Sm2O3对放电等离子烧结AlN陶瓷致密化和导热性能的影响

针对AlN陶瓷难以烧结致密的特点,采用放电等离子烧结(Spark Plasma Sintering,SPS)技术,利用SPS过程中脉冲电流产生局部高温来加强扩散作用,促进颗粒间颈部接触点形成,并通过添加适量烧结助剂Sm2O3,在短时间内实现了AlN陶瓷的烧结致密化.重点研究了烧结助剂Sm2O3的加入量、烧结温度等工艺参数对AlN陶瓷致密化钩毯统潭鹊挠跋?研究发现Sm2O3的加入使AlN致密化过程提前,烧结温度降低;SPS制备的AlN陶瓷晶粒尺寸均匀一致,晶粒发育良好烧结过程中Sm2O3与AlN粉体表面的Al2O3膜层在晶界处形成Sm-Al-O化合物,该反应有效促进了AlN颗粒间的相互扩散和烧结体的致密,对于AlN晶格完整性的保留非常有利,使AlN烧结体获得了良好的导热性能,其热导率达到150W/(m·K).     

Y2O3对SPS烧结纳米AlN粉末的影响

利用低温燃烧法合成出了平均粒度为100 nm的AlN粉末,将合成的粉末采用放电等离子(SPS)技术进行低温强化烧结,研究Y2O3对烧结过程以及烧结试样特性的影响.XRD进行物相分析,SEM观察断口形貌,排水法测烧结试样的密度,激光闪光法测烧结试样的热导率.实验表明采用低温燃烧法合成出的AlN粉末具有非常好的烧结性能,采用SPS烧结技术,40 MPa压力下,在1600℃保温4 min,就能得到非常致密的AlN陶瓷;Y2O3对纳米AlN粉末在SPS低温强化烧结过程仍有促进作用,使试样在更低的温度下烧结致密,并且晶粒更细小,从而热导率也较低;加入Y2O3的烧结试样晶界强度增加,断口中有较多的穿晶断裂形式,而不加入Y2O3的烧结试样主要以沿晶形式断裂.     

CaF2助剂放电等离子烧结透明AlN陶瓷的微观结构和光学性能

采用放电等离子烧结技术,添加质量分数为3%的CaF2作为烧结助剂,制备了透明氮化铝(AlN)陶瓷.样品在烧结温度1 800℃,30 MPa压力下保温15 min,达到了99.5%的相对密度和52.7%的最大透过率.SEM、XRD、TEM和EDX结果表明,烧结体具有很高的致密度、纯度,良好的晶粒形貌和微观晶体结构,晶界和三角晶界处观察不到第二相的存在.CaF2的添加引入液相烧结,促进AlN晶粒的生长和烧结体的致密化,并且与AlN颗粒反应生成的氟化物和Ca-Al-O化合物能够从烧结体中逸出,进一步净化烧结体,是制备透明AlN陶瓷的有效助剂.放电等离子烧结技术具有烧结快速、烧结体致密度高的特点,是制备透明AlN陶瓷的有效方法.     

可加工AlN-BN复合陶瓷的制备

以碳热还原法合成的 AlN 粉末和市售 BN 粉末为原料,添加 5%Y2O3 为烧结助剂,利用无压烧结制备 AlN-15BN复合陶瓷,研究了烧结温度对 AlN-15BN 复合陶瓷相变、致密度、微观结构以及性能的影响,结果表明:Y2O3 可与 AlN粉末表面的 Al2O3 发生反应生成液相促进烧结,随着烧结温度的升高,复合陶瓷的致密度、热导率和硬度逐渐增加,片状的 BN 形成的卡片房式结构会阻碍复合陶瓷的收缩和致密。在 1 850℃烧结 3 h,可以制备出相对密度为 86.4%,热导率为104.6 W?m-1?K-1,硬度为 HRA56.2的 AlN-15BN复合陶瓷。研究表明,通过添加加工性能良好的 BN制备可加 AIN-BN复合陶瓷,是解决 AIB 陶瓷复杂形状成形问题的一个重要途径。     

热处理高压烧结AlN陶瓷的显微组织和热导率

在流动N2保护下,对高压烧结制备的AlN(Y2O3)陶瓷进行了热处理,研究了热处理对AlN陶瓷显微组织及导热性能的影响.结果表明:在970℃热处理2 h后的AlN陶瓷材料与未热处理的试样相比,晶粒尺寸显著增大,晶粒形状越发规整,析出相均位于晶界处或者三角晶界区域,热导率从77.3 W/(m·K)提高到了156.7 W/(m·K).但是,将热处理时间延长到4 h,AlN陶瓷的气孔增大,出现了反致密化现象,热导率也降低到92.6 W/(m·K).     

