CN101654371A - Magnesium aluminum spinel-corundum-Sialon complex phase high-temperature resistant material and preparation method thereof - Google Patents
Magnesium aluminum spinel-corundum-Sialon complex phase high-temperature resistant material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a magnesium aluminum spinel-corundum-Sialon complex phase high-temperature resistant material and a preparation method thereof, belonging to the technical field of high-temperature resistant material. The main raw materials of the complex phase high-temperature resistant material contain high-aluminum fly ash, aluminum ash and magnesite. The main raw materials are mixed according to the following percentages: 0.1% to 90% of high-aluminum fly ash, 0.1% to 99% of aluminum ash and 0.1% to 40% of magnesite. The metallic aluminum in the aluminum fly ash is used as reducingagent. The magnesium aluminum spinel-corundum-Sialon complex phase high-temperature resistant material is acquired by adding binding material for forming after ball milling and mixing with dry methodand then performing aluminothermic reduction reaction under nitrogen atmosphere at 1350 DEG C to 1700 DEG C. The prepared complex phase high-temperature resistant material of the invention has the advantages of heat-resistant property, spalling resistance property and scour erosion-resisting property. The invention can efficiently lower the cost of magnesium aluminum spinel-corundum-Sialon complexphase high-temperature resistant material and find a new way to comprehensively use high-aluminum fly ash, aluminum ash and magnesite.
Description
Technical field:
The present invention relates to a kind of method of utilizing aluminous fly-ash, aluminium ash and magnesite to prepare the magnesium aluminum spinel-corundum-Sialon complex phase high-temperature resistant material, belong to technical field of refractory materials.
Background technology:
Flyash is the waste of a large amount of dischargings of fluidized-bed combustion boiler in coal-burning power plant and other coal-fired industry, and it is by the coal dust of wearing into certain fineness thin ash through being collected by dust-precipitator behind the high-temp combustion in fluidized-bed combustion boiler.It is a kind of active material that has, and its main chemical compositions is silicon-dioxide (SiO
2), aluminium sesquioxide (Al
2O
3), small amounts iron (Fe
2O
3) and calcium oxide (CaO) when sweetening agent (do not add during coal combustion calcareous).SiO wherein
2And Al
2O
3Content is the highest, and both sums generally account for more than 60%, is the main active ingredient and the high temperature resistant composition of flyash.By the end of 2002, the flyash volume of cargo in storage of China was up to 1,400,000,000 tons.According to incompletely statistics, the flyash of discharging from the coal-burning power plant present domestic every year is above 100,000,000 tons.Quantity is huge flyash so, and what have is discharged into ash, occupies a large amount of farmlands, and what have is discharged into rivers, and environment is polluted.How to solve so a large amount of lime-ash dischargings, eliminate harm,, become an important topic of electric power, environmental protection and materials industry obtaining increment utilization after the reprocessing of flyash process.
At present domestic generally all is directly or indirectly flyash to be used for cement (to produce the method for cement with high-calcium fly ass, CN1012951B), mortar (utilizes solid waste to prepare the method for thermal insulation mortar, CN 101033124A), produce vitrified brick (coal ash red mud baked bricks and manufacture method thereof, CN 1181363A), hollow block (flyash, the pearlite light hollow block, CN 1060459A), steam-pressing aero-concrete (a kind of gas concrete and making method, CN 1329334C), concrete adulterant and raw material (a kind of load larrying member eco-concrete compound and preparation method thereof, CN 1562858A), haydite (non-autoclaved and unburned haydite and using method thereof, CN 1304320C), produce fertilizer and improve the soil (a kind of nutrition base that is used for the plant ecological cultivation and preparation method thereof, CN 1255020C), the making road, construct dam body, the backfill of subsidence area, colliery and mine etc.But mainly based on building material industries such as cement and concrete, the increment effect of its utilization is not high.Therefore, increase the flyash especially comprehensive Utilization Ways of aluminous fly-ash and the added value that improves its utilization, become present problem demanding prompt solution.At present for high Al
2O
3Al in the flyash
2O
3Extraction and utilize research that some reports are also arranged, as: a kind of flyash that utilizes is produced silicon-dioxide and method of alumina, CN101049935A; A kind of production method of alumina, CN 1275860C.But from high Al
2O
3Extract Al in the flyash
2O
3Technological process have serious pollution problem, Al
2O
3The production cost height, and 1 ton of Al of every production
2O
3Will produce about 10 tons industrial solid castoff, cause solid waste to roll up, handle these solid waste and also will bring great difficulty.How efficiently to utilize high Al
2O
3Flyash is present problem demanding prompt solution.
