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Effect of Cold Drawing on Mechanical Properties of Biodegradable Fibers 冷拔对可生物降解纤维力学性能的影响
Pub Date : 2016-10-01 DOI: 10.5301/jabfm.5000328
F. L. La Mantia, M. Ceraulo, M. Mistretta, M. Morreale
Purpose Biodegradable polymers are currently gaining importance in several fields, because they allow mitigation of the impact on the environment related to disposal of traditional, nonbiodegradable polymers, as well as reducing the utilization of oil-based sources (when they also come from renewable resources). Fibers made of biodegradable polymers are of particular interest, though, it is not easy to obtain polymer fibers with suitable mechanical properties and to tailor these to the specific application. The main ways to tailor the mechanical properties of a given biodegradable polymer fiber are based on crystallinity and orientation control. However, crystallinity can only marginally be modified during processing, while orientation can be controlled, either during hot drawing or cold stretching. In this paper, a systematic investigation of the influence of cold stretching on the mechanical and thermomechanical properties of fibers prepared from different biodegradable polymer systems was carried out. Methods Rheological and thermal characterization helped in interpreting the orientation mechanisms, also on the basis of the molecular structure of the polymer systems. Results and conclusions It was found that cold drawing strongly improved the elastic modulus, tensile strength and thermomechanical resistance of the fibers, in comparison with hot-spun fibers. The elastic modulus showed higher increment rates in the biodegradable systems upon increasing the draw ratio.
生物可降解聚合物目前在若干领域越来越重要,因为它们可以减轻处置传统的、不可生物降解的聚合物对环境的影响,并减少对油基来源(当它们也来自可再生资源时)的利用。由可生物降解聚合物制成的纤维是特别感兴趣的,尽管,获得具有适当机械性能的聚合物纤维并根据具体应用进行定制并不容易。定制给定生物可降解聚合物纤维的机械性能的主要方法是基于结晶度和取向控制。然而,在加工过程中,结晶度只能略微改变,而取向可以在热拉伸或冷拉伸期间控制。本文系统地研究了冷拉伸对不同可生物降解聚合物体系制备的纤维力学和热力学性能的影响。方法基于聚合物体系的分子结构,通过流变学和热特性来解释取向机理。结果与结论与热纺纤维相比,冷拔能明显提高纤维的弹性模量、抗拉强度和耐热性。在生物降解体系中,随着拉伸比的增加,弹性模量呈现出较高的增长速率。
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引用次数: 9
Does Acid Etching Morphologically and Chemically Affect Lithium Disilicate Glass Ceramic Surfaces? 酸蚀对二硅酸锂玻璃陶瓷表面的形态和化学影响?
Pub Date : 2016-09-17 DOI: 10.5301/jabfm.5000303
Y. Maruo, G. Nishigawa, M. Irie, K. Yoshihara, T. Matsumoto, S. Minagi
Background This study evaluated the surface morphology, chemical composition and adhesiveness of lithium disilicate glass ceramic after acid etching with hydrofluoric acid or phosphoric acid. Methods Lithium disilicate glass ceramic specimens polished by 600-grit silicon carbide paper were subjected to one or a combination of these surface treatments: airborne particle abrasion with 50-μm alumina (AA), etching with 5% hydrofluoric acid (HF) or 36% phosphoric acid (Phos), and application of silane coupling agent (Si). Stainless steel rods of 3.6-mm diameter and 2.0-mm height were cemented onto treated ceramic surfaces with a self-adhesive resin cement (Clearfil SA Cement). Shear bond strengths between ceramic and cement were measured after 24-hour storage in 37°C distilled water. Results SEM images of AA revealed the formation of conventional microretentive grooves, but acid etching with HF or Phos produced a porous surface. Bond strengths of AA+HF+Si (28.1 ± 6.0 MPa), AA+Phos+Si (17.5 ± 4.1 MPa) and HF+Si (21.0 ± 3.0 MPa) were significantly greater than those of non-pretreated controls with Si (9.7 ± 3.7 MPa) and without Si (4.1 ± 2.4 MPa) (p<0.05). In addition, HF etching alone (26.2 ± 7.5 MPa) had significantly higher bond strength than AA alone (11.5 ± 4.0 MPa) (p<0.05). AA+HF, AA+Phos and HF showed cohesive failures. Conclusions Etching with HF or Phos yielded higher bond strength between lithium disilicate glass ceramic and self-adhesive resin cement without microcrack formation.