AlN陶瓷基板材料的典型性能及其制备技术

AlN陶瓷是一种新型的基板材料,具有优异的电性能和热性能,被誉为新一代高密度封装的理想基板材料。介绍AlN陶瓷的典型性能和导热机理;讨论AlN粉末的5种合成方法：铝粉直接氮化法、Al2O3碳热还原法、化学气相沉积法、溶胶？凝胶法、自蔓延高温合成法和等离子化学合成法;分析AlN烧结助剂的选择和5种烧结工艺：热压烧结、无压烧结、放电等离子烧结、微波烧结及自蔓延烧结;阐述AlN基板的制备工艺及其影响因素。     

β-氮化硅粉烧结氮化硅陶瓷热导率

以自蔓延高温合成β-氮化硅粉为原料,添加稀土化合物Y2O3和MgO复合烧结助剂,采用放电等离子烧结后高温热处理的方法制备氮化硅陶瓷。研究β-氮化硅粉体制备致密氮化硅陶瓷的条件。讨论粉体种类(β-氮化硅或α-氮化硅)及SPS保温时间对氮化硅陶瓷热导率的影响。研究表明,采用β-氮化硅粉体制备的氮化硅陶瓷的热导率比采用相同工艺α-氮化硅粉体制备的氮化硅陶瓷高15%以上。采用SPS工艺在1873K烧结5min,然后再在2173K保温3h可以获得致密的氮化硅陶瓷,其热导率高达105W·(m·K)-1。     

LaF3-MgO助烧剂配比对Si3N4陶瓷烧结及性能的影响

采用放电等离子烧结(SPS)后高温热处理的方法,制备烧结助剂总量为8%(质量分数),LaF3/MgO配比不同的Si3N4陶瓷,研究助烧剂配比对Si3N4陶瓷烧结及热导率、抗弯强度等性能的影响。结果发现,添加LaF3后SPS初期烧结速率明显减小,烧结温度区间变宽,当LaF3/MgO配比超过4:4后烧结密度急剧下降。烧结后陶瓷中形成La-Si-O化合物。热导率随LaF3/MgO比增加先升后降;而抗弯强度初期随LaF3/MgO比变化不大,但当比值超过1后,陶瓷中出现异常长大晶粒,抗弯强度下降。控制LaF3/MgO配比为3:5可以获得热导率为80W/m·K,抗弯强度超过1000MPa的高热导率高强度Si3N4陶瓷。     

两面顶技术超高压热压烧结AlN陶瓷的研究

利用两面顶压机实现了AlN陶瓷材料的超高压热压烧结,借助于XRD、SEM、热导仪、激光粒度分析等分析测试手段,系统地研究了工艺因素对AlN陶瓷的显微结构、性能的影响,获得了超高压热压烧结AlN陶瓷的较佳烧结工艺,并对超高压热压烧结的机理进行了分析、探讨.研究结果表明:Y2O3是有效的低温烧结助剂,烧结助剂的预处理有助于减弱晶界相的局部富集,是提高AlN陶瓷热导率的有效措施;在压力为5.15 GPa、温度为1 700 ℃、烧结周期为115 min的超高压热压烧结条件下,获得了显微结构致密均匀、晶粒形貌大小难以分辨、晶界不明显的AlN陶瓷,其热率导达到200 W/(m·K).     

