CN109608198A - 一种Ta2AlC-Ta4AlC3复合材料的制备方法 - Google Patents
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- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 229910004470 Ta4AlC3 Inorganic materials 0.000 title claims description 38
- 239000000843 powder Substances 0.000 claims abstract description 39
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910003468 tantalcarbide Inorganic materials 0.000 claims abstract description 27
- 238000005245 sintering Methods 0.000 claims abstract description 22
- 239000002994 raw material Substances 0.000 claims abstract description 20
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 16
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 8
- 239000010439 graphite Substances 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 16
- 239000004411 aluminium Substances 0.000 claims description 15
- 238000003763 carbonization Methods 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 9
- 230000036316 preload Effects 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 2
- 238000007580 dry-mixing Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 22
- 239000000919 ceramic Substances 0.000 abstract description 14
- 230000008569 process Effects 0.000 abstract description 11
- 230000008901 benefit Effects 0.000 abstract description 2
- 238000003825 pressing Methods 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 238000002490 spark plasma sintering Methods 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 239000004615 ingredient Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 229910004447 Ta2AlC Inorganic materials 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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Abstract
本发明公开了一种Ta2AlC‑Ta4AlC3复合材料的制备方法,其特征在于,包括以下步骤:以钽粉、铝粉和碳化钽粉为原料,按一定摩尔比进行配比并加入质量分数为10%~50%的碳化钽粉末配置复合材料的原料;将上述原料置入球磨罐中,在行星式球磨机上湿混15h;采用旋转蒸发仪将混料烘干,然后置入石墨磨具中进行预压;将模具放在放电等离子烧结炉中,在Ar气保护下,加热;与现有技术相比具有以下优点:提出一种制备Ta2AlC‑Ta4AlC3复合材料块体陶瓷的新方法,工艺简单,合成时间较短;在加压过程中烧结,脉冲电流产生的等离子体及烧结过程中的加压有利于降低粉末的烧结温度,同时低电压、高电流的特征,能使粉末快速烧结致密。
