CN103880448B - A kind of casting is large-scale from combined silicon carbide product - Google Patents

A kind of casting is large-scale from combined silicon carbide product Download PDF

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CN103880448B
CN103880448B CN201410116797.1A CN201410116797A CN103880448B CN 103880448 B CN103880448 B CN 103880448B CN 201410116797 A CN201410116797 A CN 201410116797A CN 103880448 B CN103880448 B CN 103880448B
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silicon carbide
powder
silicon
carbon black
scale
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CN103880448A (en
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李志刚
禄向阳
王守业
张振燕
惠先磊
王鹏
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Sinosteel Luoyang Institute of Refractories Research Co Ltd
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Sinosteel Luoyang Institute of Refractories Research Co Ltd
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Abstract

The present invention relates to a kind of casting large-scale from combined silicon carbide product.The present invention for powder, using silicon sol as bonding agent, adopts vibrating casting shaping with silicon-carbide particle and fine powder, silicon carbide micro-powder, fine silica powder, silica flour, carbon black, molybdenum disilicide micro mist, activated magnesia and water reducer.Shaping rear base substrate is after maintenance, drying, and burn till under protective atmosphere, maximum sintering temperature is 1300 ~ 1500 DEG C, burns till after cooling to room temperature with the furnace obtained this from combined silicon carbide product.The present invention can prepare large-scale, special-shaped from combined silicon carbide product, there is product size and the advantage such as shape is unrestricted, excellent performance, preparedly can be applicable to steel industry blast-furnace tuyere and the field such as cooling wall inlaid brick, coloured industry aluminium cell from combined silicon carbide product.

