CN104003733A - Preparation method of silicon nitride-combined silicon carbide fireproof material - Google Patents
Preparation method of silicon nitride-combined silicon carbide fireproof material Download PDFInfo
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Abstract
The invention discloses a preparation method of a silicon nitride-combined silicon carbide fireproof material. The preparation method includes steps of material proportioning, moulding, drying and nitridation sintering. The preparation method particularly includes steps of: employing 65%-85% silicon carbide and 15%-35% silicon powder as main raw materials, adding calcium lignosulphonate as a combination agent, feeding the raw materials and the combination agent in an edge runner mill for mixing, carrying out a mechanical press moulding process and a drying process under specific conditions, performing a glue-discharging process and a nitridation sintering process in a vacuum resistance furnace below 1400 DEG C to finally obtain a silicon nitride-combined silicon carbide fireproof material product with a good mechanical performance, a specific content of the silicon nitride and a specific crystal form. Through control of a moulding density, the adding amount of the silicon powder and the sintering conditions, the silicon nitride-combined silicon carbide fireproof material product with the specific content of the silicon nitride and the specific crystal form. The preparation method is reduced in cost and is beneficial to an industrial production.
Description
Technical field
The present invention relates to a kind of refractory materials preparation method, particularly relate to a kind of carborundum refractory preparation method, be applied to novel material production technical field.
Background technology
Silicon carbide articles belongs to high grade refractory, have that physical strength is high, thermal conductivity is high, thermal shock resistance and wearability is good, alkali resistant aggressiveness is good, slag resistance and oxidation-resistance good, and to features such as partial melting metal resistivity are strong, the industrial circles such as iron and steel, nonferrous metallurgy, oil, chemistry, electric power, pottery and aerospace have been widely used in.Silicon carbide is strong covalent bond and thing, and covalent linkage accounts for 88%, and it is difficult to sintering under general technology, often needs to add sintering aid when sintering, or by second-phase the method in conjunction with sintering, could form fine and close carborundum sintered body.The performance of carbofrax material also depends on the bonding state between silicon-carbide particle in material to a great extent.Silicon nitride has similar chemical structure and physical properties to silicon carbide, is strong covalent bond compound with silicon carbide.The thermal expansivity of silicon nitride is little, and oxidation rate is very slow, and hot strength is large, and volume stability is good, has good thermal conductivity, for most chemical substances, all stablizes, and is not melted non-ferrous metal and corrodes, and is the desirable bond material of silicon carbide.Silicon nitride is introduced and in silicon carbide, made silicon nitride combined silicon carbide material, when having kept silicon carbide natural characteristics, can effectively improve the performances such as hot strength, thermal shock resistance and anti-molten iron erosional competency of carbofrax material, and can under the lesser temps of 1200 ~ 1450 ℃, prepare, reaction sintering process is net-shape-sinter, be beneficial to and prepare special-shaped products, adapt to large-scale commercial production.
Although silicon nitride combined with silicon carbide refractory material prepared by reaction sintering has been widely used in iron and steel, coloured and building materials industry, but along with scientific and technological progress, the Technology development of modern industry, the required Working environment of facing of refractory materials is harsh all the more, and this just has higher requirement to the fire-resistant performance of original use.Also there are now a lot of problems in the production of silicon nitride combined with silicon carbide refractory material, as, how to guarantee silica flour nitriding rate, how to control silicon nitride crystalline phase form, how anti-fluid stopping silicon phenomenon generation and how further to improve product strength.
In industrial production, in order to shorten the production cycle, improve nitriding rate, tend to add various sintering aids in raw material, and carry out above sintering at 1400 ℃.The intensity silicon nitride amount of silicon nitride combined with silicon carbide refractory material goods increases and improves, but this higher sintering temperature has limited the add-on of silica flour in raw material, if add in raw material again silicon nitride powder cost can greatly improve.At 1400 ℃, carrying out above sintering, can there is the α crystal conversion of β phase in opposite directions in silicon nitride, and sintering aid also can promote this transformation, and if want to make the silicon nitride combined silicon carbide refractory product of excellent property, in goods, should contain more α phase silicon nitride.
