CN109320251B - 一种高性能无压烧结碳化硅复合陶瓷的制备方法 - Google Patents
一种高性能无压烧结碳化硅复合陶瓷的制备方法 Download PDFInfo
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 78
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 239000000919 ceramic Substances 0.000 title claims abstract description 41
- 239000002131 composite material Substances 0.000 title claims abstract description 37
- 238000001272 pressureless sintering Methods 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 43
- 238000000498 ball milling Methods 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 35
- 239000004642 Polyimide Substances 0.000 claims abstract description 33
- 229920001721 polyimide Polymers 0.000 claims abstract description 33
- 229910033181 TiB2 Inorganic materials 0.000 claims abstract description 31
- 239000004698 Polyethylene Substances 0.000 claims abstract description 30
- -1 polyethylene Polymers 0.000 claims abstract description 30
- 229920000573 polyethylene Polymers 0.000 claims abstract description 30
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 claims abstract description 26
- 230000008569 process Effects 0.000 claims abstract description 26
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 21
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 21
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 239000005011 phenolic resin Substances 0.000 claims abstract description 19
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 19
- 239000002002 slurry Substances 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 229910003465 moissanite Inorganic materials 0.000 claims abstract description 15
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- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
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- 238000007873 sieving Methods 0.000 claims abstract description 9
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- 238000004321 preservation Methods 0.000 claims description 8
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 8
