CN1793038A - Process for sintering Sialong binding silicon carbide refractory by microwave tech. - Google Patents
Process for sintering Sialong binding silicon carbide refractory by microwave tech. Download PDFInfo
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- CN1793038A CN1793038A CN 200510086915 CN200510086915A CN1793038A CN 1793038 A CN1793038 A CN 1793038A CN 200510086915 CN200510086915 CN 200510086915 CN 200510086915 A CN200510086915 A CN 200510086915A CN 1793038 A CN1793038 A CN 1793038A
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Abstract
The invention relates to a technology that uses microwave quickly reacting nitriding sintering Sialon associated with silicon carbide refractory. The feature of the invention is that its bulk density is 2.68-3.2g/cm<SUP>3</SUP>, compressive strength is over 180MPa, bending strength is over 45MPa, degree of porosity is below 15%, good thermal shock resistance, good anti-oxygenic property and excellent alkali resistance. It also solves the technology problem of super thickness (100mm-200mm) Sialon nitriding reacting sintering with silicon carbide refractory material.
Description
Technical field
The present invention relates to a kind of nitridation sintered Sialon of microwave technology rapid reaction (match dragon) carborundum refractory material method of utilizing, belong to technical field of refractory materials.
Background technology
Sialon (match dragon) carborundum refractory material is a kind of inner lining refractory that is widely used in high temperature equipment such as smelting iron and steel, thermal power generation and casting, kiln furnitures in the high temperature kilns such as pottery, emery wheel, electroceramics, the novel senior non-oxidized substance refractory materials in the high temperature equipment such as all kinds of incinerators.Relatively the conventional oxide refractory materials relatively, the content height that possesses skills, use temperature height, characteristics such as wear-resistant ability is strong, and compare antioxidant property and alkali resistant erosion performance with silicon nitride combined silicon carbide good especially, and the market requirement is big.
Up to now, prescription and the sintering process of matching imperial carborundum refractory material carried out a large amount of research-and-development activitys both at home and abroad, be widely used.Produce at present selected sintering technology and mainly adopt molybdenum disilicide rod, silication carbon-point constant resistance Heating element indirec radiation heating, or utilize fuel combustion such as Sweet natural gas, oil liquefied gas and isolate the indirect heating mode with goods.But, the sintering temperature that adopts the traditional industry mode of production is generally all below 1450 ℃, because the reaction and the sintering temperature of the imperial based on silicon carbide of match are higher, above traditional sintering processing is difficult to reach nitrogenizing reaction and matches imperial material completely, thereby is difficult to obtain the match dragon based on silicon carbide of excellent property.Higher temperature of reaction proposes very high requirement to the nitrogenize calcination equipment, makes that also production cost increases substantially.
Shortcomings such as in addition, there is the sintering period long (common laboratory or industrial one-period often need a week even more time) in above-mentioned traditional reaction sintering mode, and energy consumption is bigger, and thermo-efficiency is low.Under the conventional sintering mode, because the green compact surface preferentially is heated reaction and forms fine and close match dragon based on silicon carbide sintered layer, form " duricrust effect ", rely on slowly gaseous diffusion and penetrate into green compact inside and carry out the difficulty that nitrogenizing reaction becomes suitable, it is incomplete to make that also the inner nitrogenizing reaction of goods generates the imperial chemical reaction of match, inconsistent control, the homogeneity of composition, weave construction and physical and chemical performance inside and outside particularly being difficult to guarantee of also being not easy of inside and outside quality that causes goods for the bigger parts of thickness.
Summary of the invention
The objective of the invention is to propose a kind ofly to utilize microwave technology to carry out reaction sintering to match imperial carborundum refractory material, can reach is rapidly heated and reaches complete reaction easily generates the imperial needed temperature condition of match.Microwave field also has the promoter action of fast reaction speed to the formation reaction of matching dragon.In addition, microwave is to while even heating inside and outside the blank integral body, and reaction of match dragon and sintering can be inside and outside evenly abundant.The microwave reaction sintering have efficiency of energy utilization height, goods excellent performance and reliable and stable, with short production cycle, make advantage cheaply.
The method of utilizing microwave technology sintering Sialon carborundum refractory material that the present invention proposes, the industrial microwave source that this method employing frequency is 900～3000 megahertzes is as reaction and agglomerating microwave source, it is characterized in that: described method is with silicon-carbide particle and fine powder, silica flour, aluminum oxide fine powder, behind aluminium powder and the binding agent uniform mixing, be pressed into adobe by pressure forming machine, after oven dry of adobe process and the pre-degreasing carbonization treatment, the microwave that utilizes the industrial microwave source to produce under nitrogen atmosphere carries out nitrogenizing reaction and densification sintering with adobe, and the steps in sequence of described method is:
(1) raw material is selected silicon carbide for use, and silica flour is alumina powder jointed, aluminium powder, normal temperature wedding agent;
(2) with above-mentioned silicon carbide by weight percentage 90%～50%; Silica flour by weight percentage 5%～20%; Alumina powder jointed according to weight percent 1%～20%; Aluminium powder by weight percentage 0.5%～10%; Normal temperature wedding agent, add-on are 0.2～10% of total batching quality; Add together to force to stir in the sand mill and mix;
(3) the above-mentioned material that mixes is pressed into adobe in brick pressing machine;
(4) adobe of forming is dry under 30 ℃～200 ℃ temperature, the moisture controlled of dry back adobe is less than 0.4%;
(5) with dried adobe in 300～500 ℃ of temperature ranges, air atmosphere down insulation carried out degreasing and de-carbon in 2～8 hours, heat-up rate is not more than 50 ℃/minute;
(6) put into microwave agglomerating furnace with above-mentioned through the blank behind the degreasing de-carbon, feed the nitrogen sintering; When being warming up to 1350 ℃～1650 ℃ temperature ranges, and be incubated 0.5～8 hour under this temperature range, heat-up rate is controlled at 800 ℃～1700 ℃/hour;
When (7) naturally cooling to 750 ℃, stop logical nitrogen, be the imperial carborundum refractory material goods of match after being cooled to room temperature.