Summary of the invention
In order to solve prior art problem, the object of the invention is to overcome the deficiency that prior art exists, a kind of preparation method of silicon nitride combined with silicon carbide refractory material is provided, being prepared by existing reaction sintering to the method for silicon nitride combined silicon carbide refractory product improves and optimizes, by regulating raw material to form and compact density, under the system of optimizing, carry out nitridation sintered, thereby the speed of controlling metallic silicon power and nitrogen reaction with, to realize the control of the content of silicon nitride in material and crystal formation and to improve nitriding rate.
For reaching foregoing invention, create object, the present invention adopts following technical proposals:
A preparation method for silicon nitride combined with silicon carbide refractory material, comprises the steps:
1. blank preparation: fully mixed by main raw material and binding agent, after ageing mixture, complete again batching, when concrete batching, select silicon carbide and metallic silicon power as main raw material, in main raw material, silicon carbide quality mark is 65%～85%, metallic silicon power massfraction is 15%～35%, silicon-carbide particle and fine powder adopt specific grating, select granularity to be respectively 1.43～2.5 mm, 0.5～1.43 mm, 0～0.5 mm and 240 object sic powders, and be that 2:3:3:2 prepares burden according to the descending mass ratio of different grain size, the granularity of metallic silicon power is 1000 orders, binding agent adopts calcium lignin sulphonate as the bonding agent of main raw material, the add-on of calcium lignin sulphonate be main raw material and binding agent total mass 3%, calcium lignin sulphonate and water are made into 1:1 solution, use wheel roller to carry out batch mixing, the sic powder that by granularity is first 1.43～2.5 mm, 0.5～1.43 mm and 0～0.5 mm is poured in wheel roller, mixing 5min, and then to pouring calcium lignosulfonate solution in wheel roller, granularity is that 240 order silicon carbide micro-powders and granularity are 1000 object metallic silicon powers, mixing 40min, then, approaching under the condition of 16 ℃ after 4～96h ageing mixture, complete blank preparation,
2. forming of green body: the compound that completes batching in above-mentioned steps in is 1. carried out to pressure forming, obtain plain embryo; In preparation during plain embryo, preferably adopt dry-pressing formedly, control pressure can be 53～328 MPa, and pressurize 15s;
3. green compact are dry: under the temperature condition of 40～110 ℃, the plain embryo of preparing in 2. in above-mentioned steps is dried, obtain dried green compact; When preparing green compact, preferred furnace drying method is that biscuit is placed in and in maintaining box, is respectively incubated successively at 40 ℃, 60 ℃, 80 ℃ and 110 ℃ 6h;
4. green compact binder removal: adopt high temperature draft glue discharging furnace, in the temperature range of 200～700 ℃, the green compact of preparing in 3. in above-mentioned steps are being carried out to binder removal; When binder removal, preferably controlling dump temperature is 200～700 ℃, and preferably in the time of 300 ℃ and 600 ℃ time, is respectively incubated respectively 2h;
5. nitridation sintered: under the temperature condition of 1150～1380 ℃, 4. the green compact that complete binder removal in above-mentioned steps in are put into the sealed sintering that sintering oven carries out 36～72h, it is nitrogen that sintering process is used atmosphere, nitrogen gas purity >=99.999%, and to maintain nitrogen pressure in sintering oven be 0.03～0.1MPa, finally obtain silicon nitride combined with silicon carbide refractory material goods; The equipment of nitridation sintered use preferably adopts vacuum resistance furnace,, before sintering, first, by being evacuated to-0.08～-0.09MPa in vacuum resistance furnace, then in vacuum resistance furnace, passes into nitrogen, and maintains nitridation sintered nitrogen atmosphere; Under the temperature condition of 1150～1380 ℃, preferably, heat-up rate according to 2～3 ℃/min heats up, nitridation sintered employing segmentation is sintering successively, within the scope of 1150～1200 ℃, be incubated 5～10h, within the scope of 1200～1300 ℃, be incubated 5～30h, within the scope of 1300～1380 ℃, be incubated 5～30h; Preferably nitridation sintered temperature increasing schedule is: segmentation heats up successively, within the scope of 0～200 ℃, heat-up rate is 5 ℃/min, within the scope of 200～700 ℃, heat-up rate is 3 ℃/min, within the scope of 700～1150 ℃, heat-up rate is 5 ℃/min, and within the scope of 1150～1380 ℃, heat-up rate is 2 ℃/min.
