CN112500171A - 一种致密化硼化锆-碳化硅复合陶瓷的制备方法 - Google Patents
一种致密化硼化锆-碳化硅复合陶瓷的制备方法 Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 60
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 53
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910052726 zirconium Inorganic materials 0.000 title claims abstract description 50
- 239000000919 ceramic Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000005245 sintering Methods 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 39
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 18
- 229910007948 ZrB2 Inorganic materials 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 239000011230 binding agent Substances 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 229910052580 B4C Inorganic materials 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 8
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 7
- 239000005011 phenolic resin Substances 0.000 claims description 7
- 229920001568 phenolic resin Polymers 0.000 claims description 7
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000006229 carbon black Substances 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 3
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 3
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 3
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims description 3
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 2
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 238000000465 moulding Methods 0.000 claims 1
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 31
- 239000011159 matrix material Substances 0.000 abstract description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052796 boron Inorganic materials 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 238000011065 in-situ storage Methods 0.000 abstract description 4
- 238000001272 pressureless sintering Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000005260 corrosion Methods 0.000 abstract description 2
- 238000005520 cutting process Methods 0.000 abstract description 2
- 239000007772 electrode material Substances 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 230000035939 shock Effects 0.000 abstract description 2
- 238000001035 drying Methods 0.000 description 17
- 238000000498 ball milling Methods 0.000 description 11
