CN108059461A - 一种无压烧结制备高致密度Ti3AlC2块体的方法 - Google Patents
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- 238000002360 preparation method Methods 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 4
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- 229910052602 gypsum Inorganic materials 0.000 abstract 2
- 239000010440 gypsum Substances 0.000 abstract 2
- 238000002347 injection Methods 0.000 abstract 2
- 239000007924 injection Substances 0.000 abstract 2
- 238000000227 grinding Methods 0.000 abstract 1
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- 238000001513 hot isostatic pressing Methods 0.000 description 2
- 238000002490 spark plasma sintering Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
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Abstract
本发明公开了一种无压烧结制备高致密度Ti3AlC2块体的方法,该块体由Ti3AlC2注浆成型制成素坯后无压烧结制成,其中注浆成型用Ti3AlC2浆料的固相含量为40~75%,具体制备步骤:将Ti3AlC2粉末、分散剂和去离子水按比例湿法球磨混合1h~24h后,将浆料倒入硅胶石膏模具,固化后制得素坯,在惰性气氛,将烧结炉升温至1100~1600℃烧结1~24h,待炉温降到室温后,即制备出高致密度、高硬度的Ti3AlC2块体。本发明优势在于:(1)在素坯成型过程中无需加压,免去了昂贵的金属模具费用和加压设备费用,只需廉价的硅胶石膏模具;(2)在成品烧结过程中无需加压烧结,只需要通入惰性气氛或真空烧结。该材料具有组织均匀、致密度高、硬度高等特点。
Description
技术领域
本发明涉及一种无压烧结制备高致密度Ti3AlC2块体的低成本工艺,属于陶瓷材料制备技术领域。
背景技术
Ti3AlC2是一种具有优异性能的新材料。这种材料同时具有金属和陶瓷的优点,如导电、导热、可加工、耐高温、抗热震、自润滑等综合性能,在高温结构部件、化学防腐材料、电极电刷材料等很多领域有着十分广阔的应用前景(文献 1:Int.Mater.Rev.,2011,56:143~166)。
目前制备Ti3AlC2块体材料的方法主要有两种:热等静压烧结(文献2:J.Am.Ceram.Soc.,2000,83:825~832)和放电等离子烧结[专利申请号: CN03145959.5]。这两种方法都是利用高温高压烧结制备Ti3AlC2块体,需要大量的电力和昂贵的设备、模具。这两种方法的共同特点是成型和烧结过程中需要施加高达数十甚至数百兆帕的压力。
注浆成型工艺是一种在陶瓷工业中传统的成型技术,这种方法已被公认是制备复杂形状、大件制品的有效方法。注浆成型生产过程所用设备简单,生产费用低。
注浆成型工艺已成功制备各种陶瓷材料[专利申请号:CN201710091883.5、CN200910079972.3、CN200910014078.8],到目前为止,关于用注浆成型制备 Ti3AlC2块体材料的技术尚未见报道。
发明内容
技术问题:本发明旨在提供一种无压烧结制备高致密度Ti3AlC2块体的方法,所要解决的技术难题是无压成型、素坯成型问题,以及以无压烧结取代热等静压、放电等离子烧结技术,制备出性能优异Ti3AlC2块体材料。
技术方案:本发明是一种无压烧结制备高致密度Ti3AlC2块体的方法,该制备方法包括以下步骤:
1)配料:采用过80~300目筛的Ti3AlC2粉末和去离子水为原料,加入聚丙烯酸为分散剂得到固相含量40~75wt.%的混合料;
2)将步骤1)中得到的混合料湿法球磨1~24h,得到混合浆料;
3)将混合后的浆料倒入模具注浆成型,12~36h后浆料固化成型为素坯;
4)将步骤3)中注浆成型制得的素坯置于真空气氛烧结炉中,以2~10℃/min 的升温速率将炉温升到1100~1600℃,整个烧结过程在保护性气氛中进行;
5)将素坯在步骤4)中设定的烧结温度保温,最终得到Ti3AlC2块体材料。
其中,
步骤1)中的加入定量聚丙烯酸为分散剂。
所述步骤3)注浆成型所用模具为硅胶石膏模具。
所述步骤4)中烧结温度为1100~1600℃。
所述步骤4)中保护性气氛为:Ar气氛。
所述步骤5)中将素坯在步骤4)中设定的烧结温度保温,保温时间为1~24 h。
