AlN-SiC固溶体陶瓷研究进展

评述了国内外ＡｌＮ－ＳｉＣ固体溶体陶瓷研究工作的最新进展。着重阐述了烧结工艺,包括粉体机械混合传统烧结工艺及化学活化烧结新工艺,并对其优缺点进行了评价。认为化学活化烧结新工艺是今后制备ＡｌＮ－ＳｉＣ固溶体陶瓷的发展趋势,介绍了该领域的最新发展动态。     

燃烧合成AlN—SiC固溶体陶瓷

在氮气氛中,占燃铝粉,硅粉和碳黑的混合粉末,合成ＡｌＮ－ＳｉＣ陶瓷。研究了氮气压力和反应物配比对燃烧温度,燃烧波蔓延速度以及燃烧产物的影响。结合热力学解释了ＡｌＮ－ＳｉＣ固溶体的形成机理及反应次序。用扫描电镜观察了反应的形貌。     

CaO-Y2O3添加剂对AlN陶瓷显微结构及性能的影响

研究了掺杂ＣａＯ－Ｙ２Ｏ３热压烧结和常压烧结ＡｌＮ陶瓷的性能和显微结构．结果表明：热压烧结ＡｌＮ陶瓷的第二相为Ｙ３Ａｌ５Ｏ１２，常压烧结ＡｌＮ陶瓷的第二相为Ｙ３Ａｌ５Ｏ１２和Ｃａ３Ｙ２Ｏ６；热压烧结ＡｌＮ的第二相体积百分数和晶格氧含量均低于常压烧结；热压烧结ＡｌＮ陶瓷的微观结构良好，其热导率达到２００Ｗ／ｍ·Ｋ．     

添加CaF2—Y2O3的AlN陶瓷的显微结构及热导性质

本文探讨了影响添加ＣａＦ２－Ｙ２Ｏ３的ＡｌＮ陶瓷热导率的显微结构因素，利用ＸＲＤ、ＸＰＳ研究了伴随烧结过程的晶格畸变规律，确定了氧及杂质碳在ＡｌＮ晶格中的扩散行为，从而导致了晶胞的收缩和膨胀，ＴＥＭ和ＨＲＥＭ观察到类似转相区的面缺陷和不同于ＡｌＮ结构的微区，结果表明，除了晶粒内部的缺陷，第二相强烈地影响烧结体的热导率，挥发性第二相有助于提高热导率。     

β‘—Sialon—AlN多型体陶瓷研究

在Ｓｉ－Ａｌ－Ｏ－Ｎ系统中，研究了β－Ｓｉａｌｏｎ－１２Ｈ ＡｌＮ多型体自补强复相陶瓷、利用气压吉工艺制备了致密的β－Ｓｉａｌｏｎ－１２Ｈ ＡｌＮ多型体材料，研究结果表明，材料的主晶相是β－Ｓｉａｌｏｎ－１２Ｈ ＡｌＮ多型体，晶界由含Ｌａ－Ｓｉ－Ａｌ－Ｏ－Ｎ的玻璃相和微量的结晶相组成。     

低温共烧多层AlN陶瓷基片

介绍由高热导率ＡｌＮ陶瓷与金属Ｗ制备的低温共烧多层ＡｌＮ基片，研究了以Ｄｙ２Ｏ３为主的添加系统对低温烧结ＡｌＮ性能，显微结构的影响。     

添加Y2O3-Dy2O3的AlN陶瓷的烧结特性及显微结构

本文探索了以自蔓延高温（ＳＨＳ）法合成并经抗水化处理的ＡｌＮ粉为原料,以Ｙ２Ｏ３－Ｄｙ２Ｏ３作为助烧结剂的ＡｌＮ陶瓷的烧结特性及显微结构,结果表明,晶界处存在Ｄｙ４Ａｌ２Ｏ９、Ｙ３Ａｌ２Ｏ９、ＤｙＡｌＯ３、Ｄｙ２Ｏ３和ＤｙＮ等第二相物质,随烧结温度变化,第二相的种类、数量和分布不同,显微结构也随之变化,从而影响ＡｌＮ的热导率,在１８５０℃下,可获得热导率为１４８Ｗ／ｍ·Ｋ的ＡｌＮ陶瓷。     