In the above-mentioned method of utilizing microwave technology sintering Sialon carborundum refractory material, the chemical constitution of the compound of described Sialon and silicon carbide bonded refractory materials meets Si
6-zAl
zO
zN
8-z(0＜z≤4.2).
In the above-mentioned method of utilizing microwave technology sintering Sialon carborundum refractory material, it is that about 30% industrial dextrin or concentration are that about 30% calcium lignosulfonate solution or concentration are any in about 10% the polyvinyl alcohol solution that described normal temperature wedding agent adopts concentration.
In the above-mentioned method of utilizing microwave technology sintering Sialon carborundum refractory material, described is the industrial microwave source of 915～2450 megahertzes as reaction and agglomerating microwave source employing frequency.
The imperial carborundum refractory material volume density of match of the present invention is 2.68～3.2g/cm
3, ultimate compression strength is greater than 180MPa, and bending strength (or folding strength) is greater than 45MPa, and void content is less than 15%, and thermal shock resistance is good, the alkali resistant erosion performance is outstanding.Promptly get product of the present invention.The present invention can significantly improve the homogeneity of the imperial carborundum refractory material product properties of match, particularly solves super thick (the nitrogenizing reaction agglomerating technical barrier of goods of thickness 100mm～200mm).Simultaneously, goods have good various physicochemical properties, mechanical property and high-temperature behavior.Utilizing microwave technology to carry out quick nitrogenizing reaction sintering Sialon carborundum refractory material can shorten the production cycle, enhance productivity, cut down the consumption of energy, reduce cost, improve the competitiveness of product in market.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is described further:
Match in the microwave sintering process of imperial based on silicon carbide, because the thermal capacitance of silicon carbide is less relatively, microwave absorbing is good, the range of frequency that the technology of the present invention adopts be the industrial microwave source of 900～3000 megahertzes as nitrogenizing reaction and agglomerating microwave source, the penetrativity of microwave in this agglomerated material is strong.Match the required energy derive of reaction in the imperial combined silicon carbide material in micro-wave energy, thermal source derives from the interaction of microwave and material, so the evenly heating of blank inside, homogeneous reaction and sintering in the reaction sintering process.Simultaneously, the interaction of microwave and silica flour and silicon carbide can promote nitrogenizing reaction and material diffusion, the energy utilization rate height of the technology of the present invention.Therefore utilizing microwave technology to carry out reaction sintering matches imperial carborundum refractory material and can reach quick, efficient, high-quality and target cheaply.
The present invention proposes utilizes microwave technology to carry out the nitrogenizing reaction sintering to match imperial carborundum refractory material method, comprise following each concrete implementation step:
(1) raw material selects for use carborundum granularity to be distributed as 0.2 μ m～6mm (comprising particle and powder), and purity is: weight percent is greater than 95%; Silica flour, granularity is less than 70 μ m, and purity is: weight percent is greater than 95%; Alumina powder jointed, size-grade distribution is 0.1 μ m～30 μ m, and purity is: weight percent is greater than 95%; Aluminium powder, size-grade distribution are 0.1 μ m～30 μ m, and purity is: weight percent is greater than 95wt%; Normal temperature wedding agent (generally can adopt concentration is that about 30% industrial dextrin, concentration are that about 30% calcium lignosulfonate solution or concentration are about 10% polyvinyl alcohol solution).
(2) with above-mentioned silicon carbide by weight percentage 90%～50%; Silica flour by weight percentage 5%～20%; Alumina powder jointed according to weight percent 1%～20%; Aluminium powder silica flour by weight percentage 0.5%～10%; With add the normal temperature wedding agent (generally can adopt concentration is that about 30% industrial dextrin or concentration are that about 30% calcium lignosulfonate solution or concentration are about 10% polyvinyl alcohol solution, add-on be total batching quality 0.2～10%) add together to force to stir in the sand mill and mixed 20 minutes～50 minutes.
(3) material that mixes is pressed into adobe in brick pressing machine, brick pressing machine can be the large-scale vibrating pressure forming machine, also can be 200～1000 tons friction press, also can be high tonnage hydropress.
(4) adobe of forming is dry under 100 ℃ temperature, and the moisture of dry back adobe should be controlled at less than 0.4%.
(5) in kiln, blank is warming up to 300 ℃ under air atmosphere insulation carried out degreasing in 4 hours, be warming up to 500 ℃ then, air atmosphere insulation down carried out de-carbon in 6 hours.Heat-up rate is not more than 50 ℃/minute.
(6) with the above-mentioned microwave agglomerating furnace of putting into, feed nitrogen (purity is weight percentage greater than 99.9wt%) sintering through blank behind the degreasing de-carbon.It is the industrial microwave source of 915 or 2450 megahertzes (MHz) that reaction and agglomerating plant adopt frequency.Heat-up rate is controlled at 800 ℃～1700 ℃/hour, when being warming up to 1350 ℃～1650 ℃ temperature ranges and be incubated 0.5～8 hour under this temperature range (decide soaking time with products thickness, products thickness is big more, and soaking time is long more.For example, the goods that 90mm is thick, soaking time generally will reach more than 2 hours).Can stop logical nitrogen when naturally cooling to 750 ℃.Be cooled to the match dragon carborundum refractory material goods of the different shape that can obtain excellent property after the room temperature.
