CN113213942A - 一种复合碳化硅陶瓷窑具及其制备方法 - Google Patents
一种复合碳化硅陶瓷窑具及其制备方法 Download PDFInfo
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- CN113213942A CN113213942A CN202110574984.4A CN202110574984A CN113213942A CN 113213942 A CN113213942 A CN 113213942A CN 202110574984 A CN202110574984 A CN 202110574984A CN 113213942 A CN113213942 A CN 113213942A
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- silicon carbide
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- kiln furniture
- oxide
- sisic
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 159
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 137
- 239000000919 ceramic Substances 0.000 title claims abstract description 60
- 239000002131 composite material Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 42
- 238000001035 drying Methods 0.000 claims abstract description 40
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000002002 slurry Substances 0.000 claims abstract description 31
- 239000011230 binding agent Substances 0.000 claims abstract description 23
- 239000000654 additive Substances 0.000 claims abstract description 20
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 19
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 230000000996 additive effect Effects 0.000 claims abstract description 15
- 239000004202 carbamide Substances 0.000 claims abstract description 11
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910016384 Al4C3 Inorganic materials 0.000 claims abstract description 10
- 238000004381 surface treatment Methods 0.000 claims abstract description 8
- 239000001095 magnesium carbonate Substances 0.000 claims abstract description 7
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims description 50
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 33
- 238000003756 stirring Methods 0.000 claims description 26
