CN108178634A - 塞隆结合碳化硅陶瓷的制备法 - Google Patents
塞隆结合碳化硅陶瓷的制备法 Download PDFInfo
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- CN108178634A CN108178634A CN201810130333.4A CN201810130333A CN108178634A CN 108178634 A CN108178634 A CN 108178634A CN 201810130333 A CN201810130333 A CN 201810130333A CN 108178634 A CN108178634 A CN 108178634A
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- slurry
- silicon carbide
- high temperature
- temperature
- aging
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 46
- 239000000919 ceramic Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000002002 slurry Substances 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 26
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 22
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 21
- 230000003647 oxidation Effects 0.000 claims abstract description 20
- 238000000498 ball milling Methods 0.000 claims abstract description 19
- 230000032683 aging Effects 0.000 claims abstract description 17
- 230000008569 process Effects 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 235000015895 biscuits Nutrition 0.000 claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 13
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 11
- 229910052602 gypsum Inorganic materials 0.000 claims abstract description 10
- 239000010440 gypsum Substances 0.000 claims abstract description 10
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 9
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 8
- 239000010703 silicon Substances 0.000 claims abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- 238000001514 detection method Methods 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 18
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 14
- 229910003454 ytterbium oxide Inorganic materials 0.000 claims description 13
- 229940075624 ytterbium oxide Drugs 0.000 claims description 13
- 238000010792 warming Methods 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000004321 preservation Methods 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 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 6
- 238000000465 moulding Methods 0.000 claims description 6