The present invention compared with prior art, has following apparent outstanding substantive distinguishing features and remarkable advantage:
1. the present invention can adopt the silicon carbide of specified particle diameter as aggregate at various forming under the pressure, by specific grating, can not only be dry-pressing formed in very large pressure range, and can also make silica flour be disperseed fully, improve the homogeneity of green compact;
2. the present invention controls density and the void content of green compact by controlling forming pressure, thereby control nitrogen to the speed of material internal diffusion, in conjunction with regulating the content of silica flour in goods, control speed of response, when avoiding local reaction heat release too much to cause silica flour to melt, the control of realization to the content of silicon nitride in goods and crystal formation, improves nitriding rate;
3. the present invention carries out sintering 1400 ℃ of following temperature, reduces silicon nitride the α crystal conversion of β phase in opposite directions occurs, and makes the silicon nitride combined silicon carbide refractory product of excellent property, reduces the cost of preparation simultaneously;
4. the silicon nitride combined with silicon carbide refractory material goods that prepared by the present invention increase in mechanical property, less demanding to raw material, and preparation process is simple, with low cost, and sintering temperature is low, is beneficial to and realizes suitability for industrialized production.
Embodiment
Details are as follows for the preferred embodiments of the present invention:
embodiment mono-:
In the present embodiment, select granularity to be respectively 1.43～2.5mm, 0.5～1.43mm, 0～0.5mm and 240 object silicon carbide and form gradating material, mass ratio is 2:3:3:2, and silicon carbide quality mark is that 85%, 1000 order silica flour massfraction is 15%, the silicon carbide of each granularity and silica flour purity >=98%, 240 order silicon carbide d50 are 32.718 μ m, and 1000 order silica flour d50 are 4.694 μ m, and calcium lignin sulphonate is not counted in total mass, add-on is total mass 3%, and calcium lignin sulphonate and water are made into 1:1 solution.Use wheel roller to carry out batch mixing, during batch mixing, first the silicon carbide of 1.43～2.5 mm, 0.5～1.43 mm and 0～0.5 mm is poured in wheel roller, mixing 5min, then pours calcium lignosulfonate solution, 240 order silicon carbide and 1000 object metallic silicon powers into, mixing 40min.After mixed material under 16 ℃ of conditions ageing mixture 4h, use four-column hydraulic press dry-pressing formed, forming pressure 53MPa, dwell time 15s, system is of a size of the batten of 25mm * 25mm * 150mm.Batten is dried in climatic chamber, and oven dry system is 40 ℃, 60 ℃, 80 ℃ and 110 ℃ of each 6h.Style after oven dry is put into test furnace, is evacuated to-0.08～-0.09MPa, then passes into nitrogen, and nitrogen gas purity >=99.999% maintains nitridation sintered nitrogen atmosphere malleation 0.03～0.1MPa.The heating that switches on power, heat-up rate is 5 ℃/min within the scope of 0～200 ℃; Within the scope of 200～700 ℃, heat-up rate is 2 ℃/min, is wherein respectively incubated 2h at 300 ℃ and 600 ℃ and carries out binder removal; Within the scope of 700～1150 ℃, heat-up rate is 5 ℃/min, is incubated 5h at 1150 ℃; Within the scope of 1150～1350 ℃, heat-up rate is 3 ℃/min, is incubated 5h at 1200 ℃, is incubated 20h at 1300 ℃, is incubated 10h at 1380 ℃, carries out segmentation nitridation sintered.Powered-down, is cooled to below 60 ℃, takes out sample.Burn till rear sample without dimensional change.
