原位反应结合多孔Si3N4陶瓷的制备及其介电性能

以氮化硅(Si₃N₄)和氧化铝(Al₂O₃)为起始原料, 利用原位反应结合技术制备Si₃N₄多孔陶瓷. 研究烧结温度和保温时间对Si₃N₄多孔陶瓷的微观结构、力学性能以及介电性能的影响. 结果表明: 烧结温度在1350℃以下, 保温时间<4h时, 随着烧结温度的升高, 保温时间的延长, 样品的强度和介电常数增大; 但条件超出这个范围, 结果刚好相反; 物相分析表明多孔陶瓷主要由Si3N4和Al₂O₃以及Si₃N₄氧化生成的SiO₂(方石英)组成. 所制备的多孔Si₃N₄陶瓷的气孔率范围为25.34%～48.86%, 抗弯强度为34.77～127.85MPa, 介电常数为3.0～4.6, 介电损耗约为0.002.     

Y-α/β-Sialon陶瓷材料及疲劳特性研究

本文通过组份设计,选用Si₃N₄、AIN和Y₂O₃等粉末为原料,在1800～1950℃进行气氛加压烧结（GPS）,制备了性能优良的Y-α/β-Sialon陶瓷材料;利用XRD、EDAX和HREM详细地研究了相组成和晶界特性,其主晶相为β-Sialon和α-Sialon,晶界由少量的J－Y₄Si₂O₇N₂结晶相以及微量的玻璃相构成;并进一步探讨了材料在循环疲劳载荷下Vickers压痕短裂纹扩展特性,结果表明,最大应力强度因子与裂纹扩展速率之间呈V型扩展行为,并对外加应力水平非常敏感．     

熔盐热析出反应金属化Si3N4与Si3N4的连接

在采用熔盐热析出反应在Si₃N₄陶瓷表面沉积钛金属膜的基础上,对CuAg合金在金属化表面的润湿性进行了研究,结果表明,CuAg合金能对采用该方法金属化的Si₃N₄陶瓷实现良好润湿．在此基础上,成功实现了钛金属化Si₃N₄陶瓷与Si₃N₄陶瓷的连接并对连接工艺进行了系统研究．连接界面的TEM研究发现,界面上广泛存在Ti-Cu－Si-N相并对这种相对连接强度的影响进行了讨论．     

CVI制备C/Si3N4复合材料及其表征

以SICl₄-NH₃-H₂为反应体系,采用化学气相渗透法CVI)制备C/Si₃N₄复合材料.渗透产物的能谱和X射线衍射表明渗透产物为非晶态Si₃N₄,经1350℃真空热处理后,产物仍然为非晶态Si₃N₄;经1450℃真空热处理后,产物已经发生晶型转变,由非晶态转变为晶态的α-Si₃N₄和β-Si₃N₄.渗透温度、渗透时间、气体流量对试样致密化、增重及微观结构的影响研究表明渗透温度为900℃、SiCl4流量为30mL/min、H2流量为100mL/min、NH₃流量为80mL/min、渗透时间120h、系统压力1000Pa时,气体渗透进入碳布预制体后,在预制体内反应均匀,制备的复合材料较均匀.     

多孔氮化硅/碳化硅复合材料制备的反应机理分析

为了探索碳热还原法制备多孔氮化硅/碳化硅(Si₃N₄/SiC)复合陶瓷材料在高温阶段的反应机理,采用固化的酚醛树脂为碳源,通过热解产生具有反应性的碳,使之在1300-1780℃等不同温度下与表面包裹的氮化硅粉反应,氩气为保护气氛.通过对试样的XRD、TEM分析和显微结构观察,结合反应的热力学和动力学结果计算推测,树脂裂解碳与Si₃N₄反应生成SiC的机理主要为Si₃N₄分解生成Si(l)与C进一步发生的液-固反应,和Si(l)与反应过程中的中间产物CO(g)之间发生的液-气反应.其他还包括C与Si₃N₄间直接进行的固-固反应;C与Si₃N₄表面的SiO₂间的气-固反应以及由SiO(g)、Si(g)参与的气-固反应.树脂裂解碳与Si₃N₄从1400℃左右开始发生反应形成SiC,温度升高对SiC层的生长有促进,保温时间的延长对SiC层的生长厚度影响较大.     