- 238000000498 ball milling Methods 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 20
- 239000000377 silicon dioxide Substances 0.000 claims description 17
- 235000012239 silicon dioxide Nutrition 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 16
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 15
- 239000004408 titanium dioxide Substances 0.000 claims description 15
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 10
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 9
- 239000007822 coupling agent Substances 0.000 claims description 9
- 229910052708 sodium Inorganic materials 0.000 claims description 9
- 239000011734 sodium Substances 0.000 claims description 9
- 235000015895 biscuits Nutrition 0.000 claims description 8
- 238000001746 injection moulding Methods 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- -1 oleoyl diethanol amine Chemical compound 0.000 claims description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 7
- 229940043237 diethanolamine Drugs 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- BITAPBDLHJQAID-KTKRTIGZSA-N 2-[2-hydroxyethyl-[(z)-octadec-9-enyl]amino]ethanol Chemical compound CCCCCCCC\C=C/CCCCCCCCN(CCO)CCO BITAPBDLHJQAID-KTKRTIGZSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 230000035939 shock Effects 0.000 abstract description 22
- 230000003647 oxidation Effects 0.000 abstract description 11
- 238000007254 oxidation reaction Methods 0.000 abstract description 11
- 239000011819 refractory material Substances 0.000 abstract description 4
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- 229910052814 silicon oxide Inorganic materials 0.000 abstract 1
- 238000007569 slipcasting Methods 0.000 abstract 1
- 238000001816 cooling Methods 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 2
- 235000014380 magnesium carbonate Nutrition 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Abstract