本研究对氢氟酸和磷酸刻蚀后的二硅酸锂玻璃陶瓷的表面形貌、化学成分和粘附性进行了研究。方法采用600磨粒碳化硅纸对二硅酸锂玻璃陶瓷试样进行50-μm氧化铝(AA)空气粒子磨蚀、5%氢氟酸(HF)或36%磷酸(Phos)蚀刻以及硅烷偶联剂(Si)的表面处理。用自粘树脂水泥(Clearfil SA cement)将直径3.6 mm、高度2.0 mm的不锈钢棒粘合在处理过的陶瓷表面上。在37°C蒸馏水中保存24小时后,测量陶瓷与水泥之间的剪切粘结强度。结果AA的SEM图像显示形成了常规的微保留槽,而用HF或Phos酸蚀则形成了多孔表面。AA+HF+Si(28.1±6.0 MPa)、AA+Phos+Si(17.5±4.1 MPa)和HF+Si(21.0±3.0 MPa)的结合强度均显著高于未预处理Si(9.7±3.7 MPa)和未预处理Si(4.1±2.4 MPa)的对照组(p<0.05)。此外,HF蚀刻单独(26.2±7.5 MPa)的结合强度显著高于AA单独(11.5±4.0 MPa) (p<0.05)。AA+HF、AA+Phos和HF均表现为内聚失败。结论用HF或Phos蚀刻可以提高二硅酸锂玻璃陶瓷与自粘树脂水泥的粘结强度,且不会形成微裂纹。
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引用次数: 20
Measuring the Remineralization Potential of Different Agents with Quantitative Light-Induced Fluorescence Digital Biluminator 用定量光致荧光数字发光仪测定不同药剂的再矿化电位
Pub Date : 2016-09-14 DOI: 10.5301/jabfm.5000317
E. Kucukyilmaz, S. Savaş
Background The aim of this study was to investigate the effectiveness of different remineralization agents by quantitative light-induced fluorescence digital Biluminator™ (QLF-D). Methods Artificial caries lesions were created, and the teeth were divided according to the tested materials: (i) distilled water, (ii) acidulated phosphate fluoride (APF), (iii) Curodont Repair (CR), (iv) ammonium hexafluorosilicate (SiF) and (v) ammonium hexafluorosilicate plus cetylpyridinium chloride (SiF + CPC). After treatment procedures, each of the samples was placed in artificial saliva. After demineralization and 1 and 4 weeks of remineralization procedures, fluorescence loss and lesion areas were measured with QLF-D. Data were statistically analyzed (α = 0.05). Results The fluorescence values of the demineralized enamel specimens treated with the various agents differed significantly compared with pretreatment values for both 1 and 4 weeks (p<0.05). At 4 weeks, the highest fluorescence gain was calculated in the CR, APF and SiF groups compared with the control (p<0.05). Conclusions APF, SiF and CR groups yielded greater remineralization ability than SiF + CPC and control groups.
