球磨时间对放电等离子烧结合成Ti_3SiC_2纯度的影响

本文采用原料配比为3Ti/Si/2C/0.2Al(摩尔比)的单质混合粉体为原料,进行机械合金化(MA)和随后的放电等离子烧结(SPS),以制备高纯Ti3SiC2陶瓷,研究了球磨时间对放电等离子烧结制备Ti3SiC2的影响。结果表明,机械合金化混合粉体后,粉体颗粒明显细化。球磨10h,单质混合粉体会发生化学反应,生成TiC,Ti3SiC2混合粉体。继续球磨至20h,生成物混合粉体会显著细化。球磨时间对SPS烧结合成Ti3SiC2有显著的影响。球磨10h,即反应刚刚完毕,最有利于SPS合成致密高纯的Ti3SiC2,球磨时间较短(5h),对Ti3SiC2陶瓷的烧结促进作用不显著,而反应后继续延长球磨时间至20h,会降低烧结体中Ti3SiC2的纯度。采用球磨10h的粉体为原料,经850℃放电等离子烧结可获得纯度高达96%(质量分数,下同)的Ti3SiC2疏松块体,烧结温度提高到1100℃,可获得纯度为99.3%、相对密度高达98.9%的TiSiC致密块体。     

稀释剂对Al2O3(f)/Ti-Al原位复合材料纤维相的影响

以Ti、Al、TiO2及Al2O3为原料,制成预制体,通过石墨与Al2O3混合粉对预制体的覆埋实现气氛保护并进行热处理,使其原位合成Al2O3纤维增强Ti-Al金属间化合物复合材料.考察了Al2O3对材料断口形貌组织、物相成分的影响,并结合DTA进行了热力学分析.XRD表明,外加Al2O3后材料氮化严重,主晶相由Al3Ti变为AlN.SEM表明,材料基体周围分布大量纤维,稀释剂Al2O3的加入有利于纤维的生长及分布.     

(Cu-50TiH_2)+SiC_p复合粉体焊料连接石墨/铜接头的微观结构

碳材料与铜的连接在汽车及能源等领域具有潜在的应用。采用Cu、TiH2和SiC粉末组成的复合粉体焊料在950℃/10min工艺条件下真空钎焊石墨与铜,并研究复合粉体焊料中SiC含量对石墨/铜接头剪切强度的影响。结果表明,复合焊料中添加SiC有利于接头室温剪切强度的提高。当SiC体积分数为10%时,接头室温剪切强度最高,为19.2MPa。微观分析表明,连接过程中,复合粉体焊料中TiH2分解产生的Ti与SiC发生原位反应,生成TiC、Ti5Si3及Ti3SiC2等反应产物;另外,Ti与石墨母材发生界面反应形成厚度为2~3μm的TiC反应层,Ti和Cu则形成Ti3Cu4等金属间化合物。由于Ti3SiC2在高温下具有塑性,可在一定程度上缓解石墨/铜接头的残余热应力。同时,晶须状和颗粒状的反应产物弥散分布在连接层中,对接头起强化作用,也有利于石墨/铜接头性能的提高。     

机械合金化+热处理制备Ti_3AlC_2材料

采用3Ti/1.1Al/2C粉体为原料,通过机械合金化与热处理,制备高纯Ti3AlC2材料。采用XRD、SEM和EDS对试样的物相组成、微观形貌和微区成分进行分析与表征。结果表明,3Ti/1.1Al/2C粉体机械合金化9 h后,元素粉末间会发生化学反应,合成了TiC和Ti3AlC2的复合粉体材料。粉体材料的晶粒比较细小,颗粒直径约为0.5~2μm。同时产物中有一些坚硬、细小的块体出现,小块体中的TiC和Ti3AlC2晶粒发育良好,TiC晶粒大小约2μm,Ti3AlC2晶粒长约10μm、宽约2μm。对得到的机械合金化粉体进行热处理,经900℃保温2 h可获得组织细小(颗粒直径0.5~1μm)、高纯(96.6%)的Ti3AlC2材料。继续升温,会导致Ti3AlC2材料分解。温度升至1 300℃时,物相分析表明试样仅由TiC相组成,组织致密,TiC晶粒大小约5~10μm。     