本发明公开一种复合碳化硅陶瓷窑具及其制备方法,涉及耐火材料技术领域。本发明公开的复合碳化硅陶瓷窑具,是由以下重量份数的原料组成:反应烧结碳化硅40~60份、氧化物结合碳化硅28~54份、莫来石6~12份、氧化钇1.5~3份、添加剂5~8份、粘结剂3~6份、烧结助剂5~10份和水10~15份,所述添加剂为尿素和MgCO3,所述烧结助剂为B4C和Al4C3;其制备方法为:将反应烧结碳化硅进行表面处理,然后将各组分混合得浆料,注浆成型,脱模,干燥,烧结即得。本发明提供的复合碳化硅陶瓷窑具具有优异的强度、韧性、抗热震性和高温抗氧化性,其使用温度较高,延长了窑具的使用寿命。
Description
技术领域
本发明属于耐火材料技术领域,尤其涉及复合碳化硅陶瓷窑具及其制备方法。
背景技术
窑具是一种高级耐火材料,是用耐火土制成的在焙烧过程中对坯件起间隔、支托、承垫、保护等作用的器具,其质量好坏为烧成制品的质量、生产成本有着直接的影响。随着磁性材料、电子陶瓷等新型功能陶瓷的迅速发展,对窑具的品质要求也越来越高,而窑具属于消耗品,则要求窑具的材料应具备较高的耐火度、良好的热稳定性,较高的常温和高温强度,必须经受的起制品及窑具本身的负荷,良好的导热性、低蓄热性、抗热震性和抗氧化性能。自上世纪80年代以来,国内外推行陶瓷快速烧结技术,碳化硅陶瓷成为了快速烧结窑炉用高温窑具的首先材料。
碳化硅质窑具的热膨胀系数小,尤其是其热导率高,热震稳定性好,而且在高温下不产生形变。但与其他氧化物高温窑具相比,碳化硅质窑具的高温氧化性问题突出,高温氧化产物方石英会发生体积膨胀,使窑具结构疏松,以致产生裂纹而直接影响窑具的使用寿命和质量。而反应烧结碳化硅(SiSiC)继承了碳化硅的优点,自身又有低烧结温度、高致密度等优点,适于制备大尺寸、复杂形状陶瓷构件。目前在碳化硅质窑具材料中,反应烧结碳化硅的抗氧化性最好,且具有良好的耐磨性和导热性,但也存在一些问题:由于反应烧结碳化硅中存在游离硅,若使用温度接近或高于1410℃,其断裂强度将会因游离硅的软化或熔化而降低。
碳化硅窑具具有优良的高温性能,用以烧成高质量的陶瓷制品,由于SiC是共价键化合物,烧结温度高达2000℃以上,在一般窑炉中难于烧结,制品的致密化程度低,要作为耐火材料使用,必须采用结合剂结合,而窑具的使用寿命与结合剂的性能有关。根据结合剂的不同,目前碳化硅窑具的结合方式分为氧化物结合和非氧化物结合,而氧化物结合包括粘土结合、二氧化硅结合和莫来石结合,非氧化物结合包括自结合SiC、塞隆结合、氮化硅结合、氧氮化硅结合等。而目前应用最广、价格低廉的是氧化物结合碳化硅,其生产工艺简单,烧结温度较低,具有优良的抗热震性,但是使用温度较低,高温性能较差,影响了窑具的使用寿命。
发明内容
本发明主要目的是提供一种复合碳化硅陶瓷窑具及其制备方法,该窑具具有优异的强度、韧性、抗热震性和高温抗氧化性,其使用温度较高,延长了窑具的使用寿命。
为了实现本发明的目的,本发明提供了一种复合碳化硅陶瓷窑具,是由以下重量份数的原料组成:反应烧结碳化硅40~60份、氧化物结合碳化硅28~54份、莫来石6~12份、氧化钇1.5~3份、添加剂5~8份、粘结剂3~6份、烧结助剂5~10份和水10~15份,所述反应烧结碳化硅、莫来石和氧化物结合碳化硅的总组分以100重量份数计;
所述添加剂为尿素和MgCO3,所述烧结助剂为B4C和Al4C3。
进一步的,所述尿素和MgCO3的质量比为(2.5~3.3):1。
进一步的,所述粘结剂为聚乙烯醇和硅溶胶,其质量比为(0.5~1):(1~0.5)。
进一步的,所述B4C和Al4C3的质量比为(2~4):1。
进一步的,所述氧化物结合碳化硅是以复合氧化物结合碳化硅制得的。
进一步的,所述氧化物结合碳化硅的重量份数组成为:碳化硅82~90份、二氧化硅5~10份、三氧化二铝3~5份和二氧化钛2~3份,即复合氧化物为二氧化硅、三氧化二铝和二氧化钛。
进一步的,所述碳化硅为碳化硅颗粒和碳化硅细粉的混合物,所述碳化硅颗粒与所述碳化硅细粉的质量比为1:0.8;
所述碳化硅颗粒的粒径为0.1~0.2mm,所述碳化硅细粉的粒径≤50μm;
所述复合氧化物的粒径均≤50μm。
本发明复合碳化硅陶瓷窑具的制备方法,具体包括以下步骤:
(1)反应烧结碳化硅的表面处理:在反应釜中加入质量比为1:0.5的反应烧结碳化硅和去离子水,搅拌均匀,升温至80℃,然后加入锆酸酯偶联剂,搅拌反应1-1.5h,再加入油酰二乙醇胺和腐殖酸钠,在此温度继续反应2-3h,过滤,干燥,球磨,得改性后的SiSiC;