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 238000004018 waxing Methods 0.000 claims description 4
- 229920002635 polyurethane Polymers 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- 229910001938 gadolinium oxide Inorganic materials 0.000 claims description 2
- 229940075613 gadolinium oxide Drugs 0.000 claims description 2
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 claims description 2
- 230000035939 shock Effects 0.000 abstract description 13
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 230000007797 corrosion Effects 0.000 abstract description 4
- 238000005260 corrosion Methods 0.000 abstract description 4
- 238000007569 slipcasting Methods 0.000 abstract description 4
- 238000007493 shaping process Methods 0.000 abstract description 2
- 102220043159 rs587780996 Human genes 0.000 description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 15
- 238000013001 point bending Methods 0.000 description 13
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 239000000377 silicon dioxide Substances 0.000 description 8
- 229910052581 Si3N4 Inorganic materials 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 4
- 235000013312 flour Nutrition 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 description 4
- 238000002347 injection Methods 0.000 description 3
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- 239000011819 refractory material Substances 0.000 description 3
- 229920001817 Agar Polymers 0.000 description 2
- 101100373011 Drosophila melanogaster wapl gene Proteins 0.000 description 2
- 229910052769 Ytterbium Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000008272 agar Substances 0.000 description 2
- 229910021431 alpha silicon carbide Inorganic materials 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
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- 210000004483 pasc Anatomy 0.000 description 2
- 239000011505 plaster Substances 0.000 description 2
- 238000001272 pressureless sintering Methods 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 229910021332 silicide Inorganic materials 0.000 description 2
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 2
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 2
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 1