纳米Mg_2Si材料的制备及热电性能研究

以高纯Mg,Si粉合成得到的Mg_2Si微米粉体为原料,采用机械球磨方法制备纳米Mg_2Si粉体。对球磨过程中球磨介质、球料比、转速及球磨时间进行分析,发现:通过机械球磨微米Mg_2Si的方法,以正己烷为球磨介质,选取WC球和罐,在球料比为20:1、转速为370r/min、球磨70h时即可获得平均晶粒尺寸约为十几纳米的Mg_2Si纳米粉体。采用放电等离子体烧结(SPS)烧结纳米Mg_2Si粉体,块体晶粒长大,但仍在100nm左右;由于晶界散射作用,纳米块体Mg_2Si热导率明显降低,电导率、Seebeck系数一定程度下降,综合热电三因素,纳米Mg_2Si块材在800K时获得最大ZT值,为0.36,明显优于微米块体材料。     

以铝为助剂通过机械合金化和热处理制备Ti3SiC2

采用Ti、Si、C单质粉末为原料,添加少量Al元素粉末为助剂,通过机械合金化和热处理制备高纯Ti3SiC2材料。采用XRD和SEM研究该材料的物相组成和显微结构。研究结果表明,机械合金化Ti、Si、C单质混合粉末,会诱发自蔓延反应,生成组成相为TiC、Ti3SiC2、TiSi2和Ti5Si3的粉末与颗粒产物。添加适量的Al元素可消除硅化物,明显促进Ti3SiC2的反应合成。采用Ti、Si、C、Al单质粉末进行机械合金化,可制备出主相为TiC与Ti3SiC2的粉末与颗粒产物。对掺Al机械合金化粉末产物压制后,在900~1 100℃热处理2 h,可制备出纯度大于95%(质量分数)的Ti3SiC2材料,而颗粒产物在900~1 200℃进行热处理,亦可获得纯度为96%的Ti3SiC2材料。但在1 300℃,热处理产物中的Ti3SiC2会发生严重分解,部分分解为TiC和少量硅化物,使产物纯度降低。     

球磨参数对机械合金化制备Al_2O_3/Mo_5Si_3复合粉体特性的影响

以MoO3粉、Mo粉、Si粉及Al粉为原料,采用机械化学还原法制备了Al2O3/Mo5Si3复合粉体。利用XRD、SEM等对复合粉体在球磨过程中的物相转变和形貌进行表征,并对球磨参数对机械合金化过程的影响进行探讨。结果表明,原料粉体球磨10 h后转变为Al2O3/Mo5Si3复合粉体,反应较完全。随球磨时间延长,复合粉体细小均化,粉体粒度较小,球磨20h后粉体粒度在3~5μm之间,随球磨转速的提高,球磨时间延长,球磨提供能量提高,反应开始时间变短。     

包覆法制备Gp/SiC 复合材料的显微结构和性能

以不同粒径的石墨颗粒和SiC粉体为原料,采用SiC粉体包覆石墨颗粒的方法,于2000℃热压制备了石墨/碳化硅(Gp/SiC)复合材料.利用扫描电子显微镜(SEM,EDS)分析了材料的金相和断口显微结构.研究表明,石墨粒径较小且质量分数较少的复合材料比石墨粒径较大且质量分数较多的复合材料在热压工艺中更致密.石墨颗粒呈岛状紧密地镶嵌在SiC基体中,石墨与SiC界面处C和Si的扩散不明显.复合材料的相对密度、抗折强度,断裂韧性和硬度随石墨粒径和质量分数的减少而增加.断口形貌表明SiC陶瓷基体为脆性,石墨为韧性断裂.当石墨粒径为125μm、SiC与石墨的质量比为3.5时,复合材料的综合性能最佳,开口气孔率为0.3%,相对密度为97.9%,抗折强度为75±15 MPa,断裂韧性为5.4±0.5 MPa.m1/2,硬度为26.8±3GPa.     

高能球磨制备NiCr-Cr_2O_3-BaF_2/CaF_2复合粉末及其爆炸喷涂层的性能

为了制备高性能复合涂层,以70%NiCr、20%Cr2O3及10%BaF2/CaF2为原料,采用高能球磨方法制备了复合粉体,并通过特定的爆炸喷涂工艺制得复合涂层。利用扫描电子显微镜(SEM)、能谱分析(EDS)、X射线衍射(XRD)等对球磨后粉体和喷涂层的微观形貌、组织结构、成分及物相组成进行了分析。根据HB5143-96测定了爆炸喷涂复合涂层与基体间的结合强度。结果表明:随球磨时间的延长,粉体球形化程度逐步加大,颗粒尺寸逐步减小,粒度分布趋于集中,颗粒成分及结构均匀性逐步提高;当球磨11h后,粉体中的BaF2和CaF2固溶于NiCr合金,Cr2O3颗粒在NiCr基体内部镶嵌;通过爆炸喷涂将球磨粉喷涂在不锈钢基体上,其涂层微观组织均匀致密,显微硬度Hv为578,涂层与基体结合强度为67MPa,综合性能优于混合粉喷涂层。     