(2)将氧化物结合碳化硅、莫来石和氧化钇混合均匀,球磨,过筛200目后,加入到上述改性后的SiSiC和粘结剂中,搅拌0.5h,然后加入烧结助剂、添加剂和水混合,搅拌3-4h,制得浆料;
(3)将上述浆料注入到模具中,注浆成型后的素坯阴干48h后脱模,于干燥箱中进行干燥,干燥后含水量≤1%,获得坯料;
(4)将上述坯料置于高温窑炉中,升温至600℃,保温1h,然后再升温至1400~1450℃,保温4~7h,即得复合碳化硅陶瓷窑具。
进一步的,所述步骤(1)中球磨速率为320~350r/min,球磨的改性后的SiSiC的粒径≤100μm。
进一步的,所述步骤(1)中所述锆酸酯偶联剂的质量为所述SiSiC质量的0.3~0.42%,所述油酰二乙醇胺的质量为所述SiSiC质量的0.12~0.18%,所述腐殖酸钠的质量为所述SiSiC质量的0.6~0.8%。
本发明取得了以下有益效果:
1、本发明使用SiSiC和氧化物结合碳化硅作为主要原料,使陶瓷窑具的烧结温度较低,降低了生产成本,并有还具有较高的致密度,较好的抗氧化性、耐磨性和导热性。
2、本发明中加入莫来石,莫来石的线膨胀系数和碳化硅的接近,能使莫来石和SiSiC、氧化物结合碳化硅之间结合力很好,使陶瓷窑具有很好的致密度,提高了陶瓷窑具的力学性能,并且提高了陶瓷窑具的高温抗氧化性、抗热震稳定性和使用温度。
3、本发明的添加剂为尿素和MgCO3的组合物,尿素在高温条件下热分解,为SiSiC中的游离硅提供C和N,高温反应生成SiC和SiN,提高了陶瓷窑具的致密度和使用温度,使其在高于1400℃下不易软化或熔化,进一步增强了陶瓷窑具的强度和韧性;MgCO3的加入,可进一步降低陶瓷窑具的烧结温度,促进陶瓷窑具中的莫来石生长,从而使陶瓷窑具的致密度进一步提高,增强了陶瓷窑具的强度和韧性。
4、本发明中加入氧化钇,可与SiSiC表面的SiO2、氧化物结合碳化硅中的SiO2和Al2O3以及莫来石中的组分,在高温下反应形成液相,提高了各组分之间的界面结合力,使各组分间分散更加的均匀,促进本发明的烧结致密度,从而增强了陶瓷窑具的强度和韧性。
5、本发明的粘结剂为聚乙烯醇和硅溶胶的复配物,该复配物提高了陶瓷窑具各有机组分和无机组分间的结合力,提高了浆料体系的稳定性,消除表面起皮和开裂现象,并且陶瓷窑具的力学性能和抗热震性有很大程度的提高。
6、本发明在陶瓷窑具的制备过程中,对SiSiC进行表面处理,提高了SiSiC与其它组分间的界面结合力,使SiSiC能更加均匀的分散在浆料之中,促进了陶瓷窑具的烧结致密化;采用锆酸酯偶联剂、油酰二乙醇胺和腐殖酸钠对SiSiC进行表面改性,可使浆料的粘度降低,使SiSiC更易均匀分散在浆料中,从而使坯料内部致密、均匀、有很少的小气孔,提高陶瓷窑具的致密度、力学强度和高温使用性能;高温烧结过程中分解出的氧化锆和氧化物结合碳化硅中的氧化钛形成固溶体,稳定碳化硅的晶型,抑制碳化硅晶粒的长大,并加快气孔的排出,促进其烧结。
7、本发明的氧化物结合碳化硅是以碳化硅为主要原料,二氧化硅、三氧化二铝和二氧化钛为结合剂,该复合氧化物的加入,提高了碳化硅的活性,使表面积大,在高温下可促进窑具的烧结,使氧化物结合碳化硅的抗氧化性、热导性、抗热震性和高温强度均可大幅度提高,从而进一步提高了本发明的抗氧化性、热导性、抗热震性和高温强度。
8、本发明的制备方法简单,易操作,可在1400~1450℃的温度下烧结,降低了生产成本;本发明具有高温抗氧化性、抗热震性,并提升了窑具的使用温度,可在1500℃的高温中使用,其寿命是同类SiSiC制品的两倍;本发明的制备过程中,在600℃保温1h,可使坯料中有机成分分解,从而提高了陶瓷窑具的致密度。
具体实施方式
下面对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。
本发明的实施例中氧化物结合碳化硅的制备方法为:将单体丙烯酰胺、N,N-二甲基双丙烯酰胺和去离子水混合均匀;然后加入0.1~0.2mm的碳化硅颗粒、粒径≤50μm的碳化硅细粉、粒径≤50μm的SiO2、Al2O3和TiO2复合氧化物,混合均匀,球磨,制得浆料;往浆料中加入过硫酸铵,在60~70℃搅拌2~3h,再进行真空脱泡处理;注入到模具中,注浆成型,阴干,脱模,自然干燥后,于1400℃烧结,制得氧化物结合碳化硅。
实施例1
一种复合碳化硅陶瓷窑具的制备方法包括以下步骤:
(1)将60份SiSiC(粒径≤100μm)、28份氧化物结合碳化硅、12份莫来石和1.5份氧化钇混合均匀,球磨,过筛200目后,加入6份粘结剂,搅拌0.5h,然后加入10份烧结助剂、8份添加剂和10份水混合,搅拌3-4h,制得浆料。
(2)将上述浆料注入到模具中,注浆成型后的素坯阴干48h后脱模,于干燥箱中进行干燥,干燥后含水量≤1%,获得坯料。
(3)将上述坯料置于高温窑炉中,升温至600℃,保温1h,然后再升温至1400~1450℃,保温4~7h,即得复合碳化硅陶瓷窑具。
上述加入的添加剂为质量比为3.3:1的尿素和MgCO3。烧结助剂为质量比为2:1的B4C和Al4C3。粘结剂为质量比为1:1的聚乙烯醇和硅溶胶。
上述的氧化物结合碳化硅是以复合氧化物结合碳化硅制得的,其重量份数组成为:碳化硅82份、二氧化硅10份、三氧化二铝5份和二氧化钛3份,即复合氧化物为二氧化硅、三氧化二铝和二氧化钛。该碳化硅为碳化硅颗粒和碳化硅细粉的混合物,碳化硅颗粒与碳化硅细粉的质量比为1:0.8,碳化硅颗粒的粒径为0.1~0.2mm,碳化硅细粉的粒径≤50μm,复合氧化物的粒径均≤50μm。
经测试,本实施例制品的性能指标为:
体积密度2.76g/cm3,常温耐压强度206.9MPa,常温抗折强度58.8MPa,耐蠕变性0.7mm,耐热冲击温度800℃,热震稳定性100℃水冷42次,1500℃使用89次。
实施例2
一种复合碳化硅陶瓷窑具的制备方法包括以下步骤:
(1)SiSiC的表面处理:在反应釜中加入40份SiSiC和20份去离子水,搅拌均匀,升温至80℃,然后加入0.12份锆酸酯偶联剂,搅拌反应1-1.5h,再加入0.072份油酰二乙醇胺和0.32份腐殖酸钠,在此温度继续反应2-3h,过滤,干燥,球磨,球磨速率为320~350r/min,球磨后的粒径≤100μm,得改性后的SiSiC。
(2)将54份氧化物结合碳化硅、6份莫来石和3份氧化钇混合均匀,球磨,过筛200目后,加入到上述改性后的SiSiC和3份粘结剂中,搅拌0.5h,然后加入8份烧结助剂、5份添加剂和15份水混合,搅拌3-4h,制得浆料。
(3)将上述浆料注入到模具中,注浆成型后的素坯阴干48h后脱模,于干燥箱中进行干燥,干燥后含水量≤1%,获得坯料。
(4)将上述坯料置于高温窑炉中,升温至600℃,保温1h,然后再升温至1400~1450℃,保温4~7h,即得复合碳化硅陶瓷窑具。
上述加入的添加剂为质量比为2.5:1的尿素和MgCO3。烧结助剂为质量比为3:1的B4C和Al4C3。粘结剂为质量比为2:1的聚乙烯醇和硅溶胶。
上述的氧化物结合碳化硅是以复合氧化物结合碳化硅制得的,其重量份数组成为:碳化硅90份、二氧化硅5份、三氧化二铝3份和二氧化钛2份,即复合氧化物为二氧化硅、三氧化二铝和二氧化钛。该碳化硅为碳化硅颗粒和碳化硅细粉的混合物,碳化硅颗粒与碳化硅细粉的质量比为1:0.8,碳化硅颗粒的粒径为0.1~0.2mm,碳化硅细粉的粒径≤50μm,复合氧化物的粒径均≤50μm。
经测试,本实施例制品的性能指标为:
体积密度2.8g/cm3,常温耐压强度208MPa,常温抗折强度56MPa,耐蠕变性0.5mm,耐热冲击温度811℃,热震稳定性100℃水冷51次,1500℃使用91次。
实施例3
一种复合碳化硅陶瓷窑具的制备方法包括以下步骤:
(1)SiSiC的表面处理:在反应釜中加入50份SiSiC和25份去离子水,搅拌均匀,升温至80℃,然后加入0.21份锆酸酯偶联剂,搅拌反应1-1.5h,再加入0.06份油酰二乙醇胺和0.3份腐殖酸钠,在此温度继续反应2-3h,过滤,干燥,球磨,球磨速率为320~350r/min,球磨后的粒径≤100μm,得改性后的SiSiC。
(2)将43份氧化物结合碳化硅、7份莫来石和2.4份氧化钇混合均匀,球磨,过筛200目后,加入到上述改性后的SiSiC和4.5份粘结剂中,搅拌0.5h,然后加入5份烧结助剂、6.7份添加剂和12份水混合,搅拌3-4h,制得浆料。
(3)将上述浆料注入到模具中,注浆成型后的素坯阴干48h后脱模,于干燥箱中进行干燥,干燥后含水量≤1%,获得坯料。
(4)将上述坯料置于高温窑炉中,升温至600℃,保温1h,然后再升温至1400~1450℃,保温4~7h,即得复合碳化硅陶瓷窑具。
上述加入的添加剂为质量比为3:1的尿素和MgCO3。烧结助剂为质量比为4:1的B4C和Al4C3。粘结剂为质量比为1:2的聚乙烯醇和硅溶胶。
