CN105712718A - 一种层状C/ZrC复合材料及其制备方法 - Google Patents
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- 239000002131 composite material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 19
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000005470 impregnation Methods 0.000 claims description 16
- 239000011268 mixed slurry Substances 0.000 claims description 15
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 15
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 15
- 238000000498 ball milling Methods 0.000 claims description 10
- 238000005516 engineering process Methods 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- 238000007598 dipping method Methods 0.000 claims description 5
- 239000002270 dispersing agent Substances 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000003475 lamination Methods 0.000 claims description 5
- 239000010893 paper waste Substances 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 238000004381 surface treatment Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000007158 vacuum pyrolysis Methods 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 abstract 1
- 229910052726 zirconium Inorganic materials 0.000 abstract 1
- 229910026551 ZrC Inorganic materials 0.000 description 19
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 description 18
- 238000000034 method Methods 0.000 description 10
- 239000000919 ceramic Substances 0.000 description 9
- 238000005452 bending Methods 0.000 description 3
- 229910007948 ZrB2 Inorganic materials 0.000 description 2
- VWZIXVXBCBBRGP-UHFFFAOYSA-N boron;zirconium Chemical compound B#[Zr]#B VWZIXVXBCBBRGP-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910003864 HfC Inorganic materials 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 229910033181 TiB2 Inorganic materials 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000003026 anti-oxygenic effect Effects 0.000 description 1
- 239000011204 carbon fibre-reinforced silicon carbide Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/5607—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides
- C04B35/5622—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on zirconium or hafnium carbides
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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Abstract
本发明涉及一种层状C/ZrC复合材料及其制备方法，属于层状材料制备技术领域。本发明通过对原料中各相组分含量配比进行限定，对烧结温度、压力和保温时间进行限定，从而制备出成分可控的层状C/ZrC复合材料。该制备方法采用成本低廉的氧化锆及滤纸作为锆源和碳源，具有广阔的应用前景；所述复合材料的制备方法简单，制备周期短，易于规模化实施，具有较好的实用价值。
Description
技术领域
本发明涉及一种层状耐超高温复合材料及其制备方法，具体涉及一种层状C/ZrC复合材料及其制备方法，属于复合材料技术领域。
背景技术
层状复合结构设计已经成为当前国际上陶瓷增韧技术研究的热点，是陶瓷增韧的方法之一。目前，Ti/Al2O3,ZrC/SiC,ZrB2/SiC,HfC/SiC,ZrO-Zr2CN/Si3N4,SiCw/SiC,Ni/Cu,Ti-TiBw/Ti,TiB2-SiC/graphiteflake和HfC-SiC/BN等层状复合材料被报道。但是，从原材料来看（比如HfC,ZrC和ZrB2）价格都比较昂贵。这大大限制了层状复合材料的发展。因此，许多研究集中在优化制备工艺和制备条件来降低成本。
目前常用的耐高温材料体系主要包括：C/C复合材料、SiC陶瓷基复合材料(C/SiC、SiC/SiC)、难熔金属、耐超高温陶瓷等。C/ZrC复合材料具有高熔点、耐超高温、耐烧蚀性能和抗氧化性能好、尺寸稳定性优良等特点，是目前最有潜力的一种耐超高温材料。结合层状材料及耐高温材料体系的优点，在优化复合材料性能的前提下，最大限度地降低制备成本是亟需解决的问题。