本研究的目的是通过定量光诱导荧光数字发光器™(QLF-D)研究不同再矿化剂的有效性。方法人工造龋,并按试验材料分为(1)蒸馏水、(2)酸化氟化磷酸酯(APF)、(3)牙形修复剂(CR)、(4)六氟硅酸铵(SiF)和(5)六氟硅酸铵+氯化十六烷基吡啶(SiF + CPC)。处理程序后,每个样本都被放置在人工唾液中。在脱矿和再矿化1周和4周后,用QLF-D测量荧光损失和病变面积。对数据进行统计学分析(α = 0.05)。结果各药物处理1、4周后脱矿牙釉质标本的荧光值与预处理值比较差异均有统计学意义(p<0.05)。第4周时,计算CR、APF和SiF组与对照组相比荧光增益最高(p<0.05)。结论APF、SiF和CR组的再矿化能力明显高于SiF + CPC组和对照组。
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引用次数: 3
From Honeycomb- to Microsphere-Patterned Surfaces of Poly(Lactic Acid) and a Starch-Poly(Lactic Acid) Blend via the Breath Figure Method 通过呼吸图法从蜂窝状到微球状的聚乳酸和淀粉-聚乳酸混合表面
Pub Date : 2016-09-14 DOI: 10.5301/jabfm.5000281
A. Duarte, D. Maniglio, Nuno Sousa, J. Mano, R. Reis, C. Migliaresi
Background This study investigated the preparation of ordered patterned surfaces and/or microspheres from a natural-based polymer, using the breath figure and reverse breath figure methods. Methods Poly(D,L-lactic acid) and starch poly(lactic acid) solutions were precipitated in different conditions – namely, polymer concentration, vapor atmosphere temperature and substrate – to evaluate the effect of these conditions on the morphology of the precipitates obtained. Results The possibility of fine-tuning the properties of the final patterns simply by changing the vapor atmosphere was also demonstrated here using a range of compositions of the vapor phase. Porous films or discrete particles are formed when the differences in surface tension determine the ability of polymer solution to surround water droplets or methanol to surround polymer droplets, respectively. In vitro cytotoxicity was assessed applying a simple standard protocol to evaluate the possibility to use these materials in biomedical applications. Moreover, fluorescent microscopy images showed a good interaction of cells with the material, which were able to adhere on the patterned surfaces after 24 hours in culture. Conclusions The development of patterned surfaces using the breath figure method was tested in this work for the preparation of both poly(lactic acid) and a blend containing starch and poly(lactic acid). The potential of these films to be used in the biomedical area was confirmed by a preliminary cytotoxicity test and by morphological observation of cell adhesion.
本研究利用呼吸图法和反呼吸图法研究了从天然聚合物制备有序图案表面和/或微球的方法。方法将聚乳酸(D, l -乳酸)和淀粉型聚乳酸(淀粉型聚乳酸)溶液在不同的条件下(即聚合物浓度、蒸汽气氛温度和底物)进行沉淀,评价这些条件对所得沉淀物形貌的影响。结果利用气相的一系列组成,简单地通过改变蒸汽气氛来微调最终图案性质的可能性也得到了证明。当表面张力的差异分别决定了聚合物溶液包围水滴的能力或甲醇包围聚合物水滴的能力时,形成多孔膜或离散颗粒。采用简单的标准方案评估体外细胞毒性,以评估在生物医学应用中使用这些材料的可能性。此外,荧光显微镜图像显示细胞与材料的良好相互作用,在培养24小时后,细胞能够粘附在图案表面上。结论在制备聚乳酸和含有淀粉和聚乳酸的共混物时,使用呼吸图法测试了图案表面的发展。初步的细胞毒性试验和细胞粘附的形态学观察证实了这些薄膜在生物医学领域的应用潜力。
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引用次数: 10
Effect of Graphene Oxide on Bacteria and Peripheral Blood Mononuclear Cells 氧化石墨烯对细菌和外周血单核细胞的影响
Pub Date : 2016-09-07 DOI: 10.5301/jabfm.5000325
J. Campos-Delgado, K. L. Castro, J. Munguia-Lopez, Ana K. González, M. Mendoza, B. Fragneaud, R. Verdan, J. Araujo, F. J. González, H. Navarro‐Contreras, I. Pérez-Maldonado, A. De León-Rodríguez, C. Achete
Background Driven by the potential biological applications of graphene, many groups have studied the response of cells exposed to graphene oxide (GO). In particular, investigations of bacteria indicate that there are 2 crucial parameters, which so far have only been investigated separately: GO size and exposure methodology. Our study took into account both parameters. We carefully characterized the samples to catalog sizes and structural properties, and tested different exposure methodologies: exposure in saline solution and in the presence of growth media. Furthermore, we performed experiments with peripheral blood mononuclear cells exposed to our GO materials. Methods Atomic force microscopy, scanning electron microscopy, Raman spectroscopy, X-ray photoelectron spectroscopy and transmission electron microscopy were used to characterize the morphology and composition of different samples of GO: GO-H2O, GO-PBS and GO-MG. Our samples had 2D sizes of ∼100 nm (GO-H2O and GO-PBS) and >2 µm (GO-MG). We tested antibacterial activity and cytotoxicity toward peripheral blood mononuclear cells of 3 different GO samples. Results A size-dependent growth inhibition of Escherichia coli (DH5 α) in suspension was found, which proved that this effect depends strongly on the protocol followed for exposure. Hemocompatibility was confirmed by exposing peripheral blood mononuclear cells to materials for 24 hours; viability and apoptosis tests were also carried out. Conclusions Our experiments provide vital information for future applications of GO in suspension. If its antibacterial properties are to be potentiated, care should be taken to select 2D sizes in the micrometer range, and exposure should not be carried out in the presence of grow media.