SiC—AlN—Y2O3复相陶瓷的制备与性能

通过热压烧结技术，ＳｉＣ、ＡｌＮ和Ｙ２Ｏ３粉末混合体在１９２０￣２０５０℃、Ａｒ气氛下形成了致密的复相陶瓷。在室温下ＳｉＣ－ＡｌＮ－Ｙ２Ｏ３复相材料的抗弯强度和断裂韧性分别达到６００ＭＰａ和７ＭＰａ·ｍ＾１／２以上。运用ＸＲＤ、ＳＥＭ和ＴＥＭ分析致密样品的断裂裂纹、形貌和组成。ＳｉＣ－ＡｌＮ－Ｙ２Ｏ３复相陶瓷在１３７０℃氧化试验３０ｈ，其氧化产物为莫来石。     

SiC－AlN－Y_2O_3复相陶瓷的制备与性能

通过热压烧结技术，ＳｉＣ、ＡｌＮ和Ｙ２Ｏ３粉末混合作在１９２０～２０５０℃、Ａｒ气氛下形成了致密的复相陶瓷．在室温下ＳｉＣ－ＡｌＮ－Ｙ２Ｏ３复相材料的抗弯强度和断裂韧性分别达到６００ＭＰａ和７ＭＰａ·ｍ１／２以上运用ＸＲＤ、ＳＥＭ和ＴＥＭ分析致密样品的断裂裂纹、形貌和组成．ＳｉＣ－ＡｌＮ－Ｙ２Ｏ３复相陶瓷在１３７０℃氧化试验３０ｈ，其氧化产物为莫来石．     

晶内型Al2O3—SiC纳米复合陶瓷的制备

研究了沉淀法制备Ａｌ２Ｏ３－ＳｉＣ纳米复合陶瓷的工艺过程，利用Ａｌ２Ｏ３从γ相到α相的蠕虫状生长过程，使大部分纳米ＳｉＣ颗粒位于Ａｌ２Ｏ３晶粒内，用沉淀法制得的、含有５ｖｏｌ％ＳｉＣ的Ａｌ２Ｏ３－ＳｉＣ纳米复合陶瓷，其强度为４６７ＭＰａ，韧性为４．７ＭＰａ．ｍ＾１／２，与一般的Ａｌ２Ｏ３陶瓷相比有较大的提高，显示了沉淀法制备Ａｌ２Ｏ３－ＳｉＣ纳米复合陶瓷的优点。     

温度对高压烧结氮化铝陶瓷热导率的影响

以直接氮化法合成的AlN微米粉为原料,添加3%(质量分数)的CaC2为烧结助剂,在5GPa的压力下烧结30min,考察不同烧结温度对AlN陶瓷热导率的影响。用阿基米德排水法、XRD、SEM等技术手段对AlN烧结体进行性能检测。研究表明,在1500～1800℃范围内,温度的升高能促使AlN陶瓷内部晶粒长大,晶型饱满,尺寸均一,晶界相减少,实现烧结致密化,利于热导率的提高。     

透明氮化铝陶瓷研究的新进展

氮化铝（AIN）陶瓷是近年来受到广泛关注的新一代先进陶瓷,有着广泛的应用前景．由于AIN陶瓷的高热导性和低电导率、介电常数和介电损耗,使之在大功率微电子领域成为高密度集成电路基板和封装的理想候选材料,具有巨大的潜在应用市场．但是普通AIN陶瓷因为相对低的纯度和烧结性而不能满足高热导的期望．国际上关于AIN透明陶瓷的报道极少[1,2],而国内尚未见报道．最近我们开展了透明氨化铝陶瓷材料的烧结及其热性能和结构的表征研究．从研究氨化铝低温烧结所需的烧结助剂出发,根据在不同烧结助剂体系下,氨化铝表现出的不同烧结行…     