- 239000011812 mixed powder Substances 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000000748 compression moulding Methods 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 238000005452 bending Methods 0.000 description 5
- 238000005469 granulation Methods 0.000 description 5
- 230000003179 granulation Effects 0.000 description 5
- 238000007731 hot pressing Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 239000011268 mixed slurry Substances 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 238000000280 densification Methods 0.000 description 2
- 230000008707 rearrangement Effects 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000011215 ultra-high-temperature ceramic Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
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- 230000002708 enhancing effect Effects 0.000 description 1
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- 238000009776 industrial production Methods 0.000 description 1
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- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
本发明提供一种致密化硼化锆‑碳化硅复合陶瓷的制备方法,所述复合陶瓷的原料中,ZrB2粉、碳化钛粉、烧结助剂、锆源、碳化硼、C源的质量配比为(30‑75):(5‑45):(0‑5):(0‑30):(10‑35):(5‑25),在原料中,引入锆源、硼源和C源,通过原位反应,在硼化锆陶瓷基体中合成超细的硼化锆晶粒,提高了硼化锆的烧结活性,本发明采用无压烧结的技术,具有工艺简单、设备要求度低、生产成本低、便于批量化生产的优点,制得的ZrB2复合陶瓷材料具有致密度高、抗高温氧化、高硬度、耐腐蚀、耐热震性好、电阻小等优异性能,在航空航天耐高温材料、耐磨材料、切削工具、热电偶保护管以及电极材料等领域具有非常大的实用前景。
Description
技术领域
本发明属于陶瓷材料技术领域,具体涉及一种致密化硼化锆-碳化硅复合陶瓷的制备方法。
背景技术
复合陶瓷具有强度高、导热良好、电阻小、抗高温氧化、耐化学腐蚀、耐热震性好等优良的特性,被用在切削刀具、耐磨部件、电极材料、热电偶保护管等领域。但是硼化锆属于超硬材料,原子自扩散系数小,难以烧结致密化。目前,虽然使用热压、SPS、自蔓延等烧结方式可以获得致密化的硼化锆-碳化硅复合陶瓷;但是,硼化锆-碳化硅复合陶瓷的形状和数量受到限制,难以实现大规模产业化生产,导致了硼化锆-碳化硅复合陶瓷的实际应用领域比较狭窄。
CN101602597B公开一种硼化锆-碳化硅-碳黑三元高韧化超高温陶瓷基复合材料及其制备方法,硼化锆-碳化硅-碳黑三元高韧化超高温陶瓷基复合材料按体积比由50%~75%的硼化锆粉末、20%的碳化硅粉末和5%~30%的碳黑粉末制成,经烘干研磨烧结后,得到的陶瓷基复合材料强度为132.03~695.54MPa,断裂韧性为 2.01~6.57MPa·m1/2。但是,该技术采用常规的热压烧结工艺,采用热压烧结工艺,产品上下两面要承受很大的压力,产品的形状往往是板材或片材,形状简单不能复杂,所以形状受到限制;此外,由于产品受压的原因,每一批次烧结的产品数量也会受到限制。热压烧结工艺,样品虽然能获得较高的综合性能,但是样品的形状、尺寸和数量受到了极大的限制,不适用于规模化大批量生产。
发明内容
为解决现有技术存在的问题,对现有工艺进行进一步优化,本发明提供一种致密化硼化锆-碳化硅复合陶瓷的制备方法,以实现制备具有高致密度、形状可塑性强、便于大规模量产的硼化锆-碳化硅复合陶瓷的发明目的。
为解决以上技术问题,本发明采用以下技术方案:
一种致密化硼化锆-碳化硅复合陶瓷的制备方法,其特征在于,所述复合陶瓷的原料,包括ZrB2粉、碳化钛粉、烧结助剂、锆源、碳化硼和C源,ZrB2粉、碳化钛粉、烧结助剂、锆源、碳化硼、C源的质量配比为(30-75):(5-45):(0-5):(0-30):(10-35):(5-25);
所述锆源可以是锆粉、ZrO2粉、硅酸锆中的一种或几种;
所述C源可以是酚醛树脂、石墨粉、炭黑、石墨烯中的一种或几种;
