CN114988879A - 一种大型复相反应烧结碳化硅制品及制备方法 - Google Patents
一种大型复相反应烧结碳化硅制品及制备方法 Download PDFInfo
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- CN114988879A CN114988879A CN202210754421.8A CN202210754421A CN114988879A CN 114988879 A CN114988879 A CN 114988879A CN 202210754421 A CN202210754421 A CN 202210754421A CN 114988879 A CN114988879 A CN 114988879A
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 97
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title abstract description 17
- 238000004519 manufacturing process Methods 0.000 title abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 36
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 28
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 22
- 150000004767 nitrides Chemical class 0.000 claims abstract description 21
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 18
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 17
- 229910052751 metal Inorganic materials 0.000 claims abstract description 16
- 239000002184 metal Substances 0.000 claims abstract description 16
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 13
- 235000015895 biscuits Nutrition 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000010703 silicon Substances 0.000 claims abstract description 11
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 10
- 239000002245 particle Substances 0.000 claims abstract description 10
- 229910018540 Si C Inorganic materials 0.000 claims abstract description 9
- 238000001746 injection moulding Methods 0.000 claims abstract description 9
- 239000007787 solid Substances 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000000465 moulding Methods 0.000 claims abstract description 8
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000002344 surface layer Substances 0.000 claims abstract description 3
- 239000000047 product Substances 0.000 claims description 44
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 14
- 229910052786 argon Inorganic materials 0.000 claims description 11
- 239000011230 binding agent Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 9
- 239000012298 atmosphere Substances 0.000 claims description 8
- 238000010304 firing Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 239000006229 carbon black Substances 0.000 claims description 6
- 239000004568 cement Substances 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 6
- 239000011449 brick Substances 0.000 claims description 5