Influence of tungsten particles on the electrical properties of AlN ceramic

AlN-W composite ceramics were prepared by spark plasma sintering using AlN powder and tungsten powder. Effect of size and content of tungsten particles on the densification, electrical and dielectric properties of AlN ceramic was studied. The result indicates that AlN ceramic with fine tungsten powder is easy to obtain higher densification. The dielectric constant and loss of the composites obviously increased with the increase of content and size of tungsten below the percolation threshold. When R _c (the mean size of AlN powder) equals approximately R _i (the mean size of tungsten powder), the composites obtain the highest percolation threshold (22vol.?%), dielectric constant ε _r and tgδ are 110.90 and 0.02, respectively.     

电泳沉积制备氮化铝陶瓷的研究

采用电泳沉积法成功制备相对密度达到61.9%的均匀氮化铝素坯, 经无压烧结后可获得热导率为200W/(m·K)的氮化铝陶瓷. 研究表明, 以无水乙醇为溶剂、加入0.1wt%聚丙烯酸（PAA）做分散剂、pH值控制在9.7左右的悬浮液具有最佳分散性. 电泳沉积（EPD）成型比干压成型制备的预烧体孔容减小, 比湿法成型制得的预烧体大孔显著减少. 用扫描电子显微镜（SEM）对三种不同成型方法制得氮化铝陶瓷的显微结构进行了研究, 结果表明, EPD法所得氮化铝陶瓷的显微结构均匀, 晶粒尺寸5μm左右.     

多晶铈掺杂硅酸镥闪烁陶瓷的制备和发光性能

本工作对铈离子掺杂多晶硅酸镥(LSO:Ce)闪烁材料的制备方法进行了系统研究。将LSO:Ce前驱体溶胶喷雾干燥后得到了球形LSO:Ce前驱粉体, 该前驱粉体在1000℃和1100℃的温度下煅烧后分别得到了不同晶型的的单相LSO : Ce球形粉体。显微结构观察显示: 粉体颗粒的平均直径约为2 µm, 是由几十纳米大小的LSO:Ce纳米晶粒堆积而成。A型球形LSO:Ce粉体经1200℃/80MPa的放电等离子体烧结(SPS)后获得了平均晶粒尺寸为1.3 µm, 相对密度高达99.7%的LSO:Ce闪烁陶瓷。由A型球形LSO:Ce粉体压制的素坯在1650℃的空气气氛下烧结4 h后可获得相对密度达98.6%, 平均晶粒尺寸为1.6 μm的LSO:Ce陶瓷。该陶瓷经1650℃/150 MPa的热等静压(HIP)处理1 h后, 获得了相对密度为99.9%的半透明LSO:Ce闪烁陶瓷, 其平均晶粒尺寸为1.7 μm, 晶界干净。该LSO:Ce陶瓷的光产额可达28600 photons/MeV, 发光衰减时间为25 ns。     

Microstructure and properties of spark plasma sintered AlN ceramics

Spark plasma sintering (SPS) is a newly developed technique that enables poorly sinterable aluminum nitride (AlN) powder to be fully densified. It is addressed that pure AlN sintered by SPS has relatively low thermal conductivity. In this work, SPS of AlN ceramic was carried out with Y₂O₃, Sm₂O₃ and Li₂O as sintering aids. Effects of additives on AlN densification, microstructure and properties were investigated. Addition of sintering aids accelerated the densification, lowered AlN sintering temperature and was advantageous to improve properties of AlN ceramic. Thermal conductivity and strength were found to be greatly improved with the present of Sm₂O₃ as sintering additive, with a thermal conductivity value about 131 Wm⁻¹K⁻¹ and bending strength about 330 MPa for the 2 wt% Sm₂O₃-doped AlN sample SPS at 1,780 °C for 5 min. XRD measurement revealed that additives had no obvious effect on the AlN lattice parameters. Observation by SEM showed that AlN ceramics prepared by SPS method manifested quite homogeneous microstructure. However, AlN grain sizes and shapes, location of secondary phases varied with the additives. The thermal conductivity of AlN ceramics was mainly affected by the additives through their effects on the growth of AlN grain and the location of liquid phases.     