所述烧结助剂可以是氧化钙、氧化镁、氧化钇、氧化铈、氧化镧、碳化钨、碳化钛、氧化铝、氧化硅、氮化硅、氮化铝中的一种或几种;
所述ZrB2粉平均粒度为0.5~5μm,纯度大于99%;
所述碳化硅粉平均粒度为0.5~3μm,纯度大于99.5%;
所述制备方法,包括以下步骤:
(1)将原料、结合剂与液体介质一起混合成浆料,在球磨罐中球磨;
(2)将混合浆料进行喷雾造粒或在40~100℃干燥箱中烘干后手工过筛造粒;
(3)将造粒粉放入模具中,经过模压成型制成陶瓷生坯;
(4)将压制好的陶瓷生坯放入100~250℃干燥箱中干燥;
(5)将生坯放入高温烧结中,1800~2200℃下反应烧结获得致密化ZrB2-SiC复合陶瓷材料;
所述混合成浆,原料、结合剂和液体介质的质量比为100:(15-25):(100-180);
所述结合剂可以是酚醛树脂、PVA或PVB;
所述液体介质可以是水或丙酮或乙醇;
所述过筛造粒,筛网规格为40~100目;
所述模压成型,压力为100~250MPa;
所述烧结气氛可以是真空、氩气、氢气中的一种或两种。
本专利采用无压烧结工艺,制备样品的形状、尺寸和数量不受限制;在原料中,引入烧结助剂,有利于形成液相,促进颗粒之间重新排列,便于形成烧结颈,从而降低烧结温度;且在原料中,引入锆源、硼源和C源,通过原位反应合成硼化锆,在硼化锆陶瓷基体中合成超细的硼化锆晶粒,提高了硼化锆的烧结活性,而且超细的硼化锆颗粒对陶瓷基体和形成的液相均有弥散强化作用,有利于致密化,本发明无压烧结工艺得到的复合陶瓷综合性能与热压烧结的相近,适用于规模化大批量生产。
采用上述技术方案,本发明的有益效果为:
1、采用本发明致密化硼化锆-碳化硅复合陶瓷的制备方法,在原料中,引入锆源、硼源和C源,通过原位反应,在硼化锆陶瓷基体中合成超细的硼化锆晶粒,提高了硼化锆的烧结活性,有利于致密化,相对密度达到95-99%;
2、采用本发明致密化硼化锆-碳化硅复合陶瓷的制备方法,在原料中,引入烧结助剂,有利于形成液相,促进颗粒之间重新排列,便于形成烧结颈,从而降低了烧结温度,烧结温度在2100-2200℃;
3、采用本发明致密化硼化锆-碳化硅复合陶瓷的制备方法,提高了复合陶瓷的弯曲强度和断裂韧性,弯曲强度达到584-706MPa,断裂韧性达到5.92-6.69MPa·m1/2;
4、采用本发明致密化硼化锆-碳化硅复合陶瓷的制备方法,降低了硼化锆-碳化硅复合陶瓷的气孔率,气孔率为0.24-0.87%;同时维氏硬度达到23.66-25.24GPa;
5、采用本发明致密化硼化锆-碳化硅复合陶瓷的制备方法,硼化锆-碳化硅复合陶瓷材料的电阻率可达到3.12×10-6-9.48×10-5Ω·m;
6、本发明采用无压烧结工艺,可以制备出形状可塑的产品,工艺简单,对设备要求度低,便于大规模自动化生产,产品成本低且性能高,具有巨大的市场实用价值。
说明书附图
图1为本发明实施例中制备的ZrB2-SiC复合陶瓷材料条状样品实物图,图中(a)为实施例1的ZrB2-SiC复合陶瓷材料条状样品实物图,(b)为实施例2的ZrB2-SiC复合陶瓷材料条状样品实物图,(c)为实施例3的ZrB2-SiC复合陶瓷材料条状样品实物图,(d)为实施例4的ZrB2-SiC复合陶瓷材料条状样品实物图。
图2为本发明实施例中制备的ZrB2-SiC复合陶瓷材料X射线衍射图,图中(a)为实施例1的ZrB2-SiC复合陶瓷材料X射线衍射图,(b)为实施例2的ZrB2-SiC复合陶瓷材料X射线衍射图,(c)为实施例3的ZrB2-SiC复合陶瓷材料X射线衍射图,(d)为实施例4的ZrB2-SiC复合陶瓷材料X射线衍射图。
图3为本发明实施例1的ZrB2-SiC复合陶瓷材料金相显微图。
图4为本发明实施例2的ZrB2-SiC复合陶瓷材料扫描电镜照片图。
图5为本发明实施例3的ZrB2-SiC复合陶瓷材料扫描电镜照片图。
图6为本发明实施例4的ZrB2-SiC复合陶瓷材料扫描电镜照片图。
具体实施方式:
下面结合具体的实施例,进一步阐述本发明。
实施例1
一种致密化硼化锆-碳化硅复合陶瓷的制备方法,步骤如下:
(1)按质量比,将ZrB2粉、碳化硅、烧结助剂碳化钛、ZrO2粉、碳化硼粉、炭黑=45:35:5:25:10:9混合成混合粉料,将混合粉料、浓度为5%PVA溶液的结合剂、液体介质去离子水=100:25:160一起混合成浆料,在球磨罐中球磨;
所述ZrB2粉,平均粒度1μm;
所述碳化硅粉,平均粒度为0.5μm;
(2)将混合浆料进行喷雾造粒;
(3)将造粒粉放入模具中,经压力机模压成型,压力200MPa,获得生坯;
(4)将压制好的陶瓷生坯放入150℃干燥箱中干燥排出体内水分;
(5)将生坯放入烧结中,在真空状态下,升温至1800℃保温60min,之后充氩气,达到烧结温度2125℃时,保温150min,获得ZrB2-SiC复合陶瓷材料;
本实施例制得的ZrB2-SiC复合陶瓷材料的金相显微图如图3所示;经测试,该ZrB2-SiC复合陶瓷材料的相对密度为98.15%、气孔率为0.27%、弯曲强度为625MPa、断裂韧性为6.69MPa·m1/2、维氏硬度为25.15GPa、电阻率为6.87×10-5Ω·m。
实施例2
一种致密化硼化锆-碳化硅复合陶瓷的制备方法,步骤如下:
(1)按质量比,将ZrB2粉、碳化硅、烧结助剂氧化钇、Zr粉、碳化硼粉、石墨烯=40:45:3:15:25:5混合成混合粉料,将混合粉料、浓度为8%酚醛树脂结合剂、液体介质乙醇=100:15:120一起混合成浆料,在球磨罐中球磨;
所述ZrB2粉,平均粒度1μm;