发明内容
为了解决以上技术问题，本发明提供了一种层状C/ZrC复合材料，同时提供了其制备方法。本发明制备成本低，制备成的复合材料具有良好的微观结构、力学性能和致密性。
本发明中的层状C/ZrC复合材料，由以下步骤制备而成：
1）将粒径为20-30nm纳米氧化锆粉体和无水乙醇按照1:20质量比进行混合，在常温下进行磁力搅拌加超声分散1h得到混合料浆；之后将混合料浆放入聚四氟乙烯罐中球磨24h，球磨介质为氧化锆球，分散剂为0.5-1wt%聚乙二醇；将混好的浆料倒入真空浸渍设备备用；将滤纸或吸水率大的废纸裁剪成直径为45mm的圆片；对滤纸进行表面处理之后放入真空浸渍设备进行真空浸渍；将浸渍后的滤纸圆片在真空干燥箱中100℃条件下干燥24h制备成氧化锆/滤纸预制体；
2）氧化锆/滤纸预制体叠层之后放入石墨磨中并在真空热解烧结炉中进行高温烧结，得到层状C/ZrC复合材料；高温烧结条件为1650-1700℃、20-30MPa条件下烧结2-4h，其升温速度为0-1200℃升温速率为5℃/分钟，1200-1700℃为3℃/分钟；加压工艺为初始压力至目标压力的时间为20-30min。
制备成的复合材料的相对密度为1.89-1.97g/m3，弯曲强度为109.6-224.3MPa。
本发明是采用滤纸薄片在氧化锆浆料中真空浸渍法制备得到坯体，然后经过叠层在真空热压烧结条件下得到致密的层状碳/碳化锆超高温陶瓷，其工艺流程如图1所示。
本发明相比现有技术的优越性在于：
本发明相较于其他烧结工艺制备的层状复合材料制备成本更低，并有较好的力学综合性能；本发明中采用原位反应生成纳米碳化锆，层与层之间有良好的结合性，不引入其他杂质相；另外，原料获得容易，产品性能优异，有较高的成本性价比。
附图说明
图1为层状碳/碳化锆超高温复合材料的制备工艺流程图；
图2为层状碳/碳化锆超高温陶瓷的平面低倍金相图；
图3为层状碳/碳化锆超高温陶瓷的断面图。
具体实施方式
实施例1
将纳米氧化锆粉体（粒径为20-30nm）和无水乙醇按照1:20质量比进行混合，在常温下进行磁力搅拌加超声分散1h得到混合料浆；之后将混合料浆放入聚四氟乙烯罐中球磨24h，球磨介质为氧化锆球，分散剂为0.5-1wt%聚乙二醇；将混好的浆料倒入真空浸渍设备备用；将滤纸（或吸水率大的废纸）裁剪成直径为45mm的圆片；对滤纸进行表面处理之后放入真空浸渍设备进行真空浸渍；将浸渍后的滤纸圆片在真空干燥箱中100℃条件下干燥24h制备成氧化锆/滤纸预制体；氧化锆/滤纸预制体经过45层叠片后放入石墨磨中并在真空热压烧结炉中进行高温处理。其制备工艺流程图如图1所示。高温处理条件为：1700℃、30MPa条件下烧结4h，得到层状C/ZrC复合材料；升温速度为0-1200℃升温速率为5℃/分钟，1200-1700℃为3℃/分钟；加压工艺为初始压力至目标压力的时间为20-30min；如图2所示，层状C/ZrC复合材料被成功制备。样品呈现明显的层状。图3为层状碳/碳化锆超高温陶瓷的断面图。从图中可以观察到样品中颗粒生长良好，颗粒尺寸均匀，且可观察到明显的界面结合。层状样品相组成主要为C、ZrC，层厚约为100μm，层间分布均匀。对样品进行断裂实验，观察其断裂过程，可以明显观察到裂纹偏转现象。证明层状陶瓷可以改变裂纹传播路径，从而增加断裂韧性。其相对密度为1.89g/m3，弯曲强度为127MPa。
实施例2
将纳米氧化锆粉体（粒径为20-30nm）和无水乙醇按照1:20质量比进行混合，在常温下进行磁力搅拌加超声分散1h得到混合料浆；之后将混合料浆放入聚四氟乙烯罐中球磨24h，球磨介质为氧化锆球，分散剂为0.5-1wt%聚乙二醇；将混好的浆料倒入真空浸渍设备备用；将滤纸（或吸水率大的废纸）裁剪成直径为45mm的圆片；对滤纸进行表面处理之后放入真空浸渍设备进行真空浸渍；将浸渍后的滤纸圆片在真空干燥箱中100℃条件下干燥24h制备成氧化锆/滤纸预制体；氧化锆/滤纸预制体经过56层叠片后放入石墨磨中并在真空热压烧结炉中进行高温处理。高温处理条件为：1700℃、30MPa条件下烧结4h，得到层状C/ZrC复合材料；升温速度为0-1200℃升温速率为5℃/分钟，1200-1700℃为3℃/分钟；加压工艺为初始压力至目标压力的时间为20-30min；样品中颗粒生长良好，颗粒尺寸均匀，且可观察到明显的界面结合。层状样品相组成主要为C、ZrC，层厚约为100μm，层间分布均匀。对样品进行断裂实验，观察其断裂过程，可以明显观察到裂纹偏转现象。证明层状陶瓷可以改变裂纹传播路径，从而增加断裂韧性。其相对密度为1.95g/m3，弯曲强度为218MPa。
Claims (4)
1.一种层状C/ZrC复合材料，其特征在于，由以下步骤制备而成：
1)将粒径为20-30nm纳米氧化锆粉体和无水乙醇按照1:20质量比进行混合，在常温下进行磁力搅拌加超声分散1h得到混合料浆；之后将混合料浆放入聚四氟乙烯罐中球磨24h，球磨介质为氧化锆球，分散剂为0.5-1wt%聚乙二醇；将混好的浆料倒入真空浸渍设备备用；将滤纸或吸水率大的废纸裁剪成直径为45mm的圆片；对滤纸进行表面处理之后放入真空浸渍设备进行真空浸渍；将浸渍后的滤纸圆片在真空干燥箱中100℃条件下干燥24h制备成氧化锆/滤纸预制体；
2)氧化锆/滤纸预制体叠层之后放入石墨磨中并在真空热解烧结炉中进行高温烧结，得到层状C/ZrC复合材料。
2.根据权利要求1所述的层状C/ZrC复合材料，其特征在于，所述的高温烧结的条件为1650-1700℃、20-30MPa条件下烧结2-4h，其升温速度为0-1200℃升温速率为5℃/分钟，1200-1700℃为3℃/分钟；加压工艺为初始压力至目标压力的时间为20-30min。
3.一种权利要求1或2任一项所述的层状C/ZrC复合材料的制备方法，其特征在于，包括如下步骤：
1)将粒径为20-30nm纳米氧化锆粉体和无水乙醇按照1:20质量比进行混合，在常温下进行磁力搅拌加超声分散1h得到混合料浆；之后将混合料浆放入聚四氟乙烯罐中球磨24h，球磨介质为氧化锆球，分散剂为0.5-1wt%聚乙二醇；将混好的浆料倒入真空浸渍设备备用；将滤纸或吸水率大的废纸裁剪成直径为45mm的圆片；对滤纸进行表面处理之后放入真空浸渍设备进行真空浸渍；将浸渍后的滤纸圆片在真空干燥箱中100℃条件下干燥24h制备成氧化锆/滤纸预制体；
2)氧化锆/滤纸预制体叠层之后放入石墨磨中并在真空热解烧结炉中进行高温烧结，得到层状C/ZrC复合材料。
4.根据权利要求3所述的制备方法，其特征在于，所述的高温烧结的条件为1650-1700℃、20-30MPa条件下烧结2-4h，其升温速度为0-1200℃升温速率为5℃/分钟，1200-1700℃为3℃/分钟；加压工艺为初始压力至目标压力的时间为20-30min。
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