CN104058754B - β-SiC/Si2N2O complex phase is in conjunction with SiC kiln furnitures and preparation method - Google Patents
β-SiC/Si2N2O complex phase is in conjunction with SiC kiln furnitures and preparation method Download PDFInfo
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Abstract
β-SiC/Si
2n
2o complex phase, in conjunction with SiC kiln furnitures and preparation method, belongs to fire resisting material field.Raw material consists of silicon carbide, metal Si, polycrystalline silicon wastes, and the spent pulping liquor of additional above-mentioned raw materials total amount 2-6% is as bonding agent.Take various raw material by proportioning during production, obtain pug through mixing, compression moulding, dry 24-48h at 110 ± 10 DEG C, burn till under burying carbon condition in 1200-1500 DEG C.This product physical performance index is excellent: apparent porosity 9-22%, volume density 2.3-2.9g/cm
3, cold crushing strength 60-200MPa, strength at normal temperature 20-75Mpa, have good oxidation-resistance and heat-shock resistance.The present invention take polycrystalline silicon wastes as raw material, adopts carbon burial sintering mode to simplify production technique, not only reduces the production cost of SiC kiln furnitures, also achieve the recycling of polycrystalline silicon wastes, decrease the wasting of resources and environmental pollution.
Description
Technical field
The present invention relates to a kind of β-SiC/Si of fire resisting material field
2n
2o complex phase is in conjunction with SiC kiln furnitures and preparation method.
Background technology
Kiln furnitures are a kind of high grade refractories, and its quality has extremely important impact to the quality of burnt product and energy consumption.Along with applying of ceramic industry quick sintering technology of ultra, the loop cycle that kiln furnitures use is shorter and shorter, working conditions is more harsh, and an urgent demand kiln furniture material improves constantly its normal temperature, hot strength and heat-shock resistance, to meet the needs of ceramic industry quick sintering technology of ultra development.Silicon carbide series refractory material is obtained development and application because having the premium propertiess such as high thermal conductivity, low thermal expansivity, good high-temperature behavior and heat-shock resistance by the kiln furnitures being widely used as ceramic kiln.
SiC has very strong covalent linkage characteristic, under general processing condition, be difficult to sintering, usually need add sintering aid or obtain fine and close silicon carbide sintering block by the parcel of second-phase (in conjunction with phase).β-SiC and Si
2n
2o is well in conjunction with phase, has very excellent performance, SiC particle can be combined, promote its density, improves the physicochemical property of SiC kiln furnitures.β-SiC hot strength is high, has stronger creep resistance, alkali-resistivity, oxidation-resistance; Si
2n
2o has and Si
3n
4similar performance, but its oxidation-resistance and heat-shock resistance are better than Si
3n
4.Therefore, simultaneously with Si
2n
2o and β-SiC has higher normal temperature, hot strength and excellent heat-shock resistance in conjunction with the SiC goods of phase, is being better than Si as in kiln furnitures
3n
4with the goods of silicate in conjunction with phase.The research such as Liu Chunxia shows Si
2n
2o is better than Si in conjunction with the heat-shock resistance of SiC sample
3n
4in conjunction with SiC sample.Japan realizes Si
2n
2the suitability for industrialized production of O silicon carbide kiln furnitures, but be domesticly still in developmental stage.Accelerate long lifetime β-SiC/Si
2n
2o complex phase has urgent demand in conjunction with the development of SiC high-quality kiln furnitures.Domestic and international Si at present
2n
2the production of O silicon carbide kiln furnitures is mainly through with SiC, SiO
2micro mist, silica flour, clay are that raw material burns till obtained at high-temperature ammonolysis kiln, and the performance of material is still needed and improved further and improve, and there is the drawbacks such as production cost is high, energy consumption is large, processing condition are complicated, expensive.