Embodiment 1
A kind of production process of utilizing microwave technology to carry out quick nitrogenizing reaction sintering Sialon carborundum refractory material (hereinafter referred is the imperial carborundum refractory material of match):
Raw material:
The sic raw material specification of quality is, SiC is greater than 95%, Fe
2O
3Less than 0.5%.
The proportioning of each silicon-carbide particle granularity is: 6.0mm～3mm accounts for 20%; 3～1mm accounts for 20%; 1～0.5mm, 8%; ≤ 0.5mm accounts for 8%, less than the carbide fine powder 4% of 0.08mm; Total add-on of silicon carbide is 60% (weight percent).
The specification of quality of silica flour raw material is, Si is greater than 95%, Fe
2O
3Less than 0.5%.The grain graininess granularity is less than 70 μ m, and add-on is 20%.
Alumina powder jointed specification of quality is Al
2O
3Greater than 95%, Fe
2O
3Less than 0.5%, size-grade distribution is 0.1 μ m～10 μ m, and add-on is 15%.
The specification of quality of aluminium powder is, Al is greater than 95%, Fe
2O
3Less than 0.5%, size-grade distribution is 0.1 μ m～10 μ m, and add-on is 5%.
Batching:
Earlier the silicon-carbide particle adding of each granularity is forced to stir in the sand mill and mixed 3 minutes, the back added carbide fine powder, silica flour, aluminum oxide powder and aluminium powder remix after 5 minutes, it is concentration 30% industrial dextrin solution that adding adds the normal temperature wedding agent, add-on is 5% of total batching quality, after mixed 50 minutes forcing to stir in the sand mill together.
Moulding:
The material that mixes is suppressed into the thick goods of the wide 200mm of the long 220mm of 300mm in brick pressing machine, brick pressing machine is 1000 tons a friction press.
Dry:
The based on silicon carbide firebrick billet of forming under 100 ℃ temperature dry 10 hours, the moisture of dry back adobe should be controlled at less than 0.4%.
The degreasing decarburization:
In kiln, blank is warming up to 300 ℃ under air atmosphere insulation carried out degreasing in 4 hours, be warming up to 500 ℃ then, air atmosphere insulation down carried out de-carbon in 6 hours.Heat-up rate is not more than 50 ℃/minute.
Nitrogenize is burnt till:
With the above-mentioned microwave agglomerating furnace of putting into, feed nitrogen (purity is weight percentage greater than 99.9wt%) sintering through blank behind the degreasing de-carbon.It is the industrial microwave source of 2450 megahertzes (MHz) that reaction and agglomerating plant adopt frequency.Heat-up rate is controlled at 1000 ℃/hour, is warming up to 1350 ℃ of insulations 2 hours, continues to be warming up to 1650 ℃ of temperature and be incubated 7 hours under this temperature.Can stop logical nitrogen when naturally cooling to 750 ℃.Can obtain matching imperial carborundum refractory material goods after being cooled to room temperature.
The physicochemical property of brick body is: silicon carbide, 56.66%; Sialon, 34.22%; Aluminum oxide, 5.32%; Apparent porosity, 11%; Volume density 2.89g/cm
3Compressive strength 295.3Mpa; Strength at normal temperature 70.1Mpa; 1400 ℃ of folding strength 48.3Mpa.The alkali resistant erosional competency is good.
Embodiment 2
A kind of production process of utilizing microwave technology to carry out quick nitrogenizing reaction sintering Sialon carborundum refractory material (hereinafter referred is the imperial carborundum refractory material of match):
Raw material:
The sic raw material specification of quality is, SiC is greater than 98%, Fe
2O
3Less than 0.5%.
The proportioning of each silicon-carbide particle granularity is: 6.0mm～3mm accounts for 22%; 3～1mm accounts for 17%; 1～0.5mm, 11%; ≤ 0.5mm accounts for 8%, less than the carbide fine powder 7% of 0.08mm; Total add-on of silicon carbide is 65% (weight percent).
The specification of quality of silica flour raw material is, Si is greater than 98%, Fe
2O
3Less than 0.5%.Granularity is less than 50 μ m, and add-on is 16%.
Alumina powder jointed specification of quality is Al
2O
3Greater than 99%, Fe
2O
3Less than 0.2%, size-grade distribution is 0.1 μ m～2 μ m, and add-on is 15%.
The specification of quality of aluminium powder is, Al is greater than 99%, Fe
2O
3Less than 0.2%, size-grade distribution is 0.1 μ m～3 μ m, and add-on is 4%.
Batching:
Earlier the silicon-carbide particle adding of each granularity is forced to stir in the sand mill and mixed 4 minutes, the back added carbide fine powder, silica flour, aluminum oxide powder and aluminium powder remix after 6 minutes, add that to add the normal temperature wedding agent be 30% calcium lignosulfonate solution, add-on is 5.8% of total batching quality, after mixed 38 minutes forcing to stir in the sand mill together.
Moulding:
The material that mixes is suppressed into the thick goods of the wide 100mm of the long 150mm of 300mm in brick pressing machine, brick pressing machine is 1000 tons a friction press.
