CN1609057A - Fast microwave sintering process of combined silicon nitride-silicon carbide refractorg material - Google Patents
Fast microwave sintering process of combined silicon nitride-silicon carbide refractorg material Download PDFInfo
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Abstract
The present invention relates to refractory material technology. By means of the fast homogeneous heating of microwave to material and reaction promoting effect of microwave field on nitriding reaction, homogeneously mixed silicon nitride, silicon powder and small amount of organic adhesive pressed into blank, stoved and defatted are heated with microwave of industrial microwave source of 900-3000 MHz frequency to 1100-1500 deg.c under the nitrogen atmosphere for nitriding reaction and sintering to densify. After cooling naturally to room temperature, combined refractory silicon nitride-silicon carbide material in specific shape and with bulk weight 2.65-2.80 g/cu cm, compression strength higher than 250 MPa, bending strength higher than 60 MPa, porosity lower than 15 % and excellent heat shock resistance is prepared.
Description
Technical field
The present invention relates to a kind of method of utilizing microwave technology rapid reaction sintered silicon nitride carborundum refractory material, belong to technical field of refractory materials.
Background technology
Silicon nitride combined silicon carbide is a kind of be widely used in Metal smelting and casting, the kiln furnitures in the high temperature kilns such as pottery, the novel non-oxidized substance refractory materials in the high temperature equipment such as all kinds of incinerators.Relatively the conventional oxide refractory materials relatively, characteristics such as the content height that possesses skills, the market requirement are big.
Up to now, domestic and international prescription and sintering process to silicon nitride combined with silicon carbide refractory material carried out a large amount of research-and-development activitys.Be widely used.But produce selected sintering technology at present and mainly adopt Si-Mo rod, globars constant resistance Heating element indirec radiation heating, or utilize fuel combustion such as natural gas and isolate the indirect heating mode with goods.
Shortcomings such as there is the sintering period long (common laboratory or industrial production often need a week) in reaction sintering mode in the past, and energy consumption is big, and thermo-efficiency is low.Simultaneously, under the conventional sintering mode, because the blank surface preferentially is heated reaction and forms fine and close silicon nitride combined silicon carbide, and blank inside relies on the inside and outside quality of gaseous diffusion reaction slowly so goods to be not easy control, particularly be difficult to guarantee inside and outside composition, the homogeneity of weave construction and performance for the bigger parts of thickness.
Summary of the invention
The objective of the invention is to propose a kind of method of utilizing microwave technology to carry out the reaction sintering silicon nitride carborundum refractory material, this method can realize being rapidly heated, the inside and outside even heating simultaneously of blank, whole nitrogenizing reaction evenly fully, high, the superior product quality of efficiency of energy utilization, manufacturing low cost.
What the present invention proposed carries out the method for sintered silicon nitride carborundum refractory material with microwave technology, comprises following each step:
(1) raw material is selected silicon carbide powder, silica flour, organic binder bond for use, and described organic binder bond is any in calcium lignin sulphonate or methylcellulose gum or the yellow starch gum;
(2) with above-mentioned silicon carbide according to mass percent 90wt%～70wt%, silica flour is according to mass percent 10wt%～30wt%, mass percent is not more than the 3wt% binding agent, adds the suitable quantity of water wet method and fully mixes;
(3) blank is made in above-mentioned compound moulding;
(4) blank is dry under air atmosphere, temperature is no more than 100 ℃, and heat-up rate is not more than 50 ℃/minute, soaking time 1～64 hour;
(5) in 300～500 ℃ of temperature ranges, carry out degreasing, de-carbon under the air atmosphere, heat-up rate is not more than 50 ℃/minute, temperature hold-time 1～10 hour;
(6) put into microwave agglomerating furnace with above-mentioned through the blank behind the degreasing de-carbon, feed the nitrogen sintering, it is the industrial microwave source of 900～3000 megahertzes (MHz) that reaction and agglomerating plant adopt frequency;
(7) blank is warming up to 1000～1200 ℃ by room temperature under nitrogen atmosphere, in 1000～1200 ℃ of temperature ranges, kept temperature 1～10 hour, heat-up rate is controlled at 10～50 ℃/minute, then temperature is risen in 1350～1450 ℃ of temperature ranges and kept temperature 1～10 hour, heat-up rate is controlled at 10～50 ℃/minute, naturally cool to room temperature then, promptly get the good silicon nitride combined with silicon carbide refractory material of thermal shock resistance.
In aforesaid method, the described drying means of step (4) adopts and utilizes microwave or electrically heated or other heater means.
In aforesaid method, described step (6) adopts sapphire whisker plate or alumina bubble brick or the porous alumina brick lagging material as sintering process.