In recent years, the energy, information industry are flourish, and the polysilicon market as main raw material also constantly expands thereupon.But polysilicon can use after needing to cut into silicon chip.At cutting process because cutter damages enter cutting slurry by there being the crystalline silicon of 50% ~ 52% to become silicon powder, cause cutting efficiency to reduce, final cutting slip lost efficacy and became slug, caused the wasting of resources and environmental pollution, brought huge pressure to enterprise.Generally adopt at present silicon carbide as cutting abrasive material, therefore cut in slug main containing HIGH-PURITY SILICON, polyoxyethylene glycol (dispersion agent), silicon carbide and a small amount of metal, but silicon and silicon carbide are in physics and chemistry less, the separation difficulty of difference in nature.Therefore, Pure Silicon Metal in cutting waste material how is recycled cost-effectively and silicon carbide is current problem demanding prompt solution.
Summary of the invention
The present invention is intended to, according to the performance requirement of current ceramic industry to kiln furniture material, overcome existing Si
2n
2the defects such as improvement that O silicon carbide kiln furnitures production cost is high, energy consumption is large, processing condition are complicated, performance is still needed, make full use of β-SiC and Si
2n
2the performance characteristics of O, proposing a kind of take polycrystalline silicon wastes as the β-SiC/Si of raw material
2n
2o complex phase, in conjunction with SiC kiln furnitures and preparation method, not only increases the performance of kiln furnitures, reduces the production cost of kiln furnitures, also achieves the comprehensive recycling of polycrystalline silicon wastes, decreases the wasting of resources and environmental pollution.
Technical solution of the present invention:
(1). raw material composition and mass ratio: by weight percentage, 25-55% particle diameter is the SiC particle of 3-1mm, 10-25% particle diameter is 1-0.2mmSiC particle, 5-25% particle diameter≤0.088mmSiC fine powder, 0-25% metal Si, 5-30% polycrystalline silicon wastes, the spent pulping liquor of additional above-mentioned raw materials total amount 2-6% is as bonding agent.In described silicon carbide, SiC content is greater than 98%; In described metal Si, Si content is greater than 98%, and granularity is≤0.088mm; The granularity of described polycrystalline silicon wastes is discrete distribution, is between 1um and 240um, and mean particle size is 20um ± 10um; In polycrystalline silicon wastes, contents of free si is 25-60%, carborundum content is 25-60%, alumina content is 3-7%, metal Fe content is 1-5%, CaO content is less than 0.5%, it is 0.5-3% that content of MgO is less than 1%, PEG (polyoxyethylene glycol, English full name polyethyleneglycol) content.
(2). burden process: take various raw material by proportioning, will in advance load weighted SiC thick, in two kinds of granulated aggregates mix to pour in wheel roller and mix further, stop after 3 ~ 5min stirring, pour the half weighing the bonding agent prepared in advance into wheel roller, open switch again and stir 5min, make bonding agent be evenly distributed on particle surface; Then load weighted SiC fine powder, polycrystalline silicon wastes are poured into wheel roller and stirred 5min, more remaining bonding agent is all poured into wherein continuation stirring 8 ~ 12min, stop stirring.
(3). molding procedure: the raw material vibrating forming machine mixed or friction press are pressed into firebrick billet.
(4). baking operation: the firebrick billet of forming is put into moisture eliminator 110 ± 10 DEG C of dry 24-48h, controls moisture content below 0.5%.
(5). firing process: burn till preparation β-SiC/Si under obtained adobe is buried carbon condition at 1200-1500 DEG C
2n
2o complex phase is in conjunction with SiC refractory material.
Compared with prior art, feature of the present invention and positively effect:
1. the present invention adopts and buries carbon process for calcining and prepared β-SiC/Si
2n
2o complex phase is in conjunction with SiC kiln furnitures.Compared with originally nitridation sintered, simplify technique, reduce production cost.
2. product of the present invention is with β-SiC and Si
2n
2o in conjunction with phase, is closely wrapped in around SiC particle, improves the density of material.β-SiC hot strength is high, has stronger creep resistance, alkali-resistivity, oxidation-resistance; Si
2n
2o has and Si
3n
4similar performance, but its oxidation-resistance and heat-shock resistance are better than Si
3n
4.Product combines both performance advantage, has higher normal temperature, hot strength and excellent oxidation-resistance and thermal shock resistance.