纳米AlN粉末的低温烧结

研究了低温燃烧合成前驱物制备纳米级AlN粉末的低温烧结行为,利用XRD,SEM等手段对陶瓷粉末及烧结体进行了表征。结果表明:由于该粉末的粒径小(约为100nm),比表面积大(17.4m2/g),具有很好的烧结活性,在未使用烧结助剂时,在常压下1700℃获得了致密的陶瓷材料;添加5%Y2O3烧结助剂后,AlN的烧结致密化温度又降低为1600℃,比通常采用的比表面积低于5m2/g的AlN粉末的烧结致密化温度降低了200℃。分析了该种粉末促进烧结的机理,并在1650℃时制备出热导率为132.4W·m-1·K-1的AlN陶瓷。     

烧结方式对TiB2/Cu复合材料组织和性能的影响

采用微波烧结和真空烧结制备了Cu及不同TiB2含量的TiB2/Cu复合材料。测试了试样的密度、硬度、电导率,并对不同烧结法方式制备的Cu及TiB2/Cu复合材料的组织和性能进行了分析。结果表明,微波烧结技术可以在较短的时间和较低的能耗下完成烧结,且烧结体的性能要明显优于真空烧结的。但微波烧结试样的组织比较粗大,有孪晶存在,并且孪晶数量随TiB2含量的增加而减少。     

Plasma-Activated Sintering of Aluminum Nitride

The use of a new plasma- activated sintering (PAS) process to densify aluminum nitride (AIN) powders to nearly full theoretical density (97 to >99%) in 5 to 10 min was investigated. The process consists of a pulse activation step, followed by sintering at 1730 to 1800 °C using resistance heating in carbon dies. Submicron size (~0.44 μm) AIN powders of low oxygen content (<1 wt%) were consolidated to near full density in both air and vacuum with no sintering aids or binders. Transmission electron microscopy (TEM) examination revealed an equiaxed, submicron grain structure (~0.77 μm) with no apparent pores or intergranular phases. X- ray powder diffraction revealed no secondary crystalline phases.     

Gradient cemented carbide with β-phase free surface layer formed by nitrogen source AlN

Using AlN as nitrogen source, the gradient cemented carbide with β-phase free surface layer was fabricated in situ by one-step vacuum sintering. The β-phase free layer was explored by phase characterization, elemental-distribution analysis, microstructure and fracture observation. The results indicated that it was feasible to obtain β-phase free layer when utilizing AlN as the nitrogen source. The AlN decomposition fell appreciably to lower temperature in the presence of binder Co and Ni under vacuum sintering. The thickness of β-phase free layer could be tailored by controlling AlN contents, and the nitride former Al remained in the β-phase free layer. When applying nitrogen source AlN, the relative Ti content in the subsurface layer was lower than that with the conventional nitrogen source Ti(C,N) or TiN. By contrast, Co enrichment in the β-phase free layer is less significant than Ni as a result of higher solidification temperature. WC phases were much coarser averagely in the β-phase free layer than in the bulk, which was considered to be favorable for resisting against fracture. The β-phase free layer containing Al played a substantially improved role on the transverse rupture strength when AlN addition was 0.6 wt% and 1.2 wt%, while it is detrimental to the transverse rupture strength due to the formation of the intermetallic phase of Al and binder when AlN addition was 1.8 wt%.     

Material properties and machining performance of hybrid Ti2AlN bulk material for micro electrical discharge machining

Mn+1AXn(MAX) phases are a family of nanolaminated compounds that possess unique combination of typical ceramic properties and typical metallic properties.As a member of MAX phase,Ti2 AlN bulk materials are attractive for some high-temperature applications.The synthesis,characteristics and machining performance of hybrid Ti2 AlN bulk materials were focused on in this work.The bulk samples mainly consisting of Ti2 AlN MAX phase with density close to theoretic one were synthesized by a spark plasma sintering method.Scanning electron microscopy results indicate homogenous distribution of Ti2 AlN grains in the samples.Micro-hardness values are almost constant under different loads (6-6.5 GPa).A machining test was carried out to compare the effect of material properties on micro-electrical discharge machining (micro-EDM) performance for Ti2 AlN bulk samples and Ti6242 alloy.The machining performance of the Ti2 AlN sample is better than that of the Ti6242 alloy.The inherent mechanism was discussed by considering their electrical and thermal conductivity.`     

添加微量Y_2O_3对WC-8%Ni合金微观组织与性能的影响

采用冷等静压与真空烧结工艺制备硬质合金试样,利用排水法、SEM、EDS、三点弯曲法等研究了添加微量Y2O3对WC-8%Ni合金微观组织与性能的影响。结果表明,添加微量Y2O3可以降低WC-8%Ni合金的烧结温度及孔隙度,WC-8%Ni合金的真空烧结温度在1510℃左右,而WC-8%Ni-Y2O3的真空烧结温度为1480℃左右;添加的Y2O3弥散分布于粘结相,起到弥散强化的作用,提高了合金的抗弯强度。     