在石墨烯潜在的生物学应用的驱动下,许多研究小组研究了细胞暴露于氧化石墨烯(GO)的反应。特别是,对细菌的调查表明,有两个关键参数,迄今为止只分别进行了调查:氧化石墨烯的大小和暴露方法。我们的研究考虑了这两个参数。我们仔细地描述了样品的目录大小和结构特性,并测试了不同的暴露方法:在盐水溶液中暴露和在生长介质中暴露。此外,我们对暴露于氧化石墨烯材料的外周血单个核细胞进行了实验。方法采用原子力显微镜、扫描电镜、拉曼光谱、x射线光电子能谱和透射电镜对不同样品GO- h2o、GO- pbs和GO- mg的形貌和组成进行表征。我们的样品的二维尺寸为~ 100 nm (GO-H2O和GO-PBS)和bbb20µm (GO-MG)。我们测试了3种不同氧化石墨烯样品对外周血单个核细胞的抗菌活性和细胞毒性。结果在悬浮液中发现了大肠杆菌(DH5 α)的大小依赖性生长抑制作用,证明这种作用与暴露方案密切相关。外周血单个核细胞与材料接触24小时,确认血液相容性;同时进行细胞活力和细胞凋亡试验。我们的实验为氧化石墨烯在悬浮液中的应用提供了重要的信息。如果要增强其抗菌性能,应注意选择微米范围内的2D尺寸,并且不应在生长介质存在的情况下进行暴露。
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引用次数: 4
Investigation into the Elastic Properties of ex vivo Porcine Corneas Subjected to Inflation Test after Cross-Linking Treatment 交联处理后猪离体角膜充气试验弹性性能的研究
Pub Date : 2016-05-01 DOI: 10.5301/jabfm.5000262
S. Matteoli, A. Virga, I. Paladini, R. Mencucci, A. Corvi
Background The aim of this work was to evaluate the effect of cross-linking (CXL) on ex vivo porcine corneal elastic properties, using an inflation procedure. Methods Twelve corneas were subjected to standard CXL (370 nm, 3 mW/cm2, 30 minutes), while 12 were used as controls. Corneal thickness was measured by Visante optical coherence tomography, before and immediately after treatment, and before inflation test. Both intraocular pressure and radial apical cornea displacement were measured during inflation. Stress-strain curves were obtained by applying the linear shell theory. The elastic modulus was evaluated by calculating the slope of the stress-strain curves. Results Results showed a statistically significant increase in elastic modulus (p<0.0001), with a mean of 3,868 ± 502 kPa for cross-linked corneas and 2,727 ± 238 kPa for untreated corneas, when subjected to high pressure (40-60 kPa). CXL significantly increased porcine cornea stiffness by about 42%. Findings did not show any significant difference within the physiological range of pressure (2-4 kPa). Conclusions The inflation test has been proven to be a valuable tool for the investigation of corneal biomechanics, maintaining both integrity and geometry of corneal tissue.