The present embodiment obtains the silicon nitride combined with silicon carbide refractory material goods with specific crystal formation content and silicon nitride content by controlling compact density, silicon powder doping quantity and sintering schedule.The present embodiment method comprises batching, moulding, dries and burns till, specifically take silicon carbide and silica flour as main raw material, take calcium lignin sulphonate as bonding agent, raw material is put into wheel roller mixing, mechanical pressing, then under specific system, dry, in vacuum resistance furnace, experience binder removal and nitridation sintered, finally obtain that specific silicon nitride that mechanical property is good forms and the silicon nitride combined with silicon carbide refractory material goods of crystal formation.
embodiment bis-:
The present embodiment and embodiment mono-are basic identical, and special feature is:
In the present embodiment, select granularity to be respectively 1.43～2.5mm, 0.5～1.43mm, 0～0.5mm and 240 object silicon carbide and form gradating material, mass ratio is 2:3:3:2, and silicon carbide quality mark is that 80%, 1000 order silica flour massfraction is 20%, the silicon carbide of each granularity and silica flour purity >=98%, 240 order silicon carbide d50 are 32.718 μ m, and 1000 order silica flour d50 are 4.694 μ m, and calcium lignin sulphonate is not counted in total mass, add-on is total mass 3%, and calcium lignin sulphonate and water are made into 1:1 solution.Use wheel roller to carry out batch mixing, during batch mixing, first the silicon carbide of 1.43～2.5 mm, 0.5～1.43 mm and 0～0.5 mm is poured in wheel roller, mixing 5min, then pours calcium lignosulfonate solution, 240 order silicon carbide and 1000 object metallic silicon powers into, mixing 40min.After mixed material under 16 ℃ of conditions ageing mixture 10h, use four-column hydraulic press dry-pressing formed, forming pressure 73MPa, dwell time 15s, system is of a size of the batten of 25mm * 25mm * 150mm.Batten is dried in climatic chamber, and oven dry system is 40 ℃, 60 ℃, 80 ℃ and 110 ℃ of each 6h.Style after oven dry is put into test furnace, is evacuated to-0.08～-0.09MPa, then passes into nitrogen, and nitrogen gas purity >=99.999% maintains nitridation sintered nitrogen atmosphere malleation 0.03～0.1MPa.The heating that switches on power, heat-up rate is 5 ℃/min within the scope of 0～200 ℃; Within the scope of 200～700 ℃, heat-up rate is 2 ℃/min, is wherein respectively incubated 2h at 300 ℃ and 600 ℃ and carries out binder removal; Within the scope of 700～1150 ℃, heat-up rate is 5 ℃/min, is incubated 5h at 1150 ℃; Within the scope of 1150～1350 ℃, heat-up rate is 3 ℃/min, is incubated 5h at 1200 ℃, is incubated 10h at 1250 ℃, is incubated 20h at 1300 ℃, is incubated 10h at 1380 ℃, carries out segmentation nitridation sintered.Powered-down, is cooled to below 60 ℃, takes out sample.Burn till rear sample without dimensional change.