Zhi Bei silicon nitride combined with silicon carbide refractory material silicon nitride content is 10～30 mass percents according to the method described above, and carborundum content is 70～90 mass percents.
Utilize method of the present invention can significantly improve quality and various physics and chemistry and the machinery and the high-temperature behavior of silicon nitride combined with silicon carbide refractory material goods, resulting silicon nitride combined with silicon carbide refractory material, its unit weight are 2.65～2.80g/cm
3, ultimate compression strength is greater than 250MPa, and bending strength (or folding strength) is greater than 60MPa, and void content is less than 15%.Present method also can shorten the production cycle, enhances productivity, and cuts down the consumption of energy, and reduces cost, and improves the competitiveness of product in market.
Embodiment
Below in conjunction with embodiment method of the present invention is described further:
The thermal capacitance of carbofrax material is less relatively, and microwave absorbing is good.The range of frequency that present technique adopts be the industrial microwave producer of 900～3000 megahertzes as reaction and agglomerating microwave source, the penetrativity of the microwave of this frequency band in agglomerated material is strong.The required energy derive of the nitrogenizing reaction of the raw silicon in the silicon nitride combined silicon carbide material is in the interaction of microwave and silicon carbide, so even heating, homogeneous reaction and the sintering of blank inside in the reaction sintering process.Simultaneously, microwave field and silica flour interact and can promote silicon powder nitride reaction and material diffusion, energy utilization rate height.Therefore utilizing microwave technology to carry out the reaction sintering silicon nitride carborundum refractory material can reach quick, efficient, high-quality and target cheaply.
Embodiment one,
(1) raw material selects for use purity to be: mass percent is greater than 95wt%, and size distribution is 1 μ m～2mm, and grain graininess is according to the silicon carbide powder of certain grating; Silica flour: size-grade distribution is 0.1～50 μ m, and purity is mass percent 99wt%; Select calcium lignin sulphonate as binding agent, purity is mass percent 98wt%.
(2) with above-mentioned silicon carbide powder according to mass percent 90wt%, silica flour is according to mass percent 8wt%, content of binder is added suitable quantity of water according to mass percent 2wt%, the abundant mechanical stirring of wet method is mixed.
(1) above-mentioned compound adopts the vibration pressure moulding to make the blank of definite shape.
(2) blank heat drying 24 hours, temperature under air atmosphere are no more than 100 ℃, add the heating of thermal recovery resistance wire, heat-up rate is 2 ℃/minute.Then in debinding furnace with 5 ℃ of/minute heat-up rates to 300 ℃, be incubated 3 hours, in air atmosphere, carry out degreasing.Heating up then is warming up to 500 ℃ with 5 ℃ of/minute speed, is incubated 2 hours, de-carbon in the air atmosphere.Type of heating is the resistance wire heating.
(3) put into the microwave agglomerating furnace that frequency is 900 megahertzes (MHz) with above-mentioned through the blank behind the degreasing de-carbon, feed nitrogen (purity is more than 99.9%), under nitrogen atmosphere, be warming up to 1200 ℃, heat-up rate is controlled at 20 ℃/minute, kept temperature 2 hours at 1200 ℃, then temperature is risen to 1350 ℃ of temperature and kept temperature 1 hour, heat-up rate is controlled at 40 ℃/minute, naturally cools to room temperature then.
(4) obtaining unit weight is 2.75g/cm
3, ultimate compression strength 301MPa, bending strength (or folding strength) 75MPa, void content 10%, the silicon nitride combined with silicon carbide refractory material that thermal shock resistance is good.Promptly get product of the present invention.
Embodiment two,
(1) raw material selects for use purity to be: mass percent is greater than 95wt%, and size distribution is 1 μ m～2mm, and grain graininess is according to the silicon carbide powder of certain grating; Silica flour: size-grade distribution is 0.1～50 μ m, and purity is mass percent 99wt%; Select calcium lignin sulphonate as binding agent, purity is mass percent 98wt%.
(2) with above-mentioned silicon carbide powder according to mass percent 85wt%, silica flour is according to mass percent 13wt%, content of binder is according to mass percent 2wt%, suitable quantity of water, the abundant mechanical stirring of wet method is mixed.
(3) adopt the vibration pressure moulding to make the blank of definite shape above-mentioned compound.
(4) blank heat drying 24 hours, temperature under air atmosphere are no more than 100 ℃, add the heating of thermal recovery resistance wire, heat-up rate is 2 ℃/minute.In debinding furnace, be warming up to 300 ℃ then, be incubated 3 hours, in air atmosphere, carry out degreasing with 5 ℃ of/minute speed.Be warming up to 500 ℃ with 5 ℃ of/minute speed then, be incubated 2 hours, de-carbon in the air atmosphere.Type of heating is the resistance wire heating.