Dry:
The based on silicon carbide firebrick billet of forming under 120 ℃ temperature dry 6 hours, the moisture of dry back adobe should be controlled at less than 0.3%.
The degreasing decarburization:
In kiln, blank is warming up to 320 ℃ under air atmosphere insulation carried out degreasing in 4 hours, be warming up to 500 ℃ then, air atmosphere insulation down carried out de-carbon in 6 hours.Heat-up rate is not more than 50 ℃/minute.
Nitrogenize is burnt till:
With the above-mentioned microwave agglomerating furnace of putting into, feed nitrogen (purity is weight percentage greater than 99.9wt%) sintering through blank behind the degreasing de-carbon.It is the industrial microwave source of 2450 megahertzes (MHz) that reaction and agglomerating plant adopt frequency.Heat-up rate is controlled at 1100 ℃/hour, is warming up to 1350 ℃ of insulations 1.5 hours, continues to be warming up to 1650 ℃ of temperature and be incubated 4 hours under this temperature.Can stop logical nitrogen when naturally cooling to 750 ℃.Can obtain matching imperial carborundum refractory material goods after being cooled to room temperature.
The physicochemical property of brick body is: SiC, 63.73%; Sialon, 28.29%; Al
2O
3, 3.28%; Apparent porosity, 13%; Volume density 2.85g/cm
3Compressive strength 305.3Mpa; Strength at normal temperature 66.5Mpa; 1400 ℃ of folding strength 68.4Mpa.The alkali resistant erosional competency is good.
Embodiment 3
A kind of production process of utilizing microwave technology to carry out quick nitrogenizing reaction sintering Sialon carborundum refractory material (hereinafter referred is the imperial carborundum refractory material of match):
Raw material:
The sic raw material specification of quality is, SiC is greater than 97%, Fe
2O
3Less than 0.5%.
The proportioning of each silicon-carbide particle granularity is: 6.0mm～3mm accounts for 18%; 3～1mm accounts for 30%; 1～0.5mm, 10%; ≤ 0.5mm accounts for 8%, less than the carbide fine powder 24% of 0.08mm; Total add-on of silicon carbide is 90% (weight percent).
The specification of quality of silica flour raw material is, Si is greater than 98%, Fe
2O
3Less than 0.5%.Granularity is less than 70 μ m, and add-on is 7.5%.
Alumina powder jointed specification of quality is Al
2O
3Greater than 99%, Fe
2O
3Less than 0.1%, size-grade distribution is 0.1 μ m～2 μ m, and add-on is 2%.
The specification of quality of aluminium powder is, Al is greater than 99%, Fe
2O
3Less than 0.1%, size-grade distribution is 0.1 μ m～3 μ m, and add-on is 0.5%.
Batching:
Earlier the silicon-carbide particle adding of each granularity is forced to stir in the sand mill and mixed 4 minutes, the back added carbide fine powder, silica flour, aluminum oxide powder and aluminium powder remix after 6 minutes, add that to add the normal temperature wedding agent be 30% calcium lignosulfonate solution, add-on is 4.8% of total batching quality, after mixed 40 minutes forcing to stir in the sand mill together.
Moulding:
The material that mixes is suppressed into the thick goods of the wide 30mm of the long 450mm of 500mm in brick pressing machine, brick pressing machine is 1000 tons a friction press.
Dry:
The based on silicon carbide firebrick billet of forming under 30 ℃～200 ℃ temperature dry 4 hours, the moisture of dry back adobe should be controlled at less than 0.3%.
The degreasing decarburization:
In kiln, blank is warming up to 310 ℃ under air atmosphere insulation carried out degreasing in 4 hours, be warming up to 490 ℃ then, air atmosphere insulation down carried out de-carbon in 6 hours.Heat-up rate is not more than 50 ℃/minute.
Nitrogenize is burnt till:
With the above-mentioned microwave agglomerating furnace of putting into, feed nitrogen (purity is weight percentage greater than 99.9wt%) sintering through blank behind the degreasing de-carbon.It is the industrial microwave source of 2450 megahertzes (MHz) that reaction and agglomerating plant adopt frequency.Heat-up rate is controlled at 1200 ℃/hour, is warming up to 1350 ℃ of insulations 1 hour, continues to be warming up to 1600 ℃ of temperature and be incubated 2 hours under this temperature.Can stop logical nitrogen when naturally cooling to 750 ℃.Can obtain matching imperial carborundum refractory material goods after being cooled to room temperature.
The physicochemical property of brick body is: SiC, 87.23%; Sialon, 11.33%; Al
2O
3, 0.01%; Apparent porosity, 15%; Volume density 2.69g/cm
3Compressive strength 195.5Mpa; Strength at normal temperature 48.6Mpa; 1400 ℃ of folding strength 49.8Mpa.Thermal shock resistance is good, antioxidant property is good, the alkali resistant erosional competency is good.
Embodiment 4
A kind of production process of utilizing microwave technology to carry out quick nitrogenizing reaction sintering Sialon carborundum refractory material (hereinafter referred is---match imperial carborundum refractory material):
Raw material:
The sic raw material specification of quality is, SiC is greater than 98%, Fe
2O
3Less than 0.5%.
The proportioning of each silicon-carbide particle granularity is: 6.0mm～3mm accounts for 20%; 3～1mm accounts for 22%; 1～0.5mm, 14%; ≤ 0.5mm accounts for 10%, less than the carbide fine powder 14% of 0.08mm; Total add-on of silicon carbide is 80% (weight percent).