3. the present invention is using polycrystalline silicon cut waste as raw material, replaces all or part of industrial silicon carbide and metallic silicon power, and in realizing under the condition of not separating silicon carbide and Pure Silicon Metal, the recycling of polycrystalline silicon wastes, had both reduced β-SiC/Si
2n
2o complex phase, in conjunction with the preparation cost of SiC kiln furnitures, additionally reduces the waste of resource and the pollution of environment.
4. in the polycrystalline silicon cut waste that the present invention adopts, contain a small amount of PEG, the effect of bonding agent can be played at shaping and initial stage of sintering, improve filling properties and the processability of raw material, replace original resol to use with spent pulping liquor, improve the raw-material feature of environmental protection.
5. the polycrystalline silicon cut waste granularity that the present invention adopts is discrete distribution, is conducive to raw-material grain composition, improves the density of material.Free silica granularity in polycrystalline silicon wastes is little, and surface-area is large, and reactive behavior is large, when existing with industrial silica fume simultaneously, and energy CO, N preferentially and in atmosphere
2rapid reaction, forms gradient reaction step by step, optimizes the structure of material.
6. product of the present invention has excellent physical performance index.Apparent porosity 9-22%, volume density 2.3-2.9g/cm
3, cold crushing strength 60-200MPa, strength at normal temperature 20-75Mpa, there is good oxidation-resistance and heat-shock resistance.
7. the requirement of the aspect such as the kiln furnitures product of the present invention intensity that can meet ceramic industry is high, heat-shock resistance is strong, oxidation-resistance is strong, and production technique is relatively simple, production cost is low, market potential is large, is suitable for applying, will has good economic and social benefit.
Embodiment
Embodiment 1:
A kind of β-SiC/Si
2n
2o complex phase is in conjunction with SiC kiln furnitures and preparation method thereof, and by weight percentage, raw material consists of: the SiC particle 45% of particle diameter 3-1mm, particle diameter 1-0.2mmSiC particle 15%, particle diameter≤0.088mmSiC fine powder 13%, Industrial Metal silica flour 17%, polycrystalline silicon wastes 10%, the spent pulping liquor of additional 3%.
(1). batching: take various raw material by proportioning, will in advance load weighted SiC thick, in two kinds of granulated aggregates mix to pour in wheel roller and mix further, stop after 3 ~ 5min stirring, wheel roller is poured into by weighing the bonding agent half prepared in advance, open switch again and stir 5min, make bonding agent be evenly distributed on particle surface; Then load weighted SiC fine powder, polycrystalline silicon wastes are poured into wheel roller and stirred 5min, more remaining bonding agent is all poured into wherein continuation stirring 8min, stop stirring.
(2). shaping: the raw material mixed is pressed into firebrick billet with vibrating forming machine or friction press.
(3). dry: the refractory brick of forming is put into moisture eliminator 110 DEG C of dry 48h, control moisture content below 0.5%.
(4). burn till: under obtained adobe is buried carbon condition at 1450 DEG C, burn till preparation β-SiC/Si
2n
2o complex phase is in conjunction with SiC refractory material.
The physical and chemical index of products obtained therefrom is: apparent porosity 15%, volume density 2.65g/cm
3, cold crushing strength 168MPa, strength at normal temperature 65MPa, heat-shock resistance, oxidation-resistance are all better.
Embodiment 2:
Raw material composition is identical with embodiment 1, and production technique is substantially identical with example 1, and difference is: sintering temperature is 1500 DEG C.
The performance index of products obtained therefrom are: apparent porosity 16%, volume density 2.61g/cm
3, cold crushing strength 157MPa, high temperature break resistant intensity 56MPa, its heat-shock resistance, oxidation-resistance are all better.