- 238000000748 compression moulding Methods 0.000 claims description 5
- 239000011162 core material Substances 0.000 claims description 5
- 239000002270 dispersing agent Substances 0.000 claims description 5
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- 229910007991 Si-N Inorganic materials 0.000 claims description 4
- 229910006294 Si—N Inorganic materials 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical compound [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 claims description 4
- 239000004927 clay Substances 0.000 claims description 4
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- 238000011068 loading method Methods 0.000 claims description 4
- 239000005011 phenolic resin Substances 0.000 claims description 4
- 229920001568 phenolic resin Polymers 0.000 claims description 4
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 3
- 229920001353 Dextrin Polymers 0.000 claims description 2
- 239000004375 Dextrin Substances 0.000 claims description 2
- 229920000877 Melamine resin Polymers 0.000 claims description 2
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- 150000007513 acids Chemical class 0.000 claims description 2
- 239000010426 asphalt Substances 0.000 claims description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- 230000007547 defect Effects 0.000 claims description 2
- 235000019425 dextrin Nutrition 0.000 claims description 2
- 238000007723 die pressing method Methods 0.000 claims description 2
- 238000009792 diffusion process Methods 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000002006 petroleum coke Substances 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 2
- 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 2
- 239000006104 solid solution Substances 0.000 claims description 2
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 239000012466 permeate Substances 0.000 claims 1
- 239000011819 refractory material Substances 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 3
- 238000009434 installation Methods 0.000 abstract description 2
- 238000003825 pressing Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 14
- 238000001816 cooling Methods 0.000 description 10