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 8
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 8
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 239000012188 paraffin wax Substances 0.000 claims description 4
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 4
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- 229910052582 BN Inorganic materials 0.000 claims description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 2
- 239000004927 clay Substances 0.000 claims description 2
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 2
- 239000010445 mica Substances 0.000 claims description 2
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- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 2
- 229920000058 polyacrylate Polymers 0.000 claims description 2
- 230000000052 comparative effect Effects 0.000 description 25
- 229910052580 B4C Inorganic materials 0.000 description 24
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 239000000463 material Substances 0.000 description 10
- 238000005452 bending Methods 0.000 description 6
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- 229910052786 argon Inorganic materials 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000007731 hot pressing Methods 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000012790 adhesive layer Substances 0.000 description 2
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- 239000010703 silicon Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 2
- 238000007792 addition Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
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- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
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- 238000005520 cutting process Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
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- 238000009792 diffusion process Methods 0.000 description 1
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- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920003223 poly(pyromellitimide-1,4-diphenyl ether) Polymers 0.000 description 1
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- 238000004062 sedimentation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
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- 238000009736 wetting Methods 0.000 description 1
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Abstract
本发明属于碳化硅陶瓷领域,涉及一种无压烧结碳化硅复合陶瓷的制备方法。制备方法包括以下步骤:按照原料配比称取各成分,将SiC、TiB2、B4C、聚酰亚胺、分散剂以及40‑60%的水混合球磨4‑8h;静置1‑5h后,入蒸汽干燥箱中干燥;加入酚醛树脂以及剩余40‑60%的水,继续球磨1‑3h;加入聚乙烯和聚乙烯醇,球磨1‑3h,得浆液;将浆液喷雾干燥造粒;造粒料过50‑100目筛,加入脱模剂,采用压制成型工艺制得生坯;将生批放入高温真空烧结炉内,采用无压烧结工艺进行烧结。
Description
技术领域
本发明属于碳化硅陶瓷领域,涉及一种无压烧结碳化硅复合陶瓷的制备方法。
背景技术
烧结过程根据有无加压分为热压烧结和无压烧结,热压烧结是在烧结过程中同时施加一定的外力,使材料加速流动、重排和致密化。而无压烧结是指在常压下,通过对制品加热而烧结的一种方法。在碳化硅烧结中,由于SiC共价键比例较高,自扩散系数很小,从而导致碳化硅很难烧结。相对于无压烧结,碳化硅陶瓷采用热压烧结虽然更容易获得细晶粒的组织,实现晶体的趋向效应和控制含有高蒸气压成分系统的组成变化,因而容易得到良好机械性能的产品,但是热压烧结仅适合形状简单的制品,对于形状复杂的制品,后期还需要金刚石切割机的再次加工,很难规模生产;而无压烧结制备的SiC陶瓷不仅具备烧结助剂含量低,不会在晶界处残留低熔点的物质,可使SiC陶瓷材料拥有良好的高温稳定性的优点,而且,对于降低烧结成本和制备形状复杂且厚度较大的产品,常压烧结具有比较突出的优势。但常压烧结过程中碳化硅样品容易产生孔隙,其致密化程度较热压烧结有所欠缺,得到的碳化硅密度在3.1g/cm3左右,弯曲强度在400MPa左右,维氏硬度0.5约2400-2500kgF/mm2,无法满足复杂工况下对耐冲击、耐颠震的性能要求,因此如何利用无压烧结获得高性能的碳化硅复合陶瓷以达到复杂工况下的使用要求是十分必要的。
发明内容
本发明的目的是针对目前碳化硅陶瓷无压烧结的缺陷,引入SiC-TiB2-B4C复合相,以增强陶瓷材料的弯曲强度、硬度等性能,再通过聚酰亚胺在粘合剂添加之前覆盖在SiC、TiB2、B4C表面,以降低烧结过程中的孔隙率,提高烧结致密度,进一步提高材料的性能。
为了达到上述发明目的,本发明采用以下技术方案:一种高性能无压烧结碳化硅复合陶瓷的制备方法,所述碳化硅复合陶瓷的制备原料包括以下重量份成分:
SiC:70-80份,TiB2:13-18份,B4C:5-12份,分散剂:0.3-0.5份,酚醛树脂:5-8份,聚乙烯:1-2份,聚乙烯醇:4-6份,脱模剂:2-5份,聚酰亚胺:5-7份,水150-300份。
作为优选,所述制备方法包括以下步骤:
(1)按照权利要求1的原料配比称取各成分,将SiC、TiB2、B4C、聚酰亚胺、分散剂以及40-60%的水混合球磨4-8h;
(2)静置1-5h后,入蒸汽干燥箱中干燥;
(3)加入酚醛树脂以及剩余40-60%的水,继续球磨1-3h;
(4)加入聚乙烯和聚乙烯醇,球磨1-3h,得浆液;
(5)将浆液喷雾干燥造粒;
(6)造粒料过50-100目筛,加入脱模剂,采用压制成型工艺制得生坯;
(7)将生批放入高温真空烧结炉内,采用无压烧结工艺进行烧结。
作为优选,所述球磨机转速为50~500转/分钟,步骤(1)球磨后的粒度0.1-2μm。
作为优选,所述喷雾干燥造粒大小为50-100μm,含水率0.5-1.5%。
作为优选,所述成型压力为300-500MPa。
作为优选,所述无压烧结工艺为:以10-15℃/min的速度升温至1200-1400℃,然后通入惰性气体,随后以≥50℃/min的速度加热至2000-2200℃,保温烧结2-4h。
作为优选,所述分散剂为六偏磷酸钠、聚丙烯酸铵、柠檬酸铵、十二烷基硫酸钠、四甲基氢氧化铵中的一种或多种。
作为优选,所述脱模剂为微晶石蜡、聚乙烯蜡、氮化硼、硬脂酸盐类、滑石粉、白粘土、云母中的一种或多种。
本发明与现有技术相比,有益效果体现在:
本发明在SiC的基础上,引入TiB2和B4C,形成SiC-TiB2-B4C复合相,增强陶瓷材料的弯曲强度、硬度等性能。并加入聚酰亚胺干燥固定在SiC、TiB2、B4C颗粒表面,通过烧结过程中的缓慢升温,降低材料的孔隙度并建立起共格晶界,提高烧结致密度,进一步提高材料的性能。本发明所获得的复合陶瓷性能选超无压烧结碳化硅,满足复杂工况下,耐冲击、耐颠震等性能要求。
具体实施方式
下面通过具体实施例对本发明的技术方案作进一步描述说明。如果无特殊说明,本发明的实施例中所采用的原料均为本领域常用的原料,实施例中所采用的方法,均为本领域的常规方法。
本发明的一个实施例中,碳化硅复合陶瓷的制备原料包括以下重量份成分:SiC:70-80份,TiB2:13-18份,B4C:5-12份,分散剂:0.3-0.5份,酚醛树脂:5-8份,聚乙烯:1-2份,聚乙烯醇:4-6份,脱模剂:2-5份,聚酰亚胺:5-7份,水150-300份。
B4C是硬度很大的材料,将其作为增强相分散在SiC基体中可以极大提高材料的硬度。TiB2在碳化硅和碳化硼表面形成,碳化硅和碳化硼成为附着二硼化钛的基体,因此颗粒小的二硼化钛颗粒包围在碳化硅和碳化硼周围,防止二硼化钛颗粒成团聚集,并利用陶瓷中的二硼化钛颗粒使得部件承受弯曲的能力加大:在高温下,TiB2可以与碳化硅表面的残留Si形成固溶体,固溶强化体提高材料的弯曲强度。且TiB2能够润湿SiC和B4C,形成SiC-TiB2-B4C复合相,三者具有良好的界面相容性,以促进烧结,提高材料的力学性能。
酚醛树脂作为碳源,在烧结过程中,使碳化硅表面的二氧化硅形成碳化硅,从而增加碳化硅的表面能,促进烧结,烧结过后产品内部没有残留的硅,提高产品的耐腐蚀性。聚乙烯以及聚乙烯醇作为粘结剂,将碳化硅等颗粒粘结在一起,无压烧结中增加致密度,粘结剂的含量需要控制合理,粘结剂含量越多,干燥后形成的网络越密实,粘结力也越强,但是粘结剂含量过多会降低碳化硅复合陶瓷的密度。
本发明的一个实施例中,碳化硅复合陶瓷的制备方法包括以下步骤:
(1)按照原料配比称取各成分,将SiC、TiB2、B4C、聚酰亚胺、分散剂以及40-60%的水混合球磨4-8h,湿法球磨不仅能均匀分散粉体,还可以细化陶瓷颗粒粒径,获得晶粒细化的均匀分散体系。
(2)静置1-5h后,入蒸汽干燥箱中干燥;
(3)加入酚醛树脂以及剩余40-60%的水,继续球磨1-3h。
(4)加入聚乙烯和聚乙烯醇,球磨1-3h,得浆液。
(5)将浆液喷雾干燥造粒。将混合好的浆料直接喷雾到热空气中,在非常短的时间内干燥,得到形状规则的球状粉粒。压制成型前的造粒可以避免各组分的再团聚和沉降分离,保持浆料原有的均匀性,得到的粉体粒度分布均匀,流动性好。
(6)造粒料过50-100目筛,加入脱模剂,采用压制成型工艺制得生坯;
(7)将生批放入高温真空烧结炉内,采用无压烧结工艺进行烧结。
本实施例中,先将聚酰亚胺与SiC、TiB2、B4C颗粒混合球磨,静置过程中,聚酰亚胺吸附在颗粒表面,通过干燥将颗粒表面的聚酰亚胺固定住。粘结剂聚乙烯和聚乙烯醇在后续球磨中形成在聚酰亚胺外周围,由此SiC、TiB2和B4C颗粒从内到外形成聚酰亚胺层和粘结剂层。粘结剂层的热分解速度低于聚酰亚胺,在烧结过程中,粘结剂层最先热分解挥发,形成的孔隙由聚酰亚胺填充,随后聚酰亚胺再热分解,SiC、TiB2、B4C颗粒相互粘结,从而降低无压烧结过程中的孔隙,提高致密度。
在本发明的一个实施例中,所述球磨机转速为50~500转/分钟,步骤(1)球磨后的粒度为0.1-2μm。复合陶瓷由SiC、TiB2、B4C粉末制成,粉末大小决定烧结部件中的晶粒大小,从而影响陶瓷性能,将SiC、TiB2、B4C粉末的粒度控制在0.1-2μm,有助于获得合适粒径的晶粒。
在本发明的一个实施例中,所述喷雾干燥造粒大小为50-100μm,含水率0.5-1.5%。造粒料中的水分含量对烧结具有很大影响,残余的水分在烧结过程中形成水蒸气,而水蒸气与碳化硅在高温下反应强烈,会生成硅、碳或二氧化硅,影响颗粒间的粘结,降低材料致密度。
在本发明的一个实施例中,所述成型压力为300-500MPa。
在本发明的一个实施例中,所述无压烧结工艺为:以10-15℃/min的速度升温至1200-1400℃,然后通入惰性气体,随后以≥50℃/min的速度加热至2000-2200℃,保温烧结2-4h。
烧结过程中,在温度升至1200-1400℃之前,以10-15℃/min的速度的温度升温,可以延长粘结层和聚酰亚胺层的热分解间隔时间,使得聚酰亚胺层由足够的时间填充粘结层分解留下的孔隙。烧结过程中的高温段再充入惰性气体进行保护。
以下实施例中,聚酰亚胺具体选自杜邦Vespel,聚乙烯醇采用日本可乐丽PVA-217,聚乙烯蜡为泰国SCG化工的LP0020P,聚乙烯为中国石油化工的3300F,酚醛树脂购自河南滨海实业有限责任公司,型号为2130。