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 230000018199 S phase Effects 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000001934 delay Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011268 mixed slurry Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 239000002023 wood Substances 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
- C04B35/56—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
- C04B35/565—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 silicon carbide
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Abstract
本发明公开了一种塞隆结合碳化硅陶瓷的制备法,包括配料、球磨混合、料浆陈腐、石膏模注浆成型、素坯烘干、高温烧结;所述配料为:由以下重量含量的成分组成基础料:粒度为60~150μm的粗碳化硅颗粒30~41.5wt%、粒度为1~50μm细碳化硅颗粒30~41.5wt%、15~30wt%的金属硅,2~5wt%的氧化铝,0~1wt%氧化铁,0~1.6wt%稀土氧化物。本发明采用注浆成型工艺可以简化生产工艺流程,降低生产成本,制备出的制品高温下抗氧化性好,机械强度高,抗热震性好,耐磨耐腐蚀。
Description
技术领域
本发明涉及一种塞隆结合碳化硅陶瓷的制备方法,该陶瓷主要含有α-SiC和β-SiAlON(塞隆)相。
背景技术
碳化硅由于其极佳的热导率,耐化学腐蚀性好,耐磨性好,高温抗氧化性好,作为高端耐火材料广泛应用于窑炉,熔炉,环保节能设备改造,高端换热器等领域。
目前市场上主要的碳化硅制品有氮化硅结合碳化硅,重结晶烧结碳化硅,反应烧结碳化硅,无压烧结碳化硅陶瓷。氮化硅结合碳化硅制品体积密度较低,一般存在12%以上的气孔率,严重影响到高温机械强度和高温抗氧化性;重结晶碳化硅制品采用粗细碳化硅颗粒注浆成型,在2400℃保护气氛下烧结而成,可以耐1650℃以上的高温,但是体积密度较低一般为2.70g/cm3,存在15%左右的气孔率,高温机械强度低,抗氧化性差,而且生产成本高;反应烧结碳化硅陶瓷制品,体积密度高,机械强度高,但是存在15%左右的金属硅,使用温度低于1350℃,同时金属硅的存在,限制其在氧化、强酸、强碱腐蚀领域的应用。无压烧结碳化硅,烧结温度在2100-2200℃之间,烧结温度较高,对烧结设备要求严格,生产成本较高,高温下制品有16-17%的线性收缩,因此收缩变形不好控制,大件制品的变形比较严重,出现开裂的概率也增大。
专利CN201210287828.0一种轻质高强氮化硅结合碳化硅耐火材料及其制备方法,该材料主要以碳化硅和硅粉为原料制成,碳化硅与硅粉的重量比为65~85:15~30;其中,碳化硅粒径D50=0.1μm~150μm,硅粉粒径D50=0.1μm~1μm;将全部原料混合后进行球磨,球磨时间为8~12小时,球磨后烘干,加原料重的8~12%的PVA造粒,过40~80目筛,室温放置24小时以上,干压成型,成型压力为40~80MPa,排胶,氮化烧结。该方法制备的氮化硅结合碳化硅制品中含有12%以上的气孔,同时含有游离的SiO2相,影响其在高温下的机械强度,制备的制品壁厚和体积较大,降低了材料的抗热震性,影响了窑炉的装载率,增加了能源的消耗。
专利CN2009100222627一种生产塞隆/氮化硅复相结合碳化硅制品的方法。碳化硅做主原料,配有硅粉、金属铝粉、二氧化硅微粉、氧化铝微粉、铝酸盐水泥、外加剂,其质量分数分别为60%~80%、5%~16%、0~5%、0.5%~6%、1%~5%、2%~8%、0.01%~0.06%;采用浇注成型的方法生产异形件,在氮化条件下烧结制备复相结合碳化硅耐火材料制品,该方法制备的制品主要含有氮氧化硅、α-Si3N4、β-Si3N4和玻璃相,其中氮氧化硅和玻璃相,严重影响制品的耐高温、抗热震和抗氧化性,限制了其在高温窑炉领域的应用。
发明内容
本发明要解决的技术问题是提供一种塞隆(SiAlON)结合碳化硅(SiC)陶瓷的制备法。
为了解决上述技术问题,本发明提供一种塞隆结合碳化硅陶瓷的制备法(注浆成型塞隆结合碳化硅陶瓷的方法),包括配料、球磨混合、料浆陈腐、石膏模注浆成型、素坯烘干、高温烧结;
所述配料为:
由以下重量含量的成分组成基础料:粒度为60~150μm的粗碳化硅颗粒30~41.5wt%、粒度为1~50μm细碳化硅颗粒30~41.5wt%、15~30wt%的金属硅,2~5wt%的氧化铝,0~1wt%氧化铁,0~1.6wt%稀土氧化物;
所述球磨混合为:
先在基础料中加入四甲基氢氧化铵和去离子水后进行球磨搅拌(转速为5~30r/min),直至搅拌均匀(搅拌时间为3~8h);然后加入质量浓度10wt%的聚乙烯吡咯烷酮PVP(PVPK90)水溶液进行球磨搅拌(转速为20-30r/min),直至搅拌均匀(持续搅拌时间为2~6h),最后过筛,得料浆;所述四甲基氢氧化铵占基础料总重的0.2~1.5wt%,去离子水占基础料总重的10~30wt%,质量浓度10wt%的聚乙烯吡咯烷酮PVPK90水溶液占基础料总重的0.2~3wt%;
将球磨混合所得的料浆先进行真空搅拌;所述真空搅拌为:将球磨混合所得的料浆置于搅拌桶内,于真空条件(真空表的压力为10-1Pa)、20~30r/min的转速下持续搅拌0.5~4h,从而实现脱泡;
备注说明:碳化硅和氧化铝均为α相(阿尔法相),金属硅使用冶金硅,纯度≥98%;四甲基氢氧化铵作为分散剂,PVPK90水溶液作为悬浮剂和粘结剂;去离子水作为溶剂;
所述料浆陈腐为:取消真空条件,将真空搅拌所得的料浆(脱泡处理后的料浆)于20-30r/min的转速下进行刮壁搅拌,从而实现陈腐,陈腐时间3~5天;将陈腐后料浆进行石膏模注浆成型;
所述素坯烘干为:将石膏模注浆成型所得的素坯先于室温***干1~2天,然后于50~60℃保温干燥3~8h,然后升温至90~120℃保温干燥1~3h;
所述高温烧结为:先将烘干后素坯整齐装入高温窑炉中,充入流动氮气,升温过程始终保证炉内微正压(氮气压力高于大气压200Pa),以1~3℃/min升温至600±30℃,保温0.5~2.0h,进行排蜡处理;以1~3℃/min升温至1380±30℃,保温10~18h,然后以0.5~2℃/min升温至1450±30℃,保温4~6h后停止加热,关掉氮气进气阀,然后降温(带电降温),降温速率为1~3℃/min,待温度降至1250~1350℃实施高温氧化处理;
所述高温氧化处理为:待温度降至1250~1350℃,打开进气阀充入(缓慢充入)流动空气进行高温氧化处理,处理时间为0.5~2.0h,处理完后停止加热,随炉冷却至室温开炉。
作为本发明的塞隆结合碳化硅陶瓷的制备法的改进:
将陈腐后料浆进行性能的检测:包括PH值、体积密度和黏度。
备注:用PH试纸检测料浆的PH值,PH值介于7-9之间,采用空杯法检测料浆的体积密度>2.4g/cm3,采用NDJ-8S数字式粘度计检测料浆黏度控制在100-300mPa·S。对陈腐后的料浆性能进行检测,为后续生产提供参考和追溯问题提供参考。
作为本发明的塞隆结合碳化硅陶瓷的制备法的进一步改进:
所述稀土氧化物为氧化钇、氧化镱、氧化镧、氧化钆中的至少一种。
作为本发明的塞隆结合碳化硅陶瓷的制备法的进一步改进:
所述球磨混合步骤为:于内衬聚氨酯球磨机中进行球磨;过200目筛,得料浆。
作为本发明的塞隆结合碳化硅陶瓷的制备法的进一步改进:
所述真空搅拌步骤,在搅拌过程中一直抽取真空,从而确保真空度。
在本发明中,石膏模注浆成型是常规技术。
本发明的性能检测所采取的方法为:
制备规格为10*10*10mm的试样块,煮沸法结合排水法检测体积密度和显气孔率;制备规格为3*4*36mm的测试条检测室温和1450℃下的三点抗弯强度;制备规格20*5*100mm试验条,在加热炉中加热至1100℃,空气气氛下保温500h,冷却至室温后检测质量损失率:(测试前质量-测试后质量)*100/测试后质量,检测抗氧化性好坏;制备规格20*5*100mm的测试条在加热炉中加热至1450℃,然后取出放置在空气中冷却,待降至室温,观察表面是否出现裂纹,检测其抗热震性好坏。
本发明相比较现有技术具有以下技术优势:
1.本发明制备出的制品气孔率较低,室温和工作温度下机械强度高,耐磨耐酸碱腐蚀,抗热震性和抗氧化性好;
2.引入稀土氧化物作为烧结助剂,高温下稀土氧化物与游离金属硅反应,生成比二氧化硅更耐高温氧化的稀土金属硅化物晶界相,极大提高制品的高温抗氧化性;
3.采用粗细搭配的两种α-SiC粉,结合传统的注浆工艺,极大降低生产成本,提高生产产品种类的灵活性,可以做些复杂异形大件制品;
4.本发明的制备的窑炉耐火材料,以较轻的质量承担较重的载荷,增大窑炉的装载率,极佳的抗热震性可以进行制品的快速烧结和快速降温,提高窑炉的利用率,降低生产周期;
综上所述,本发明采用注浆成型工艺可以简化生产工艺流程,降低生产成本,可以制备大件和形状复杂的制品,同时加入稀土氧化物,高温下稀土氧化物与游离金属硅反应,生成比二氧化硅更耐高温氧化的稀土金属硅化物晶界相,制备出的制品具高温下抗氧化性好,机械强度高,抗热震性好,耐磨耐腐蚀。
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,以下实施例中所用原材料均能通过市购形式获得。
本发明的步骤中没有明确告知的,均是在室温下进行。
实施例1、一种塞隆结合碳化硅陶瓷的制备方法,依次进行以下步骤:
1)、配料:
由以下重量含量的成分组成基础料:
120#(粒度为120μm)的粗碳化硅颗粒40wt%,
F240(粒度为40μm)的细碳化硅颗粒35wt%,
金属Si 19wt%,
三氧化二铝(α相)4wt%,
氧化铁0.4wt%,
氧化钇0.8wt%,
氧化镱0.8wt%。