本刊2006年第1～6期总目次

文题期页.研究与开发.粉体的新压制方程研究13反应钎涂碳化物/铁基自熔合金复合涂层及组织形成机理18喷射成形时雾化压力与静压头对雾化熔滴尺寸影响的理论分析113汽车发动机用无Co排气阀座圈材料的开发118注射成形纯钛脱粘和烧结工艺研究283外应力及磁场对粘接Ni52Mn24.4Ga23.6合金马氏体相变的影响288球磨材质对纳米SiC/Al复合体系混合粉形貌及块体材料微观组织的影响294活性粉末Ni-Al与SiC陶瓷的界面润湿特性和润湿机理研究3163快速凝固喷射沉积制备Al-40Si组织分析3166约束弧等离子体制备铝纳米粉体的研究3170熔体自生原位增韧Al2…     

放电等离子烧结Ti/(1-x)Ti_3SiC_2+xSiC层状材料的显微结构

以钛粉,硅粉和石墨粉为原料,采用放电等离子烧结技术制备密度为4.14 g/cm3的Ti3SiC2和密度为4.03 g/cm3的0.8 Ti3SiC2+0.2 SiC复合材料,并以此为基础制备Ti/Ti3SiC2/0.8Ti3SiC2+0.2SiC层状材料。通过扫描电镜(SEM)和X射线衍射仪(XRD)分析材料的显微结构与相组成。结果表明:该层状材料的界面结合紧密,没有明显的孔洞、裂纹等缺陷,各层的相组成符合设计要求。经800℃热处理40 h后Ti/Ti3SiC2界面处生成稳定的TiC层,在高温下该层状材料的界面基本稳定。     

层状可加工陶瓷Ti3SiC2自蔓延高温合成反应机理的研究

采用燃烧波淬熄法,以Ti粉、Si粉和C粉为原料研究了层状可加工陶瓷Ti3SiC2在自蔓延高温合成(SHS)中的反应机理.淬熄试样中保留未反应区、反应区和已反应区,用扫描电子显微镜观察燃烧反应中显微组织的转变过程,用能谱仪分析各微区的成分变化,并通过差热分析(DSC-TGA)和XRD分析考察了从600℃到1500℃ Ti-C-Si系统的反应合成过程和相形成规律.结果表明:层状可加工陶瓷Ti3SiC2自蔓延高温合成的机理为溶解-析出机制,Ti粉与Si粉的固态扩散导致低熔点Ti-Si溶液形成,Ti、Si、C粉粒逐渐向Ti-Si溶液中溶解,当溶液中的Ti、Si、C浓度饱和时,从中析出TiC、SiC颗粒,最后形成最终产物Ti3SiC2.     

反应烧结制备TiC-Ti3SiC2梯度材料

采用Ti、Si、TiC粉末为原料,通过放电等离子反应烧结制备TiC-Ti<,3>SiC<,2>梯度功能材料.采用X射线衍射(XRD)、扫描电镜(SEM)和能谱分析(EDS)等手段,分析梯度材料的相组成和微观结构特征.结果表明,采用放电等离子烧结,升温速度为100℃/min时,在1 350℃保温15min、加压40MPa...     

Correlation of microstructure with hardness and wear resistance in (TiC,SiC)/stainless steel surface composites fabricated by high-energy electron-beam irradiation

Stainless-steel-based surface composites reinforced with TiC and SiC carbides were fabricated by high-energy electron beam irradiation. Four types of powder/flux mixtures, i.e., TiC, (Ti + C), SiC, and (Ti + SiC) powders with 40 wt. pct of CaF₂ flux, were deposited evenly on an AISI 304 stainless steel substrate, which was then irradiated with an electron beam. TiC agglomerates and pores were found in the surface composite layer fabricated with TiC powders because of insufficient melting of TiC powders. In the composite layer fabricated with Ti and C powders having lower melting points than TiC powders, a number of primary TiC carbides were precipitated while very few TiC agglomerates or pores were formed. This indicated that more effective TiC precipitation was obtained from the melting of Ti and C powders than of TiC powders. A large amount of precipitates such as TiC and Cr₇C₃ improved the hardness, high-temperature hardness, and wear resistance of the surface composite layer two to three times greater than that of the stainless steel substrate. In particular, the surface composite fabricated with SiC powders had the highest volume fraction of Cr₇C₃ distributed along solidification cell boundaries, and thus showed the best hardness, high-temperature hardness, and wear resistance.     