The aluminium ash is the solid waste of slag after cooling processing that produces in the technological processs such as aluminum casting industry, aluminium regeneration industry and electrolytic aluminum industry.Oven-fresh aluminium slag contains 50%～70% metallic aluminium usually, after conventional recycling, still contains 15～30% metallic aluminium in the remaining aluminium scrap ash, because of grade is lower, generally no longer further extracts aluminium and discards.Also there is 10～25% Al in the aluminium ash simultaneously
2O
3AlN with 5～20% contains in addition than high basic metal and heavy metal compound, is deposited in plant area or landfill, not only causes the waste of resource, the pollution that also brings environment simultaneously.If can realize the high efficiente callback and the use of aluminium ash resource circulation of aluminium slag, will reduce the influence that ecotope is caused effectively.The processing mode of aluminium ash is except that landfill both at home and abroad at present, and the cycling and reutilization of aluminium ash mainly contains following several approach: (1) synthesized polymer aluminum chloride (water purification agent) (manufacture method of water purification agent, CN 1089240A; A kind of production method of sewage flocculant, CN 1009279B).Polymerize aluminum chloride has characteristics such as purification efficiency height, few, the easy filtration of dosage, production technique be simple, is good flocculation agent, has been widely used in the processing of trade effluent and sanitary wastewater.Produce water purification agent and produce a large amount of harmful chemical spent materials, have the secondary pollution problem that produces.(2) steel-making covering slag (insulating covering agent, sweetening agent etc.) (Clean Steel tundish covering flux and manufacture method thereof, CN1238134C; Desulfurizing agent for smelting iron and steel, CN 1223302A).The beginning of the eighties, in the Japan plate Co., Ltd. at first according to the grade of different aluminum ash, the molten steel oxidation of using it for the 200t electric furnace dust temperature raising and refinement and deoxidation desulfurization.At present, domestic aluminium ash composition complexity deals with difficulty, and molten steel is easy to generate pollution, can't apply.(3) preparing brown corundum, fireproof magnesia alumina spinel starting material (utilizes wasted aluminium ash to make the method for fireproof raw material (brown corundum), CN 1927770A; Produce the method for electric melting magnesium aluminum spinel, CN 1919739A).This approach can effectively improve the added value that the aluminium ash utilizes, but in the aluminium ash a certain amount of SiO will be arranged
2Be wasted with available composition such as AlN, and from the aluminium ash electric smelting to obtain the preparation technology of target product comparatively complicated.
Sialon and composite diphase material thereof have unique over-all properties, and promptly good, the high strength of high-temperature stability, wear-resistant, corrosion-resistant and the anti-thermal shock stability is good in and difficult advantages such as wetting metals is the non-oxidized substance refractory materials that a class has development potentiality.Traditional Sialon synthetic method adopts chemical feedstocks usually, and cost is higher, has limited its large-scale commercial applications application.In recent years, adopting natural aluminosilicate and industrial solid castoff is synthetic Sialon of raw material and composite diphase material thereof, has become a direction of high temperature ceramic material development.
According to document, some reports also appear in succession for aluminium ash and fly-ash Preparation Sialon and matrix material thereof, Chinese invention patent " a kind of magnesium-aluminium spinel/Sialon composite ceramic material and preparation method thereof " (CN 101066865A) utilizes aluminium ash synthetic MgAl spinal/Sialon matrix material, has utilized part raw mineral materials (bauxitic clay grog fine powder) and synthesis material (MgO fine powder, silica flour and aluminium powder).Chinese invention patent " utilizes the method for aluminium ash and the synthetic Sialon ceramic powder of flyash " and (CN101353256A) utilizes aluminium ash and flyash to be raw material, add carbon black as reductive agent, prepared the Sialon ceramic powder by the hot composite reduction nitriding process of aluminothermy carbon.At present, still finding no employing aluminous fly-ash, aluminium ash and magnesite is raw material prepares the magnesium aluminum spinel-corundum-Sialon complex phase high-temperature resistant material by original position thermite reduction nitrogenize patent documentation report.