- 230000001276 controlling effect Effects 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 235000012239 silicon dioxide Nutrition 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000002893 slag Substances 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000005485 electric heating Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 238000005121 nitriding Methods 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- YXTPWUNVHCYOSP-UHFFFAOYSA-N bis($l^{2}-silanylidene)molybdenum Chemical compound [Si]=[Mo]=[Si] YXTPWUNVHCYOSP-UHFFFAOYSA-N 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 229920005551 calcium lignosulfonate Polymers 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000013066 combination product Substances 0.000 description 1
- 229940127555 combination product Drugs 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229910021343 molybdenum disilicide Inorganic materials 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
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Abstract
本发明属于耐火材料制备技术领域，涉及一种大型复相反应烧结碳化硅制品及制备方法。涉及的一种大型复相反应烧结碳化硅制品的主原料选用碳化硅颗粒和细粉、碳粉或固碳残留≥30%的液态碳源、硅含量98%以上金属硅粉；金属硅粉的加入量高于Si‑C反应的理论配比，其富余量用于形成氮化物结合相；根据制品尺寸形状用半干法模压或湿法注模成型为所需外形，素坯经烘干后装窑；纯氮气气氛，1150‑1250℃初步形成部分氮化物；特定温度转换氩气气氛，氮化反应停止，表层和芯部形成β‑SiC结合相；最后通入氮气，达到最终烧结。本发明大幅度降低安装周期和成本，生产和应用环节具备节能降耗的效果。
Description
技术领域
本发明属于耐火材料制备技术领域，具体涉及一种大型复相反应烧结碳化硅制品及制备方法。
背景技术
高炉炼铁技术正朝着大型化、高效、节能、环保等方向发展，其炉内工况环境更加复杂苛刻，选择具备优良使用效果的关键部位用耐火材料，对高炉使用寿命、运行成本等起至关重要的作用。碳化硅质耐火材料内衬在高炉中已有广泛应用，但多年来很少有新产品突破。不同种类碳化硅耐火材料制品，Sialon结合SiC具有优良的抗碱性能，易挂渣，因此非常适合在高炉内使用；β-SiC结合SiC与高温熔渣润湿性差，抗渣和抗碱能力强，同时具有较高的热导率和优良的抗热震性能；Si3N4结合SiC相对于前两种制造费用低，各项高温性能优良，国内产量据世界前列，具有较高的综合性价比，在炼铁、有色、陶瓷等多个行业广泛应用。
不同碳化硅质耐火材料的制造过程，氮化物结合碳化硅制品需要把外部N2渗入到含Si坯体内，坯体烧后增重密度增加，不需要很高的成型密度，但坯体尺寸受氮化深度限制，标准产品一般氮化厚度不大于150mm。烧成原理上，β-SiC结合SiC可制备大尺寸产品，但其成型和烧成工艺技术苛刻，工业化制备难度高。本发明所制备大型复相反应烧结碳化硅制品综合β-SiC和氮化物结合SiC制品的制备优势和性能特点，优化结合相种类，可适应不同工况环境。例如，在高炉内使用，可制备β-SiC和Sialon为主的复相结合碳化硅制品，产品具有更好的抗碱和挂渣性能，同时降低大型制品制造难度和成本，扩展高性能碳化硅制品的应用能力和范围。
大型碳化硅质耐火材料制品制备技术，中国专利“一种浇注成型大型氮化物结合碳化硅制品”（CN103936437B）提出了以氮化物结合相为主的浇注成型碳化硅制品。所述浇注成型大型氮化物结合碳化硅制品，以碳化硅颗粒和细粉、碳化硅微粉、二氧化硅微粉、氧化铝微粉、活性氧化镁和减水剂为粉料，未添加金属硅粉，硅溶胶为结合剂，烧成制备原理存在较大差异；中国专利“一种浇注成型自结合碳化硅制品”（CN103880448B）提出了以自结合（β-SiC）为主的浇注成型碳化硅制品。所述一种浇注成型自结合碳化硅制品以碳化硅颗粒和细粉、碳化硅微粉、二氧化硅微粉、硅粉、炭黑、二硅化钼微粉、活性氧化镁和减水剂为粉料，硅溶胶为结合剂，保护气氛下，最高（1300-1500）℃烧制而成，可制备大尺寸制品。该自结合制品制备技术，浇注成型坯体具有较高的自由水份，加上坯体烧成失重，要求成型坯体具有更高的成型密度，才能保证制品的基本性能指标。
复相结合碳化硅制品的制备，中国专利“水泥窑预热器用复合氮化物结合碳化硅挂板的烧制方法”（CN101602607B）提出以多种氮化物为结合相的碳化硅制品，所述水泥窑预热器用复合氮化物结合碳化硅挂板的烧制方法，素坯由碳化硅、硅粉、二氧化硅微粉、三氧化二铝微粉和有机液体结合剂组成，氮气气氛下（1400-1500）℃下烧成，制备由氮化硅、氧氮化硅、赛隆复相结合的碳化硅材料。所述水泥窑预热器用复合氮化物结合碳化硅挂板纯氮气气氛烧成，只能制备薄壁型挂板，且未包含β-SiC结合相。
发明内容
本发明的目的是提出一种大型复相反应烧结碳化硅制品及制备方法，通过反应烧结工艺，生成以β-SiC和氮化物作为复相结合相的大型碳化硅制品，所述制备方法具有制造成本低、易实现工业化、高温使用性能优异的特点。
本发明为完成上述目的采用如下技术方案：