上述的氧化物结合碳化硅是以复合氧化物结合碳化硅制得的,其重量份数组成为:碳化硅86份、二氧化硅8份、三氧化二铝4份和二氧化钛2份,即复合氧化物为二氧化硅、三氧化二铝和二氧化钛。该碳化硅为碳化硅颗粒和碳化硅细粉的混合物,碳化硅颗粒与碳化硅细粉的质量比为1:0.8,碳化硅颗粒的粒径为0.1~0.2mm,碳化硅细粉的粒径≤50μm,复合氧化物的粒径均≤50μm。
经测试,本实施例制品的性能指标为:
体积密度2.79g/cm3,常温耐压强度205MPa,常温抗折强度56.1MPa,耐蠕变性0.6mm,耐热冲击温度812℃,热震稳定性100℃水冷49次,1500℃使用90次。
实施例4
一种复合碳化硅陶瓷窑具的制备方法包括以下步骤:
(1)SiSiC的表面处理:在反应釜中加入46份SiSiC和23份去离子水,搅拌均匀,升温至80℃,然后加入0.184份锆酸酯偶联剂,搅拌反应1-1.5h,再加入0.069份油酰二乙醇胺和0.322份腐殖酸钠,在此温度继续反应2-3h,过滤,干燥,球磨,球磨速率为320~350r/min,球磨后的粒径≤100μm,得改性后的SiSiC。
(2)将48份氧化物结合碳化硅、6份莫来石和1.8份氧化钇混合均匀,球磨,过筛200目后,加入到上述改性后的SiSiC和5.4份粘结剂中,搅拌0.5h,然后加入7份烧结助剂、7.3份添加剂和15份水混合,搅拌3-4h,制得浆料。
(3)将上述浆料注入到模具中,注浆成型后的素坯阴干48h后脱模,于干燥箱中进行干燥,干燥后含水量≤1%,获得坯料。
(4)将上述坯料置于高温窑炉中,升温至600℃,保温1h,然后再升温至1400~1450℃,保温4~7h,即得复合碳化硅陶瓷窑具。
上述加入的添加剂为质量比为2.8:1的尿素和MgCO3。烧结助剂为质量比为3.2:1的B4C和Al4C3。粘结剂为质量比为3:4的聚乙烯醇和硅溶胶。
上述的氧化物结合碳化硅是以复合氧化物结合碳化硅制得的,其重量份数组成为:碳化硅86份、二氧化硅8份、三氧化二铝4份和二氧化钛2份,即复合氧化物为二氧化硅、三氧化二铝和二氧化钛。该碳化硅为碳化硅颗粒和碳化硅细粉的混合物,碳化硅颗粒与碳化硅细粉的质量比为1:0.8,碳化硅颗粒的粒径为0.1~0.2mm,碳化硅细粉的粒径≤50μm,复合氧化物的粒径均≤50μm。
经测试,本实施例制品的性能指标为:
体积密度3.53g/cm3,常温耐压强度204MPa,常温抗折强度55.5MPa,耐蠕变性0.5mm,耐热冲击温度816℃,热震稳定性100℃水冷53次,1500℃使用87次。
实施例5
一种复合碳化硅陶瓷窑具的制备方法包括以下步骤:
(1)SiSiC的表面处理:在反应釜中加入55份SiSiC和28份去离子水,搅拌均匀,升温至80℃,然后加入0.187份锆酸酯偶联剂,搅拌反应1-1.5h,再加入0.088份油酰二乙醇胺和0.418份腐殖酸钠,在此温度继续反应2-3h,过滤,干燥,球磨,球磨速率为320~350r/min,球磨后的粒径≤100μm,得改性后的SiSiC。
(2)将35份氧化物结合碳化硅、10份莫来石和2份氧化钇混合均匀,球磨,过筛200目后,加入到上述改性后的SiSiC和3.9份粘结剂中,搅拌0.5h,然后加入7.5份烧结助剂、6.1份添加剂和12份水混合,搅拌3-4h,制得浆料。
(3)将上述浆料注入到模具中,注浆成型后的素坯阴干48h后脱模,于干燥箱中进行干燥,干燥后含水量≤1%,获得坯料。
(4)将上述坯料置于高温窑炉中,升温至600℃,保温1h,然后再升温至1400~1450℃,保温4~7h,即得复合碳化硅陶瓷窑具。
上述加入的添加剂为质量比为2.6:1的尿素和MgCO3。烧结助剂为质量比为2.5:1的B4C和Al4C3。粘结剂为质量比为1:1的聚乙烯醇和硅溶胶。
上述的氧化物结合碳化硅是以复合氧化物结合碳化硅制得的,其重量份数组成为:碳化硅90份、二氧化硅5份、三氧化二铝3份和二氧化钛2份,即复合氧化物为二氧化硅、三氧化二铝和二氧化钛。该碳化硅为碳化硅颗粒和碳化硅细粉的混合物,碳化硅颗粒与碳化硅细粉的质量比为1:0.8,碳化硅颗粒的粒径为0.1~0.2mm,碳化硅细粉的粒径≤50μm,复合氧化物的粒径均≤50μm。
经测试,本实施例制品的性能指标为:
体积密度3.02g/cm3,常温耐压强度280MPa,常温抗折强度250MPa,耐蠕变性0.3mm,耐热冲击温度820℃,热震稳定性100℃水冷60次,1500℃使用280次。
对比例1