本研究的目的是评估交联(CXL)对离体猪角膜弹性性能的影响。方法将12只角膜进行标准CXL (370 nm, 3 mW/cm2, 30 min)处理,12只角膜作为对照。在治疗前、治疗后和充气试验前,用Visante光学相干断层扫描测量角膜厚度。充气过程中测量眼压和径向角膜顶位移。应用线性壳理论得到了应力-应变曲线。通过计算应力-应变曲线的斜率来计算弹性模量。结果结果显示,交联角膜的弹性模量在高压(40-60 kPa)下平均增加3,868±502 kPa,未处理角膜的弹性模量平均增加2,727±238 kPa,具有统计学意义(p<0.0001)。CXL可显著提高猪角膜硬度约42%。结果显示,在生理压力范围(2 ~ 4 kPa)内无显著差异。结论膨胀试验是研究角膜生物力学的有效工具,可保持角膜组织的完整性和几何形状。
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引用次数: 16
Synthesis Variants of Quaternary Ammonium Polyethyleneimine Nanoparticles and Their Antibacterial Efficacy in Dental Materials 季铵盐聚乙烯亚胺纳米颗粒的合成及其在口腔材料中的抗菌作用
Pub Date : 2016-05-01 DOI: 10.5301/jabfm.5000269
Nathan Zaltsman, Dana Kesler-Shvero, E. Weiss, N. Beyth
Background Resin-based dental materials allow bacterial growth on their surface and lack antibacterial activity, leading to functional and esthetic failure. Quaternary ammonium polyethyleneimine (QPEI) nanoparticles (NPs) incorporated in resin-based composite at 2% wt/wt have demonstrated prolonged and complete inhibition of bacterial growth. This study focused on optimization of QPEI NP synthesis to reduce the concentration required for bacterial growth inhibition. The objective here was to enhance antimicrobial efficacy by excess base neutralization, using phosphoric or hydrochloric acid, and by using surfactants. Methods QPEI NP variants were prepared (i) under controlled neutralization of acid, using NaHCO3, (ii) under controlled carbonate ion neutralization with HCl or H3PO4 and (iii) by treatment with N-lauroylsarcosine or glycerol monostearate. NPs incorporated in the dental materials were examined for their antibacterial effect against Enterococcus faecalis. Results Controlled addition of NaHCO3 resulted in modified QPEI NPs with an increased ability to inhibit bacterial growth. Surface treatment with N-lauroylsarcosine resulted in enhanced antibacterial activity at 0.5% wt/wt concentration in acrylate and epoxy resin-based dental materials. Conclusions The antimicrobial efficacy of QPEI NP may be improved significantly by controlling the addition of NaHCO3, neutralization of excess base and the surface-agent effect.
基于树脂的牙科材料允许细菌在其表面生长,并且缺乏抗菌活性,导致功能和美观失败。季铵聚乙烯亚胺(QPEI)纳米颗粒(NPs)以2% wt/wt掺入树脂基复合材料中,已证明对细菌生长有长期和完全的抑制作用。本研究的重点是优化QPEI NP的合成,以降低细菌生长抑制所需的浓度。这里的目的是通过过量碱中和,使用磷酸或盐酸,并通过使用表面活性剂来提高抗菌效果。方法:采用NaHCO3控制中和酸,HCl或H3PO4控制中和碳酸盐离子,n -月桂酰肌氨酸或单硬脂酸甘油处理,制备QPEI NP变体。研究了掺入口腔材料的NPs对粪肠球菌的抗菌作用。结果控制NaHCO3的添加导致修饰的QPEI NPs具有增强的抑制细菌生长的能力。在丙烯酸酯和环氧树脂基牙科材料中,n-月桂酰肌氨酸表面处理在0.5% wt/wt浓度下增强了抗菌活性。结论通过控制NaHCO3的加入、过量碱的中和和表面剂效应,可显著提高QPEI NP的抗菌效果。
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引用次数: 18
Promotion of Osteogenic Differentiation by Amnion/Chorion Membrane Extracts 羊膜/绒毛膜提取物促进成骨分化
Pub Date : 2016-05-01 DOI: 10.5301/jabfm.5000264
Y. Go, Sung Eun Kim, G. Cho, S. Chae, J. Song
Background The amniotic membrane is a favorable biomaterial to apply in the field of tissue engineering because of its unique biological properties. Human amniotic membranes consist of 2-layered sheets containing numerous growth factors, cytokines and other bioactive substances. Methods In this study, we explored the potential of amnion membrane extracts (AME) and amnion/chorion membrane extracts (A/CME) to promote osteogenic differentiation of osteoblast-like (MG-63) cells. MG-63 cells were cultured in osteogenic induction medium (OIM) with or without 100 µg/mL of AME or A/CME. To determine the early and late differentiation of osteogenesis, alkaline phosphatase (ALP) activity and calcium deposition were measured at 3, 7, 10 and 24 days. Expression of specific genes associated with osteogenic differentiation, including osteocalcin (OCN), osteopontin (OPN), runt domain-containing transcription factor (Runx2) and osterix (OSX) was also determined. Results In vitro experiments demonstrated that A/CME increased ALP activity, osteogenic gene expression and mineralization under osteogenic-inducing conditions. Notably, we found that A/CME contained growth factors related to osteogenesis, including fibroblast growth factors and transforming growth factors, which potentially promoted osteogenic differentiation of MG-63 cells to a greater extent than AME. Conclusions These results indicate that A/CME is capable of providing growth factors and other substrates for osteogenic differentiation, which significantly increased the efficacy of osteogenesis in MG-63 cells. Taken together, the results of this study suggest that human A/CME is a promising biomaterial with therapeutic potential in bone regeneration applications.