实施例1
本实施例的碳化硅复合陶瓷制备方法中,原料为以下重量份成分:SiC:75份,TiB2:15份,B4C:10份,六偏磷酸钠:0.4份,酚醛树脂:6份,聚乙烯:1.5份,聚乙烯醇:5份,聚乙烯蜡:3份,聚酰亚胺:6份,水200份。
按照上述原料配比称取各成分,将SiC、TiB2、B4C、聚酰亚胺、六偏磷酸钠以及60%的水混合球磨6h,球磨机转速为100r/min,球磨后粒度为1μm左右;静置3h后,入蒸汽干燥箱中干燥;然后加入酚醛树脂以及剩余40%的水,继续球磨2h;加入聚乙烯和聚乙烯醇,球磨2h,得浆液;将浆液喷雾干燥造粒,造粒大小为80μm左右,含水率1.0%左右;造粒料过60目筛,加入聚乙烯蜡,在400MPa下压制成生坯;将生批放入高温真空烧结炉内,先以11℃/min左右的速度升温至1300℃,然后通入氩气,随后以70℃/min的速度加热至2100℃,保温烧结3h,得无压烧结碳化硅复合陶瓷。
实施例2
本实施例的碳化硅复合陶瓷制备方法中,原料为以下重量份成分:SiC:75份,TiB2:15份,B4C:10份,六偏磷酸钠:0.4份,酚醛树脂:6份,聚乙烯:1.5份,聚乙烯醇:5份,聚乙烯蜡:3份,聚酰亚胺:6份,水200份。
按照上述原料配比称取各成分,将SiC、TiB2、B4C、聚酰亚胺、六偏磷酸钠以及60%的水混合球磨6h,球磨机转速为100r/min,球磨后粒度为5μm左右;静置3h后,入蒸汽干燥箱中干燥;然后加入酚醛树脂以及剩余40%的水,继续球磨2h;加入聚乙烯和聚乙烯醇,球磨2h,得浆液;将浆液喷雾干燥造粒,造粒大小为80μm左右,含水率1.0%左右;造粒料过60目筛,加入聚乙烯蜡,在400MPa下压制成生坯;将生批放入高温真空烧结炉内,先以11℃/min左右的速度升温至1300℃,然后通入氩气,随后以70℃/min的速度加热至2100℃,保温烧结3h,得无压烧结碳化硅复合陶瓷。
实施例3
本实施例的碳化硅复合陶瓷制备方法中,原料为以下重量份成分:SiC:75份,TiB2:15份,B4C:10份,六偏磷酸钠:0.4份,酚醛树脂:6份,聚乙烯:1.5份,聚乙烯醇:5份,聚乙烯蜡:3份,聚酰亚胺:6份,水200份。
按照上述原料配比称取各成分,将SiC、TiB2、B4C、聚酰亚胺、六偏磷酸钠以及60%的水混合球磨6h,球磨机转速为100r/min,球磨后粒度为1μm左右;静置3h后,入蒸汽干燥箱中干燥;然后加入酚醛树脂以及剩余40%的水,继续球磨2h;加入聚乙烯和聚乙烯醇,球磨2h,得浆液;将浆液喷雾干燥造粒,造粒大小为200μm左右,含水率1.0%左右;造粒料过60目筛,加入聚乙烯蜡,在400MPa下压制成生坯;将生批放入高温真空烧结炉内,先以11℃/min左右的速度升温至1300℃,然后通入氩气,随后以70℃/min的速度加热至2100℃,保温烧结3h,得无压烧结碳化硅复合陶瓷。
实施例4
本实施例的碳化硅复合陶瓷制备方法中,原料为以下重量份成分:SiC:70份,TiB2:13份,B4C:6份,柠檬酸铵:0.3份,酚醛树脂:5份,聚乙烯:1份,聚乙烯醇:4份,微晶石蜡:2份,聚酰亚胺:5份,水150份。
按照上述原料配比称取各成分,将SiC、TiB2、B4C、聚酰亚胺、柠檬酸铵以及50%的水混合球磨5h,球磨机转速为200r/min,球磨后粒度为1μm左右;静置2h后,入蒸汽干燥箱中干燥;然后加入酚醛树脂以及剩余50%的水,继续球磨1h;加入聚乙烯和聚乙烯醇,球磨3h,得浆液;将浆液喷雾干燥造粒,造粒大小为50μm左右,含水率0.5%左右;造粒料过80目筛,加入微晶石蜡,在300MPa下压制成生坯;将生批放入高温真空烧结炉内,先以15℃/min左右的速度升温至1200℃,然后通入氩气,随后以60℃/min的速度加热至2000℃,保温烧结2h,得无压烧结碳化硅复合陶瓷。
实施例5
本实施例的碳化硅复合陶瓷制备方法中,原料为以下重量份成分:SiC:80份,TiB2:18份,B4C:10份,十二烷基硫酸钠:0.3份,酚醛树脂:8份,聚乙烯:2,聚乙烯醇:6份,硬脂酸盐锌:4份,聚酰亚胺:7份,水300。
按照上述原料配比称取各成分,将SiC、TiB2、B4C、聚酰亚胺、十二烷基硫酸钠以及60%的水混合球磨7h,球磨机转速为100r/min,球磨后粒度为1.2μm左右;静置4h后,入蒸汽干燥箱中干燥;然后加入酚醛树脂以及剩余40%的水,继续球磨3h;加入聚乙烯和聚乙烯醇,球磨2h,得浆液;将浆液喷雾干燥造粒,造粒大小为100μm左右,含水率1.5%左右;造粒料过60目筛,加入硬脂酸盐锌,在400MPa下压制成生坯;将生批放入高温真空烧结炉内,先以10℃/min左右的速度升温至1400℃,然后通入氩气,随后以90℃/min的速度加热至2200℃,保温烧结3h,得无压烧结碳化硅复合陶瓷。
