CN117700230A - 形状复杂的碳化硅陶瓷材料及其制备方法及其应用 - Google Patents
形状复杂的碳化硅陶瓷材料及其制备方法及其应用 Download PDFInfo
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 78
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 27
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 26
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 22
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims abstract description 22
- 239000000178 monomer Substances 0.000 claims abstract description 20
- 229910052580 B4C Inorganic materials 0.000 claims abstract description 13
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000919 ceramic Substances 0.000 claims abstract description 13
- 238000001272 pressureless sintering Methods 0.000 claims abstract description 13
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 12
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000465 moulding Methods 0.000 claims abstract description 11
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- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical group CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 14
- 235000015895 biscuits Nutrition 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- 238000005238 degreasing Methods 0.000 claims description 10
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
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- 229910052757 nitrogen Inorganic materials 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
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- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
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- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 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
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
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- 239000002270 dispersing agent Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
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- 239000011707 mineral Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000007569 slipcasting Methods 0.000 description 1
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Abstract
本发明属于陶瓷材料制备技术领域,涉及一种凝胶注模成型配合无压烧结制备形状复杂碳化硅陶瓷材料及其制备方法。该碳化硅陶瓷材料的原料由以下重量份的成分组成:W0.5碳化硅微粉(碳化硅无压微粉)90‑110份;W1.5碳化硼1‑5份;四甲基氢氧化铵0.4‑1.0份;单体A和单体B共8‑12份;甲叉双丙烯酰胺0.1‑0.5份;过硫酸铵0.04‑0.1份;四甲基乙二胺0.01‑0.1份;去离子水35‑45份。本发明使用未经处理的碳化硅粉,直接用于凝胶注模成型,整体工艺简单,操作性强,结合无压烧结可制备多种形状复杂致密度高的碳化硅陶瓷制件。
Description
技术领域
本发明属于陶瓷材料制备技术领域,涉及一种凝胶注模成型配合无压烧结制备形状复杂碳化硅陶瓷材料的制备方法。
背景技术
无压碳化硅作为一种结构陶瓷材料,相对于反应碳化硅未受内部颗粒间残余硅的影响,在强度、耐磨损、耐高温和耐腐蚀等物理化学性能上更有优势,使之在化工、冶炼、矿产、航天军工等领域应用广泛。
凝胶注模成形利用高分子单体聚合成形,使液态浆料转变成固态坯体的方法,结合相应陶瓷的烧结工艺可制备出常规压力成型无法得到的异形制件,且对于其他异形产品成型工艺,如注射成型、注浆成型、热压成型,具有工艺设备要求简单、有机物添加少,成型坯体密度强度高,产品壁厚大等特点,除碳化硅外可应用其他陶瓷材料中,如氧化铝、氧化锆、氮化硅等。
凝胶注模需要具有粘度低(小于1000mPa.s),分散性好,固化可控,固相含量较高的浆料,所以对原料用量和过程控制有一定要求。公开号为102875150B的中国申请专利公开了一种凝胶注模成型、无压烧结制备碳化硅陶瓷叶轮的方法,原料为预处理粉,即,将碳化硅粉末、炭黑粉末和碳化硼粉或硼粉加入到去离子水介质中,以丙三醇为分散剂,进行球磨混料、振动磨混料或者搅拌磨混料,料浆经真空烘干、破碎、过筛,或者喷雾干燥,获得混合均匀的混合粉末,浆料中引发剂和催化剂在真空脱泡中同时加入搅拌,易发生“暴聚”造成提前固化的可能。公开号为114988880B的中国申请专利公开了一种凝胶注模成型无压烧结制备碳化硅陶瓷的制备方法,以改性碳化硅粉为原料,浆料额外加入阻凝剂延长聚合的时间,而在注模前未进行真空易引入气泡。
上述预处理和改性均是为了增加碳化硅在浆料中的质量比即固相含量,以达到匹配该工艺的固相含量和分散性,另外还为了避免收缩大导致干燥开裂。因此属于必备的前处理工艺。
发明内容
本发明要解决的技术问题是提供一种形状复杂碳化硅陶瓷材料及其制备方法及其应用。
为解决上述技术问题,本发明提供一种可用于形状复杂的碳化硅陶瓷材料(碳化硅陶瓷制件),该碳化硅陶瓷材料的原料由以下重量份的成分组成:W0.5碳化硅微粉(碳化硅无压微粉)90-110份;W1.5碳化硼1-5份;四甲基氢氧化铵0.4-1.0份;单体A和单体B共8-12份;甲叉双丙烯酰胺0.1-0.5份;过硫酸铵0.04-0.1份;四甲基乙二胺0.01-0.1份;去离子水35-45份。
甲叉双丙烯酰胺作为交联剂,过硫酸铵作为引发剂,四甲基乙二胺作为催化剂。
作为本发明的可用于形状复杂的碳化硅陶瓷材料的改进:单体A为丙烯酰胺,单体B为甲基丙烯酸羟乙酯,单体A与B质量比为5~8:2~6。
本发明还提供了上述可用于形状复杂的碳化硅陶瓷材料的制备方法,包括以下步骤:
1)、预置液调配:
将单体A、甲叉双丙烯酰胺加入去离子水中,混合溶解,得预置液Ⅰ;将四甲基氢氧化铵及过硫酸铵加入去离子水中,混合溶解,得预置液Ⅱ,将四甲基乙二胺加入单体B中混合,得预置液Ⅲ;