粗碳化硅颗粒、细碳化硅颗粒的纯度均≥98%,均为α相;
金属Si纯度≥98%,选用200目,
三氧化二铝(α相),D50=2.5μm,纯度≥99.8%,
氧化铁,D50=0.3μm,纯度≥96%,
氧化钇,D50=1.5μm,纯度≥99.9%,
氧化镱,D50=1.5μm,纯度≥99.9%。
2)、球磨混合:
采用聚氨酯内衬的球磨机,首先在球磨机中加入基础料相同重量的碳化硅研磨球,研磨球的平均直径控制在8mm,在球磨机内加入基础料,然后加入占基础料0.5wt%四甲基氢氧化铵和占基础料15wt%的去离子水、进行球磨搅拌(转速为30r/min),球磨时间为8h;
再以基础料1wt%的比例加入质量浓度10wt%的PVPK90水溶液,进行球磨搅拌(转速为30r/min),球磨时间为4h;
3)、真空搅拌脱泡:
将上述混好的料浆,采用200目筛网过筛后,加入到真空搅拌机的搅拌桶中进行缓慢搅拌,搅拌轴的转速30r/min,同时开启真空泵抽真空,保证搅拌桶内为负压(真空表的压力在10-1Pa),持续时间2h,从而实现脱泡;时间到后关闭真空泵。
4)、料浆陈腐:
将脱泡处理后的料浆在搅拌桶中进行刮壁搅拌(转速为20r/min)从而实现陈腐,陈腐时间3天;
备注说明:此步骤不进行抽真空。
5)、料浆性能的检测:
用PH试纸检测料浆的PH值,PH值介于7-8之间,采用空杯法检测料浆的体积密度为2.43g/cm3,采用NDJ-8S数字式粘度计检测料浆黏度为260mPa·S。
6)、石膏模注浆成型(此为常规技术,因此只进行如下的简述):
将放置在真空搅拌机中检测合格的料浆,再次抽真空处理。开启真空泵,真空表的压力控制在10-1Pa,持续30min后,关闭真空泵,打开真空搅拌机的进气阀和出料阀门,向注浆桶中倒入所需的料浆,然后进行注浆成型,将料浆倒入准备好的石膏模具中,静置0.5h,静置过程中石膏模开始吸收料浆中的水分,注浆口料浆液面会下降,中途根据注浆口料浆的下降程度及时补浆2次,用游标卡尺检测注浆毛坯顶端口的内外径,达到要求的壁厚8mm后,倒出多余的料浆,把石膏模具注浆口部位朝下放置5min,待内部多余的料浆全部倒出,然后注浆口朝上放置在室内,静置5h后待坯体成型稳定后,拆掉石膏模,用刮刀清理掉素坯表面毛刺;
7)、素坯烘干:
先将素坯整齐摆放在室内台面上,室温***干1天,然后放置在烘箱中50℃保温5h,然后升温至100℃保温2h;
8)、高温烧结及氧化处理:
将烘干后素坯整齐装入高温窑炉中,充入流动氮气,升温过程始终保证炉内微正压(氮气压力高压大气压200Pa),以1.5℃/min升温至600℃,保温1.0h,进行排蜡处理,以2.0℃/min升温至1380℃,保温15h,然后以1.0℃/min升温至1450℃,保温6h后停止加热,关掉氮气进气阀,然后带电降温,降温速率为2.0℃/min,待温度降至1350℃,打开进气阀,缓慢充入流动空气,进行高温氧化处理,处理时间为1.0h,处理完后停止加热,随炉冷却至室温开炉。
9)、性能检测:
检测体积密度为2.84g/cm3,气孔率为9%;室温下三点抗弯强度为220MPa,1450℃下三点抗弯强度为210MPa;氧化处理后质量损失率为1.12%,抗氧化性很好;试样表面没有肉眼可以观察到的微裂纹,抗热震性极好。
实施例2、
以“氧化钇占1.6wt%,D50=1.5μm,纯度≥99.9%”替代实施例1中“氧化钇占0.8wt%,D50=1.5μm,纯度≥99.9%;氧化镱占0.8wt%,D50=1.5μm,纯度≥99.9%”,其余等同于实施例1。
检测体积密度为2.81g/cm3,气孔率为10%;室温下三点抗弯强度为190MPa,1450℃下三点抗弯强度为185MPa;质量损失率为1.5%,抗氧化性较好;试样表面没有肉眼可以观察到的微裂纹,抗热震性很好。
实施例3、
以“氧化镱占0.8wt%,D50=1.5μm,纯度≥99.9%”替代实施例1中“氧化钇占0.8wt%,D50=1.5μm,纯度≥99.9%;氧化镱占0.8wt%,D50=1.5μm,纯度≥99.9%”,相应增加金属Si至19.8wt%,其余等同于实施例1。
检测体积密度为2.78g/cm3,气孔率为11%;室温下三点抗弯强度为170MPa,1450℃下检测三点抗弯强度为165MPa;质量损失率为2.0%,抗氧化性较好;试样表面没有肉眼可以观察到的微裂纹,抗热震性很好。
实施例4、
以“氧化镧占1.6wt%,D50=1.5μm,纯度≥99.9%”替代实施例1中“氧化钇占0.8wt%,D50=1.5μm,纯度≥99.9%。氧化镱占0.8wt%,D50=1.5μm,纯度≥99.9%”,其余等同于实施例1。
检测体积密度为2.81g/cm3,气孔率为10%;室温下三点抗弯强度为175MPa,1450℃下三点抗弯强度为170MPa,质量损失率为1.8%,抗氧化性较好;试样表面没有肉眼可以观察到的微裂纹,抗热震性很好。
实施例5、
以“氧化镱占1.6wt%,D50=1.5μm,纯度≥99.9%”替代实施例1中“氧化钇占0.8wt%,D50=1.5μm,纯度≥99.9%。氧化镱占0.8wt%,D50=1.5μm,纯度≥99.9%”,其余等同于实施例1。