The specification of quality of silica flour raw material is, Si is greater than 97%, Fe
2O
3Less than 0.5%.Granularity is less than 50 μ m, and add-on is 11%.
Alumina powder jointed specification of quality is Al
2O
3Greater than 99%, Fe
2O
3Less than 0.1%, size-grade distribution is 0.1 μ m～10 μ m, and add-on is 8%.
The specification of quality of aluminium powder is, Al is greater than 99%, Fe
2O
3Less than 0.1%, size-grade distribution is 0.1 μ m～10 μ m, and add-on is 3%.
Batching:
Earlier the silicon-carbide particle adding of each granularity is forced to stir in the sand mill and mixed 5 minutes, the back added carbide fine powder, silica flour, aluminum oxide powder and aluminium powder remix after 6 minutes, it is concentration 30% industrial dextrin solution that adding adds the normal temperature wedding agent, add-on is 4.6% of total batching quality, after mixed 42 minutes forcing to stir in the sand mill together.
Moulding:
The material that mixes is suppressed into the thick goods of the wide 75mm of the long 250mm of 400mm in brick pressing machine, brick pressing machine is 1000 tons a friction press.
Dry:
The based on silicon carbide firebrick billet of forming under 30 ℃～200 ℃ temperature dry 8 hours, the moisture of dry back adobe should be controlled at less than 0.3%.
The degreasing decarburization:
In kiln, blank is warming up to 350 ℃ under air atmosphere insulation carried out degreasing in 4 hours, be warming up to 480 ℃ then, air atmosphere insulation down carried out de-carbon in 6 hours.Heat-up rate is not more than 50 ℃/minute.
Nitrogenize is burnt till:
With the above-mentioned microwave agglomerating furnace of putting into, feed nitrogen (purity is weight percentage greater than 99.9wt%) sintering through blank behind the degreasing de-carbon.It is the industrial microwave source of 915 megahertzes (MHz) that reaction and agglomerating plant adopt frequency.Heat-up rate is controlled at 1000 ℃/hour, is warming up to 1350 ℃ of insulations 2.5 hours, continues to be warming up to 1600 ℃ of temperature and be incubated 4 hours under this temperature.Can stop logical nitrogen when naturally cooling to 750 ℃.Can obtain matching imperial carborundum refractory material goods after being cooled to room temperature.
The physicochemical property of brick body is: silicon carbide, 77.96%; Sialon, 19.02%; Aluminum oxide, 0.02%; Apparent porosity, 13%; Volume density 2.80g/cm
3Compressive strength 291.4Mpa; Strength at normal temperature 63.1Mpa; 1400 ℃ of folding strength 57.8Mpa.Thermal shock resistance is good, the alkali resistant erosional competency is good.
Embodiment 5
A kind of production process of utilizing microwave technology to carry out quick nitrogenizing reaction sintering Sialon carborundum refractory material (hereinafter referred is the imperial carborundum refractory material of match):
Raw material:
The sic raw material specification of quality is, SiC is greater than 98%, Fe
2O
3Less than 0.5%.
The proportioning of each silicon-carbide particle granularity is: 6.0mm～3mm accounts for 19%; 3～1mm accounts for 22%; 1～0.5mm accounts for 10%; ≤ 0.5mm accounts for 8%, accounts for 14% less than the carbide fine powder of 0.08mm; Total add-on of silicon carbide is 73% (weight percent).
The specification of quality of silica flour raw material is, Si is greater than 97%, Fe
2O
3Less than 0.5%.Granularity is less than 60 μ m, and add-on is 18%.
Alumina powder jointed specification of quality is Al
2O
3Greater than 99%, Fe
2O
3Less than 0.2%, size-grade distribution is 0.1 μ m～2 μ m, and add-on is 5%.
The specification of quality of aluminium powder is, Al is greater than 99%, Fe
2O
3Less than 0.2%, size-grade distribution is 0.1 μ～3 μ m, and add-on is 4%.
Batching:
Earlier the silicon-carbide particle adding of each granularity is forced to stir in the sand mill and mixed 4 minutes, the back added carbide fine powder, silica flour, aluminum oxide powder and aluminium powder remix after 5 minutes, it is that concentration is 12% polyvinyl alcohol solution that adding adds the normal temperature wedding agent, add-on is 6% of total batching quality, after mixed 40 minutes forcing to stir in the sand mill together.
Moulding:
The material that mixes is suppressed into the thick goods of the wide 130mm of the long 350mm of 400mm in brick pressing machine, brick pressing machine is 1000 tons a friction press.
Dry:
The based on silicon carbide firebrick billet of forming under 30 ℃～200 ℃ temperature dry 6 hours, the moisture of dry back adobe should be controlled at less than 0.3%.
The degreasing decarburization:
In kiln, blank is warming up to 300 ℃ under air atmosphere insulation carried out degreasing in 4 hours, be warming up to 500 ℃ then, air atmosphere insulation down carried out de-carbon in 6 hours.Heat-up rate is not more than 50 ℃/minute.
Nitrogenize is burnt till:
With the above-mentioned microwave agglomerating furnace of putting into, feed nitrogen (purity is weight percentage greater than 99.9wt%) sintering through blank behind the degreasing de-carbon.It is the industrial microwave source of 915 megahertzes (MHz) that reaction and agglomerating plant adopt frequency.Heat-up rate is controlled at 1100 ℃/hour, is warming up to 1350 ℃ of insulations 2 hours, continues to be warming up to 1600 ℃ of temperature and be incubated 2 hours under this temperature.Can stop logical nitrogen when naturally cooling to 750 ℃.Can obtain matching imperial carborundum refractory material goods after being cooled to room temperature.