2)、浆料搅拌及除泡:
在室温下,取(60±5)%预置溶液Ⅱ加入预置液Ⅰ中,再继续加入W0.5碳化硅微粉(碳化硅无压微粉)、W1.5碳化硼,机械搅拌1~5h进行分散(制得分散的混合物),之后加入剩余预置液Ⅱ搅拌1~5min,再继续加入预置液Ⅲ进行搅拌1~10min,接着改为真空搅拌2~10min从而实现脱泡(真空脱泡),得到碳化硅浆料;
步骤2)可在真空搅拌机下进行;
3)、素坯成型:
将步骤2)所得的碳化硅浆料注入模具中进行浆料浇注成型,在烘箱中进行加热固化,加热固化结束后脱模,所得素坯(素坯底部垫海绵)自然冷却至室温并于室温下放置一段时间,而后继续放入烘箱中分段加热干燥;
说明:模具可按照实际所需进行设置,从而获得复杂形状的制件;
4)、素坯脱脂:
将步骤3)所得物经过机加工成所需形状后放入脱胶炉中,或者将步骤3)所得物直接放入脱胶炉中,在惰性气体保护下(即,脱胶炉中通流动氮气或氩气等),升温至800~900℃保温1~3h进行脱脂;
5)、烧结:
将步骤4)所得物升温至2100~2200℃保温1~3h进行无压烧结,得到碳化硅陶瓷毛坯。
作为本发明的可用于形状复杂的碳化硅陶瓷材料的制备方法的改进:预置液Ⅰ中所用的去离子水:预置液Ⅱ所用的去离子水=8.8~9.2:0.8~1.2的质量比。
作为本发明的可用于形状复杂的碳化硅陶瓷材料的制备方法的进一步改进:所述步骤3)中:
所述加热固化的温度为40~80℃,时间为0.5~1.5小时;
冷却至室温后于室温下放置时间为6~24h;
分段加热干燥:升温至60±5℃保持4~12h,再升温至80±5℃保持4~12h,再升温至120±5℃保持4~12h。
作为本发明的可用于形状复杂的碳化硅陶瓷材料的制备方法的进一步改进:
所述步骤3)分段加热干燥中的升温速率为1~5℃/min;
步骤4)中的升温速率1~5℃/min;
步骤5)中的升温速率2~10℃/min。
作为本发明的可用于形状复杂的碳化硅陶瓷材料的制备方法的进一步改进:所述步骤2)中的搅拌速率为200~400r/min。
本发明是涉及一种凝胶注模成型配合无压烧结制备形状复杂碳化硅陶瓷材料的制备方法。本发明针对在真空脱泡过程浆料容易反应导致粘度增高的问题提供一种工艺简单,可操作性强,原料无需改性的无压碳化硅制备方法。本发明使用未经处理的碳化硅粉,直接用于凝胶注模成型,整体工艺简单,操作性强,结合无压烧结可制备多种形状复杂致密度高的碳化硅陶瓷制件。
本发明具有如下技术优势:
1、本发明使用两种单体,即,使用甲基丙烯酸羟乙酯部分替代丙烯酰胺,保证坯体成型和烧结稳定性下,减少有毒性的丙烯酰胺用量,同时延长注模前浆料凝胶时间,避免提前固化,从而顺利完成搅拌真空(脱泡)+浆料浇注成型这两个步骤;
2、本发明无需对碳化硅原料粉进行改性或预处理,原料及工艺简单,节约成本,可操作性强,适合小批量生产。
3、采用凝胶注模成型结合无压烧结方法,本发明素坯干燥收缩均匀,不易开裂,气孔率低,可生产出致密度高,外观良好的异形碳化硅陶瓷制品。
采用本发明方法,可制备密度大、强度高、形状复杂的碳化硅陶瓷制品,由于碳化硅材料具有耐腐蚀是特性,因此本发明可应用于制备形状复杂的例如叶轮的有耐腐蚀需求的构件。
附图说明
下面结合附图对本发明的具体实施方式作进一步详细说明。
图1为采用本发明的材料制备而得的碳化硅陶瓷叶轮制件;
图2为采用本发明的材料制备而得的碳化硅陶瓷异形制件(左右图分别代表正反面)。
具体实施方式
下面结合具体实施例对本发明进行进一步描述,但本发明的保护范围并不仅限于此:
W0.5、W1.5代表不同的粒度号,W0.5的粒径为0~0.5μm,W1.5的粒径为0.5~~1.5μm。此为本行业的常识。
实施例1、一种形状复杂碳化硅陶瓷材料的方法,依次进行以下步骤:
S1:按重量份称取,包括W0.5碳化硅微粉(碳化硅无压微粉)90份;W1.5碳化硼1份;四甲基氢氧化铵1.0份;丙烯酰胺5.6份;甲基丙烯酸羟乙酯2.4份;甲叉双丙烯酰胺0.5份;过硫酸铵0.1份;四甲基乙二胺0.01份;去离子水35份;