embodiment tri-:
The present embodiment and previous embodiment are basic identical, and special feature is:
In the present embodiment, select granularity to be respectively 1.43～2.5mm, 0.5～1.43mm, 0～0.5mm and 240 object silicon carbide and form gradating material, mass ratio is 2:3:3:2, and silicon carbide quality mark is that 75%, 1000 order silica flour massfraction is 25%, the silicon carbide of each granularity and silica flour purity >=98%, 240 order silicon carbide d50 are 32.718 μ m, and 1000 order silica flour d50 are 4.694 μ m, and calcium lignin sulphonate is not counted in total mass, add-on is total mass 3%, and calcium lignin sulphonate and water are made into 1:1 solution.Use wheel roller to carry out batch mixing, during batch mixing, first the silicon carbide of 1.43～2.5 mm, 0.5～1.43 mm and 0～0.5 mm is poured in wheel roller, mixing 5min, then pours calcium lignosulfonate solution, 240 order silicon carbide and 1000 object metallic silicon powers into, mixing 40min.After mixed material under 16 ℃ of conditions ageing mixture 15h, use four-column hydraulic press dry-pressing formed, forming pressure 113MPa, dwell time 15s, system is of a size of the batten of 25mm * 25mm * 150mm.Batten is dried in climatic chamber, and oven dry system is 40 ℃, 60 ℃, 80 ℃ and 110 ℃ of each 6h.Style after oven dry is put into test furnace, is evacuated to-0.08～-0.09MPa, then passes into nitrogen, and nitrogen gas purity >=99.999% maintains nitridation sintered nitrogen atmosphere malleation 0.03～0.1MPa.The heating that switches on power, heat-up rate is 5 ℃/min within the scope of 0～200 ℃; Within the scope of 200～700 ℃, heat-up rate is 2 ℃/min, is wherein respectively incubated 2h at 300 ℃ and 600 ℃ and carries out binder removal; Within the scope of 700～1150 ℃, heat-up rate is 5 ℃/min, is incubated 5h at 1150 ℃; Within the scope of 1150～1350 ℃, heat-up rate is 3 ℃/min, is incubated 10h at 1200 ℃, is incubated 10h at 1250 ℃, is incubated 20h at 1300 ℃, is incubated 10h at 1380 ℃, carries out segmentation nitridation sintered.Powered-down, is cooled to below 60 ℃, takes out sample.Burn till rear sample without dimensional change.
embodiment tetra-:
The present embodiment and previous embodiment are basic identical, and special feature is:
In the present embodiment, select granularity to be respectively 1.43～2.5mm, 0.5～1.43mm, 0～0.5mm and 240 object silicon carbide and form gradating material, mass ratio is 2:3:3:2, and silicon carbide quality mark is that 75%, 1000 order silica flour massfraction is 25%, the silicon carbide of each granularity and silica flour purity >=98%, 240 order silicon carbide d50 are 32.718 μ m, and 1000 order silica flour d50 are 4.694 μ m, and calcium lignin sulphonate is not counted in total mass, add-on is total mass 3%, and calcium lignin sulphonate and water are made into 1:1 solution.Use wheel roller to carry out batch mixing, during batch mixing, first the silicon carbide of 1.43～2.5 mm, 0.5～1.43 mm and 0～0.5 mm is poured in wheel roller, mixing 5min, then pours calcium lignosulfonate solution, 240 order silicon carbide and 1000 object metallic silicon powers into, mixing 40min.After mixed material under 16 ℃ of conditions ageing mixture 15h, use four-column hydraulic press dry-pressing formed, forming pressure 127MPa, dwell time 15s, system is of a size of the batten of 25mm * 25mm * 150mm.Batten is dried in climatic chamber, and oven dry system is 40 ℃, 60 ℃, 80 ℃ and 110 ℃ of each 6h.Style after oven dry is put into test furnace, is evacuated to-0.08～-0.09MPa, then passes into nitrogen, and nitrogen gas purity >=99.999% maintains nitridation sintered nitrogen atmosphere malleation 0.03～0.1MPa.The heating that switches on power, heat-up rate is 5 ℃/min within the scope of 0～200 ℃; Within the scope of 200～700 ℃, heat-up rate is 2 ℃/min, is wherein respectively incubated 2h at 300 ℃ and 600 ℃ and carries out binder removal; Within the scope of 700～1150 ℃, heat-up rate is 5 ℃/min, is incubated 10h at 1150 ℃; Within the scope of 1150～1350 ℃, heat-up rate is 3 ℃/min, is incubated 10h at 1200 ℃, is incubated 15h at 1300 ℃, is incubated 10h at 1380 ℃, carries out segmentation nitridation sintered.Powered-down, is cooled to below 60 ℃, takes out sample.Burn till rear sample without dimensional change.