The physicochemical property of brick body is: SiC, 70.23%; Sialon, 28.43%; Aluminum oxide, 0.03%; Apparent porosity, 13%; Volume density 2.80g/cm
3Compressive strength 242.6Mpa; Strength at normal temperature 65.7Mpa; 1400 ℃ of folding strength 62.9Mpa.Thermal shock resistance is good, and the alkali resistant erosional competency is good.
Embodiment 6
A kind of production process of utilizing microwave technology to carry out quick nitrogenizing reaction sintering Sialon carborundum refractory material (hereinafter referred is the imperial carborundum refractory material of match):
Raw material:
The sic raw material specification of quality is, SiC is greater than 98%, Fe
2O
3Less than 0.5%.
The proportioning of each silicon-carbide particle granularity is: 6.0mm～3mm accounts for 19%; 3～1mm accounts for 22%; 1～0.5mm accounts for 10%; ≤ 0.5mm accounts for 8%, accounts for 14% less than the carbide fine powder of 0.08mm; Total add-on of silicon carbide is 73% (weight percent).
The specification of quality of silica flour raw material is, Si is greater than 97%, Fe
2O
3Less than 0.5%.Granularity is less than 60 μ m, and add-on is 18%.
Alumina powder jointed specification of quality is Al
2O
3Greater than 99%, Fe
2O
3Less than 0.2%, size-grade distribution is 0.1 μ m～2 μ m, and add-on is 5%.
The specification of quality of aluminium powder is, Al is greater than 99%, Fe
2O
3Less than 0.2%, size-grade distribution is 0.1 μ m～3 μ m, and add-on is 4%.
Batching:
Earlier the silicon-carbide particle adding of each granularity is forced to stir in the sand mill and mixed 4 minutes, the back added carbide fine powder, silica flour, aluminum oxide powder and aluminium powder remix after 5 minutes, it is that concentration is 12% polyvinyl alcohol solution that adding adds the normal temperature wedding agent, add-on is 6% of total batching quality, after mixed 40 minutes forcing to stir in the sand mill together.
Moulding:
The material that mixes is suppressed into the thick goods of the wide 130mm of the long 350mm of 400mm in brick pressing machine, brick pressing machine is 1000 tons a friction press.
Dry:
The based on silicon carbide firebrick billet of forming under 30 ℃～200 ℃ temperature dry 6 hours, the moisture of dry back adobe should be controlled at less than 0.3%.
The degreasing decarburization:
In kiln, blank is warming up to 300 ℃ under air atmosphere insulation carried out degreasing in 4 hours, be warming up to 500 ℃ then, air atmosphere insulation down carried out de-carbon in 6 hours.Heat-up rate is not more than 50 ℃/minute.
Nitrogenize is burnt till:
With the above-mentioned microwave agglomerating furnace of putting into, feed nitrogen (purity is weight percentage greater than 99.9wt%) sintering through blank behind the degreasing de-carbon.It is the industrial microwave source of 915 megahertzes (MHz) that reaction and agglomerating plant adopt frequency.Heat-up rate is controlled at 1100 ℃/hour, is warming up to 1350 ℃ of insulations 2 hours, continues to be warming up to 1600 ℃ of temperature and be incubated 6 hours under this temperature.Can stop logical nitrogen when naturally cooling to 750 ℃.Can obtain matching imperial carborundum refractory material goods after being cooled to room temperature.
The physicochemical property of brick body is: SiC, 70.23%; Sialon, 28.43%; Aluminum oxide, 0.03%; Apparent porosity, 12%; Volume density 2.80g/cm
3Compressive strength 242.6Mpa; Strength at normal temperature 65.7Mpa; 1400 ℃ of folding strength 65.9Mpa.Thermal shock resistance is good, and the alkali resistant erosional competency is good.
Embodiment 7
A kind of production process of utilizing microwave technology to carry out quick nitrogenizing reaction sintering Sialon carborundum refractory material (hereinafter referred is the imperial carborundum refractory material of match):
Raw material:
The sic raw material specification of quality is, SiC is greater than 98%, Fe
2O
3Less than 0.5%.
The proportioning of each silicon-carbide particle granularity is: 6.0mm～3mm accounts for 19%; 3～1mm accounts for 22%; 1～0.5mm accounts for 10%; ≤ 0.5mm accounts for 8%, accounts for 14% less than the carbide fine powder of 0.08mm; Total add-on of silicon carbide is 73% (weight percent).
The specification of quality of silica flour raw material is, Si is greater than 97%, Fe
2O
3Less than 0.5%.Granularity is less than 60 μ m, and add-on is 18%.
Alumina powder jointed specification of quality is Al
2O
3Greater than 99%, Fe
2O
3Less than 0.2%, size-grade distribution is 0.1 μ m～2 μ m, and add-on is 5%.
The specification of quality of aluminium powder is, Al is greater than 99%, Fe
2O
3Less than 0.2%, size-grade distribution is 0.1 μ m～3 μ m, and add-on is 4%.
Batching:
Earlier the silicon-carbide particle adding of each granularity is forced to stir in the sand mill and mixed 4 minutes, the back added carbide fine powder, silica flour, aluminum oxide powder and aluminium powder remix after 5 minutes, it is that concentration is 12% polyvinyl alcohol solution that adding adds the normal temperature wedding agent, add-on is 6% of total batching quality, after mixed 40 minutes forcing to stir in the sand mill together.