S2:将丙烯酰胺、甲叉双丙烯酰胺加入去离子水中,混合溶解,得预置液Ⅰ,将四甲基氢氧化铵及过硫酸铵加入去离子水中,混合溶解,得预置液Ⅱ,其中预置液Ⅰ中所用的去离子水:预置液Ⅱ所用的去离子水=9:1的质量比,将四甲基乙二胺加入甲基丙烯酸羟乙酯中混合,得预置液Ⅲ;
S3:在室温下,取60%预置液Ⅱ加入预置液Ⅰ中,继续加入碳化硅微粉、碳化硼,在转速为200r/min下,机械搅拌1h制得分散的混合物,之后加入剩余预置液Ⅱ搅拌1min,再继续加入预置溶液Ⅲ搅拌1min,最后改为真空搅拌3min从而实现真空脱泡,得到碳化硅浆料;
此步骤可在真空搅拌机下进行;
S4:将碳化硅浆料注入模具中进行浆料浇注成型,在烘箱内加热至80℃进行固化(约0.5小时),固化结束后脱模,所得素坯底部垫海绵,自然冷却至室温并室温放置24h,而后将素坯(连同海绵)继续放入烘箱中分段升温至60℃、80℃和120℃分别保温12h干燥;
S5:步骤S4干燥后所得物,按照实际所需,经过机加工成所需形状后放入脱胶炉中,或者直接放入脱胶炉中,通流动氮气下(即,于氮气保护下),以升温速率1℃/min,800℃保温1h进行脱脂;
S6:脱脂后,以2℃/min的升温速率加热到2100℃,保温1h进行无压烧结得到致密碳化硅毛坯。
实施例2、一种形状复杂碳化硅陶瓷材料的方法,依次进行以下步骤:
S1:按重量份称取,包括W0.5碳化硅微粉(碳化硅无压微粉)100份;W1.5碳化硼3份;四甲基氢氧化铵0.7份;丙烯酰胺6份;甲基丙烯酸羟乙酯4份;甲叉双丙烯酰胺0.25份;过硫酸铵0.04份;四甲基乙二胺0.055份;去离子水40份;
S2:将丙烯酰胺、甲叉双丙烯酰胺加入去离子水中,混合溶解,得预置液Ⅰ,将四甲基氢氧化铵及过硫酸铵加入去离子水中,混合溶解,得预置液Ⅱ,其中预置液Ⅰ中所用的去离子水:预置液Ⅱ所用的去离子水=9:1的质量比,将四甲基乙二胺加入甲基丙烯酸羟乙酯中混合,得预置液Ⅲ;
S3:在室温下,取60%预置液Ⅱ加入预置液Ⅰ中,继续加入碳化硅微粉、碳化硼,在转速为300r/min下,机械搅拌2.5h制得分散的混合物,之后加入剩余预置液Ⅱ搅拌2min,再继续加入预置溶液Ⅲ搅拌2min,最后改为真空搅拌6.5min从而实现真空脱泡,得到碳化硅浆料;
此步骤可在真空搅拌机下进行;
S4:将碳化硅浆料注入模具中进行浆料浇注成型,在烘箱内加热至60℃进行固化(约1.0小时),固化结束后脱模,所得素坯底部垫海绵,自然冷却至室温并室温放置15h,而后将素坯(连同海绵)继续放入烘箱中分段升温至60℃、80℃和120℃保温8h干燥;
S5:步骤S4干燥后所得物,按照实际所需,经过机加工成所需形状后放入脱胶炉中,或者直接放入脱胶炉中,通流动氮气下(即,于氮气保护下),以升温速率3℃/min,850℃保温1h进行脱脂;
S6:脱脂后,以6℃/min的升温速率加热到2150℃,保温2h进行无压烧结得到致密碳化硅毛坯。
实施例3、一种形状复杂碳化硅陶瓷材料的方法,依次进行以下步骤:
S1:按重量份称取,包括W0.5碳化硅微粉(碳化硅无压微粉)110份;W1.5碳化硼5份;四甲基氢氧化铵0.4份;丙烯酰胺6份;甲基丙烯酸羟乙酯6份;甲叉双丙烯酰胺0.5份;过硫酸铵0.07份;四甲基乙二胺0.1份;去离子水45份;
S2:将丙烯酰胺、甲叉双丙烯酰胺加入去离子水中,混合溶解,得预置液Ⅰ,将四甲基氢氧化铵及过硫酸铵加入去离子水中,混合溶解,得预置液Ⅱ,其中预置液Ⅰ中所用的去离子水:预置液Ⅱ所用的去离子水=9:1的质量比,将四甲基乙二胺加入甲基丙烯酸羟乙酯中混合,得预置液Ⅲ;
S3:在室温下,取60%预置液Ⅱ加入预置液Ⅰ中,继续加入碳化硅微粉、碳化硼,在转速为400r/min下,机械搅拌5h制得分散的混合物,之后加入剩余预置液Ⅱ搅拌3min,再继续加入预置溶液Ⅲ搅拌3min,最后改为真空搅拌10min从而实现真空脱泡,得到碳化硅浆料;
此步骤可在真空搅拌机下进行;
S4:将碳化硅浆料注入模具中进行浆料浇注成型,在烘箱内加热至40℃进行固化(约1.5小时),固化结束后脱模,所得素坯底部垫海绵,自然冷却至室温并室温放置6h,而后将素坯(连同海绵)继续放入烘箱中分段升温至60℃、80℃和120℃保温4h干燥;
S5:步骤S4干燥后所得物,按照实际所需,经过机加工成所需形状后放入脱胶炉中,或者直接放入脱胶炉中,通流动氮气下(即,于氮气保护下),以升温速率5℃/min,900℃保温2h进行脱脂;