(5) put into the microwave agglomerating furnace that frequency is 2450 megahertzes (MHz) with above-mentioned through the blank behind the degreasing de-carbon, feed nitrogen (purity is more than 99.9%), under nitrogen atmosphere, be warming up to 1000 ℃, heat-up rate is controlled at 20 ℃/minute, kept temperature 2 hours at 1000 ℃, then temperature is risen to 1450 ℃ of temperature and kept temperature 1 hour, heat-up rate is controlled at 20 ℃/minute, naturally cools to room temperature then.
(6) obtaining unit weight is 2.70g/cm
3, ultimate compression strength 310MPa, bending strength (or folding strength) 73MPa, void content 14%, the silicon nitride combined with silicon carbide refractory material that thermal shock resistance is good.Promptly get product of the present invention.
Embodiment three,
(1) raw material selects for use purity to be: mass percent is greater than 95wt%, and size distribution is 1 μ m～2mm, and grain graininess is according to the silicon carbide powder of certain grating; Silica flour: size-grade distribution is 0.1～50 μ m, and purity is mass percent 99wt%; Select calcium lignin sulphonate as binding agent, purity is mass percent 98wt%.
(2) with above-mentioned silicon carbide powder according to mass percent 80wt%, silica flour is according to mass percent 18wt%, content of binder is according to mass percent 2wt%, suitable quantity of water, the abundant mechanical stirring of wet method is mixed.
(3) adopt the vibration pressure moulding to make the blank of definite shape above-mentioned compound.
(4) blank heat drying 24 hours, temperature under air atmosphere are no more than 100 ℃, add the heating of thermal recovery resistance wire, heat-up rate is 2 ℃/minute.In debinding furnace, be warming up to 300 ℃ then, be incubated 3 hours, in air atmosphere, carry out degreasing with 5 ℃ of/minute speed.Be warming up to 500 ℃ with 5 ℃ of/minute speed then, be incubated 2 hours, de-carbon in the air atmosphere.Type of heating is the resistance wire heating.
(5) put into the microwave agglomerating furnace that frequency is 3000 megahertzes (MHz) with above-mentioned through the blank behind the degreasing de-carbon, feed nitrogen (purity is more than 99.9%), under nitrogen atmosphere, be warming up to 1100 ℃, heat-up rate is controlled at 20 ℃/minute, kept temperature 2 hours at 1100 ℃, then temperature is risen to 1400 ℃ of temperature and kept temperature 1 hour, heat-up rate is controlled at 20 ℃/minute, naturally cools to room temperature then.
(6) obtaining unit weight is 2.75g/cm
3, ultimate compression strength 315MPa, bending strength (or folding strength) 74MPa, void content 10%, the silicon nitride combined with silicon carbide refractory material that thermal shock resistance is good.Promptly get product of the present invention.
Embodiment four,
(1) raw material selects for use purity to be: mass percent is greater than 95wt%, and size distribution is 1 μ m～2mm, and grain graininess is according to the silicon carbide powder of certain grating; Silica flour: size-grade distribution is 0.1～50 μ m, and purity is mass percent 99wt%; Select yellow starch gum as binding agent, purity is mass percent 98wt%.
(3) with above-mentioned silicon carbide powder according to mass percent 75wt%, silica flour is according to mass percent 23wt%, content of binder is according to mass percent 2wt%, suitable quantity of water, the abundant mechanical stirring of wet method is mixed.
(4) adopt the vibration pressure moulding to make the blank of definite shape above-mentioned compound.
(5) blank heat drying 24 hours, temperature under air atmosphere are no more than 100 ℃, add other modes such as thermal recovery microwave or resistive heating or combustion gas etc., heat-up rate is 2 ℃/minute.
(6) with above-mentioned through the oven dry after blank in frequency is the microwave agglomerating furnace of 2450 megahertzes (MHz), be warming up to 300 ℃ in the air atmosphere, be incubated 3 hours, carry out degreasing, heat-up rate is 5 ℃/minute.Be warming up to 500 ℃ with 5 ℃ of/minute speed then, be incubated 2 hours, de-carbon.Then furnace atmosphere is replaced into nitrogen (purity is more than 99.9%), under nitrogen atmosphere, be warming up to 1200 ℃, heat-up rate is controlled at 20 ℃/minute, kept temperature 2 hours at 1200 ℃, then temperature is risen to 1400 ℃ of temperature and kept temperature 1 hour, heat-up rate is controlled at 20 ℃/minute, naturally cools to room temperature then.