TZP陶瓷的高温润滑研究

研究了TZP陶瓷在固体润滑下,室温（25℃）至600℃制备范围内的摩擦学特性．结果表明,使用石墨和MoS₂润滑剂,可在室温至600℃范围内降低TZP／Si₃N₄摩擦副的摩擦系数和磨损率,但当环境温度过高时,摩擦系数和磨损量有所增加;使用CeO₂和Cu对TZP／Si₃N₄摩擦副的摩擦系数影响不大,但可以降低TZP陶瓷的磨损量;CeF₃在高温时,由于结晶化趋势完善及沿（002）面的滑移取向,故可对TZP陶瓷起到良好的润滑作用．     

放电等离子快速烧结SiC晶须增强Si3N4BN层状复合材料

采用放电等离子烧结技术(SPS)快速烧结了SiC晶须增强的Si₃N₄/BN层状复合材料.利用SPS技术,在烧结温度为1650℃、保温15min的条件下,材料的密度可达3.18g/cm³,抗弯强度高达600MPa,断裂功达到3500J/m².研究表明:特殊的层状结构、SiC晶须的拔出与折断是材料断裂功提高的主要原因.X射线衍射及扫描电子显微镜研究表明:α-Si₃N₄已经在短短的烧结过程中全部转变成长柱状的β-Si₃N₄,并且长柱状的β-Si₃N₄和SiC晶须具有明显的织构.     

α/β-Sialon陶瓷材料及其疲劳寿命研究

通过组成设计,以Si₃N₄、AIN、Al₂O₃和Y₂O₃粉末为原料,采用气氛加压烧结工艺,在1800～1980℃,1．0～3、0MPaN₂压力下烧结,制备了α／β-Sialon陶瓷材料,通过XRD,SEM和HREM等分析可见,其材料的显微结构是由棒状的β-Sialon和近似等轴的α-Sialona组成,在晶界存在微量的结晶相和玻璃相．并进一步研究了α／β-Sialon陶瓷材料的疲劳寿命,实验证明,该材料的疲劳极限约为其静态强度的75％．     

自蔓延高温合成Y-α/β-Sialon粉末

本文通过组成设计,以Si、Al、Y₂O₃为原料,Si₃N₄为稀释剂,利用自蔓延高温合成法（SHS）制备了Y－α／β－Sialon粉末;并利用XRD、化学分析法分别研究了α－Sialon简称α′）、β－Sialon简称β′）相组成和游离硅含量;且详细讨论了氮气压力、稀释剂含量对生成物Y－α／β－Sialon中的α′、β′相及残余硅含量的影响．     

Sialon结合SiC复合材料的制备与性能

利用天然高岭土,通过碳热还原氮化法合成β-Sialon（Si₃Al₃O₃N₅）粉体,并制备出Sialon结合SiC复合材料,同时测定该材料的机械性能和热力学性能,Sialon结合SiC复合材料可在1550～1640℃烧结,烧结体的体积密度可达2．26g／cm³,三点抗弯强度42．0MPa,1200℃恒温20min后,经15℃冷水淬冷10次仍保持原有强度,1350℃空气流中灼烧失重率低于0．035％／cm²．     

可切削的氧化锆陶瓷牙科修复体的制备

通过控制CaO_₂-Al_₂O_₃-SiO_₂硅酸盐玻璃粉体,在1300℃低温下液相烧结获得热膨胀系数在7.19×10 ^-6/℃和8.15×10^-6/℃范围内,与修复体饰瓷相近,其强度在340～360MPa,韧性在2.7～3.5 MPa·m^I/2,可切削性与In-Ceram相当的氧化锆陶瓷牙科修复体.     