Synthesis of boride and nitride ceramics in molten aluminium by reactive infiltration

The infiltration of solid powder mixtures with molten aluminium has been investigated as a potential route for the synthesis of ceramic/metal composites. Either titanium or tantalum powder was mixed with boron nitride flakes for the reaction powder mixture. The infiltration occurred spontaneously at 1473K for both [Ti+BN] and [Ta+BN] powder mixtures. Owing to reactions between the starting materials, both boride and nitride ceramics were produced in molten aluminium. TiB2 and AlN were produced from the [Ti+BN] powder mixture, and TaB2 and AlN were produced from the [Ta+BN] powder mixture. When the [Ti+BN] powder mixture was used, a reaction producing Al3Ti took place immediately after the infiltration of the molten aluminium, and a subsequent reaction producing TiB2 and AlN proceeded gradually. The time required to convert BN flakes to TiB2 and AlN particles at 1473K was in the range of 1800–3600 s. On the other hand, when the [Ta+BN] powder mixture was used, there was an initial incubation period to allow the tantalum and molten aluminium to react with each other. The reaction between tantalum, BN and aluminium took place after this incubation period. This revised version was published online in November 2006 with corrections to the Cover Date.     

溶胶–凝胶法制备不同形态的半透明羟基磷灰石陶瓷

为探索制备不同形态半透明羟基磷灰石(T-HA)陶瓷的方法, 采用微米级HA粉体为原料, 甲壳素为粘结剂, 用溶胶–凝胶法制备出球状和纤维状的陶瓷初坯, 然后进行常压烧结得到纯HA陶瓷, 最后经过热等静压烧结得到T-HA陶瓷。溶胶–凝胶法赋形简单, 制备出的球状T-HA陶瓷的球形度良好, 纤维状T-HA陶瓷的纵横比高, 其致密度为99.1%, 平均晶粒尺寸为2.2 μm。其中球状半透明HA陶瓷的抗压强度为10.2 MPa, 高于常规烧结得到的球状致密和多孔HA陶瓷(分别为8.9和4.7 MPa)。仿生矿化和细胞培养的结果显示半透明HA陶瓷具有良好的生物相容性。     

Preparation and properties of ALCON (Al28C6O21N6) ceramics

The synthesis of Al₂₈C₆O₂₁N₆ powder (ALCON), starting from the binary compounds is described. The powder is resistant to oxidation in air up to 760°C. From the prepared powder, fully dense ceramics have successfully been prepared using hot pressing. The as-prepared ceramics had a thermal conductivity of 20 W m^–1 K^–1. Experiments showed that it is also possible to prepare ALCON ceramics by reactive hot-pressing, starting from Al₂O₃, AlN and Al₄C₃. Further optimization is expected to raise the thermal conductivity significantly. The strength, about 300 MPa, is similar to that of AlN. The thermal expansion coefficient of 4.8 × 10^–6K^–1 closely matches that of silicon, making application of ALCON ceramics as heat sinks an interesting possibility.     

微波低温烧结制备氮化铝透明陶瓷

微波烧结(Microwave Sintering)是一种新型、高效的烧结技术, 具有传统烧结技术无可比拟的优越性. 本文在不添加任何烧结助剂的前提下, 采用高纯微米级氮化铝(AlN)粉, 在1700℃/2h的微波低温烧结工艺条件下制备出透明度较高的AlN透明陶瓷. 分析结果表明, 采用微波低温烧结工艺制备的AlN透明陶瓷晶粒尺寸细小(<10μm), 晶粒发育完善且分布均匀, 晶界平直光滑且无第二相分布, 从而证明用微波烧结可以实现AlN透明陶瓷的低温烧结.