Description

A kind of casting is large-scale from combined silicon carbide product
Technical field
The invention belongs to technical field of inorganic nonmetallic materials.Be specifically related to a kind of casting large-scale from combined silicon carbide product, can prepare large-scale or abnormal shape from combined silicon carbide product, prepared silicon carbide articles can be applicable to steel industry blast-furnace tuyere and the field such as cooling wall inlaid brick, coloured industry aluminium cell.
Background technology
SiC based refractories has that hot strength is high, thermal conductivity is high, thermal expansivity is low, thermal shock resistance is good, alkali resistant erosion performance is good, the liquation erosional competency such as anti-slag and zinc-aluminium copper-lead is strong and the advantage such as wear resistance at elevated temperature is good, has application prospect widely in smelting iron and steel, non-ferrous metal metallurgy, ceramic industry etc.The combination of silicon carbide articles comprises oxide compound combination, nitride bonded and certainly combines, and compared with combining with oxide compound, nitride bonded and certainly combination have more excellent high-temperature behavior and erosion-resisting characteristics,
Nitride combined silicon carbide goods are generated the nitride such as silicon nitride and produce bonding strength by silica flour nitridation in situ in preparation process, the abundant nitrogenize of silica flour is the key of these goods of preparation.Along with the carrying out of silicon powder nitride, in material, air vent aperture reduction, void content reduce.Silicon powder nitride is thermopositive reaction, and it is too high that nitridation process controls the slightly improper local temperature that easily causes, and makes silica flour melt blocking pore.Above-mentioned two aspect effects make compared with the nitrogenizing reaction of thick product inside become very difficult.Therefore, adopt silica flour nitridation in situ to generate nitride combined silicon carbide material generating process control overflow higher, it is complete that dimensional thickness is difficult to nitrogenize at more than 250mm, easily occurs residual silicon and affect product performance.Above shortcoming makes silica flour nitridation in situ technique cannot prepare the nitride combined silicon carbide goods of large-size.
Compared with nitride combined silicon carbide goods, from silicon carbide by reaction in－situ production silicon carbide whisker generation combination between carbon raw material and silica flour under high temperature, its reaction is carried out between material internal material, do not have external reactant gases to infiltrate condition restriction in preparation process, be thus more suitable for preparing large-size, complex-shaped silicon carbide articles.As described in " ZL200910227624.6 carborundum content be greater than 92% from combined silicon carbide product and preparation method thereof ", usually combination is adopted at present from combined silicon carbide product, pass through mechanical pressing, thus limit its size and dimension to a certain extent, hinder it and apply.
Compared with mechanical pressing, casting has the advantages such as less investment, molding mode is flexible, moulded products size and dimension is unrestricted, in the large-scale fire resistive material product of preparation, have unique advantage.About pouring forming technology be applied to from combined silicon carbide product time Problems existing do following explanation: 1) adopt the bonding agent such as cement, hydrated aluminum oxide during casting, to introduce except SiC and SiO unavoidably 2impurity in addition, the high-temperature behavior of reduction material and resistance to fouling etc.For from combined silicon carbide product, silicon sol is most suitable bonding agent, and silicon sol solidifies by adjusting its pH value or introducing alkaline-earth metal ions usually, and then makes its base substrate produce intensity.Compared with introducing alkaline-earth metal ions, the base substrate of adjusted to ph solidification is only by silicon-dioxide Coagulating binding each other, intensity low being difficult to meets the requirements such as carrying, makes material internal in the operation process before the bakings such as form removal easily produce defect, adds the scrap rate of material.Alkaline-earth metal ions solidification blank strength is higher, but Ca 2+or Mg 2+introducing Deng foreign ion is unfavorable for material at high temperature performance.How when introducing minute quantity impurity, material is reached key that higher blank strength is such articulated system successful Application.2) generation of in-situ carbon SiClx mainly two reactions: Si and C direct reaction and mass transferring in gas phase generate SiC.Generate SiC with Si with C direct reaction to compare, the SiC generated by mass transferring in gas phase mostly is fibrous whisker, is more conducive to the improvement of material property.In material, the existence of SiO gas is the key that mass transferring in gas phase generates SiC, improves SiO partial pressure and is more conducive to the generation of fibrous whisker.Have decisive influence from the generation pattern of combined silicon carbide product situ silicon carbide to its mechanical property etc., how promoting that in-situ carbon SiClx is evenly distributed in whole material with crystal whisker-shaped is prepare the key of high-performance from combined silicon carbide product.3) must contain some amount carbon source after combined silicon carbide product is shaping, being spontaneously wet out by water property of the carbon source such as crystalline flake graphite, coke difference, when causing material casting after adding, mobility is deteriorated, water requirement significantly increases, and reduces material property.Pitch particularly ball pitch on shaping hourly water demand and mobility impact little, but its comparatively high-volatile increase material and burn posterior spiracle rate, unfavorable to the many performances of material.Visible, the selection of suitable carbon source is to most important from combined silicon carbide product.4) in material add silica flour and carbon raw material quantity determine and generate quantity from combined silicon carbide product situ silicon carbide, increasing in-situ carbon SiClx generation quantity can improve from combined silicon carbide product performance, but in-situ carbon SiClx quantity is not The more the better, this is because adding of too much carbon raw material considerably reduces material volume density, in-situ carbon SiClx enhancement can not make up the disadvantageous effect that material density reduces, thus is unfavorable for the raising of material property.In-situ carbon SiClx generates quantity and there is an OK range.
Summary of the invention
For the problems referred to above, the present invention proposes a kind of casting large-scale from combined silicon carbide product, the present invention can prepare large-size, complex-shaped from carborundum refractory material.
Object of the present invention is achieved through the following technical solutions: described casting is large-scale is be raw material by silicon-carbide particle and fine powder, silicon carbide micro-powder, fine silica powder, silica flour, carbon black and molybdenum disilicide micro mist from combined silicon carbide product, and additional activated magnesia, water reducer and silicon sol form; Described carbon black is middle particle pyrolysis method carbon black, i.e. N900 series carbon black; Described molybdenum disilicide powder size requires≤5 μm; Described activated magnesia chemical composition requires MgO >=92.0%, tap density≤0.1g/ml;