背景羊膜具有独特的生物学特性,是一种很有前途的生物材料,可应用于组织工程领域。人羊膜由两层膜组成,其中含有大量的生长因子、细胞因子和其他生物活性物质。方法探讨羊膜提取物(AME)和羊膜/绒毛膜提取物(A/CME)促进成骨细胞样细胞(MG-63)成骨分化的潜力。MG-63细胞在含或不含100µg/mL AME或A/CME的成骨诱导培养基(OIM)中培养。在第3、7、10、24天分别测定碱性磷酸酶(ALP)活性和钙沉积,以确定成骨分化的早、晚期。测定了与成骨分化相关的特定基因的表达,包括骨钙素(OCN)、骨桥蛋白(OPN)、含runt结构域转录因子(Runx2)和osterix (OSX)。结果体外实验表明,在成骨诱导条件下,A/CME增加了ALP活性、成骨基因表达和矿化。值得注意的是,我们发现A/CME含有与成骨相关的生长因子,包括成纤维细胞生长因子和转化生长因子,这些因子可能比AME更大程度地促进MG-63细胞的成骨分化。结论A/CME可为MG-63细胞的成骨分化提供生长因子等基质,显著提高成骨效果。综上所述,本研究结果表明,人A/CME是一种具有骨再生治疗潜力的生物材料。
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引用次数: 18
Comparison of Shear Bond Strength of Universal Adhesives on Etched and Nonetched Enamel 通用胶粘剂在蚀刻与非蚀刻搪瓷上剪切粘接强度的比较
Pub Date : 2016-04-01 DOI: 10.5301/jabfm.5000261
Riccardo Beltrami, M. Chiesa, A. Scribante, J. Allegretti, C. Poggio
Background The purpose of this study was to evaluate the effect of surface pretreatment with 37% phosphoric acid on the enamel bond strength of different universal adhesives. Methods One hundred and sixty bovine permanent mandibular incisors freshly extracted were used as a substitute for human teeth. The materials tested in this study included 6 universal adhesives, and 2 self-etch adhesives as control. The teeth were assigned into 2 groups: In the first group, etching was performed using 37% phosphoric acid for 30 seconds. In the second group, no pretreatment agent was applied. After adhesive application, a nanohybrid composite resin was inserted into the enamel surface by packing the material into cylindrical-shaped plastic matrices. After storing, the specimens were placed in a universal testing machine. The normality of the data was calculated using the Kolmogorov-Smirnov test. Analysis of variance (ANOVA) was applied to determine whether significant differences in debond strength values existed among the various groups. Results Groups with phosphoric acid pretreatment showed significantly higher shear bond strength values than groups with no enamel pretreatment (p<0.001). No significant variation in shear strength values was detected when comparing the different adhesive systems applied onto enamel after orthophosphoric acid application (p>0.05). Conclusions All adhesives provide similar bond strength values when enamel pretreatment is applied even if compositions are different. Bond strength values are lower than promised by manufacturers.