Description
技术领域
本发明属于新型结构材料制备技术领域,特别涉及一种放电等离子烧结工艺制备Ta2AlC-Ta4AlC3复合材料块体陶瓷的方法。
背景技术
三元层状陶瓷Mn+1AXn (其中:M为早期过渡金属;A为ⅢA或ⅣA族元素;X为C或N;n=1,2,3;简称MAX)。Mn+1AXn属于六方晶系结构,空间点群为P63/mmc。Ta2AlC、Ta4AlC3分别为MAX相中211相和413相的代表,其中Ta2AlC晶格参数为a=3.075Å,c=13.83Å,Ta4AlC3晶格参数为a=3.10884 ± 0.00004 Å,c=24.0776 ± 0.0004 Å。MAX相综合了金属和陶瓷的性质,既像金属一样具有良好的导电性、导热性、机械加工性、抗热震性及良好的损伤容限,又与陶瓷一样具有高熔点、高弹性模量、高热稳定性及优异的耐摩擦性及抗氧化性等性能。Ta2AlC、Ta4AlC3及其复合材料优异的综合性能使其在航天航空、核工业、机械、电子信息等领域具有广阔的应用前景。
目前的研究表明,Ta2AlC块体主要是通过热等静压法和热压法等工艺制备而成,如胡春峰等(材料研究杂志,Int. J. Mater. Res. 99(2008)8)采用原位反应/热压法,以Ta、Al和C粉为原料,在1550°C,30MPa压力下热压30min后,在1400°C热处理60min得到单相Ta2AlC块体陶瓷。但是这类工艺往往合成时间较长,经过长时间的加热,材料组织粗化,导致其力学性能降低。放电等离子烧结工艺利用上、下模冲及通电电极将特定烧结电源和压制压力施加于烧结粉末,经放电活化、热塑变形和冷却完成制取高性能材料,能够有效解决以上问题。 关于Ta4AlC3块体的合成制备报道较少,同时,至今也未有关于任何一种方法合成制备Ta2AlC-Ta4AlC3复合材料的报道,Ta2AlC-Ta4AlC3复合材料的SPS烧结合成制备更无法查询。
发明内容
本发明的目的在于利用放电等离子烧结工艺制备致密度高、晶粒细小且性能优异的Ta2AlC-Ta4AlC3复合材料块体陶瓷,首次利用了Ta-Al-TaC体系,SPS技术合成制备出细晶Ta2AlC-Ta4AlC3复合材料,制备的Ta2AlC-Ta4AlC3块体陶瓷纯度、致密度较高,晶粒细小且力学性能优异。
本发明是通过以下技术方案实现的:一种Ta2AlC-Ta4AlC3复合材料的制备方法,其特征在于,包括以下步骤:
(1) 以钽粉、铝粉和碳化钽粉为原料,按一定摩尔比进行配比并加入质量分数为10%~50%的碳化钽粉末配置Ta2AlC-Ta4AlC3复合材料的原料;
(2) 将上述原料置入球磨罐中,在行星式球磨机上湿混15h;
(3) 采用旋转蒸发仪将混料烘干,然后置入石墨磨具中进行预压;
(4) 将模具放在放电等离子烧结炉中,在Ar气保护下,以80~500°C/min升温速率加热至1300~1500°C,在30~500MPa压力下保温5~10min。
进一步的,原料钽粉、铝粉和碳化钽粉均为单质粉体,粒径大小在1μm~75μm,钽粉、铝粉和碳化钽粉按摩尔比Ta:Al:TaC =1:1.4:1混合并加入质量分数为10%~50%的碳化钽粉末配置Ta2AlC-Ta4AlC3复合材料。
进一步的,钽粉、铝粉和碳化钽粉按摩尔比 Ta:Al:TaC=1:1.4:1混合并加入质量分数为10%的碳化钽粉末配置Ta2AlC-Ta4AlC3复合材料的原料。
进一步的,钽粉、铝粉和碳化钽粉按摩尔比 Ta:Al:TaC=1:1.4:1混合并加入质量分数为20%的碳化钽粉末配置Ta2AlC-Ta4AlC3复合材料的原料。
进一步的,钽粉、铝粉和碳化钽粉按摩尔比 Ta:Al:TaC=1:1.4:1混合并加入质量分数为30%的碳化钽粉末配置Ta2AlC-Ta4AlC3复合材料的原料。
进一步的,将烘干的混料置入涂有BN石墨磨具中进行预压,预压压力为10~50Mpa。
本发明所述一种利用放电等离子烧结工艺制备Ta2AlC-Ta4AlC3复合材料块体陶瓷,与现有技术相比具有以下优点:提出一种制备Ta2AlC-Ta4AlC3复合材料块体陶瓷的新方法,工艺简单,合成时间较短;在加压过程中烧结,脉冲电流产生的等离子体及烧结过程中的加压有利于降低粉末的烧结温度,同时低电压、高电流的特征,能使粉末快速烧结致密。
附图说明
图1为放电等离子烧结工艺制备Ta2AlC-Ta4AlC3复合材料陶瓷的X射线衍射谱。
具体实施方式
下面结合附图对本发明作进一步描述。以下实施例仅用于更加清楚地说明本发明的技术方案,而不能以此来限制本发明的保护范围。
