凝胶浇注成型制备致密 SiC陶瓷材料

采用一种凝胶浇注成型预配液作为陶瓷粉体的分散介质,将亚微米级SiC粉体和烧结助剂Y2O3、Al2O3直接混合,制得了固含量>50vol％的凝胶浇注浆料,在100s-1的剪切速率下,浆料粘度<1Pa·s,可以顺利实现凝胶浇注成型;对得到的SiC素坯进行了无压烧结．在2000℃保温1h(氩气氛)的烧结条件下,烧结体相对密度为(98．1±0．2)％,抗折强度、硬度和韧性分别为(722±70)MPa、(20．18±0．75)GPa、(4．00±0．20)MPa·m1／2．     

Sintering kinetics of YAG ceramics

Solid state reactive （SSR） sintering kinetics was observed for YAG ceramics. There were two densification stages in sin- tering process due to its reaction. After the first stage, samples began to expand, then, the second densification stage began. At a heat- ing rate of 10 ℃/min, the sample warped down and warped back to straight. The apparent activation energy of the first densification process was about 522 kJ/mol for the initial shrinkage of A1203 and Y203 mixed powder green-body, which increased in the follow- ing process due to the solid state reaction. In the second densification stage, synthesis reaction of YAG still worked. Green-bodies processed with higher heating rate got more shrinkage at the same temperature than lower heating rate green bodies. And its kinetic field diagram was abnormal, compared with that of other reported ceramics, such as Al203. It was found that the reaction of YAG provided positive effect to the sintering driving force. The apparent activation energy for densification of SSR YAG sintered in ArH5 atmosphere was 855 kJ/mol at temperature holding sintering. And the apparent activation energy for grain growth was 1053 kJ/mol.     

热压碳化硅陶瓷材料的研究

碳化硅是一种应用在高温工程中有希望的候选材料。目前,许多工作正致力于研究气体透平和其它工程中需用的强度高、抗氧化性优良的SiC烧结体。 本文研究了添加剂(B_4C、C)和其它工艺参数对热压SiC的烧结性状和机械性能的影响。同时也研究了不同温度、不同时间、湿氧条件下的氧化增重和强度变化。 研究所得的结果如下: (1)B_4C和C是热压α-SiC达到致密必不可少的添加剂。达到最高密度的B_4C和C的最低限量分别为0.5wt％。 (2)热压SiC的室温抗弯强度约为500MN/m~2,且从室温到1400℃高温强度都几乎不变,高温时略有升高。另外,强度值似乎与碳的添加量(直到3wt％)无关。 (3)添加1wt％B_4C和3wt％C的SB_1C_3组成(热压条件是2050℃、保温45min、压力40MN/m~2),其性能是:密度3.17g/cm~3,室温强度480MN/m~2、热膨胀系数4.6×10~(-6)℃~(-1),洛氏硬度HRA93.5。 (4)直到1280℃,掺B_4C和C的SB_1C_3组成的抗氧化性是非常优良的,氧化速率与时间呈抛物线关系,氧化后的室温强度也是基本不变的。     

通过凝胶注模成型和无压烧结制备碳化硅陶瓷

以四甲基氢氧化铵为分散剂,糊精为碳源,通过静电稳定作用,制备了高固相含量、分散良好的碳化硅陶瓷浆料。以水溶性N,N–二甲基丙烯酰胺为单体,N,N’–亚甲基双丙烯酰胺为交联剂,采用实验室开发的偶氮[2–(2–咪唑啉–2–基)]丙烷HCl引发体系,在45～50℃引发单体聚合,制备出水基凝胶注模碳化硅素坯,素坯的相对密度达58%,抗弯强度大于40MPa。进一步通过无压烧结制备相对密度高于98%,硬度达28GPa,强度达530 MPa的SiC陶瓷。对素坯和SiC陶瓷的微结构和力学性能进行了测试和表征。结果表明:采用糊精作为碳源可以提高凝胶注模浆料的分散性,避免凝胶过程中的碳阻聚问题,有利于制备出高性能的碳化硅陶瓷材料。     

Sintering of transparent Nd:YAG ceramics in oxygen atmosphere

Yttrium aluminum garnet (YAG) transparent ceramics were fabricated by sintering at oxygen atmosphere. Tetraethyl orthosilicate (TEOS) was added as the sintering additive to control the grain growth and densification. Pores were eliminated clearly at temperature lower than 1700oC, while grain size was around 3 μm. The in-line transmittance was 80% at 1064 nm when samples were sintered at 1710oC. The effect of TEOS was studied in oxygen atmosphere sintering for Nd:YAG transparent ceramics. At higher temperature like 1710oC, the grain growth mechanism was solute drag, while at 1630 and 1550 oC the grain growth was controlled by liquid phase sintering mechanism. And 0.5 wt.% TEOS was the best adding content for Nd:YAG sintered in oxygen atmosphere.     

Na2O-B2O3-SiO2玻璃焊料连接碳化硅陶瓷接口抗热震性能

采用水淬法对以Na₂O-B₂O₃-SiO₂体系玻璃焊料连接的常压烧结碳化硅试条的抗热震性能进行了研究. 对不同温度下淬火后接口以及断面处微观结构进行了比较与分析, 并对比了不同淬火温度以及固定淬火温度为150℃时多次热循环后连接试条的残余弯曲强度. 结果表明, 对于单次淬火, 当淬火温度为150℃时, 由于热应力引起中间层内部微裂纹扩展, 导致残余弯曲强度迅速降低到(152±28) MPa. 淬火温度在150℃~320℃时, 中间层内部裂纹保持在亚临界状态, 相应弯曲强度基本保持在140 MPa. 继续升高淬火温度至420℃时, 裂纹进一步扩展, 试条残余弯曲强度迅速降低至(32±8) MPa. 对于多次热循环, 当淬火温度固定在150℃时, 经多次热循环, 残余弯曲强度与热循环次数变化不明显, 基本保持在120 MPa左右, 这说明在150℃以下淬火, 连接试条具有较好的抗热循环冲击性能.     

水基流延成型制备ZrB2和ZrB2-20vol% SiC复合材料的微观结构和抗热震性能

研究了水基流延成型和热压烧结制备的ZrB2和ZrB2-20vol% SiC(ZS20)材料的微观结构和抗热震性能.在ZS20材料中分别观察到了Zr-B-C和Zr-B-W固溶相,而在ZrB2材料中并未发现有固溶相.固溶相的形成使得晶格参数减小,因此ZS20材料中ZrB2的衍射峰向高角度偏移.采用淬火法测得ZrB2和ZS20材料的临界热震温度分别为298℃和306℃,并将实验值与理论计算值进行比较.ZrB2基体与SiC第二相及固溶相之间由于热膨胀系数的差异而在材料内部引入应力,因而ZS20材料抗热震性能的实验值低于理论计算值.     

凝胶冷冻干燥法制备透明氧化钇陶瓷

采用凝胶冷冻干燥法, 在--50℃、8Pa的真空度下制备了碱式硝酸钇前驱体. 干燥后前驱体呈疏松片状堆积, 比烘箱干燥样品具有更为清晰的轮廓. 经过1100℃煅烧后, 凝胶冷冻干燥处理的粉体具有较细的颗粒, 颗粒尺寸分布均一, 并且具有较大的比表面积. 该粉体经过干压型, 于1700℃真空保温4h烧结后得到晶粒大小均匀的致密多晶透明陶瓷, 平均晶粒尺寸在40μm左右, 样品相对密度达99.6%. 样品经抛光后可见光400nm波长透过率达60%, 并且在紫外波段也具有类似于氧化钇单晶的高透过率.