embodiment five:
The present embodiment and previous embodiment are basic identical, and special feature is:
In the present embodiment, select granularity to be respectively 1.43～2.5mm, 0.5～1.43mm, 0～0.5mm and 240 object silicon carbide and form gradating material, mass ratio is 2:3:3:2, and silicon carbide quality mark is that 75%, 1000 order silica flour massfraction is 25%, the silicon carbide of each granularity and silica flour purity >=98%, 240 order silicon carbide d50 are 32.718 μ m, and 1000 order silica flour d50 are 4.694 μ m, and calcium lignin sulphonate is not counted in total mass, add-on is total mass 3%, and calcium lignin sulphonate and water are made into 1:1 solution.Use wheel roller to carry out batch mixing, during batch mixing, first the silicon carbide of 1.43～2.5 mm, 0.5～1.43 mm and 0～0.5 mm is poured in wheel roller, mixing 5min, then pours calcium lignosulfonate solution, 240 order silicon carbide and 1000 object metallic silicon powers into, mixing 40min.After mixed material under 16 ℃ of conditions ageing mixture 15h, use four-column hydraulic press dry-pressing formed, forming pressure 177MPa, dwell time 15s, system is of a size of the batten of 25mm * 25mm * 150mm.Batten is dried in climatic chamber, and oven dry system is 40 ℃, 60 ℃, 80 ℃ and 110 ℃ of each 6h.Style after oven dry is put into test furnace, is evacuated to-0.08～-0.09MPa, then passes into nitrogen, and nitrogen gas purity >=99.999% maintains nitridation sintered nitrogen atmosphere malleation 0.03～0.1MPa.The heating that switches on power, heat-up rate is 5 ℃/min within the scope of 0～200 ℃; Within the scope of 200～700 ℃, heat-up rate is 2 ℃/min, is wherein respectively incubated 2h at 300 ℃ and 600 ℃ and carries out binder removal; Within the scope of 700～1150 ℃, heat-up rate is 5 ℃/min, is incubated 10h at 1150 ℃; Within the scope of 1150～1350 ℃, heat-up rate is 3 ℃/min, is incubated 10h at 1200 ℃, is incubated 20h at 1300 ℃, is incubated 10h at 1380 ℃, carries out segmentation nitridation sintered.Powered-down, is cooled to below 60 ℃, takes out sample.Burn till rear sample without dimensional change.
Above the embodiment of the present invention is illustrated; but the invention is not restricted to above-described embodiment; can also make multiple variation according to the object of innovation and creation of the present invention; the change of making under all spirit according to technical solution of the present invention and principle, modification, substitute, combination, simplify; all should be equivalent substitute mode; as long as goal of the invention according to the invention; only otherwise deviate from the preparation method's of silicon nitride combined with silicon carbide refractory material of the present invention know-why and inventive concept, all belong to protection scope of the present invention.
Claims (9)
1. a preparation method for silicon nitride combined with silicon carbide refractory material, is characterized in that, comprises the steps:
1. batching is prepared: by main raw material and binding agent, fully mixed, after ageing mixture, complete again batching, when concrete batching, select silicon carbide and metallic silicon power as main raw material, in main raw material, silicon carbide quality mark is 65%～85%, metallic silicon power massfraction is 15%～35%, silicon-carbide particle adopts specific grating, select granularity to be respectively 1.43～2.5 mm, 0.5～1.43 mm, 0～0.5 mm and 240 object sic powders, and be that 2:3:3:2 carries out silicon-carbide particle mix according to the descending mass ratio of different grain size, the granularity of metallic silicon power is 1000 orders, binding agent adopts calcium lignin sulphonate as the bonding agent of main raw material, the add-on of calcium lignin sulphonate be main raw material and binding agent total mass 3%, calcium lignin sulphonate and water are made into 1:1 solution,
2. forming of green body: the compound that completes batching in above-mentioned steps in is 1. carried out to pressure forming, obtain plain embryo;
3. green compact are dry: under the temperature condition of 40～110 ℃, the plain embryo of preparing in 2. in above-mentioned steps is dried, obtain dried raw embryo;
4. green compact binder removal: adopt high temperature draft glue discharging furnace, in the temperature range of 200～700 ℃, the green compact of preparing in 3. in above-mentioned steps are being carried out to binder removal;
5. nitridation sintered: under the temperature condition of 1150～1380 ℃, 4. the green compact that complete binder removal in above-mentioned steps in are put into the sealed sintering that sintering oven carries out 36～72h, it is nitrogen that sintering process is used atmosphere, nitrogen gas purity >=99.999%, and to maintain nitrogen pressure in sintering oven be 0.03～0.1MPa, finally obtain silicon nitride combined with silicon carbide refractory material goods.