对比例1
对比例1与实施例1的区别在于,对比例1的碳化硅陶瓷复合材料中没有包含聚酰亚胺,其它与实施例1相同。
对比例2
对比例1与实施例1的区别在于,对比例1的碳化硅陶瓷复合材料中聚酰亚胺与聚乙烯以及聚乙烯醇一起添加,其它与实施例1相同。
对比例3
对比例1与实施例1的区别在于,对比例1的碳化硅陶瓷复合材料中没有包含TiB2,其它与实施例1相同。
对比例4
对比例1与实施例1的区别在于,对比例1的碳化硅陶瓷复合材料中没有包含B4C,其它与实施例1相同。
对比例5
对比例1与实施例1的区别在于,对比例1的碳化硅陶瓷复合材料中没有包含TiB2和B4C,其它与实施例1相同。
对比例6
对比例1与实施例1的区别在于,对比例1的碳化硅陶瓷复合材料的无压烧结工艺为:以5℃/min左右的速度升温至1300℃,其它与实施例1相同。
对比例7
对比例1与实施例1的区别在于,对比例1的碳化硅陶瓷复合材料的无压烧结工艺为:以30℃/min左右的速度升温至1300℃,其它与实施例1相同。
将实施例1-5以及对比例1-7的碳化硅复合陶瓷进行性能测试,结果如表1所示。
表1
从表1可以看出,对比例1-7的密度和性能都要低于实施例1-5的碳化硅复合陶瓷,尤其是对比例1,因其复合材料中没有包括聚酰亚胺,呈现的性能显著低于实施例1-5,对比例3、对比例4和对比例5分别缺少TiB2、B4C以及TiB2和B4C成分,形成的陶瓷中无法形成SiC-TiB2-B4C复合相,弯曲强度、硬度等性能低于实施例1-5。而实施例1选用本发明实施例的较优参数,相对实施例2-5具有最优的性能。
本文中所描述的具体实施例仅仅是对本发明精神作举例说明。本发明所属技术领域的技术人员可以对所描述的具体实施例做各种修改或补充或采用类似的方式替代,但并不会偏离本发明的精神或者超越所附权利要求书所定义的范围。
Claims (7)
1.一种高性能无压烧结碳化硅复合陶瓷的制备方法,其特征在于,所述碳化硅复合陶瓷的制备原料包括以下重量份成分:
SiC:70-80份,TiB2:13-18份,B4C:5-12份,分散剂:0.3-0.5份,酚醛树脂:5-8份,聚乙烯:1-2份,聚乙烯醇:4-6份,脱模剂:2-5份,聚酰亚胺:5-7份,水150-300份;所述制备方法包括以下步骤:
(1)按照原料配比称取各成分,将SiC、TiB2、B4C、聚酰亚胺、分散剂以及40-60%的水混合球磨4-8h;
(2)静置1-5h后,入蒸汽干燥箱中干燥;
(3)加入酚醛树脂以及剩余40-60%的水,继续球磨1-3h;
(4)加入聚乙烯和聚乙烯醇,球磨1-3h,得浆液;
(5)将浆液喷雾干燥造粒;
(6)造粒料过50-100目筛,加入脱模剂,采用压制成型工艺制得生坯;
(7)将生坯放入高温真空烧结炉内,采用无压烧结工艺进行烧结。
2.根据权利要求1所述的制备方法,其特征在于,球磨机转速为50~500转/分钟,步骤(1)球磨后的粒度为0.1-2μm。
3.根据权利要求1所述的制备方法,其特征在于,所述喷雾干燥造粒大小为50-100μm,含水率0.5-1.5%。
4.根据权利要求1所述的制备方法,其特征在于,所述成型压力为300-500MPa。
5.根据权利要求1所述的制备方法,其特征在于,所述无压烧结工艺为:以10-15℃/min的速度升温至1200-1400℃,然后通入惰性气体,随后以≥50℃/min的速度加热至2000-2200℃,保温烧结2-4h。
6.根据权利要求1所述的制备方法,其特征在于,所述分散剂为六偏磷酸钠、聚丙烯酸铵、柠檬酸铵、十二烷基硫酸钠、四甲基氢氧化铵中的一种或多种。
7.根据权利要求1所述的制备方法,其特征在于,所述脱模剂为微晶石蜡、聚乙烯蜡、氮化硼、硬脂酸盐类、滑石粉、白粘土、云母中的一种或多种。
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Application publication date: 20190212 Assignee: Ningbo Chuangwei Machinery Co.,Ltd. Assignor: NINGBO DONGLIAN MECHANICAL SEAL Co.,Ltd. Contract record no.: X2023980053451 Denomination of invention: A preparation method for high-performance pressureless sintered silicon carbide composite ceramics Granted publication date: 20210205 License type: Common License Record date: 20231221 |