Moulding:
The material that mixes is suppressed into the thick goods of the wide 130mm of the long 350mm of 400mm in brick pressing machine, brick pressing machine is 1000 tons a friction press.
Dry:
The based on silicon carbide firebrick billet of forming under 30 ℃～200 ℃ temperature dry 6 hours, the moisture of dry back adobe should be controlled at less than 0.3%.
The degreasing decarburization:
In kiln, blank is warming up to 330 ℃ under air atmosphere insulation carried out degreasing in 4 hours, be warming up to 490 ℃ then, air atmosphere insulation down carried out de-carbon in 6 hours.Heat-up rate is not more than 50 ℃/minute.
Nitrogenize is burnt till:
With the above-mentioned microwave agglomerating furnace of putting into, feed nitrogen (purity is weight percentage greater than 99.9wt%) sintering through blank behind the degreasing de-carbon.It is the industrial microwave source of 2450 megahertzes (MHz) that reaction and agglomerating plant adopt frequency.Heat-up rate is controlled at 1100 ℃/hour, is warming up to 1350 ℃ of insulations 2 hours, continues to be warming up to 1400 ℃ of temperature and be incubated 8 hours under this temperature.Can stop logical nitrogen when naturally cooling to 750 ℃.Can obtain matching imperial carborundum refractory material goods after being cooled to room temperature.
The physicochemical property of brick body is: SiC, 70.23%; Sialon, 28.43%; Aluminum oxide, 0.03%; Apparent porosity, 11%; Volume density 2.81g/cm
3Compressive strength 245.6Mpa; Strength at normal temperature 65.7Mpa; 1400 ℃ of folding strength 65.9Mpa.Thermal shock resistance is good, and the alkali resistant erosional competency is good.
Embodiment 8
A kind of production process of utilizing microwave technology to carry out quick nitrogenizing reaction sintering Sialon carborundum refractory material (hereinafter referred is the imperial carborundum refractory material of match):
Raw material:
The sic raw material specification of quality is, SiC is greater than 98%, Fe
2O
3Less than 0.5%.
The proportioning of each silicon-carbide particle granularity is: 6.0mm～3mm accounts for 19%; 3～1mm accounts for 22%; 1～0.5mm accounts for 10%; ≤ 0.5mm accounts for 8%, accounts for 14% less than the carbide fine powder of 0.08mm; Total add-on of silicon carbide is 73% (weight percent).
The specification of quality of silica flour raw material is, Si is greater than 97%, Fe
2O
3Less than 0.5%.Granularity is less than 60 μ m, and add-on is 18%.
Alumina powder jointed specification of quality is Al
2O
3Greater than 99%, Fe
2O
3Less than 0.2%, size-grade distribution is 0.1 μ m～2 μ m, and add-on is 5%.
The specification of quality of aluminium powder is, Al is greater than 99%, Fe
2O
3Less than 0.2%, size-grade distribution is 0.1 μ m～3 μ m, and add-on is 4%.
Batching:
Earlier the silicon-carbide particle adding of each granularity is forced to stir in the sand mill and mixed 4 minutes, the back added carbide fine powder, silica flour, aluminum oxide powder and aluminium powder remix after 5 minutes, it is that concentration is 12% polyvinyl alcohol solution that adding adds the normal temperature wedding agent, add-on is 6% of total batching quality, after mixed 40 minutes forcing to stir in the sand mill together.
Moulding:
The material that mixes is suppressed into the thick goods of the wide 130mm of the long 350mm of 400mm in brick pressing machine, brick pressing machine is 1000 tons a friction press.
Dry:
The based on silicon carbide firebrick billet of forming under 30 ℃～200 ℃ temperature dry 6 hours, the moisture of dry back adobe should be controlled at less than 0.3%.
The degreasing decarburization:
In kiln, blank is warming up to 300 ℃ under air atmosphere insulation carried out degreasing in 4 hours, be warming up to 500 ℃ then, air atmosphere insulation down carried out de-carbon in 6 hours.Heat-up rate is not more than 50 ℃/minute.
Nitrogenize is burnt till:
With the above-mentioned microwave agglomerating furnace of putting into, feed nitrogen (purity is weight percentage greater than 99.9wt%) sintering through blank behind the degreasing de-carbon.It is the industrial microwave source of 2450 megahertzes (MHz) that reaction and agglomerating plant adopt frequency.Heat-up rate is controlled at 1100 ℃/hour, is warming up to 1350 ℃ of insulations 2 hours, continues to be warming up to 1400 ℃ of temperature and be incubated 6 hours under this temperature.Can stop logical nitrogen when naturally cooling to 750 ℃.Can obtain matching imperial carborundum refractory material goods after being cooled to room temperature.
The physicochemical property of brick body is: SiC, 70.23%; Sialon, 28.43%; Aluminum oxide, 0.03%; Apparent porosity, 12%; Volume density 2.8g/cm
3Compressive strength 240.6Mpa; Strength at normal temperature 65.7Mpa; 1400 ℃ of folding strength 65.9Mpa.Thermal shock resistance is good, and the alkali resistant erosional competency is good.
Embodiment 9
A kind of production process of utilizing microwave technology to carry out quick nitrogenizing reaction sintering Sialon carborundum refractory material (hereinafter referred is the imperial carborundum refractory material of match):
Raw material:
The sic raw material specification of quality is, SiC is greater than 98%, Fe
2O
3Less than 0.5%.