Summary of the invention:
In the objective of the invention is to use at present aluminous fly-ash and aluminium ash large-scale industrialization the ubiquity added value low, be easy to generate problem such as secondary waste, proposes a kind of with aluminous fly-ash, aluminium ash and and magnesite be that raw material passes through original position thermite reduction nitriding process preparation low cost, high performance magnesium aluminum spinel-corundum-Sialon complex phase high-temperature resistant material.
There is Al in the aluminium ash
2O
3, AlN, Al, MgO, SiO
2Deng, main chemical compositions SiO in the flyash
2, Al
2O
3, magnesite at high temperature is decomposed to form MgO, the metallic aluminium reduction nitridation SiO wherein in the aluminium ash
2Form Si
3N
4, Al
2O
3Admittedly be fused to Si with AlN
3N
4Middle Sialon, MgO and the Al of forming
2O
3Form magnesium-aluminium spinel.The magnesium aluminum spinel-corundum-Sialon composite diphase material is just at Al
2O
3, MgO, spinel have on the basis of good high temperature resistant, anti-scour property the matrix material of composite S ialon again, to have better heat-shock resistance and use properties, and particularly can avoid after the Sialon oxidation forming the cavity behind the oxidation of coal of carbon containing refractory and the mechanical behavior under high temperature that reduces refractory materials.Utilizing aluminous fly-ash, aluminium ash and magnesite to prepare the Sialon composite diphase material will further reduce cost, especially the metallic aluminium in the aluminium ash is active reductive agent, the gas phase of comparing the thermite reduction generation with carbothermic reduction reaction is less, so the material comparatively fine and close to preparation has more meaning, really having accomplished turns waste into wealth.
A kind of magnesium aluminum spinel-corundum-Sialon complex phase high-temperature resistant material that the present invention proposes, it is characterized in that: this complex phase high-temperature resistant material is a main raw material with aluminous fly-ash, aluminium ash and magnesite.Described aluminous fly-ash (alumina content is greater than 25%, and calcium oxide content is less than 5.0%) accounts for 0.1～90% of total batching massfraction; Described aluminium ash (content of metallic aluminium is greater than 10%, and the content of aluminum oxide is greater than 10%, and it can be the aluminium ash that produces in the technological processs such as aluminum casting industry, aluminium regeneration industry and electrolytic aluminum industry) accounts for 0.1～99% of total batching massfraction.Described magnesite (magnesium oxide is greater than 40%) accounts for 0.1～40% of total batching massfraction.
The method of a kind of magnesium aluminum spinel-corundum-Sialon complex phase high-temperature resistant material that the present invention proposes; it is characterized in that: described method is at first prepared burden above-mentioned various raw materials in required ratio; mixed 1～12 hour through dry ball milling then; the powder that mixes is added the wedding agent that accounts for powder total mass 3%～10%, and (it is about 30% industrial dextrin that wedding agent generally can adopt concentration; concentration is that about 30% calcium lignosulfonate solution or concentration are about 10% polyvinyl alcohol solution) be pressed into base substrate; base substrate is handled through 100～300MPa isostatic cool pressing; with base substrate behind 50 ℃～100 ℃ down dry 2～6h; under condition of nitrogen gas (nitrogen pressure of reaction be 0.12～1.0MPa) in 900～1000 ℃ the insulation 0.5～1h; 1200～1300 ℃ of insulation 1～2h; (temperature increasing schedule is from 5～10 ℃/min of room temperature to 900 ℃ temperature rise rate in 1350 ℃～1700 ℃ insulation 2～10h again; more than 900 ℃; 2～5 ℃/min) carry out original position thermite reduction nitrogenizing reaction, under nitrogen protection, naturally cool to room temperature at last and can obtain this complex phase high-temperature resistant material with stove.
The present invention not only can provide a new technological approaches for the comprehensive utilization of aluminous fly-ash, aluminium ash and magnesite zero release, high added value, can obtain simultaneously the senior complex fire resistant material of a kind of low cost, high comprehensive performance, for certain contribution is made in the hot industry development.
Description of drawings:
Fig. 1 is aluminous fly-ash among the embodiment 1, aluminium ash and the magnesite XRD figure spectrum at 1400 ℃ * 3h nitrogenize after product;
Fig. 2 is aluminous fly-ash among the embodiment 2, aluminium ash and the magnesite XRD figure spectrum at 1500 ℃ * 3h nitrogenize after product;
Fig. 3 is aluminous fly-ash among the embodiment 3, aluminium ash and the magnesite XRD figure spectrum at 1550 ℃ * 3h nitrogenize after product.
