for −Δf0V as 0.20 mol·L−1 NaNO3 > 0.20 mol·L−1 NaClO4 > 0.10 mol·L−1 Na2SO4. The −Δf0V response to the redox switching of the CTC/o-TD “couple” was enhanced by the introduction of CS because of the formation of the CTC-CS adduct, as also characterized and supported by UV-Vis and FTIR spectrophotometry. The molar ratio (x) of the CTC to CS in the adduct and the electrode-collection efficiency of the CTC (η) were estimated using EQCM. The values of −Δf0V increased with the increase in CS concentration, with a linear range from 0.75 to 15.2 μmol·L−1, and a detection limit down to 50 nmol·L−1. The new method proposed for CS assay was characterized by a dynamically renewed surface of the detection electrode.  相似文献   

15.
原位沉析法制备壳聚糖棒材的研究   总被引:16,自引:1,他引:15  
以壳聚糖凝胶膜为模板,将壳聚糖溶液与NaOH凝固液隔离,利用膜渗透原位沉析法制备了高性能的壳聚糖棒材(d=4.5mm),其弯曲强度、弯曲模量和剪切强度分别为92.4MPa,4.1GPa和36.5MPa.扫描电子显微镜(SEM)分析结果表明,原位沉析法制备的壳聚糖棒材具有同心筒状层叠结构,并对其成型机理进行了探讨.  相似文献   

16.
A new type of nanofibrous structure from chitosan bearing carboxymethyl-β-cyclodextrin (CS-g-β-CD) as a novel drug delivery system was synthesized by grafting carboxymethyl-β-cyclodextrin (CM β-CD) onto chitosan (CS) in the presence of water soluble 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide (EDC) as the condensing agent and N-hydroxysuccinimide (NHS). Defect free mats containing CS-g-β-CD have been fabricated using electrospinning of an aqueous solution of poly(vinyl alcohol) (PVA)/CS-g-β-CD blends. The morphology and diameter of the electrospun nanofibers were examined by scanning electron microscopy (SEM). The average fiber diameter was in the range of 130–210 nm. SEM images showed that the morphology and diameter of the nanofibers were mainly affected by weight ratio of the blend at constant applied voltage. The results revealed that increasing CS-g-β-CD content in the blends decreases the average fiber diameter. It was observed that the PVA/CS-g-β-CD nanofibrous mat provided a slower release of the entrapped drug in compare to PVA/CS nanofibrous mat.  相似文献   

17.
本文将磷酸氢钙(CaHPO4·2H2O,DCPD)添加到硅酸三钙(Ca3SiO5,C3S)骨水泥中,采用X射线衍射(XRD),扫描电镜(SEM),万能力学测试机等手段对不同添加量的骨水泥进行表征,考察添加DCPD对硅酸三钙骨水泥性能的影响。实验表明,C3S材料中添加10% DCPD有着优于单纯C3S骨水泥的水化性能,骨水泥的初凝时间从92 min缩短到80 min;添加20%~30% DCPD能提高材料的短期力学强度,可以实现其短期抗压强度的优化;添加30%~40% DCPD的材料有着优良的生物活性与适中的可降解性能。结果表明,通过添加DCPD优化C3S水泥的性能,对各种不同性能具有DCPD添加量的依赖性。通过进一步优化DCPD添加量,将可能获得优良的生物活性骨缺陷填充材料。  相似文献   

18.
The (1-x)BiFeO3-xBaTiO3 (short for (1-x)BFO-xBTO, x = 0.2–0.4) ceramics were prepared by solid-state reaction with microwave sintering (MWS) and conventional sintering (CS) methods. The crystal structure, microstructures, dielectric properties, ferroelectric properties, and magnetic properties of BFO-BTO ceramics sintered by MWS and CS were systematically investigated. It is found that the MWS can effectively decrease the grain size and enhance the compactness of BFO-BTO ceramics. The X-ray diffraction (XRD) results confirm that all ceramics exhibit a single perovskite structure, and the phase transforms from rhombohedral in BiFeO3-rich compositions to pseudo-cubic phase gradually as x increases. Introducing BTO into BFO can strengthen its dielectric relaxation behavior. Compared with CS, the MWS samples have a lower remanent polarization (Pr) and a smaller coercive field (Ec) under the same electric field. Therefore, MWS contributes to the decrease of dielectric loss. Addition of BTO can contribute to the reduction of the coercive force (Hc) of BFO-based ceramic, and so decrease the hysteresisloss. At the same time, its remanent magnetization (Mr) value can be decreased by introducing BTO into BFO and using MWS method. The present research provides a route for decreasing the dielectric loss and hysteresis loss of BiFeO3-based ceramics using the MWS method.  相似文献   

19.
原位复合法制备层状结构的壳聚糖/羟基磷灰石纳米材料   总被引:21,自引:0,他引:21  
用原位复合法制备了高性能的壳聚糖/羟基磷灰石(CS/HA)纳米复合材料.用预先沉积的壳聚糖膜将含有羟基磷灰石前驱体的壳聚糖溶液与凝固液隔离,同时控制壳聚糖沉积与羟基磷灰石前驱体转化为羟基磷灰石的过程,使其缓慢且有序地进行.当pH值改变时,质子化的壳聚糖分子链在负电层诱导下有序沉积并形成层状结构与羟基磷灰石原位生成CS/HA,并实现二者分子级复合.XRD和TEM测试证实原位生成的磷酸盐是羟基磷灰石,且其颗粒长约为100nm,宽30~50nm.SEM结果表明,用原位复合法制备的材料具有层状结构,CS/HA(质量比100/5)纳米复合材料弯曲强度高达86MPa,比松质骨的高3~4倍,相当于密质骨的1/2,有望用于可承重部位的组织修复材料.  相似文献   

20.
The core–shell nanoparticles possessing poly(methyl methacrylate) (PMMA) core coated with chitosan (CS), polyethyleneimine (PEI), and chitosan-mixed-polyethyleneimine (CS/PEI) shells were synthesized in this work. The emulsifier-free emulsion polymerization triggered by a redox initiating system from t-butylhydroperoxide (TBHP) and amine groups on CS and/or PEI was used as a synthetic method. In the CS/PEI systems, the amount of CS was kept constant (0.5 g), while the amount of PEI was varied from 0.1 to 0.5 g. The surface and physico-chemical properties of prepared nanoparticles were then examined. FTIR spectra indicated the presence of grafted PMMA on CS and/or PEI, and the weight fraction of incorporated PEI in the CS/PEI nanoparticles. All nanoparticles were spherical in shape with uniform size distribution illustrated by scanning electron microscopy (SEM). The introduction of PEI to CS nanoparticles yielded the higher monomer conversion, grafting efficiency, and grafting percentage compared with the CS nanoparticles. The size of CS/PEI nanoparticles was smaller than the original CS and PEI nanoparticles, and tended to decrease with increasing amount of PEI introduced. The introduction of PEI also brought the higher colloidal stability to the nanoparticles as indicated by zeta-potential measurement and isoelectric point analysis. The nanoparticles exhibited a promising antibacterial activity against Staphylococcus aureus and Escherichia coli. The nanoparticle–bacteria interaction was studied via SEM. The results suggested that they would be useful as effective antibacterial agents.  相似文献   

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