2. the preparation method of silicon nitride combined with silicon carbide refractory material according to claim 1, it is characterized in that: above-mentioned steps 1. in, use wheel roller to carry out batch mixing, the sic powder that by the granularity of employing is first 1.43～2.5 mm, 0.5～1.43 mm and 0～0.5 mm is poured in wheel roller, mixing 5min, and then to pouring calcium lignosulfonate solution in wheel roller, granularity is that 240 order silicon carbide micro-powders and granularity are 1000 object metallic silicon powers, mixing 40min, then, approaching under the condition of 16 ℃ after 4～96h ageing mixture, complete batching.
3. the preparation method of silicon nitride combined with silicon carbide refractory material according to claim 2, it is characterized in that: above-mentioned steps 1. in, in wheel roller, by granularity, be that 240 order silicon carbide micro-powders, granularity are that 1000 object metallic silicon powers and calcium lignosulfonate solution are when mix, first in wheel roller, pour calcium lignin sulphonate into, the mixing 5min that approaches, then to adding granularity in wheel roller, be that 240 order silicon carbide micro-powders and granularity are 1000 object metallic silicon powers, the mixing 35min that approaches again, then, after ageing mixture, complete batching.
4. according to the preparation method of silicon nitride combined with silicon carbide refractory material described in any one in claim 1～3, it is characterized in that: above-mentioned steps 2. in, in preparation during plain embryo, adopt dry-pressing formedly, control pressure can be 53～328 MPa, the dwell time is 15s.
5. according to the preparation method of silicon nitride combined with silicon carbide refractory material described in any one in claim 1～3, it is characterized in that: above-mentioned steps 3. in, when preparing green compact, furnace drying method be by above-mentioned steps 2. in the biscuit of preparation be placed in and in maintaining box, at 40 ℃, 60 ℃, 80 ℃ and 110 ℃, be respectively incubated successively 6h.
6. according to the preparation method of silicon nitride combined with silicon carbide refractory material described in any one in claim 1～3, it is characterized in that: above-mentioned steps 4. in, when binder removal, dump temperature is 200～700 ℃, wherein in the time of 300 ℃ and 600 ℃ time, is respectively incubated 2h.
7. according to the preparation method of silicon nitride combined with silicon carbide refractory material described in any one in claim 1～3, it is characterized in that: above-mentioned steps 5. in, the equipment of nitridation sintered use is vacuum resistance furnace, before sintering, first-0.08～-0.09MPa will be evacuated in vacuum resistance furnace, then in vacuum resistance furnace, pass into nitrogen, and maintain nitridation sintered nitrogen atmosphere.
8. according to the preparation method of silicon nitride combined with silicon carbide refractory material described in any one in claim 1～3, it is characterized in that, above-mentioned steps 5. in, under the temperature condition of 1150～1380 ℃, heat-up rate according to 2～3 ℃/min heats up, and nitridation sintered employing segmentation is sintering successively, within the scope of 1150～1200 ℃, is incubated 5～10h, within the scope of 1200～1300 ℃, be incubated 5～30h, within the scope of 1300～1380 ℃, be incubated 5～30h.
9. according to the preparation method of silicon nitride combined with silicon carbide refractory material described in any one in claim 1～3, it is characterized in that, above-mentioned steps 5. in, nitridation sintered temperature increasing schedule is: segmentation heats up successively, within the scope of 0～200 ℃, heat-up rate is 5 ℃/min, within the scope of 200～700 ℃, heat-up rate is 3 ℃/min, and within the scope of 700～1150 ℃, heat-up rate is 5 ℃/min, and within the scope of 1150～1380 ℃, heat-up rate is 2 ℃/min.