Embodiment:
Below in conjunction with embodiment technical scheme of the present invention is described further:
Composition of raw materials and proportioning that the present invention adopts are respectively: aluminous fly-ash accounts for 0.1～90% of total batching massfraction, and the aluminium ash accounts for 0.1～99% of total batching massfraction, and magnesite accounts for 0.1～40% of total batching massfraction.Wherein, alumina content is greater than 25% in the aluminous fly-ash, and calcium oxide content is less than 5.0%; The content of metallic aluminium is greater than 10% in the aluminium ash, and the content of aluminum oxide is greater than 10%, and it can be the aluminium ash that produces in the technological processs such as aluminum casting industry, aluminium regeneration industry and electrolytic aluminum industry; Magnesium oxide is greater than 40% in the magnesite.Guaranteeing during batching that aluminium in the aluminium ash is enough to can the reducing powder coal ash, the SiO in the aluminium ash
2Nitrogenize forms Si
3N
4
The present invention at first prepares burden above-mentioned various raw materials in required ratio; mixed 1～12 hour through dry ball milling then; the powder that mixes is added the wedding agent that accounts for powder total mass 3%～10%, and (it is about 30% industrial dextrin that wedding agent generally can adopt concentration; concentration is that about 30% calcium lignosulfonate solution or concentration are about 10% polyvinyl alcohol solution) be pressed into base substrate; base substrate is handled through 100～300MPa isostatic cool pressing; with base substrate behind 50 ℃～100 ℃ down dry 2～6h; under condition of nitrogen gas (nitrogen pressure of reaction be 0.12～1.0MPa) in 900～1000 ℃ the insulation 0.5～1h; 1200～1300 ℃ of insulation 1～2h; (temperature increasing schedule is from 5～10 ℃/min of room temperature to 900 ℃ temperature rise rate in 1350 ℃～1700 ℃ insulation 2～10h again; more than 900 ℃; 2～5 ℃/min) carry out original position thermite reduction nitrogenizing reaction, under nitrogen protection, naturally cool to room temperature at last and can obtain this complex phase high-temperature resistant material with stove.
A kind of preparation technology's flow process of magnesium aluminum spinel-corundum-Sialon complex phase high-temperature resistant material is:
Raw material → raw materials pretreatment (pulverizing and jevigating sieves) → batching → dry ball milling mixing → adding wedding agent is made static pressure processing → drying → nitrogenizing reaction sintering → magnesium aluminum spinel-corundum-Sialon complex phase high-temperature resistant material such as base substrate → wait
The complex phase high-temperature resistant material of the present invention preparation has good high temperature resistant, heat-shock resistance and anti-scour property, can effectively reduce the cost that contains magnesium-aluminium spinel, corundum, Sialon complex phase high-temperature resistant material, be that new application approach has been opened up in the aluminous fly-ash and the comprehensive utilization of aluminium ash and the efficient utilization of magnesite simultaneously.
Embodiment 1
Raw material:
Shanxi power plant fly ash, its chemical constitution are (w): Al
2O
340.37%, SiO
252.45%, Fe
2O
32.36%, CaO 0.75%, and MgO 0.54%, loss on ignition 1.56%, other 1.97%, add-on accounts for 40% of total batching massfraction;
The aluminium ash of Shanghai aluminium manufacturer, its chemical constitution are (w): Al
2O
318.02%, AlN 14.13%, and Al 28.62%, MgO7.1%, SiO
25.9%, Fe
2O
34.0%, CaO 2.8%, Na
2O 2.6%, TiO
21.6%, loss on ignition 12.8%, other 2.43%, add-on accounts for 55% of total batching massfraction;
The magnesite of Liaoning output, its chemical constitution are (w): MgO 44.66%, Al
2O
30.33%, SiO
21.35%, CaO1.52%, Fe
2O
30.51%, loss on ignition 50.40%, add-on account for 5% of total batching massfraction.
Raw materials pretreatment:
Above-mentioned raw materials is utilized levigate mistake 200 mesh sieves of vibration mill respectively, make raw material granularity before use thinner.
Batching and ball milling:
The raw material of above-mentioned various processing is prepared burden in described ratio, then with admixtion dry ball milling mixing 6h.
Be shaped with dry:
It is the interim wedding agents of about 30% industrial dextrin that above-mentioned compound is added the concentration that accounts for compound total mass 10%, is suppressed into sample base substrate, forming pressure 50MPa by brick pressing machine.The sample base substrate is closely knit through the isostatic cool pressing pressurization, pressure 200MPa pressurize 1min.Base substrate is 50 ℃ of dryings 1 hour, 100 ℃ of dryings 2 hours.
