CN103880448A - Large casting-molding self-combined silicon carbide product - Google Patents
Large casting-molding self-combined silicon carbide product Download PDFInfo
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Abstract
The invention relates to a large casting-molding self-combined silicon carbide product. The method comprises the following steps: taking silicon carbon particulates and fine powder, silicon carbon powder, silica powder, silicon powder, carbon black, molybdenum disilicide micro powder, active magnesium oxide and a water reducer as powder; by taking ludox as a binding agent, molding by adopting a vibrating casting manner; sintering the molded green body under a protective atmosphere after conserving and baking, wherein the highest sintering temperature is 1300-1500 DEG C; sintering and cooling to room temperature along with a furnace, so as to prepare the self-combined silicon carbide product. The large and profile self-combined silicon carbide product can be prepared, and has the advantages that the size and the shape of the product are not limited, performance is excellent, and the like, and the prepared self-combined silicon carbide product can be applied to the fields such as a blast-furnace tuyere and a cooling wall tile in the iron and steel industry and an aluminum electrolytic cell in the non-ferrous industry.
Description
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 special-shapedly from combined silicon carbide product, prepared silicon carbide articles can be applicable to the field such as steel industry blast-furnace tuyere and cooling wall inlaid brick, coloured industry aluminium cell.
Background technology
The advantage such as the strong and wear resistance at elevated temperature of the liquation erosional competencyes such as 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, anti-slag and zinc-aluminium copper-lead is good, has application prospect very widely at aspects such as smelting iron and steel, non-ferrous metal metallurgy, ceramic industries.The combination of silicon carbide articles comprises that oxide compound, in conjunction with, nitride bonded and from combination, be combined and compare with oxide compound, nitride bonded and there is more excellent high-temperature behavior and erosion-resisting characteristics from combination,
Nitride combined silicon carbide goods generate 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 reduce, void content reduce.Silicon powder nitride is thermopositive reaction, and the slightly improper local temperature that easily causes of nitridation process control is too high, makes silica flour fusing stop up pore.It is very difficult that above-mentioned two aspect effects make to become compared with the nitrogenizing reaction of thick product inside.Therefore, adopt silica flour nitridation in situ to generate the control of nitride combined silicon carbide material generating process and have relatively high expectations, it is complete that dimensional thickness is difficult to nitrogenize 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 high temperature under between carbon raw material and silica flour reaction in－situ produce silicon carbide whisker and produce combination, its reaction is carried out between material internal material, in preparation process, do not have external reactant gases to infiltrate condition restriction, thereby be 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 ", conventionally adopt combination from combined silicon carbide product at present, pass through mechanical pressing, thereby limited to a certain extent its size and dimension, hinder it and applied.
Compared with mechanical pressing, casting has the advantages such as less investment, molding mode is flexible, moulded products size and dimension is unrestricted, aspect the large-scale fire resistive material product of preparation, has unique advantage.Be applied to about pouring forming technology the problem existing when the combined silicon carbide product and do following explanation: 1) adopt the bonding agent such as cement, hydrated aluminum oxide, unavoidable introducing except SiC and SiO when casting
2impurity in addition, high-temperature behavior and the resistance to fouling etc. of reduction material.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 conventionally, and then makes its base substrate produce intensity.Compared with introducing alkaline-earth metal ions, adjust the curing base substrate of pH value and only depend on silicon-dioxide Coagulating binding each other, low being difficult to of intensity meets the requirements such as carrying, makes material internal in the operation process before the bakings such as form removal easily produce defect, increased the scrap rate of material.It is higher that alkaline-earth metal ions solidifies blank strength, but Ca
2+or Mg
2+be unfavorable for material at high temperature performance Deng the introducing of foreign ion.How, in the situation that introducing minute quantity impurity, make material reach the key that higher blank strength is such articulated system successful Application.2) generation of in-situ carburization silicon is mainly two reaction: Si and C direct reaction and mass transferring in gas phase generation SiC.Generate SiC with Si with C direct reaction and compare, the SiC generating 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 fibrous whisker generation.Generation pattern from combined silicon carbide product situ silicon carbide has decisive influence to its mechanical property etc., and how promoting in-situ carburization silicon to be evenly distributed in whole material with crystal whisker-shaped is to prepare the key of high-performance from combined silicon carbide product.3) after combined silicon carbide product moulding, must contain some amount carbon source, the carbon sources such as crystalline flake graphite, coke are poor by wettability, and while causing material casting after adding, mobility variation, water requirement significantly increase, and have reduced material property.Pitch when particularly ball pitch is to moulding water requirement and flowability affects little, but it has increased material compared with high-volatile and has burnt 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) quantity of adding silica flour and carbon raw material in material has determined to generate quantity from combined silicon carbide product situ silicon carbide, increasing in-situ carburization silicon generation quantity can improve from combined silicon carbide product performance, but in-situ carburization silicon quantity is not The more the better, this is owing to too much significantly having reduced material volume density adding of carbon raw material, in-situ carburization silicon enhancement can not make up the disadvantageous effect that material density reduces, thereby is unfavorable for the raising of material property.In-situ carburization silicon generates quantity and has 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 to 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, additional activated magnesia, water reducer and silicon sol composition; Described carbon black is middle particle pyrolysis method carbon black, i.e. N900 series carbon black; Described molybdenum disilicide micro mist granularity requirements≤5 μ m; 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 to select 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 μ m.