检测体积密度为2.76g/cm3,气孔率为11%,室温下三点抗弯强度为180MPa,1450℃下三点抗弯强度为163MPa,质量损失率为2.5%,抗氧化性好;试样表面没有肉眼可以观察到的微裂纹,抗热震性较好。
实施例6、
以“氧化钇占0.4wt%,D50=1.5μm,纯度≥99.9%;氧化镱占0.4wt%,D50=1.5μm,纯度≥99.9%”替代实施例1中“氧化钇占0.8wt%,D50=1.5μm,纯度≥99.9%。氧化镱占0.8wt%,D50=1.5μm,纯度≥99.9%”,相应增加金属Si至19.8wt%,其余等同于实施例1。
检测体积密度为2.72g/cm3,气孔率为12%;室温下三点抗弯强度为170MPa,1450℃下检测三点抗弯强度为160MPa;质量损失率为2.5%,抗氧化性好;试样表面没有肉眼可以观察到的微裂纹,抗热震性较好。
对比例1-1、将实施例1中的“氧化钇占0.8wt%,D50=1.5μm,纯度≥99.9%。氧化镱占0.8wt%,D50=1.5μm,纯度≥99.9%”去掉,将“金属Si,19wt%”改为“金属Si,20.6wt%”其余等同于实施例1。
对比例1-2、将实施例1中的“氧化钇占0.8wt%,D50=1.5μm,纯度≥99.9%。氧化镱占0.8wt%,D50=1.5μm,纯度≥99.9%”改成“氧化钇占0.8wt%,D50=5μm,纯度≥99.9%。氧化镱占0.8wt%,D50=5μm,纯度≥99.9%”,其余等同于实施例1。
对比例2-1、将实施例1中的“三氧化二铝(α相)4wt%,氧化铁0.4wt%”改成“三氧化二铝(α相)4.4wt%”,其余等同于实施例1。
对比例2-2、将实施例1中的“金属Si,19wt%,三氧化二铝(α相)4wt%”改为“金属Si,23wt%”,其余等同于实施例1。
对比例3、将实施例1中的步骤8)、高温烧结及氧化处理改为以下步骤:
将烘干后素坯整齐装入高温窑炉中,充入流动氮气,升温过程始终保证炉内微正压(氮气压力高压大气压200Pa),以1.5℃/min升温至600℃,保温1.0h,进行排蜡处理,以2.0℃/min升温至1380℃,保温15h,然后以1.0℃/min升温至1450℃,保温6h后停止加热,关掉氮气进气阀,随炉冷却至室温开炉。其余等同于实施例1。
上述所有对比例的性能数据如下表1所述。
表1
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 (5)
1.塞隆结合碳化硅陶瓷的制备法,包括配料、球磨混合、料浆陈腐、石膏模注浆成型、素坯烘干、高温烧结,其特征是:
所述配料为:
由以下重量含量的成分组成基础料:粒度为60~150μm的粗碳化硅颗粒30~41.5wt%、粒度为1~50μm细碳化硅颗粒30~41.5wt%、15~30wt%的金属硅,2~5wt%的氧化铝,0~1wt%氧化铁,0~1.6wt%稀土氧化物;
所述球磨混合为:
先在基础料中加入四甲基氢氧化铵和去离子水后进行球磨搅拌,直至搅拌均匀;然后加入质量浓度10wt%的聚乙烯吡咯烷酮PVP水溶液进行球磨搅拌,直至搅拌均匀,最后过筛,得料浆;所述四甲基氢氧化铵占基础料总重的0.2~1.5wt%,去离子水占基础料总重的10~30wt%,质量浓度10wt%的聚乙烯吡咯烷酮PVPK90水溶液占基础料总重的0.2~3wt%;
将球磨混合所得的料浆先进行真空搅拌;所述真空搅拌为:将球磨混合所得的料浆置于搅拌桶内,于真空条件、20~30r/min的转速下持续搅拌0.5~4h,从而实现脱泡;
所述料浆陈腐为:取消真空条件,将真空搅拌所得的料浆于20-30r/min的转速下进行刮壁搅拌,从而实现陈腐,陈腐时间3~5天;将陈腐后料浆进行石膏模注浆成型;
所述素坯烘干为:将石膏模注浆成型所得的素坯先于室温***干1~2天,然后于50~60℃保温干燥3~8h,然后升温至90~120℃保温干燥1~3h;
所述高温烧结为:先将烘干后素坯整齐装入高温窑炉中,充入流动氮气,升温过程始终保证炉内微正压,以1~3℃/min升温至600±30℃,保温0.5~2.0h,进行排蜡处理;以1~3℃/min升温至1380±30℃,保温10~18h,然后以0.5~2℃/min升温至1450±30℃,保温4~6h后停止加热,关掉氮气进气阀,然后降温,降温速率为1~3℃/min,待温度降至1250~1350℃实施高温氧化处理;
所述高温氧化处理为:待温度降至1250~1350℃,打开进气阀充入流动空气进行高温氧化处理,处理时间为0.5~2.0h,处理完后停止加热,随炉冷却至室温开炉。
2.根据权利要求1所述的塞隆结合碳化硅陶瓷的制备法,其特征是:
将陈腐后料浆进行性能的检测:包括PH值、体积密度和黏度。
3.根据权利要求1或2所述的塞隆结合碳化硅陶瓷的制备法,其特征是:
所述稀土氧化物为氧化钇、氧化镱、氧化镧、氧化钆中的至少一种。
4.根据权利要求3所述的塞隆结合碳化硅陶瓷的制备法,其特征是:
所述球磨混合步骤为:于内衬聚氨酯球磨机中进行球磨;过200目筛,得料浆。
5.根据权利要求4所述的塞隆结合碳化硅陶瓷的制备法,其特征是:所述真空搅拌步骤,在搅拌过程中一直抽取真空,从而确保真空度。
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