Original position thermite reduction nitrogenizing reaction:
Place nitriding furnace under 0.12MPa nitrogen, to react base substrate, and at 900 ℃ of insulation 1h, 1200 ℃ of insulation 2h, 1400 ℃ of insulation 3h, temperature increasing schedule: from 10 ℃/min of room temperature to 900 ℃ temperature rise rate, more than 900 ℃, 2～5 ℃/min.Under nitrogen protection, naturally cool to room temperature at last and can obtain this MgAl with stove
2O
4-Al
2O
3-Sialon complex phase high-temperature resistant material.
The physicochemical property of sample is: the XRD figure of nitrogenize product is composed as shown in Figure 1, and its principal crystalline phase is magnesium-aluminium spinel phase, Sialon phase, corundum phase; The apparent porosity of sample is 10% behind the sintering, and volume density is 3.20g/cm
3, strength at normal temperature is 153.1MPa; Slag corrosion resistance ability, thermal shock resistance are good.
Embodiment 2
Raw material:
Beijing power plant fly ash, its chemical constitution (w): SiO
254.30%, Al
2O
335.40%, Fe
2O
31.50%, CaO 1.80%, and MgO 0.70%, loss on ignition 4.30%, other 2.0%, add-on accounts for 38% of total batching massfraction;
The aluminium ash of Hebei aluminium manufacturer, its chemical constitution are (w): Al
2O
321.05%, AlN 11.03%, Al 29.55%, MgO12.5%, SiO
25.0%, Fe
2O
33.8%, CaO 3.4%, Na
2O 1.6%, TiO
21.2%, loss on ignition 8.77%, other 2.10%, account for 52% of total batching massfraction;
The magnesite of Liaoning output, its chemical constitution are (w): MgO 44.66%, Al
2O
30.33%, SiO
21.35%, CaO1.52%, Fe
2O
30.51%, loss on ignition 50.40%, add-on account for 10% of total batching massfraction.
Raw materials pretreatment:
Above-mentioned raw materials is utilized levigate mistake 200 mesh sieves of vibration mill respectively, make raw material granularity before use thinner.
Batching and ball milling:
The raw material of above-mentioned various processing is prepared burden in described ratio, then with admixtion dry ball milling mixing 8h.
Be shaped with dry:
It is about 30% calcium lignosulfonate solution that above-mentioned compound is added the concentration that accounts for compound total mass 5%, is suppressed into sample base substrate, forming pressure 50MPa by brick pressing machine.The sample base substrate is closely knit through the isostatic cool pressing pressurization, pressure 200MPa pressurize 1min.Base substrate is 50 ℃ of dryings 1 hour, 100 ℃ of dryings 2 hours.
Original position thermite reduction nitrogenizing reaction:
Place nitriding furnace under 0.12MPa nitrogen, to react base substrate, and at 900 ℃ of insulation 1h, 1300 ℃ of insulation 2h, 1500 ℃ of insulation 3h, temperature increasing schedule: from 10 ℃/min of room temperature to 900 ℃ temperature rise rate, more than 900 ℃, 2～5 ℃/min.Under nitrogen protection, naturally cool to room temperature at last and can obtain this MgAl with stove
2O
4-Al
2O
3-Sialon complex phase high-temperature resistant material.
The physicochemical property of sample is: the XRD figure of nitrogenize product is composed as shown in Figure 2, and its principal crystalline phase is corundum phase, Sialon phase MgAl
2O
4Phase also has a spot of Al
6O
3N
4Sample apparent porosity behind the sintering is 9.2%, and volume density is 3.15g/cm
3, strength at normal temperature is 147.5MPa; Slag corrosion resistance ability, thermal shock resistance are good.
Embodiment 3
Raw material:
Shanxi power plant fly ash, its chemical constitution are (w): Al
2O
340.37%, SiO
252.45%, Fe
2O
32.36%, CaO 0.75%, and MgO 0.54%, loss on ignition 1.56%, other 1.97%, add-on accounts for 41% of total batching massfraction;
The aluminium ash of Hebei aluminium manufacturer, its chemical constitution are (w): Al
2O
321.05%, AlN 11.03%, Al 29.55%, MgO12.5%, SiO
25.0%, Fe
2O
33.8%, CaO 3.4%, Na
2O 1.6%, TiO
21.2%, loss on ignition 8.77%, other 2.10%, the aluminium ash accounts for 59% of total batching massfraction.