S6:脱脂后,以10℃/min的升温速率加热到2200℃,保温3h进行无压烧结得到致密碳化硅毛坯。
将上述实施例1-3所碳化硅陶瓷制备过程中测试数据和结果如表1所示。
表1测试数据
对比例1、将实施例2中的“丙烯酰胺6份;甲基丙烯酸羟乙酯4份”改成“丙烯酰胺4份;甲基丙烯酸羟乙酯6份”,即甲基丙烯酸羟乙酯高于丙烯酰胺,而两者的总用量保持不变,其余等同于实施例2。
测试数据和结果如上表1所示。
对比例2、将实施例2中的“丙烯酰胺6份;甲基丙烯酸羟乙酯4份”改成“丙烯酰胺10份;甲基丙烯酸羟乙酯0份”,即两者的总用量保持不变,其余等同于实施例2。
测试数据和结果如上表1所示。
对比例3、取消实施例2的步骤S2、S3,改为如下:将步骤S1称取的成分混合。粉末聚结,无法制成浆料,因此无法进行后续步骤。
对比例4、将实施例2的步骤S3改为:
S3:在室温下,将预置液Ⅰ、预置液Ⅱ、预置溶液Ⅲ、碳化硅微粉、碳化硼混合后机械搅拌2.6h,再改为真空搅拌6.5min从而实现真空脱泡,得到碳化硅浆料;其余等同于实施例2。
测试数据和结果如上表1所示。
最后,还需要注意的是,以上列举的仅是本发明的若干个具体实施例。显然,本发明不限于以上实施例,还可以有许多变形。本领域的普通技术人员能从本发明公开的内容直接导出或联想到的所有变形,均应认为是本发明的保护范围。
Claims (7)
1.可用于形状复杂的碳化硅陶瓷材料,其特征在于:该碳化硅陶瓷材料的原料由以下重量份的成分组成:W0.5碳化硅微粉90-110份;W1.5碳化硼1-5份;四甲基氢氧化铵0.4-1.0份;单体A和单体B共8-12份;甲叉双丙烯酰胺0.1-0.5份;过硫酸铵0.04-0.1份;四甲基乙二胺0.01-0.1份;去离子水35-45份。
2.根据权利要求1所述的可用于形状复杂的碳化硅陶瓷材料,其特征在于:单体A为丙烯酰胺,单体B为甲基丙烯酸羟乙酯,单体A与B质量比为5~8:2~6。
3.如权利要求1或2的可用于形状复杂的碳化硅陶瓷材料的制备方法,其特征在于包括以下步骤:
1)、预置液调配:
将单体A、甲叉双丙烯酰胺加入去离子水中,混合溶解,得预置液Ⅰ;将四甲基氢氧化铵及过硫酸铵加入去离子水中,混合溶解,得预置液Ⅱ,将四甲基乙二胺加入单体B中混合,得预置液Ⅲ;
2)、浆料搅拌及除泡:
在室温下,取(60±5)%预置溶液Ⅱ加入预置液Ⅰ中,再继续加入W0.5碳化硅无压微粉、W1.5碳化硼,搅拌1~5h进行分散,之后加入剩余预置液Ⅱ搅拌1~5min,再继续加入预置液Ⅲ进行搅拌1~10min,接着改为真空搅拌2~10min从而实现脱泡,得到碳化硅浆料;
3)、素坯成型:
将步骤2)所得的碳化硅浆料注入模具中进行浆料浇注成型,在烘箱中进行加热固化,加热固化结束后脱模,所得素坯自然冷却至室温并于室温下放置,而后继续放入烘箱中分段加热干燥;
4)、素坯脱脂:
将步骤3)所得物经过机加工成所需形状后放入脱胶炉中,或者将步骤3)所得物直接放入脱胶炉中,在惰性气体保护下,升温至800~900℃保温1~3h进行脱脂;
5)、烧结:
将步骤4)所得物升温至2100~2200℃保温1~3h进行无压烧结,得到碳化硅陶瓷毛坯。
4.根据权利要求3所述的可用于形状复杂的碳化硅陶瓷材料的制备方法,其特征在于:预置液Ⅰ中所用的去离子水:预置液Ⅱ所用的去离子水=8.8~9.2:0.8~1.2的质量比。
5.根据权利要求3或4所述的可用于形状复杂的碳化硅陶瓷材料的制备方法,其特征在于:所述步骤3)中:
所述加热固化的温度为40~80℃,时间为0.5~1.5小时;
冷却至室温后于室温下放置时间为6~24h;
分段加热干燥:升温至60±5℃保持4~12h,再升温至80±5℃保持4~12h,再升温至120±5℃保持4~12h。
6.根据权利要求5所述的可用于形状复杂的碳化硅陶瓷材料的制备方法,其特征在于:
步骤4)中的升温速率1~5℃/min;
步骤5)中的升温速率2~10℃/min。
7.根据权利要求6所述的可用于形状复杂的碳化硅陶瓷材料的制备方法,其特征在于:所述步骤2)中的搅拌速率为200~400r/min。
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