有益效果:本发明具有以下优点:
1.本发明制备原材料组分少,模具成本低廉。
2.本发明烧结工艺简单,能够满足现有市场需求,进行大规模生产。
3.当注浆成型用Ti3AlC2浆料的固相含量高达65%时,素坯1400℃烧结1h 时,可以获得致密度高达98.9%,硬度高达4.37GPa。
附图说明
图1是实施方式七烧结前后的对比照片。
图2是实施方案五的扫描电镜照片。
具体实施方式
实施方式一:
采用80目筛的Ti3AlC2粉末和去离子水为原料,加入聚丙烯酸为分散剂得到固相含量40wt.%的混合料,湿法球磨1h,得到混合浆料,将浆料倒入模具注浆成型,待36h后固化成素坯,最后将素坯置于普通管式气氛炉中,Ar气氛保护下烧结,以3℃/min的升温速率升温至1300℃保温3h,得到Ti3AlC2块体。相对密度达89.1%,硬度为2.31Gpa。
实施方式二:
采用120目筛的Ti3AlC2粉末和去离子水为原料,加入聚丙烯酸为分散剂得到固相含量50wt.%的混合料,湿法球磨24h,得到混合浆料,将浆料倒入模具注浆成型,待24h后固化成素坯,最后将素坯置于普通管式气氛炉中,Ar气氛保护下烧结,以2℃/min的升温速率升温至1100℃保温24h,得到Ti3AlC2块体。相对密度达85.3%,硬度为1.31Gpa。
实施方式三:
采用200目筛的Ti3AlC2粉末和去离子水为原料,加入聚丙烯酸为分散剂得到固相含量50wt.%的混合料,湿法球磨16h,得到混合浆料,将浆料倒入模具注浆成型,待12h后固化成素坯,最后将素坯置于普通管式气氛炉中,Ar气氛保护下烧结,以5℃/min的升温速率升温至1500℃保温5h,得到Ti3AlC2块体。相对密度达94.7%,硬度为3.47Gpa。
实施方式四:
采用120目筛的Ti3AlC2粉末和去离子水为原料,加入聚丙烯酸为分散剂得到固相含量60wt.%的混合料,湿法球磨24h,得到混合浆料,将浆料倒入模具注浆成型,待18h后固化成素坯,最后将素坯置于普通管式气氛炉中,Ar气氛保护下烧结,8℃/min的升温速率升温至1600℃保温12h,得到Ti3AlC2块体。相对密度达94.3%,硬度为3.25Gpa。
实施方式五:
采用300目筛的Ti3AlC2粉末和去离子水为原料,加入聚丙烯酸为分散剂得到固相含量65wt.%的混合料,湿法球磨20h,得到混合浆料,将浆料倒入模具注浆成型,待20h后固化成素坯,最后将素坯置于普通管式气氛炉中,Ar气氛保护下烧结,以4℃/min的升温速率升温至1400℃保温1h,得到Ti3AlC2块体。相对密度达98.9%,硬度为4.37Gpa。
实施方式六:
采用120目筛的Ti3AlC2粉末和去离子水为原料,加入聚丙烯酸为分散剂得到固相含量70wt.%的混合料,湿法球磨24h,得到混合浆料,将浆料倒入模具注浆成型,待36h后固化成素坯,最后将素坯置于普通管式气氛炉中,Ar气氛保护下烧结,以8℃/min的升温速率升温至1200℃保温18h,得到Ti3AlC2块体。相对密度达92.2%,硬度为2.69Gpa。
实施方式七:
采用80目筛的Ti3AlC2粉末和去离子水为原料,加入聚丙烯酸为分散剂得到固相含量75wt.%的混合料,湿法球磨12h,得到混合浆料,将浆料倒入模具注浆成型,待24h后固化成素坯,最后将素坯置于普通管式气氛炉中,Ar气氛保护下烧结,以2℃/min的升温速率升温至1500℃保温12h,得到Ti3AlC2块体。相对密度达97.4%,硬度为3.71Gpa。
除上述实施例外,本发明还可以有其他实施方式。凡采用等同替换或等效变换形成的技术方案,均属于本发明要求的保护范围。
Claims (6)
1.一种无压烧结制备高致密度Ti3AlC2块体的方法,其特征在于该方法包括以下步骤:
1)配料:采用过80~300目筛的Ti3AlC2粉末和去离子水为原料,加入聚丙烯酸为分散剂得到固相含量40~75wt.%的混合料;
2)将步骤1)中得到的混合料湿法球磨1~24h,得到混合浆料;
3)将混合后的浆料倒入模具注浆成型,12~36h后浆料固化成型为素坯;
4)将步骤3)中注浆成型制得的素坯置于真空气氛烧结炉中,以2~10℃/min的升温速率将炉温升到1100~1600℃,整个烧结过程在保护性气氛中进行;
5)将素坯在步骤4)中设定的烧结温度保温,最终得到Ti3AlC2块体材料。
2.根据权利要求1所述的无压烧结制备高致密度Ti3AlC2块体的方法,其特征在于步骤1)中的加入定量聚丙烯酸为分散剂。
3.根据权利要求1所述的无压烧结制备高致密度Ti3AlC2块体的方法,其特征在于所述步骤3)注浆成型所用模具为硅胶石膏模具。
4.根据权利要求1所述的无压烧结制备高致密度Ti3AlC2块体的方法,其特征在于所述步骤4)中烧结温度为1100~1600℃。
5.根据权利要求1所述的无压烧结制备高致密度Ti3AlC2块体的方法,其特征在于所述步骤4)中保护性气氛为:Ar气氛。
6.根据权利要求1所述的无压烧结制备高致密度Ti3AlC2块体的方法,其特征在于所述步骤5)中将素坯在步骤4)中设定的烧结温度保温,保温时间为1~24h。
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