Correlation of microstructure with hardness and wear resistance in (TiC,SiC)/stainless steel surface composites fabricated by high-energy electron-beam irradiation

Stainless-steel-based surface composites reinforced with TiC and SiC carbides were fabricated by high-energy electron beam irradiation. Four types of powder/flux mixtures, i.e., TiC, (Ti+C), SiC, and (Ti+SiC) powders with 40 wt. pct of CaF₂ flux, were deposited evenly on an AISI 304 stainless steel substrate, which was then irradiated with an electron beam. TiC agglomerates and pores were found in the surface composite layer fabricated with TiC powders because of insufficient melting of TiC powders. In the composite layer fabricated with Ti and C powders having lower melting points than TiC powders, a number of primary TiC carbides were precipitated while very few TiC agglomerates or pores were formed. This indicated that more effective TiC precipitation was obtained from the melting of Ti and C powders than of TiC powders. A large amount of precipitates such as TiC and Cr₇C₃ improved the hardness, high-temperature hardness, and wear resistance of the surface composite layer two to three times greater than that of the stainless steel substrate. In particular, the surface composite fabricated with SiC powders had the highest volume fraction of Cr₇C₃ distributed along solidification cell boundaries, and thus showed the best hardness, high-temperature hardness, and wear resistance.     

自蔓燃高温合成碳化物陶瓷

介绍了自蔓延高温合成（SHS）制备碳化物粉体。单晶、多孔材料和致密材料。重点讨论了通过控制反应参数,控制合成材料的组织结构和性能的一些措施。以催化剂载体、泡沫陶瓷过滤器、粗TiC磨料以及Si-SiC复合材料为例,介绍了SHS在材料合成中的应用和控制方法。参考Ti3SiC2陶瓷的合成,讨论了多元SHS体系中产物相的控制问题。另外,文中还介绍了提高烧结助剂BxC在SiC中的分散性,从而提高SHSSiC烧结性的实例。     

The fracture characteristics of Al-9Ti/SiC p metal matrix composites

A fracture mechanics approach was used to determine the plane strain fracture toughness (K _IC) of a mechanically alloyed Al-9Ti 20 vol pct cobalt sol-gel-coated SiC particle-reinforced composite. Processing defects consisting of clumped SiC particulate, bonded by the sol-gel, initiated failure in tensile tests. The defects were measured and the fracture toughness was calculated using the Irwin relation. The value ofK _IC for the as-received material was determined to be equal to 4.7 MPa·m^1/2 at room temperature. Annealing the material for 120 hours and 400 hours at 500 °C increased the fracture toughness. This can be attributed to coarsening of an Al₃Ti strengthening phase. Tensile tests conducted at 200 °C show thatK _IC decreases at that temperature for each annealing condition. The sensitivity to the presence of the defects is greatest for samples annealed at 500 °C for 120 hours. The effect of the defects on the failure mechanism of the composite material as a function of temperature was determined. At room temperature, the Co/SiC processing defects provide low-energy paths for crack propagation; at 500 °C, the defects serve as void nucleation sites.     

Ti3SiC2/Cu复合材料的制备与性能

三元层状化合物Ti3SiC2兼具陶瓷和金属的性能,受到材料研究者的广泛关注.该文采用热压工艺制备Ti3SiC2/Cu复合材料,研究Ti3SiC2含量及烧结温度对复合材料密度、抗弯强度、弹性模量、电阻率等性能的影响.结果表明,复合材料的相对密度对其性能有着重要的影响.当Ti3SiC2的质量分数在60％～80％范围内,其它...     

W粉粒度对Ti-20%W合金组织和力学性能的影响

以TiH2粉和不同粒径的W粉为原料,通过粉末冶金法制备了Ti-20%W合金,利用金相显微镜、X射线衍射仪、扫描电子显微镜和能谱分析仪对合金的微观组织和成分进行分析,并测定了其显微硬度和抗压强度。结果表明:选用细W粉时,W颗粒与Ti固溶量大,显微硬度值均匀且抗压强度高,强化机理为固溶强化,断口分析表明采用纳米W粉时Ti-20%W合金发生了韧性断裂;而采用粗W粉时,W颗粒与Ti固溶量较少,显微硬度值从W颗粒中心到Ti基体呈现先升高后降低的趋势,抗压强度较差。这说明采用W增强Ti基体时固溶强化比第二相即颗粒强化的效果更明显。