实施例1:一种Ta2AlC-Ta4AlC3复合材料的制备方法包括以下步骤:
(1) 以钽粉、铝粉和碳化钽粉为原料,按Ta:Al:TaC =1:1.4:1的摩尔比并加入质量分数为10%的碳化钽粉末配料;
(2) 将上述配料置入球磨罐中,在行星式球磨机上湿混15h;
(3)采用旋转蒸发仪将混料烘干,然后置入石墨磨具中进行预压,预压压力为20Mpa;
(4) 将模具放在放电等离子烧结炉中,在Ar气保护下,以200°C/min升温速率加热至1500°C,在500MPa压力下保温5min。保温结束后随炉冷却至室温,即得Ta2AlC-Ta4AlC3复合材料块体陶瓷。
实施例2:一种Ta2AlC-Ta4AlC3复合材料的制备方法包括以下步骤:
(1) 以钽粉、铝粉和碳化钽粉为原料,按Ta:Al:TaC =1:1.4:1的摩尔比并加入质量分数为20%的碳化钽粉末配料;
(2) 将上述配料置入球磨罐中,在行星式球磨机上湿混15h;
(3)采用旋转蒸发仪将混料烘干,然后置入石墨磨具中进行预压,预压压力为20Mpa;
(4) 将模具放在放电等离子烧结炉中,在Ar气保护下,以200°C/min升温速率加热至1500°C,在500MPa压力下保温5min。保温结束后随炉冷却至室温,即得Ta2AlC-Ta4AlC3复合材料块体陶瓷。
实施例3:一种Ta2AlC-Ta4AlC3复合材料的制备方法包括以下步骤:
(1) 以钽粉、铝粉和碳化钽粉为原料,按Ta:Al:TaC =1:1.4:1的摩尔比并加入质量分数为30%的碳化钽粉末配料;
(2) 将上述配料置入球磨罐中,在行星式球磨机上湿混15h;
(3)采用旋转蒸发仪将混料烘干,然后置入石墨磨具中进行预压,预压压力为20Mpa;
(4) 将模具放在放电等离子烧结炉中,在Ar气保护下,以200°C/min升温速率加热至1500°C,在500MPa压力下保温5min。保温结束后随炉冷却至室温,即得Ta2AlC-Ta4AlC3复合材料块体陶瓷。
如图1所示,为放电等离子烧结工艺制备Ta2AlC-Ta4AlC3复合材料陶瓷的X射线衍射谱,图中显示Ta2AlC的XRD图谱,以及典型添加10%、20%和30%的TaC粉末制备的复合材料的XRD图谱。
以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明技术原理的前提下,还可以做出若干改进和变形,这些改进和变形也应视为本发明的保护范围。
Claims (6)
1.一种Ta2AlC-Ta4AlC3复合材料的制备方法,其特征在于,包括以下步骤:
(1) 以钽粉、铝粉和碳化钽粉为原料,按一定摩尔比进行配比并加入质量分数为10%~50%的碳化钽粉末配置Ta2AlC-Ta4AlC3复合材料的原料;
(2) 将上述原料置入球磨罐中,在行星式球磨机上湿混15h;
(3) 采用旋转蒸发仪将混料烘干,然后置入石墨磨具中进行预压;
(4) 将模具放在放电等离子烧结炉中,在Ar气保护下,以80~500°C/min升温速率加热至1300~1500°C,在30~500MPa压力下保温5~10min。
2.根据权利要求1所述的一种Ta2AlC-Ta4AlC3复合材料的制备方法,其特征在于,原料钽粉、铝粉和碳化钽粉均为单质粉体,钽粉、铝粉和碳化钽粉按摩尔比Ta:Al:TaC =1:1.4:1混合并加入质量分数为10%~50%的碳化钽粉末配置Ta2AlC-Ta4AlC3复合材料。
3.根据权利要求2所述的一种Ta2AlC-Ta4AlC3复合材料的制备方法,其特征在于,钽粉、铝粉和碳化钽粉按摩尔比 Ta:Al:TaC=1:1.4:1混合并加入质量分数为10%的碳化钽粉末配置Ta2AlC-Ta4AlC3复合材料的原料。
4.根据权利要求2所述的一种Ta2AlC-Ta4AlC3复合材料的制备方法,其特征在于,钽粉、铝粉和碳化钽粉按摩尔比 Ta:Al:TaC=1:1.4:1混合并加入质量分数为20%的碳化钽粉末配置Ta2AlC-Ta4AlC3复合材料的原料。
5.根据权利要求2所述的一种Ta2AlC-Ta4AlC3复合材料的制备方法,其特征在于,钽粉、铝粉和碳化钽粉按摩尔比 Ta:Al:TaC=1:1.4:1混合并加入质量分数为30%的碳化钽粉末配置Ta2AlC-Ta4AlC3复合材料的原料。
6.根据权利要求1所述的一种Ta2AlC-Ta4AlC3复合材料的制备方法,其特征在于,将烘干的混料置入涂有BN石墨磨具中进行预压,预压压力为10~50Mpa。
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