本对比例使用河南四成研磨科技有限公司型号为24-3000#的反应烧结用绿碳化硅制得碳化硅陶瓷窑具,其制备方法为:
(1)将100份SiSiC球磨,过筛200目后,加入3.9份粘结剂聚乙烯醇,搅拌0.5h,然后加入7.5份烧结助剂B4C、6.1份添加剂MgCO3和12份水混合,搅拌3-4h,制得浆料。
(2)将上述浆料注入到模具中,注浆成型后的素坯阴干48h后脱模,于干燥箱中进行干燥,干燥后含水量≤1%,获得坯料。
(3)将上述坯料置于高温窑炉中,升温至600℃,保温1h,然后再升温至1400~1450℃,保温4~7h,即得碳化硅陶瓷窑具。
经测试,本实施例制品的性能指标为:
体积密度2.43g/cm3,常温耐压强度262MPa,常温抗折强度208MPa,耐蠕变性0.9mm,耐热冲击温度680℃,热震稳定性100℃水冷19次,使用温度<1400℃。
以上所述实施例的各技术特征可以进行任意组合,为使描述简洁,未对上述实施例中的各个技术特征所有可能的组合都进行描述,然而,只要这些技术特征的组合不存在矛盾,都应当认为是本说明书记载的范围。
以上所述实施例仅表达了本发明的几种实施方式,其描述较为具体和详细,但并不能因此而理解为对本发明专利范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。
Claims (10)
1.一种复合碳化硅陶瓷窑具,其特征在于,是由以下重量份数的原料组成:SiSiC 40~60份、氧化物结合碳化硅28~54份、莫来石6~12份、氧化钇1.5~3份、添加剂5~8份、粘结剂3~6份、烧结助剂5~10份和水10~15份,所述SiSiC、莫来石和氧化物结合碳化硅的总组分以100重量份数计;
所述添加剂为尿素和MgCO3,所述烧结助剂为B4C和Al 4C3。
2.根据权利要求1所述的复合碳化硅陶瓷窑具,其特征在于,所述尿素和MgCO3的质量比为(2.5~3.3):1。
3.根据权利要求1所述的复合碳化硅陶瓷窑具,其特征在于,所述粘结剂为聚乙烯醇和硅溶胶,其质量比为(0.5~1):(1~0.5)。
4.根据权利要求1所述的复合碳化硅陶瓷窑具,其特征在于,所述B4C和Al 4C3的质量比为(2~4):1。
5.根据权利要求1所述的复合碳化硅陶瓷窑具,其特征在于,所述氧化物结合碳化硅是以复合氧化物结合碳化硅制得的。
6.根据权利要求5所述的复合碳化硅陶瓷窑具,其特征在于,所述氧化物结合碳化硅的重量份数组成为:碳化硅82~90份、二氧化硅5~10份、三氧化二铝3~5份和二氧化钛2~3份,即复合氧化物为二氧化硅、三氧化二铝和二氧化钛。
7.根据权利要求6所述的复合碳化硅陶瓷窑具,其特征在于,所述碳化硅为碳化硅颗粒和碳化硅细粉的混合物,所述碳化硅颗粒与所述碳化硅细粉的质量比为1:0.8;
所述碳化硅颗粒的粒径为0.1~0.2mm,所述碳化硅细粉的粒径≤50μm;
所述复合氧化物的粒径均≤50μm。
8.如权利要求1-7所述任一项的复合碳化硅陶瓷窑具的制备方法,其特征在于,具体包括以下步骤:
(1)SiSiC的表面处理:在反应釜中加入质量比为1:0.5的SiSiC和去离子水,搅拌均匀,升温至80℃,然后加入锆酸酯偶联剂,搅拌反应1-1.5h,再加入油酰二乙醇胺和腐殖酸钠,在此温度继续反应2-3h,过滤,干燥,球磨,得改性后的SiSiC;
(2)将氧化物结合碳化硅、莫来石和氧化钇混合均匀,球磨,过筛200目后,加入到上述改性后的SiSiC和粘结剂中,搅拌0.5h,然后加入烧结助剂、添加剂和水混合,搅拌3-4h,制得浆料;
(3)将上述浆料注入到模具中,注浆成型后的素坯阴干48h后脱模,于干燥箱中进行干燥,干燥后含水量≤1%,获得坯料;
(4)将上述坯料置于高温窑炉中,升温至600℃,保温1h,然后再升温至1400~1450℃,保温4~7h,即得复合碳化硅陶瓷窑具。
9.根据权利要求8所述的复合碳化硅陶瓷窑具的制备方法,其特征在于,所述步骤(1)中球磨速率为320~350r/min,球磨的改性后的SiSiC的粒径≤100μm。
10.根据权利要求9所述的复合碳化硅陶瓷窑具的制备方法,其特征在于,所述步骤(1)中所述锆酸酯偶联剂的质量为所述SiSiC质量的0.3~0.42%,所述油酰二乙醇胺的质量为所述SiSiC质量的0.12~0.18%,所述腐殖酸钠的质量为所述SiSiC质量的0.6~0.8%。
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