In the present invention, the weight percent of each raw material is:
Silicon-carbide particle 65 ~ 75%
Carbide fine powder 8 ~ 20%
Silicon carbide micro-powder 2 ~ 7%
Fine silica powder 2 ~ 5%
Silica flour 1 ~ 8%
Carbon black 0.5 ~ 4%
Molybdenum disilicide micro mist 0.3 ~ 1%
Activated magnesia is additional, and add-on is the 0.03-0.06% of raw material gross weight
Water reducer is additional, and add-on is the 0.05-0.12% of raw material gross weight
Silicon sol is additional;
The gross weight of goods raw material is 100%.
In the present invention, carbon black add-on preferentially selects 1.5-2.5%, silica flour add-on preferentially selects 3-5%.
The chemical composition of silicon-carbide particle described in the present invention and fine powder requires as SiC >=95%.The size range of silicon-carbide particle is 3 ~ 0.088mm, and carbide fine powder size range is 0.044 ~ 0.020mm.Described silicon carbide micro-powder Chemical Composition requires SiC >=94.0%, and granularity requirements is less than 5 μm.
Described fine silica powder Chemical Composition requires SiO 2>=95.0%, Particle size requirements≤1 μm.Described silica flour chemical composition requires Si >=95.0%, Particle size requirements≤0.074mm.
Described water reducer refers to the polyethylene glycol type water reducer CASTMENT FS-20 that BASF Aktiengesellschaft produces.
Described silicon sol is alkaline sodium form silicon sol, SiO 2content range is 20-31%, preferentially selects SiO 2content is the silicon sol of 24-26%.
Above-mentioned particle and powder are proportionally prepared burden, after fully mixing, add silicon sol, silicon sol add-on controls 60 ~ 90% according to vibration flowability.Adopt vibrating casting method shaping.Shaping rear base substrate is after maintenance, drying; heat in atmosphere furnace and burn till; under base substrate should be in protective atmosphere in sintering process; to avoid the oxidation of carbon black, silica flour and carbide fine powder; heating up process is continuous warming; maximum sintering temperature is 1300 ~ 1500 DEG C, and the treatment time adjusts according to product size size.Burn till can obtain after cooling to room temperature with the furnace this from combined silicon carbide product.
In the present invention, fine silica powder, silicon carbide micro-powder and carbon black compound add, and optimize the size composition of mould material matrix, make the size composition of its fine fraction more reasonable, flowing property when improve shaping.Silicon carbide micro-powder be added in the add-on decreasing fine silica powder to a certain extent, make the carborundum content of material higher, material is sublimate more.
The present invention adopts casting, and silicon sol used combines and belongs to non-cement articulated system, avoids the detrimentally affect that traditional casting aluminous cement bonding agent at high temperature generates eutectic.The present invention adds activated magnesia and fine silica powder simultaneously, and have employed silicon sol and make bonding agent.By the Mg generated after activated magnesia aquation 2+, by silicon sol and fine silica powder surface-Si-O -group couples together, and makes material solidification and produces higher blank strength.Activated magnesia specific surface area is large, granularity is tiny, can play good solidification effect and higher blank strength when adding little, simultaneously very little to material at high temperature performance impact.
The present invention's carbon black used is middle particle pyrolysis method carbon black, i.e. N900 series carbon black.This serial carbon black is that Sweet natural gas (methane) thermo-cracking under 1300 DEG C ~ 1400 DEG C high temperature generates, and has the feature of Large stone, low structure and low specific surface area.Add this serial carbon black very little on mobility impact during material casting, both ensure that carbon was uniformly distributed in whole material, and turn avoid the disadvantageous effect adopting the carbon sources such as crystalline flake graphite, coke, pitch.
In the present invention, bonding agent silicon sol is evenly wrapped in around silica flour, carbon black, make that there is between reactant higher contact area, increase SiO gaseous phase partial pressure under high temperature, facilitate gas-phase reaction and generate SiC, make silicon carbide is that fibrous whisker is uniformly distributed in the material more.The appropriate molybdenum disilicide micro mist added serves the effect generating in-situ carburization Si catalyst, improves the generation pattern of in-situ carburization silicon wafer palpus, makes it distribute in the material more even, and then improves bonding strength and the high-temperature behavior of material.
In invention, silica flour add-on is 1 ~ 8%, and carbon black add-on is 0.5 ~ 4%, and wherein carbon black add-on preferentially selects 1.5-2.5%, silica flour add-on preferentially selects 3-5%.The flowing property impact of above-mentioned carbon black add-on on mould material is very little, the basis not reducing material compactness ensure that the generation of some amount in-situ carbon SiClx, make material have more excellent performance.
Embodiment
Illustrate enforcement of the present invention and feature below, but the present invention is not limited to following embodiment.
Embodiment 1: feed composition and proportioning (mass percent) are silicon-carbide particle 75%, carbide fine powder 8%, silicon carbide micro-powder 5%, fine silica powder 2%, silica flour 6%, carbon black 3%, molybdenum disilicide 1%, activated magnesia (additional) 0.04%, water reducer (additional) 0.1%.
Embodiment 2: feed composition and proportioning (mass percent) are silicon-carbide particle 70%, carbide fine powder 15.6%, silicon carbide micro-powder 6%, fine silica powder 3%, silica flour 3.5%, carbon black 1.5%, molybdenum disilicide 0.4%, activated magnesia (additional) 0.05%, water reducer (additional) 0.07%.
Embodiment 3: feed composition and proportioning (mass percent) are silicon-carbide particle 65%, carbide fine powder 15%, silicon carbide micro-powder 2%, fine silica powder 5%, silica flour 8%, carbon black 4%, molybdenum disilicide 1%, activated magnesia (additional) 0.06%, water reducer (additional) 0.12%.
Embodiment 4: feed composition and proportioning (mass percent) are silicon-carbide particle 70%, carbide fine powder 18.2%, silicon carbide micro-powder 7%, fine silica powder 3%, silica flour 1%, carbon black 0.5%, molybdenum disilicide 0.3%, activated magnesia (additional) 0.03%, water reducer (additional) 0.05%.
Embodiment 5: feed composition and proportioning (mass percent) are silicon-carbide particle 65%, carbide fine powder 20%, silicon carbide micro-powder 4%, fine silica powder 4%, silica flour 4.5%, carbon black 2%, molybdenum disilicide 0.5%, activated magnesia (additional) 0.06%, water reducer (additional) 0.08%.
After proportionally fully being mixed by above-mentioned powder, add SiO 2content is the alkaline sodium form silicon sol of 25%, adjusts its vibration flowability respectively 60 ~ 90%, and the mass percent that silicon sol added by embodiment 1 ~ embodiment 5 accounts for powder is respectively: 7.0%, 6.3%, 7.5%, 6.0% and 7.2%.Fully mix after adding silicon sol, silicon sol is wrapped in around particle and powder uniformly.The material mixed is added vibration limit in limit in mould to feed in raw material, mould material is filled in whole mould uniformly.Shaping rear base substrate is after maintenance, drying, and in atmosphere furnace, the heating of protective atmosphere system is burnt till, and can obtain this from combined silicon carbide product after cooling to room temperature with the furnace.