Described fine silica powder Chemical Composition requires SiO
2>=95.0%, particle diameter requires≤1 μ m.Described silica flour chemical composition requires Si >=95.0%, particle diameter requirement≤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 type 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 is controlled 60 ~ 90% according to vibrational flow value.Adopt the moulding of vibrating casting method.After moulding, base substrate is after maintenance, drying; in atmosphere furnace, heat and burn till; base substrate should be under protective atmosphere in sintering process; to avoid the oxidation of carbon black, silica flour and carbide fine powder; heat temperature raising process is continuous warming; maximum sintering temperature is 1300 ~ 1500 ℃, and the treatment time is adjusted according to product size size.Burn till cool to the furnace can make after room temperature this from combined silicon carbide product.
In the present invention, fine silica powder, silicon carbide micro-powder and carbon black are compound adds, and has optimized the size composition of mould material matrix, makes the size composition of its fine powder part more reasonable, the flowing property while having improved moulding.Silicon carbide micro-powder be added in the add-on that has reduced to a certain extent fine silica powder, make the carborundum content of material higher, material is sublimate more.
The present invention adopts casting, and silicon sol used, in conjunction with belonging to non-cement articulated system, has avoided traditional casting aluminous cement bonding agent at high temperature to generate the detrimentally affect of eutectic.The present invention has added activated magnesia and fine silica powder simultaneously, and has adopted silicon sol to make bonding agent.By the Mg generating 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 adding when 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 series carbon black is that Sweet natural gas (methane) thermo-cracking under 1300 ℃ ~ 1400 ℃ high temperature generates, and has the feature of large particle diameter, low structure and low specific surface area.Flowability affects while adding this series carbon black to material casting is very little, has both guaranteed that carbon was uniformly distributed in whole material, has avoided again adopting the disadvantageous effect of 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 between reactant, to there is higher contact area, under high temperature, increase SiO gaseous phase partial pressure, promoted gas-phase reaction to generate SiC, made silicon carbide be fibrous whisker more and be evenly distributed in material.The appropriate molybdenum disilicide micro mist adding has played the effect that generates in-situ carburization Si catalyst, has improved the generation pattern of in-situ carburization silicon wafer palpus, it is distributed in 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 to select 3-5%.Above-mentioned carbon black add-on is very little on the flowing property impact of mould material, has guaranteed the generation of some amount in-situ carburization silicon on the basis that does not reduce material compactness, makes 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) they 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) they 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) they 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) they 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) they 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 above-mentioned powder is proportionally fully mixed, add SiO
2content is 25% alkaline sodium type silicon sol, adjusts respectively the mass percent that its vibrational flow value accounts for powder at silicon sol that 60 ~ 90%, embodiment, 1 ~ embodiment 5 adds and is respectively: 7.0%, 6.3%, 7.5%, 6.0% and 7.2%.After adding silicon sol, fully mix, silicon sol is wrapped in around particle and powder uniformly.Add vibration limit in limit in mould to feed in raw material in the material mixing, mould material is filled in whole mould uniformly.After moulding, base substrate is after maintenance, drying, and in atmosphere furnace, protective atmosphere system heating is burnt till, cool to the furnace can make after room temperature this from combined silicon carbide product.
Claims (6)
1. a casting is large-scale from combined silicon carbide product, 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 composition; Described carbon black is middle particle pyrolysis method carbon black, i.e. N900 series carbon black; Described molybdenum disilicide micro mist granularity≤5 μ m; 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 is controlled 60 ~ 90% according to vibrational flow value; Adopt the moulding of vibrating casting method; After moulding base substrate through maintenance, dry after, in atmosphere furnace, heat and burn till, base substrate in sintering process under protective atmosphere, to avoid the oxidation of carbon black, silica flour and carbide fine powder; Heat temperature raising process is continuous warming, and maximum sintering temperature is 1300 ~ 1500 ℃; After burning till, cooling to room temperature with the furnace can make this from combined silicon carbide product;
The weight percent of Raw of the present invention 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 is preferentially selected 1.5-2.5%, and silica flour add-on is preferentially selected 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 μ m.
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 diameter requires≤1 μ m; Described silica flour chemical composition requires Si>=95.0%, particle diameter requirement≤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 type silicon sol, SiO
2content range is 20-31%, preferentially selects SiO
2content is the silicon sol of 24-26%.
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| CN107324821A (en) * | 2017-07-12 | 2017-11-07 | 瑞泰科技股份有限公司 | It is a kind of that there is high-absorbility, the CFB boiler water-cooling wall carborundum wear-resistant castable of high heat conductance |
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