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| CN104016693A (en) * | 2014-06-11 | 2014-09-03 | 上海大学 | Preparation method of carbide bonded silicon nitride fireproof material |
| CN104987097A (en) * | 2015-07-30 | 2015-10-21 | 武汉科技大学 | Silicon nitride binding silicon carbide refractory material and preparation method therefor |
| CN106554212A (en) * | 2015-09-30 | 2017-04-05 | 比亚迪股份有限公司 | Porous silicon carbide precast body and Al-SiC composites and their preparation method |
| CN107353019A (en) * | 2017-06-20 | 2017-11-17 | 浙江锦诚新材料股份有限公司 | A kind of waste incinerator silicon carbide corrosive-proof plastic material |
| CN109503171A (en) * | 2018-12-18 | 2019-03-22 | 宜兴高等职业技术学校 | A kind of silicon nitride combined silicon carbide brick and preparation method thereof |
| CN109608209A (en) * | 2018-12-21 | 2019-04-12 | 郑州安联凯实业有限公司 | A kind of production method of high thermal conductivity high abrasion refractory material |
| CN113121240A (en) * | 2021-04-23 | 2021-07-16 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of high-wear-resistance nitride-combined silicon carbide composite ceramic overcurrent part |
| CN113666752A (en) * | 2021-08-05 | 2021-11-19 | 陕西中钒昌盛新材料科技有限公司 | Novel technology for producing silicon nitride magnesium by using waste magnesium refractory material |
| CN115368143A (en) * | 2022-05-30 | 2022-11-22 | 宜兴市拓邦耐火科技有限公司 | Silicon nitride microcrystal plate and its production process |
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| CN102746013A (en) * | 2012-08-13 | 2012-10-24 | 南京工业大学 | Light high-strength silicon nitride bonded silicon carbide refractory and preparation method thereof |
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| CN102746013A (en) * | 2012-08-13 | 2012-10-24 | 南京工业大学 | Light high-strength silicon nitride bonded silicon carbide refractory and preparation method thereof |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104016693A (en) * | 2014-06-11 | 2014-09-03 | 上海大学 | Preparation method of carbide bonded silicon nitride fireproof material |
| CN104987097A (en) * | 2015-07-30 | 2015-10-21 | 武汉科技大学 | Silicon nitride binding silicon carbide refractory material and preparation method therefor |
| CN106554212A (en) * | 2015-09-30 | 2017-04-05 | 比亚迪股份有限公司 | Porous silicon carbide precast body and Al-SiC composites and their preparation method |
| CN106554212B (en) * | 2015-09-30 | 2019-12-10 | 比亚迪股份有限公司 | Porous silicon carbide preform, Al-SiC composite material and preparation methods thereof |
| CN107353019A (en) * | 2017-06-20 | 2017-11-17 | 浙江锦诚新材料股份有限公司 | A kind of waste incinerator silicon carbide corrosive-proof plastic material |
| CN109503171A (en) * | 2018-12-18 | 2019-03-22 | 宜兴高等职业技术学校 | A kind of silicon nitride combined silicon carbide brick and preparation method thereof |
| CN109608209A (en) * | 2018-12-21 | 2019-04-12 | 郑州安联凯实业有限公司 | A kind of production method of high thermal conductivity high abrasion refractory material |
| CN113121240A (en) * | 2021-04-23 | 2021-07-16 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of high-wear-resistance nitride-combined silicon carbide composite ceramic overcurrent part |
| CN113666752A (en) * | 2021-08-05 | 2021-11-19 | 陕西中钒昌盛新材料科技有限公司 | Novel technology for producing silicon nitride magnesium by using waste magnesium refractory material |
| CN115368143A (en) * | 2022-05-30 | 2022-11-22 | 宜兴市拓邦耐火科技有限公司 | Silicon nitride microcrystal plate and its production process |
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