The magnesite of Liaoning output, its chemical constitution are (w): MgO 44.66%, Al
2O
30.33%, SiO
21.35%, CaO1.52%, Fe
2O
30.51%, loss on ignition 50.40%, add-on account for 5% of total batching massfraction.
Raw materials pretreatment:
Above-mentioned raw materials is utilized levigate mistake 200 mesh sieves of vibration mill respectively, make raw material granularity before use thinner.
Batching and ball milling:
The raw material of above-mentioned various processing is prepared burden in described ratio, then with admixtion dry ball milling mixing 8h.
Be shaped with dry:
It is about 30% calcium lignosulfonate solution that above-mentioned compound is added the concentration that accounts for compound total mass 5%, is suppressed into sample base substrate, forming pressure 50MPa by brick pressing machine.The sample base substrate is closely knit through the isostatic cool pressing pressurization, pressure 200MPa pressurize 1min.Base substrate is 50 ℃ of dryings 1 hour, 100 ℃ of dryings 2 hours.
Original position thermite reduction nitrogenizing reaction:
Place nitriding furnace under 0.12MPa nitrogen, to react base substrate, and at 900 ℃ of insulation 1h, 1300 ℃ of insulation 2h, 1550 ℃ of insulation 3h, temperature increasing schedule: from 10 ℃/min of room temperature to 900 ℃ temperature rise rate, more than 900 ℃, 2～5 ℃/min.Under nitrogen protection, naturally cool to room temperature at last and can obtain this MgAl with stove
2O
4-Al
2O
3-Sialon complex phase high-temperature resistant material.
The physicochemical property of sample is: the XRD figure of nitrogenize product is composed as shown in Figure 3, and its principal crystalline phase is magnesium-aluminium spinel phase, Sialon phase, corundum phase; The apparent porosity of sample is 9.5% behind the sintering; Volume density is 3.25g/cm
3, strength at normal temperature is 162.0MPa; Slag corrosion resistance ability, thermal shock resistance are good.
Claims (3)
1, a kind of magnesium aluminum spinel-corundum-Sialon complex phase high-temperature resistant material and preparation method thereof, it is characterized in that: this complex phase high-temperature resistant material is a main raw material with aluminous fly-ash, aluminium ash, magnesite, aluminous fly-ash according to account for total batching massfraction 0.1～90%, the aluminium ash according to account for total batching massfraction 0.1～99%, magnesite is according to 0.1～40% preparing burden of accounting for total batching massfraction, after dry ball milling mixes, add suitable wedding agent and be shaped.Base substrate prepares the magnesium aluminum spinel-corundum-Sialon complex phase high-temperature resistant material under the condition of high temperature and nitrogenize.
2, magnesium aluminum spinel-corundum-Sialon complex phase high-temperature resistant material according to claim 1, it is characterized in that: the alumina content in the described aluminous fly-ash is greater than 25%, and calcium oxide content is less than 5.0%.The content of metallic aluminium is greater than 10% in the described aluminium ash, and the content of aluminum oxide is greater than 10%, and it can be the aluminium ash that produces in the technological processs such as aluminum casting industry, aluminium regeneration industry and electrolytic aluminum industry.Magnesium oxide in the described magnesite is greater than 40%.
3; the method of a kind of preparation magnesium aluminum spinel-corundum-Sialon complex phase high-temperature resistant material as described; it is characterized in that: described method is at first prepared burden above-mentioned various raw materials in required ratio; mixed 1～12 hour through dry ball milling then; the powder that mixes is added the wedding agent that accounts for powder total mass 3%～10%, and (it is about 30% industrial dextrin that wedding agent generally can adopt concentration; concentration is that about 30% calcium lignosulfonate solution or concentration are about 10% polyvinyl alcohol solution) be pressed into base substrate; base substrate is handled through 100～300MPa isostatic cool pressing; with base substrate behind 50 ℃～100 ℃ down dry 2～6h; under condition of nitrogen gas, be incubated 0.5～1h prior to 900～1000 ℃; 1200～1300 ℃ of insulation 1～2h; carry out original position thermite reduction nitrogenizing reaction in 1350 ℃～1700 ℃ insulation 2～10h again, under nitrogen protection, naturally cool to room temperature at last and can obtain this complex phase high-temperature resistant material with stove.
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