(6) obtaining unit weight is 2.77g/cm
3, ultimate compression strength 332MPa, bending strength (or folding strength) 76MPa, void content 13%, the silicon nitride combined with silicon carbide refractory material that thermal shock resistance is good.Promptly get product of the present invention.
Embodiment five,
(1) raw material selects for use purity to be: mass percent is greater than 95wt%, and size distribution is 1 μ m～2mm, and grain graininess is according to the silicon carbide powder of certain grating; Silica flour: size-grade distribution is 0.1～50 μ m, and purity is mass percent 99wt%; Select methylcellulose gum as binding agent, purity is mass percent 98wt%.
(2) with above-mentioned silicon carbide powder according to mass percent 70wt%, silica flour is according to mass percent 28wt%, content of binder is according to mass percent 2wt%, suitable quantity of water, the abundant mechanical stirring of wet method is mixed.
(3) adopt the vibration pressure moulding to make the blank of definite shape above-mentioned compound.
(4) blank heat drying 24 hours, temperature under air atmosphere are no more than 100 ℃, add other modes such as thermal recovery microwave or resistive heating or combustion gas etc., heat-up rate is 2 ℃/minute.
(5) with above-mentioned through the oven dry after blank in frequency is the microwave agglomerating furnace of 2450 megahertzes (MHz), be warming up to 300 ℃ in the air atmosphere, be incubated 3 hours, carry out degreasing, heat-up rate is 5 ℃/minute.Be warming up to 500 ℃ with 5 ℃ of/minute speed then, be incubated 2 hours, de-carbon.Then furnace atmosphere is replaced into nitrogen (purity is more than 99.9%), under nitrogen atmosphere, be warming up to 1200 ℃, heat-up rate is controlled at 20 ℃/minute, kept temperature 2 hours at 1200 ℃, then temperature is risen to 1400 ℃ of temperature and kept temperature 2 hours, heat-up rate is controlled at 20 ℃/minute, naturally cools to room temperature then.
(6) obtaining unit weight is 2.78g/cm
3, ultimate compression strength 300MPa, bending strength (or folding strength) 75MPa, void content 13%, the silicon nitride combined with silicon carbide refractory material that thermal shock resistance is good.Promptly get product of the present invention.
Claims (4)
1, with the method for microwave technology Fast Sintering silicon nitride combined with silicon carbide refractory material, it is characterized in that: described method utilizes microwave to carry out the rapid reaction sintering of silicon nitride combined with silicon carbide refractory material as the energy, comprises following each step:
(1) raw material is selected silicon carbide powder, silica flour, organic binder bond for use, and described organic binder bond is any in calcium lignin sulphonate or methylcellulose gum or the yellow starch gum;
(2) with above-mentioned silicon carbide according to mass percent 90wt%～70wt%, silica flour is according to mass percent 10wt%～30wt%, mass percent is not more than the 3wt% binding agent, adds the suitable quantity of water wet method and fully mixes;
(3) blank is made in above-mentioned compound moulding;
(4) blank is dry under air atmosphere, temperature is no more than 100 ℃, and heat-up rate is not more than 50 ℃/minute;
(5) in 300～500 ℃ of temperature ranges, the base substrate to step (4) under the air atmosphere carries out degreasing, de-carbon, and heat-up rate is not more than 50 ℃/minute, temperature hold-time 1～10 hour;
(6) put into microwave agglomerating furnace with above-mentioned through the blank behind the degreasing de-carbon, feed the nitrogen sintering, it is the industrial microwave source of 900～3000 megahertzes (MHz) that reaction and agglomerating plant adopt frequency;
(7) base substrate with step (6) is warming up to 1000～1200 ℃ by room temperature under nitrogen atmosphere, in 1000～1200 ℃ of temperature ranges, kept temperature 1～10 hour, heat-up rate is controlled at 10～50 ℃/minute, then temperature is risen in 1350～1450 ℃ of temperature ranges and kept temperature 1～10 hour, heat-up rate is controlled at 10～50 ℃/minute, naturally cool to room temperature then, promptly get the good silicon nitride combined with silicon carbide refractory material of thermal shock resistance.
2, the method with microwave technology Fast Sintering silicon nitride combined with silicon carbide refractory material according to claim 1 is characterized in that: the described drying means of step (4) adopts and utilizes microwave or electrically heated or other heater means.
3, the method with microwave technology Fast Sintering silicon nitride combined with silicon carbide refractory material according to claim 1 is characterized in that: described step (6) adopts sapphire whisker plate or alumina bubble brick or the porous alumina brick lagging material as sintering process.
4, the silicon nitride combined with silicon carbide refractory material silicon nitride content according to the described method preparation of claim 1 is 10～30 mass percents, and carborundum content is 70～90 mass percents.
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