本研究的目的是评价37%磷酸表面预处理对不同通用胶粘剂牙釉质结合强度的影响。方法采用新鲜拔牙的牛恒颌门牙160颗作为人牙的替代物。本研究测试的材料包括6种通用胶粘剂和2种自蚀刻胶粘剂作为对照。将牙齿分为两组:第一组使用37%磷酸进行30秒的蚀刻。第二组不使用预处理剂。粘结后,将纳米杂化复合树脂填充到牙釉质表面,形成圆柱状的塑料基体。标本存放后,置于万能试验机中。使用Kolmogorov-Smirnov检验计算数据的正态性。采用方差分析(ANOVA)确定各组间脱粘强度值是否存在显著差异。结果磷酸预处理组与未预处理组的牙釉质抗剪强度差异有统计学意义(p0.05)。结论不同成分的粘接剂在进行牙釉质预处理时粘接剂的粘结强度相近。粘结强度值低于制造商承诺的值。
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引用次数: 38
Electrical and Microstructural Characterization of Ceramic Gadolinium-Doped Ceria Electrolytes for ITSOFCs by Sol-Gel Route 溶胶-凝胶法制备itsofc掺杂钆陶瓷电解质的电学和微观结构表征
Pub Date : 2016-04-01 DOI: 10.5301/jabfm.5000265
G. Accardo, C. Ferone, R. Cioffi, D. Frattini, L. Spiridigliozzi, G. Dell’Agli
Background Gadolinium-doped ceria (GDC) is a promising alternative as a solid electrolyte for intermediate temperature solid oxide fuel cells (ITSOFCs) due to its low operating temperature and its high electrical conductivity. The traditional synthesis processes require extended time for powder preparation. Sol-gel methodology for electrolyte fabrication is more versatile and efficient. Methods In this work, nanocrystalline ceria powders, with 10 and 20 mol% of gadolinium (Ce0.9Gd0.1O1.95 and Ce0.8Gd0.2O1.9) were synthesized by a modified sol-gel technique, featuring a nitrate-fuel exothermic reaction. GDC tablets were prepared from powders and sintered at 1500°C with a dwell time of 3 hours. The sintered pellets’ microstructure (by SEM) and electrical conductivity (by EIS) were evaluated. The powder properties, such as crystalline structure (by XRD), thermal properties (TGA/DTA), particle size and morphology (TEM) and textural properties (BET method) were determined and, in addition, for the first time an accurate chemical structural evolution (FTIR) was studied. Results Sintered GDC0.8 samples exhibited the maximum theoretical density of 97% and an average grain size of 700 nm. The electrical conductivity vs. temperature showed values ranging from 1.9∙10−2 to 5.5∙10−2 S·cm−1 at 600°C and 800°C for GDC with 20 mol% of gadolinium. Conclusions The methodology investigated showed reduced reaction time, a better control of stoichiometry and low cost. Characterization results demonstrated that these materials can be applied in ITSOFCs due to high conductivity, even at 550°C-600°C. The increased conductivity is related to the improved mobility of gadolinium ions in a high-density structure, with nanometric grains.
掺钆二氧化铈(GDC)由于其工作温度低、导电性好,是中温固体氧化物燃料电池(ITSOFCs)的理想电解质。传统的合成工艺需要延长粉末制备时间。溶胶-凝胶法制备电解质的方法更加通用和高效。方法采用改进的溶胶-凝胶法,采用硝酸盐-燃料放热反应制备了钆含量分别为10%和20% (Ce0.9Gd0.1O1.95和Ce0.8Gd0.2O1.9)的纳米晶二氧化铈粉体。以粉末为原料制备GDC片剂,在1500℃下烧结,保温时间为3小时。对烧结球团的微观结构(SEM)和电导率(EIS)进行了表征。测定了粉末的晶体结构(XRD)、热性能(TGA/DTA)、粒度和形貌(TEM)、织构性能(BET)等性能,并首次进行了精确的化学结构演化(FTIR)研究。结果烧结后的GDC0.8样品理论密度最大可达97%,平均晶粒尺寸为700 nm。在600°C和800°C时,含20 mol%钆的GDC的电导率随温度变化范围为1.9∙10−2 ~ 5.5∙10−2 S·cm−1。结论该方法具有反应时间短、化学计量控制好、成本低等优点。表征结果表明,由于这些材料具有高导电性,即使在550°C-600°C下也可以应用于itsofc。电导率的提高与钆离子在具有纳米颗粒的高密度结构中的迁移率提高有关。
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引用次数: 33
期刊
Journal of Applied Biomaterials & Biomechanics
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