Claims (1)
1. a β-SiC/Si
2n
2o complex phase is in conjunction with the preparation method of SiC kiln furnitures, it is characterized in that: raw material by weight percentage consists of SiC particle that 25-55% particle diameter is 3-1mm, 10-25% particle diameter is 1-0.2mmSiC particle and 5-25% particle diameter≤0.088mmSiC fine powder, 0-25% metal Si, 5-30% polycrystalline silicon wastes, the spent pulping liquor of additional above-mentioned raw materials total amount 2-6% is as bonding agent;
Wherein in silicon carbide, SiC content is greater than 98%, and in metal Si, Si content is greater than 98%, particle diameter is≤0.088mm; The granularity of described polycrystalline silicon wastes is discrete distribution, be between 1um and 240um, mean particle size is 20um ± 10um, in polycrystalline silicon wastes, contents of free si is 25-60%, and carborundum content is 25-60%, and alumina content is 3-7%, metal Fe content is 1-5%, CaO content is less than 0.5%, and it is 0.5-3% that content of MgO is less than 1%, PEG content;
Preparation method comprises the following steps:
A. various raw material is taken by proportioning, the SiC particle of load weighted 3-1mm in advance and 1-0.2mmSiC granulated aggregate are mixed to pour in wheel roller and mixes further, stop after 3 ~ 5min stirring, pour the half weighing the bonding agent prepared in advance into wheel roller, open switch again and stir 5min, make bonding agent be evenly distributed on particle surface; Then load weighted SiC fine powder, polycrystalline silicon wastes are poured into wheel roller and stirred 5min, more remaining bonding agent is all poured into wherein continuation stirring 8-12min, stop stirring;
B. the raw material vibrating forming machine mixed or friction press are pressed into firebrick billet;
C. the firebrick billet of forming is put into moisture eliminator 110 ± 10 DEG C of dry 24-48h, control moisture content below 0.5%;
D. preparation β-SiC/Si is burnt till under obtained adobe being buried carbon condition at 1200-1500 DEG C
2n
2o complex phase is in conjunction with SiC refractory brick.
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|---|---|---|---|---|
| CN104313678B (en) * | 2014-10-14 | 2017-04-26 | 武汉科技大学 | Whisker-like SiC/Si3N4/Si2N2O composite powder and preparation method thereof |
| CN106431431A (en) * | 2016-08-31 | 2017-02-22 | 江苏诺明高温材料股份有限公司 | In-situ generating method for Si2N2O ceramic bonding phases in aluminum-carbon fireproof material with carbon thermal reduction method |
| CN106966732B (en) * | 2017-03-09 | 2021-03-23 | 平顶山学院 | Fine powder silicon carbide ceramic and preparation method thereof |
| CN108275969B (en) * | 2018-01-31 | 2020-04-07 | 景德镇陶瓷大学 | Mullite-silicon carbide whisker composite ceramic material taking natural minerals as raw materials and preparation method thereof |
| CN109293373B (en) * | 2018-10-23 | 2021-05-28 | 河南省衡锐佳新材料科技有限公司 | Preparation of environment-friendly silicon-based additive and application method of environment-friendly silicon-based additive in refractory material |
| CN110981510A (en) * | 2019-12-18 | 2020-04-10 | 宜兴市丁山耐火器材有限公司 | Silicon oxynitride and silicon carbide combined refractory brick and preparation method thereof |
| CN114988879B (en) * | 2022-06-30 | 2023-03-21 | 中钢集团洛阳耐火材料研究院有限公司 | Large-scale complex-phase reaction sintered silicon carbide product and preparation method thereof |
| CN115215654B (en) * | 2022-07-01 | 2023-04-07 | 偃师中岳耐火材料有限公司 | Preparation method of high-wettability graphite-based composite powder |
| CN116396084A (en) * | 2023-03-20 | 2023-07-07 | 宜兴金君耐火炉料有限公司 | Preparation method of silicon oxynitride-silicon carbide composite brick for producing low-oxygen copper rod |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101602607A (en) * | 2009-06-21 | 2009-12-16 | 贾剑光 | Cement kiln preheaters complex nitride based on silicon carbide link plate and method for cooking |
| CN102275925A (en) * | 2011-06-09 | 2011-12-14 | 东北大学 | Method for sintering silicon carbide through crystalline silicon cutting waste material nitridation reaction |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101602607A (en) * | 2009-06-21 | 2009-12-16 | 贾剑光 | Cement kiln preheaters complex nitride based on silicon carbide link plate and method for cooking |
| CN102275925A (en) * | 2011-06-09 | 2011-12-14 | 东北大学 | Method for sintering silicon carbide through crystalline silicon cutting waste material nitridation reaction |
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