Claims (6)

1. casting is large-scale from a combined silicon carbide product, and the thickness of described silicon carbide articles is at more than 250mm; It is characterized in that described goods are raw material by silicon-carbide particle and fine powder, silicon carbide micro-powder, fine silica powder, silica flour, carbon black and molybdenum disilicide micro mist, additional activated magnesia, water reducer and silicon sol form; Described carbon black is middle particle pyrolysis method carbon black, i.e. N900 series carbon black; Described molybdenum disilicide powder size≤5 μm; Described activated magnesia chemical composition MgO >=92.0%, tap density≤0.1g/ml; Above-mentioned particle and powder are proportionally prepared burden, after fully mixing, add silicon sol, silicon sol add-on controls 60 ~ 90% according to vibration flowability; Adopt vibrating casting method shaping; Shaping rear base substrate, after maintenance, drying, heats and burns till, under base substrate is in protective atmosphere in sintering process, to avoid the oxidation of carbon black, silica flour and carbide fine powder in atmosphere furnace; Heating up process is continuous warming, and maximum sintering temperature is 1300 ~ 1500 DEG C; Cooling to room temperature after burning till with the furnace can obtain this from combined silicon carbide product;
The weight percent of described goods Raw is:
Silicon-carbide particle 65 ~ 75%
Carbide fine powder 8 ~ 20%
Silicon carbide micro-powder 2 ~ 7%
Fine silica powder 2 ~ 5%
Silica flour 1 ~ 8%
Carbon black 0.5 ~ 4%
Molybdenum disilicide micro mist 0.3 ~ 1%
Activated magnesia is additional, and add-on is the 0.03-0.06% of raw material gross weight
Water reducer is additional, and add-on is the 0.05-0.12% of raw material gross weight
Silicon sol is additional;
The gross weight of goods raw material is 100%.
2. a kind of casting according to claim 1 is large-scale from combined silicon carbide product, it is characterized in that: wherein carbon black add-on preferentially selects 1.5-2.5%, and silica flour add-on preferentially selects 3-5%.
3. a kind of casting according to claim 1 is large-scale from combined silicon carbide product, it is characterized in that: the chemical composition of described silicon-carbide particle and fine powder requires as SiC >=95%; The size range of silicon-carbide particle is 3 ~ 0.088mm, and carbide fine powder size range is 0.044 ~ 0.020mm; Described silicon carbide micro-powder Chemical Composition requires SiC >=94.0%, and granularity requirements is less than 5 μm.
4. a kind of casting according to claim 1 is large-scale from combined silicon carbide product, it is characterized in that: described fine silica powder Chemical Composition requires SiO 2>=95.0%, Particle size requirements≤1 μm; Described silica flour chemical composition requires Si>=95.0%, Particle size requirements≤0.074mm.
5. a kind of casting according to claim 1 is large-scale from combined silicon carbide product, it is characterized in that: described water reducer is the polyethylene glycol type water reducer CASTMENT FS-20 that BASF Aktiengesellschaft produces.
6. a kind of casting according to claim 1 is large-scale from combined silicon carbide product, it is characterized in that: described silicon sol is alkaline sodium form silicon sol, selects SiO 2content is the silicon sol of 24-26%.
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