一种大型复相反应烧结碳化硅制品的制备方法，碳化硅制品的主原料选用碳化硅含量在98%以上的碳化硅颗粒和细粉、碳含量在99%99%以上碳粉或固碳残留≥30%的液态碳源、硅含量98%以上金属硅粉；所述金属硅粉的加入量高于Si-C反应的理论配比，其富余量用于形成氮化物结合相；根据制品尺寸形状用半干法模压或湿法注模成型为所需外形，素坯经烘干后装窑；纯氮气气氛，1150-1250℃初步形成部分氮化物；特定温度转换氩气气氛，氮化反应停止，表层和芯部形成β-SiC结合相；最后通入氮气，达到最终烧结；通过Si-C和Si-N2反应形成含3-10%的β-SiC和5-20%的氮化物作为复相结合相把骨料结合，形成大型复相反应烧结碳化硅制品。
通过Si-C反应形成β-SiC结合相，同时通过Si-N2系列反应形成氮化物结合相，包括Si3N4、Si2N2O、Sialon中的其中一种或多种。
所述半干法模压成型：使用外加量2-5%的木钙、糊精、酚醛树脂、水溶性树脂等其中一种或多种作为临时粘结剂，半干法模压成型；
所述湿法注模成型：外加0.05-0.30%的三聚磷酸钠、六偏磷酸钠、聚羧酸类、密胺树脂类等无机或有机分散剂的一种或多种，且使用ρ-Al2O3、纯铝酸钙水泥、高铝粘土、二氧化硅微粉、硅溶胶、铝溶胶等其中一种或多种作为胶凝剂，其中ρ-Al2O3、纯铝酸钙水泥、高铝粘土、二氧化硅微粉加入1-5%，硅溶胶、铝溶胶外加量8-15%，实现湿法注模成型。
一种大型复相反应烧结碳化硅制品的制备方法，可根据配方设计控制结合相的物相组成及含量，制备和成型厚度150mm以上的大型制品；具体包括以下配比、混料和成型过程如下：
1）主原料配比：
碳化硅颗粒原料：粒度0-6mm，占比60-80%；
碳化硅细粉原料：粒度-320目～ -150目，占比10-30%；
D50≤25μm的固态碳源细粉包括炭黑、石油焦、石墨，固碳残留≥30%的液态碳源包括酚醛树脂、沥青，固态和液态碳源其中的一种或两种相互组合：理论碳占比1-3%；
金属硅粉：粒度-320目 ～-150目，占比5-15%；
2）混料和成型工序：
上述不同原料，半干法成型时与粘结剂，或湿法成型时与分散剂和胶凝剂，按一定比例混合均匀，采用半干法机压或湿法注模方式成型，素坯经脱模和干燥处理后，形成干素坯：
3）烧结：干素坯经烘干后装窑，烧成过程包括以下三个阶段：第一阶段，氮气气氛，初步氮化形成部分氮化物，配方内少量Al2O3、SiO2氧化物初步形成固溶或反应进入氮化物晶格，避免烧后游离氧化物残留；第二阶段，转换氩气气氛，氮化反应停止，只发生Si-C反应，碳消耗金属硅充分转化为β-SiC相，反应后坯体显气孔适量增加，有利于第三阶段氮气扩散和渗透；同时β-SiC相赋予砖体芯部材质一定结合强度，降低坯体出现缺陷的几率；第三阶段，高温下氩气转换为氮气，通过长时间保温，氮缓慢渗入坯体，与少量未反应金属硅充分反应，坯体增重，密度提高，达到最终烧结。
所述一种大型复相反应烧结碳化硅制品的制备方法，烧成过程的具体操作如下：
干素坯放入气氛炉内，400℃前通入氮气置换出炉内空气，并调节出气口保持炉内微正压60-150mmH2O柱，整个过程控制升降温速率不高于0.5℃/min，并维持炉内正压力，采用以下温度制度和气氛：
1）炉温从室温升至（1150-1250）℃，保温（0-20）h后，氮气转换为氩气，同温继续保温（3-8）h；
2）炉温从（1150-1250）℃升至（1300-1380）℃保温（5-25）h后，氩气转换为氮气，继续保温（10-20）h；
3）炉温从（1300-1380）℃升至最高（1400-1500）℃，保温（5-20）h后，保持氮气气氛，进入降温阶段；
4）炉内温度降至200℃以下出炉。
本发明提出的一种大型复相反应烧结碳化硅制品及制备方法，通过引入β-SiC结合相改善大型制品芯部无法氮化形成结合相，造成大量残硅易开裂的问题。所述一种大型复相反应烧结碳化硅制品的制备方法，通过引入氮化物结合相，产生烧成增重致密，解决自结合制品烧成致密度下降，以及高密度成型难度大的问题。解决现有同级别材料生产制备大型制品的难题。
所述一种大型复相反应烧结碳化硅制品的制备方法，制品应用时，可大幅度降低安装周期和成本，生产和应用环节具备节能降耗的效果，因此具有很好的经济和社会效益。
附图说明
图1为大型复相反应烧结碳化硅制品典型显微结构，所示为所述复相反应烧结碳化硅制品气孔内β-SiC纳米线和晶体发育不规则的氮化物穿插生长的形貌。
图2为材料内部絮状β-SiC纳米线形貌。
具体实施方式
下面通过几个实施例对本发明进行具体说明：
实施例1：
混料，（0-3）mm碳化硅颗粒，加入量70%；-240目碳化硅细粉，加入13.5%；炭黑N990加入1.5%，-320目金属硅粉加入15%，木钙外加3%，与少量水充分混合，半干法模压成型为厚200mm的砖坯。干燥后装入电加热梭式气氛窑，调节出气口保持炉内微正压100mmH2O柱，控制升温速度为0.5℃/min，炉温从室温升至1200℃，保温10h，把氮气转换为氩气，继续保温5h；氩气气氛，以0.5℃/min升温，炉温从1200℃升至1300℃，1300℃保温10h，氩气转换为氮气，继续保温15h；控制升温速度0.3℃/min，从1300℃升至1400℃，1400℃保温12h，保持氮气气氛，进入控制降温阶段；控制降温速度≤0.5℃/min，炉内温度从最高温度降温至1000℃后停炉，自由降温200℃后出炉。烧后材料典型物相组成：除SiC主晶相外，β-SiC含量3-5%，Si3N4含量15-20%。
实施例2：