The proportioning of each silicon-carbide particle granularity is: 6.0mm～3mm accounts for 19%; 3～1mm accounts for 22%; 1～0.5mm accounts for 10%; ≤ 0.5mm accounts for 8%, accounts for 14% less than the carbide fine powder of 0.08mm; Total add-on of silicon carbide is 73% (weight percent).
The specification of quality of silica flour raw material is, Si is greater than 97%, Fe
2O
3Less than 0.5%.Granularity is less than 60 μ m, and add-on is 18%.
Alumina powder jointed specification of quality is Al
2O
3Greater than 99%, Fe
2O
3Less than 0.2%, size-grade distribution is 0.1 μ m～2 μ m, and add-on is 5%.
The specification of quality of aluminium powder is, Al is greater than 99%, Fe
2O
3Less than 0.2%, size-grade distribution is 0.1 μ m～3 μ m, and add-on is 4%.
Batching:
Earlier the silicon-carbide particle adding of each granularity is forced to stir in the sand mill and mixed 4 minutes, the back added carbide fine powder, silica flour, aluminum oxide powder and aluminium powder remix after 5 minutes, it is that concentration is 12% polyvinyl alcohol solution that adding adds the normal temperature wedding agent, add-on is 6% of total batching quality, after mixed 40 minutes forcing to stir in the sand mill together.
Moulding:
The material that mixes is suppressed into the thick goods of the wide 130mm of the long 350mm of 400mm in brick pressing machine, brick pressing machine is 1000 tons a friction press.
Dry:
The based on silicon carbide firebrick billet of forming under 30 ℃～200 ℃ temperature dry 6 hours, the moisture of dry back adobe should be controlled at less than 0.3%.
The degreasing decarburization:
In kiln, blank is warming up to 300 ℃ under air atmosphere insulation carried out degreasing in 4 hours, be warming up to 500 ℃ then, air atmosphere insulation down carried out de-carbon in 6 hours.Heat-up rate is not more than 50 ℃/minute.
Nitrogenize is burnt till:
With the above-mentioned microwave agglomerating furnace of putting into, feed nitrogen (purity is weight percentage greater than 99.9wt%) sintering through blank behind the degreasing de-carbon.It is the industrial microwave source of 2450 megahertzes (MHz) that reaction and agglomerating plant adopt frequency.Heat-up rate is controlled at 1100 ℃/hour, is warming up to 1350 ℃ of insulations 2 hours, continues to be warming up to 1400 ℃ of temperature and be incubated 4 hours under this temperature.Can stop logical nitrogen when naturally cooling to 750 ℃.Can obtain matching imperial carborundum refractory material goods after being cooled to room temperature.
The physicochemical property of brick body is: SiC, 70.23%; Sialon, 28.43%; Aluminum oxide, 0.03%; Apparent porosity, 14%; Volume density 2.79g/cm
3Compressive strength 232.6Mpa; Strength at normal temperature 55.7Mpa; 1400 ℃ of folding strength 64.9Mpa.Thermal shock resistance is good, and the alkali resistant erosional competency is good.
Claims (4)
1, utilizes the method for microwave technology sintering Sialon carborundum refractory material, the industrial microwave source that this method employing frequency is 900～3000 megahertzes is as reaction and agglomerating microwave source, it is characterized in that: described method is with behind silicon-carbide particle and fine powder, silica flour, aluminum oxide fine powder, aluminium powder and the binding agent uniform mixing, be pressed into adobe by pressure forming machine, after oven dry of adobe process and the pre-degreasing carbonization treatment, the microwave that utilizes the industrial microwave source to produce under nitrogen atmosphere carries out nitrogenizing reaction and densification sintering with adobe, and the steps in sequence of described method is:
(1) raw material is selected silicon carbide for use, and silica flour is alumina powder jointed, aluminium powder, normal temperature wedding agent;
(2) with above-mentioned silicon carbide by weight percentage 90%～50%; Silica flour by weight percentage 5%～20%; Alumina powder jointed according to weight percent 1%～20%; Aluminium powder by weight percentage 0.5%～10%; Normal temperature wedding agent, add-on are 0.2～10% of total batching quality; Add together to force to stir in the sand mill and mix;
(3) the above-mentioned material that mixes is pressed into adobe in brick pressing machine;
(4) with the brick bat drying of forming, the moisture controlled of dry back adobe is less than 0.4%;
(5) with dried adobe in 300～500 ℃ of temperature ranges, air atmosphere down insulation carried out degreasing and de-carbon in 2～8 hours, heat-up rate is not more than 50 ℃/minute;
(6) put into microwave agglomerating furnace with above-mentioned through the blank behind the degreasing de-carbon, feed nitrogen; Be warming up to 1350 ℃, be incubated 0.5～2.5 hour; Continue to be warming up to 1650 ℃ of temperature, and under this temperature range, be incubated 0.5～8 hour;
When (7) naturally cooling to 700 ℃, stop logical nitrogen, be the imperial carborundum refractory material goods of match after being cooled to room temperature.
2, the method with microwave technology Fast Sintering Sialon carborundum refractory material according to claim 1, it is characterized in that: it is the microwave heating technique in the industrial microwave source of 900～3000 megahertzes that the described drying means of step (4) adopts frequency.
3, the method with microwave technology Fast Sintering Sialon carborundum refractory material according to claim 1, it 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, a kind of microwave that utilizes the certain frequency scope according to claim 1 carries out the method for rapid reaction agglomerating Sialon carborundum refractory material.It is characterized in that: it is that the industrial microwave source of 900～3000 megahertzes is as reaction and agglomerating microwave agglomerating furnace that present technique adopts frequency.
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