纳米SiO2质量分数对胶粘碳纤维增强树脂复合材料板-钢搭接界面黏结性能的影响

胶黏剂力学性能对碳纤维增强树脂复合材料(CFRP)加固钢结构的界面黏结性能影响显著。基于研制的胶黏剂配比,分析了不同纳米SiO₂质量分数对胶黏剂常温固化后基本力学性能及微观结构的影响,制作了31个CFRP板-钢板双搭接试件,对其进行了常温固化后的承载能力、有效黏结长度、传力模式、黏结-滑移本构等试验研究,得出了纳米SiO₂质量分数对CFRP板-钢板搭接试件界面黏结性能的影响规律,并与常用商品胶黏剂进行了比较。研究结果表明:随纳米SiO₂质量分数的增加,胶黏剂应力-应变关系由线性转变为非线性,应变能、断裂伸长率及剪切强度分别最高提升了292.10%、202.88%和133.12%。微观结构分析表明纳米SiO₂的添加使断面粗糙度显著增加,形成了密集的塑性空穴,产生了更多的微裂纹,使胶黏剂的韧性大幅度提高。当纳米SiO₂质量分数从0增至1wt%,搭接试件破坏模式由界面破坏逐渐变为CFRP板层离破坏。掺入纳米SiO₂能显著增加搭接试件的极限承载力(提升256.96%)及界面有效黏结长度(提升3倍),提高CFRP表面的应变及界面剪应力峰值。纳米SiO₂质量分数为0与0.5wt%的搭接试件的黏结-滑移曲线为双线性三角形模型,纳米SiO₂质量分数为1wt%的搭接试件的黏结-滑移曲线为三线性梯形模型,黏结界面韧性大幅提升。CFRP-钢界面承载能力受胶黏剂拉伸强度与断裂伸长率的双重影响,非线性高强度(即具有较高应变能)胶黏剂对应的CFRP-钢搭接接头具有更好的界面性能。      

硅氧烷改性水性聚氨酯乳液的附着性能

利用硅氧烷（γ-氨丙基三乙氧基硅烷（KH550）、γ-缩水甘油氧丙基三甲氧基硅烷（KH560））改性水性聚氨酯乳液,考察了改性后乳液成膜在无机基材表面附着力的变化。KH560改性的乳液成膜在无机基材表面具有较好的附着力,其中对玻璃的干附着力可达1级,对标准马口铁也可达1～2级;在浸水后,尤其在玻璃表面附着力保持最好,附...     

Bond strength and effective bond length of FRP sheets/plates bonded to concrete considering the type of adhesive layer

Recent experimental results of the FRP–concrete bonded joint using flexible adhesive showed that the most popular analytical models available in the literature underestimate the bond strength and the effective bond length of these experiments. Most of these existing models need to be modified to consider the type of adhesive layer. Consequently, the bond strength model proposed by Chen and Teng (2001) has been modified to consider the type of adhesive layer. An extensive database consisting of about 100 test results of FRP–concrete joint has been assembled to examine the validity of the proposed model taking the type of adhesive layer into consideration. The modified bond strength model is accurately capable of predicting the bond strength and the effective bond length.     

含Zn、Mg生物玻璃的制备及性能研究

采用溶胶-凝胶法,在58S生物玻璃的基础上,分别用0.5wt％的氧化镁和氧化锌取代氧化钙制备了含镁和含锌的生物玻璃.压制的试样分别在600、700和800℃煅烧以做强度测试,并分析了600和800℃煅烧后的物相组成.结果表明,三种试样煅烧至800℃仍为玻璃态,而镁锌的掺入大幅度提高了生物玻璃的强度,这主要是因为Mg-O和Zn-O具有比Ca-O高的键能.模拟体液浸泡试验表明,镁和锌降低了羟基磷灰石的早期成核速度,但并不影响其后期的生长.浸泡三天后所有样品表面都被羟基磷灰石覆盖,表明了样品具有良好的生物活性.     

Cooling rate-induced glass-adhesion variations using crystallizing hot-melt adhesives

Polychlorotrifluoroethylene (PCTFE) and PCTFE copolymeric films are being used in the electronic packaging industry as insulating dielectric layers between microwave circuits. Because these films are semicrystalline and, in this application, are being used as hot-melt adhesives, the cooling rate is an important processing variable, affecting the crystallinity of the PCTFE films which, in turn, affect many properties including dielectric characteristics and mechanical properties. In this study, the crystallinity of PCTFE and PCTFE copolymeric films as a function of cooling rate was characterized by wide-angle X-ray scattering. As expected, the degree of crystallinity decreased as the cooling rate increased. Analysis of mechanical properties as a function of cooling rate by tensile testing showed that the mechanical behaviour of the films became more ductile with faster cooling rates. Because the cooling rate has also been shown to significantly affect adhesion in previous studies, the effect of cooling rate on the bond strength between PCTFE and a glass substrate was analysed. Peel testing was performed on PCTFE/glass laminates revealing that the adhesive bond strength increased as the cooling rate was increased. Thus, optimum adhesion is achieved with faster cooling rates. This was attributed to the higher fracture energy and greater ductility of the adhesive. This revised version was published online in November 2006 with corrections to the Cover Date.     