混料，（0-5）mm碳化硅颗粒，加入量65%；-240目碳化硅细粉，加入17%；炭黑N990加入3.0%，-200目金属硅粉加入10%，ρ-Al2O3加入5%，三聚磷酸钠外加+0.2%，聚羧酸类分散剂外加+0.1%，与水充分混合，湿法成型为厚300mm的砖坯。养护脱模干燥后，装入电加热梭式气氛窑，调节出气口保持炉内微正压120mmH2O柱，控制升温速度为0.5℃/min，炉温从室温升至1250℃，保温12h，氮气转换为氩气，继续保温5h；氩气气氛，0.5℃/min升温，炉温从1250℃升至1330℃保温12h，氩气转换为氮气，继续保温20h；控制升温速度0.3℃/min，从1330℃升至1500℃，1500℃保温12h，保持氮气气氛，进入控制降温阶段；控制降温速度不大于0.5℃/min，炉内温度从最高温度降温至800℃后停炉，自由降温后出炉。烧后材料的物相组成：除SiC主晶相外，β-SiC%=(5-10)%，Sialon=(5-10)%，Si3N4=(1-3)%。
实施例3：
混料，（0-6）mm碳化硅颗粒，加入量68%；-240目碳化硅细粉，加入16.9%；炭黑N990加入2.1%，-150目金属硅粉加入8%，ρ-Al2O3加入2%，二氧化硅微粉加入3%，聚羧酸类外加+0.2%，与水充分混合，湿法成型为500mm的砖坯。养护脱模干燥后，装入电加热梭式气氛窑，调节出气口保持炉内微正压150mmH2O柱，控制升温速度为0.3℃/min，炉温从室温升至1230℃，保温20h，氮气转换为氩气，继续保温8h；0.3℃/min升温，炉温从1230℃升至1350℃保温25h，氩气转换为氮气，继续保温20h；控制升温速度0.3℃/min，从1350℃升至1450℃，1450℃保温20h，保持氮气气氛，进入控制降温阶段；控制降温速度不大于0.3℃/min，炉内温度从最高温度降温至600℃后停炉，自由降温后出炉。烧后材料的物相组成：除SiC主晶相外，β-SiC%=(5-10)%，Si2N2O=3-5%，Sialon=(1-3)%，Si3N4=(1-3)%。
Claims (6)
1.一种大型复相反应烧结碳化硅制品，碳化硅制品的主原料选用碳化硅含量在98%以上的碳化硅颗粒和细粉、碳含量在99%上碳粉或固碳残留≥30%的液态碳源、硅含量98%以上金属硅粉；其特征在于：所述金属硅粉的加入量高于Si-C反应的理论配比，其富余量用于形成氮化物结合相；根据制品尺寸形状用半干法模压或湿法注模成型为所需外形，素坯经烘干后装窑；纯氮气气氛，1150-1250℃初步形成部分氮化物；特定温度转换氩气气氛，氮化反应停止，表层和芯部形成β-SiC结合相；最后通入氮气，达到最终烧结；通过Si-C和Si-N2反应形成含3-10%的β-SiC和5-20%的氮化物作为复相结合相把骨料结合，形成大型复相反应烧结碳化硅制品。
2.如权利要求1所述的一种大型复相反应烧结碳化硅制品，其特征在于：通过Si-C反应形成β-SiC结合相，同时通过Si-N2系列反应形成氮化物结合相，包括Si3N4、Si2N2O、Sialon的其中一种或多种。
3.如权利要求1所述的一种大型复相反应烧结碳化硅制品，其特征在于：所述半干法模压成型：使用外加量2-5%的木钙、糊精、酚醛树脂、水溶性树脂等其中一种或多种作为临时粘结剂，半干法模压成型。
4.如权利要求1所述的一种大型复相反应烧结碳化硅制品，其特征在于：所述湿法注模成型：外加0.05-0.30%的三聚磷酸钠、六偏磷酸钠、聚羧酸类、密胺树脂类等无机或有机分散剂的一种或多种，且使用ρ-Al2O3、纯铝酸钙水泥、高铝粘土、二氧化硅微粉、硅溶胶、铝溶胶等其中一种或多种作为胶凝剂，其中ρ-Al2O3、纯铝酸钙水泥、高铝粘土、二氧化硅微粉加入1-5%，硅溶胶、铝溶胶外加量8-15%，实现湿法注模成型。
5.制备权利要求1-4任一一种大型复相反应烧结碳化硅制品的制备方法，其特征在于：可根据配方设计控制结合相的物相组成及含量，制备和成型厚度150mm以上的大型制品；具体包括以下配比、混料和成型过程如下：
1）主原料配比：
碳化硅颗粒原料：粒度0-6mm，占比60-80%；
碳化硅细粉原料：粒度-320目～ -150目，占比10-30%；
D50≤25μm的固态碳源细粉包括炭黑、石油焦、石墨，固碳残留≥30%的液态碳源包括酚醛树脂、沥青，固态和液态碳源其中的一种或两种相互组合：理论碳占比1-3%；
金属硅粉：粒度-320目 ～-150目，占比5-15%；
2）混料和成型工序：
上述不同原料，半干法成型时与粘结剂，或湿法成型时与分散剂和胶凝剂，按一定比例混合均匀，采用半干法机压或湿法注模方式成型，素坯经脱模和干燥处理后，形成干素坯：
3）烧结：干素坯经烘干后装窑，烧成过程包括以下三个阶段：第一阶段，氮气气氛，初步氮化形成部分氮化物，配方内少量Al2O3、SiO2氧化物初步形成固溶或反应进入氮化物晶格，避免烧后游离氧化物残留；第二阶段，转换氩气气氛，氮化反应停止，只发生Si-C反应，碳消耗金属硅充分转化为β-SiC相，反应后坯体显气孔适量增加，有利于第三阶段氮气扩散和渗透；同时β-SiC相赋予砖体芯部材质一定结合强度，降低坯体出现缺陷的几率；第三阶段，高温下氩气转换为氮气，通过长时间保温，氮缓慢渗入坯体，与少量未反应金属硅充分反应，坯体增重，密度提高，达到最终烧结。
6.如权利要求5一种大型复相反应烧结碳化硅制品的制备方法，其特征在于：烧成过程的具体操作如下：
干素坯放入气氛炉内，400℃前通入氮气置换出炉内空气，并调节出气口保持炉内微正压60-150mmH2O柱，整个过程控制升降温速率不高于0.5℃/min，并维持炉内正压力，采用以下温度制度和气氛：
1）炉温从室温升至（1150-1250）℃，保温（0-20）h后，氮气转换为氩气，同温继续保温（3-8）h；
2）炉温从（1150-1250）℃升至（1300-1380）℃保温（5-25）h后，氩气转换为氮气，继续保温（10-20）h；
3）炉温从（1300-1380）℃升至最高（1400-1500）℃，保温（5-20）h后，保持氮气气氛，进入降温阶段；
4）炉内温度降至200℃以下出炉。
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