烧结压力对整体PCBN刀具微结构与性能的影响及作用机理

将粒度尺寸5 μm的CBN微粉与黏结剂Al的混合粉末在国产六面顶压机上高压烧结制备整体PCBN材料,通过对样品磨耗比、显微硬度的测试与分析获得了较优的烧结工艺参数:烧结压力5.4 GPa、烧结温度1500℃和烧结时间240 s。测得样品的显微硬度为3897HV5（加载时间15 s）,磨耗比为8750。SEM、TEM观察和XRD衍射分析表明:提高烧结压力可使CBN颗粒产生一定的塑性流动,抑制烧结过程中CBN颗粒表面逆转成hBN;黏结剂Al可与CBN颗粒表面反应形成中间产物AlN和AlB₂,在CBN颗粒之间形成牢固的陶瓷中介结合,并消除CBN烧结过程中残余的hBN,从而提高整体PCBN刀具的性能。      

Dielectric properties of spark plasma sintering AlN-W composite ceramics

In order to develop AlN composites suitable for high average power electronic tube,AlN-W materials were prepared by spark plasma sintering.The effects of manufacture parameters on dielectric loss tangent and permittivity constant were investigated,which include powder-mixed method,milling time of high-energy ball milling,starting powder particle size,sintering temperature and holding time and adding amount of the conductive second phase.The results showed that AlN-W materials sintered at the temperature of 1700°C holding for 5 min with 10 vol.% W showed the best dielectric loss tangent larger than 0.81 at the frequency 1 kHz-1 MHz.In addition,magnetic stirring mixed powder and lower sintering temperature led to the better properties because of the higher porosity.The samples sintered from the starting AlN powder with smaller particle size also had the better properties.     

Sintering, characterisation, and analysis of functional gradient hardmetals

Four WC–carbonitride–Co-based hardmetal green bodies of different carbonitride and N content were sintered in vacuum and in nitrogen at two different pressures. Phase formation upon heating was investigated by interrupting the sintering process at various stages and was studied by means of standard metallographic methods. Shrinkage behaviour and magnetic properties of the partly sintered samples were measured as a function of temperature and atmosphere. The surface and the bulk of the samples were analysed by XRD, showing the homogenisation of the cubic hard phases as a function of temperature. During vacuum sintering all samples showed formation of η phases M₁₂C and M₆C, especially at the surface. M₁₂C was converted to M₆C between 1100 and 1300 °C. By the introduction of N₂ the η phases decomposed and the samples ended up with either a carbonitride-depleted or a carbonitride-enriched zone, depending on which sintering cycle was performed.     

Effects of rare earth oxide additives on the thermal behaviors of aluminum nitride ceramics

The effects of Y₂O₃ and Er₂O₃ on the sintering behaviors, thermal properties and microstructure of AlN ceramics were investigated. The experimental results show that the sintering temperature can be decreased; the relative density and thermal behavior can be improved by adding rare earth oxide in AlN ceramics. For AlN ceramics with 3 wt.% Er₂O₃ additive, the relative density is 98.8%, and the thermal conductivity reaches 106 W·m⁻¹·K⁻¹. The microstructure research found that no obvious aluminum erbium oxide was found in AlN ceramics doped with 3 wt.% Er₂O₃, which favored the improvement of the thermal conductivity of AlN ceramics.     

新型高热导率氮化铝基微波衰减陶瓷研究

针对传统氧化铍基微波损耗陶瓷存在毒性大、一致性差和焊接难度大的问题,发展了一种高热导率氮化铝基的AlN-FeSiAl微波衰减陶瓷。该材料在AlN基体中添加FeSiAl,属环境友好型材料。为获得高热导率和良好的电磁性能,开展了不同氮化铝粉末、不同FeSiAl粉末添加量以及烧结工艺对复合材料性能影响的研究。结果表明,采用日本东洋氮化铝粉末、添加10%(质量分数,下同)的FeSiAl,在1650℃和85 MPa下进行真空热压烧结,获得了衰减性能优异的微波衰减陶瓷,且材料热导率达到88.2 W/m·K,接近美国Ceradyne公司AlN基微波衰减陶瓷的热导率水平。