所述碳化硅粉,平均粒度为3μm;
(2)将球磨后的浆料在80℃干燥箱中烘干后,手工研磨破碎粉末,并过100目筛造粒;
(3)将造粒粉放入模具中,经压力机模压成型,压力150MPa,获得生坯;
(4)将压制好的陶瓷生坯放入120℃干燥箱中干燥排出体内水分;
(5)将生坯放入烧结中,在真空状态下,升温至1650℃保温90min,达到烧结温度2100℃时,保温180min,获得ZrB2-SiC复合陶瓷材料;
本实施例制得的ZrB2-SiC复合陶瓷材料的扫描电镜图如图4所示;经测试,该ZrB2-SiC复合陶瓷材料的相对密度为96.34%、气孔率为0.87%、弯曲强度为584MPa、断裂韧性为6.18MPa·m1/2、维氏硬度为23.66GPa、电阻率为9.48×10-5Ω·m。
实施例3
一种致密化硼化锆-碳化硅复合陶瓷的制备方法,步骤如下:
(1)按质量比,将ZrB2粉、碳化硅、烧结助剂氧化铈、硅酸锆、碳化硼粉、石墨粉=60:22:5:25:30:19混合成混合粉料,将混合粉料、浓度为5%酚醛树脂结合剂、液体介质去离子水=100:20:180一起混合成浆料,在球磨罐中球磨;
所述ZrB2粉,平均粒度0.5μm;
所述碳化硅粉,平均粒度为0.5μm;
(2)将球磨后的浆料在100℃干燥箱中烘干后,手工研磨破碎粉末,并过60目筛造粒;
(3)将造粒粉放入模具中,经压力机模压成型,压力250MPa,获得生坯;
(4)将压制好的陶瓷生坯放入200℃干燥箱中干燥排出体内水分;
(5)将生坯放入烧结中,在氩气状态下,升温至2000℃保温60min,之后充氢气,达到烧结温度2200℃时,保温90min,获得ZrB2-SiC复合陶瓷材料;
本实施例制得的ZrB2-SiC复合陶瓷材料的扫描电镜图如图5所示;经测试,该ZrB2-SiC复合陶瓷材料的相对密度为98.69%、气孔率为0.24%、弯曲强度为656MPa、断裂韧性为5.92MPa·m1/2、维氏硬度为24.87GPa、电阻率为3.12×10-6Ω·m。
实施例4
一种致密化硼化锆-碳化硅复合陶瓷的制备方法,步骤如下:
(1)按质量比,将ZrB2粉、碳化硅、烧结助剂氧化铝、ZrO2粉、碳化硼粉、酚醛树脂粉=55:30:4:20:35:15混合成混合粉料,将混合粉料、浓度为5%PVB结合剂、液体介质丙酮=100:15:100一起混合成浆料,在球磨罐中球磨;
所述ZrB2粉,平均粒度2μm;
所述碳化硅粉,平均粒度为1μm;
(2)将球磨后的浆料进行喷雾造粒;
(3)将造粒粉放入模具中,经压力机模压成型,压力180MPa,获得生坯;
(4)将压制好的陶瓷生坯放入250℃干燥箱中干燥排出体内水分;
(5)将生坯放入烧结中,在氩气状态下,升温至1950℃保温90min,达到烧结温度2135℃时,保温120min,获得ZrB2-SiC复合陶瓷材料;
本实施例制得的ZrB2-SiC复合陶瓷材料的扫描电镜图如图6所示;经测试,该ZrB2-SiC复合陶瓷材料的相对密度为97.21%、气孔率为0.76%、弯曲强度为706MPa、断裂韧性为6.11MPa·m1/2、维氏硬度为25.24GPa、电阻率为8.56×10-5Ω·m。
从本发明实施例中制备的ZrB2-SiC复合陶瓷材料扫描电镜图可以展示出不同工艺体系获得的复合材料显微组织,可以观察出复合材料中,各成分的含量多少,颗粒尺寸大小等;结合X射线衍射图可见,通过无压烧结工艺,原料中的锆源、硼源、碳源通过原位合成工艺,合成了硼化锆,从而在硼化锆陶瓷基体中起到了增强作用。
Claims (11)
1.一种致密化硼化锆-碳化硅复合陶瓷的制备方法,其特征在于,所述复合陶瓷的原料,包括ZrB2粉、碳化钛粉、烧结助剂、锆源、碳化硼和C源,ZrB2粉、碳化钛粉、烧结助剂、锆源、碳化硼、C源的质量配比为(30-75):(5-45):(0-5):(0-30):(10-35):(5-25)。
2.根据权利要求1所述的制备方,其特征在于,所述锆源可以是锆粉、ZrO2粉、硅酸锆中的一种或几种。
3.根据权利要求1所述的制备方法,其特征在于,所述C源可以是酚醛树脂、石墨粉、炭黑、石墨烯中的一种或几种。
4.根据权利要求1所述的制备方法,其特征在于,所述烧结助剂可以是氧化钙、氧化镁、氧化钇、氧化铈、氧化镧、碳化钨、碳化钛、氧化铝、氧化硅、氮化硅、氮化铝中的一种或几种。
5.根据权利要求1所述的制备方法,其特征在于,所述ZrB2粉平均粒度为0.5-5μm,纯度大于99%;碳化硅粉平均粒度为0.5-3μm,纯度大于99.5%。
6.根据权利要求1所述的制备方法,其特征在于,所述制备方法,包括将原料与结合剂和液体介质混合成浆;所述原料、结合剂和液体介质的质量比为100:(15-25):(100-180)。
7.根据权利要求6所述的制备方法,其特征在于,所述结合剂可以是酚醛树脂、PVA或PVB。
8.根据权利要求6所述的制备方法,其特征在于,所述液体介质可以是水或丙酮或乙醇。
9.根据权利要求6所述的制备方法,其特征在于,所述制备方法,还包括模压成型,所述模压成型,压力为100-250MPa。
10.根据权利要求6所述的制备方法,其特征在于,所述制备方法,还包括烧结,所述烧结气氛可以是真空、氩气、氢气中的一种或两种。
11.根据权利要求6所述的制备方法,其特征在于,所述制备方法,还包括过筛造粒,所述过筛造粒,筛网规格为40-100目。
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