聚醚分子量对PUA光固化胶黏剂性能的影响

采用不同分子量的聚醚合成了聚氨酯丙烯酸酯预聚体,加入其他助剂配制成光固化胶黏剂。傅里叶红外光谱表明,C=C双键有效地参与了光固化反应;透光率测试显示,聚乙二醇分子量增大,光固化后胶黏剂的透光率降低,聚醚分子量小于1000时,变化不大;DSC曲线表明,预聚体中聚醚分子量越大,玻璃化温度越低;TG曲线表明,不同分子量的聚乙二醇对胶黏剂的热稳定性区别不大;剪切强度证明,随着聚乙二醇分子量的增加,胶黏剂的剪切强度下降,聚乙二醇分子量为600时,剪切强度为1547N,且为本体破坏。聚醚分子量为600～1000时,胶黏剂具有最佳的综合性能。     

Functionally graded bioactive glass coating on magnesia partially stabilized zirconia (Mg-PSZ) for enhanced biocompatibility

The coating of magnesia partially stabilized zirconia (Mg-PSZ) with a bioactive glass was investigated for enhancing the bioactivity and bone-bonding ability of Mg-PSZ orthopedic implants. Individual coatings of three different bioactive glasses were prepared by depositing a concentrated suspension of the glass particles on Mg-PSZ substrates, followed by sintering at temperatures between 750 °C and 850 °C. Two silicate-based glass compositions (designated 13–93 and 6P68), and a borosilicate glass composition (H12) were investigated. The microstructure and adhesive strength of the coatings were characterized, and the in vitro bioactivity of the glasses was compared by measuring their conversion kinetics to hydroxyapatite in an aqueous phosphate solution at 37 °C. The 6P68 glass provided the highest adhesive strength (40 ± 2 MPa) but showed very limited bioactivity, whereas the H12 glass had lower adhesive strength (18 ± 2 MPa) but the highest bioactivity. A functionally graded coating, consisting of a 6P68 interfacial layer and an H12 surface layer, was developed to provide a coating with high adhesive strength coupled with rapid in vitro bioactivity.     

The preparation and performance of a novel room-temperature-cured heat-resistant adhesive for ceramic bonding

A novel adhesive for joining ceramic materials was made using silicon-epoxy interpenetrating polymer networks (IPNs) as matrix (based on silicon resin (SR) and diglycidyl ether of bisphenol A (DGEBA) epoxy resin (EP)), γ-glycidoxypropyltrimethoxysilane (γ-GPS) as cross-linking agent, dibutyltin dilaurate (DBTDL) as catalyst, Al, low melting point glass (GP) and B₄C powders as inorganic fillers, low molecular polyamide (LMPA 650) as curing agent. The character and heat-resistance property of the IPNs and adhesive were tested by FT-IR, DSC and TG. The compressive shear strength of ceramic joints was investigated at different temperatures in atmosphere surroundings. The modification mechanism of inorganic fillers was studied using XRD. Results showed that the IPNs were a homogeneous morphology of inter-crosslinked network structure with single T_g. The adhesive could be cured at room temperature with good heat-resistance property due to the chemical bond of epoxy group and Si-O-Si. The optimum compressive shear strength (9.44 MPa at 1000 °C) occurred at SR/EP ratio: 9/1, content of KH560: 2%, Al/GP/B₄C ratio: 3.2/4/3, fillers/IPNs ratio: 6/4. The adhesive had good heat-resistance property with 10% weight loss at 435 °C. Failure mode of joint was mixing failure due to the high chemical bonding force.     

Modification of polymer properties to minimize thermal stresses in adhesive joints

The adhesive behaviour of epoxy-glass microballoon composites was studied at 25 and 75° C for plate and tubular lap joints of various combinations. It was found that the adhesive bond for various joints is enhanced through addition of microballoons. High adhesive force is observed at higher temperatures for various joints combinations where the thermal stresses are lowered and the bond is strengthened. The obtained results for various joint combinations demonstrate that high strength can be achieved when significant thermal stresses do not exist. The filler effect on some physical properties such as density, glass transition temperature, thermal expansion and Poisson's ratio of the epoxy composites is also investigated. Simple analysis indicates the differential thermal expansion coefficient between the adhesive and metallic joints and bulk modulus of the adhesive dictates the stress state.