CN102701746B - Preparation method of infrared radiation ceramic powder in spinel-silicate multi-phase composite system - Google Patents
Preparation method of infrared radiation ceramic powder in spinel-silicate multi-phase composite system Download PDFInfo
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Abstract
The invention relates to a preparation method of infrared radiation ceramic powder in a spinel-silicate multi-phase composite system. The preparation method comprises the following steps: firstly, various raw materials are taken at a specified ratio, and then the primary processing of milling, mixing, drying and press-molding on the raw materials to form a blocky blank is carried out, and the obtained blocky blank is subjected to heating and heat preservation at the temperature in the range of 800 DEG C to 980 DEG C to form a spinel-type solid solution; then the temperature is continually heated up to 1100 DEG C to 1300 DEG C to heat and preserve heat of the blocky blank to form a silicate mineral, the spinel-type solid solution and the silicate minerals are composited in a multiphase way to form a black sintered body with a multiphase composite structure; and the obtained black sintered body is crushed, ground and sieved, so that the infrared radiation ceramic powder in the spinel-silicate multi-phase composite system can be obtained. The raw materials used in the invention are ordinary raw materials which are extensive in sources, the preparation method is simple and practical, short in production cycle and low in manufacturing cost, can be used in infrared radiation energy-saving coatings, infrared radiant heaters and the like of a high temperature industrial furnace (boiler), and has wide application prospect.
Description
Technical field
The present invention relates to infrared radiant material field, relate in particular to the preparation method of spinel-silicate multiphase composite system infrared radiation ceramic powder of the products such as a kind of infrared radiative energy-saving coating that is specially adapted to high-temperature industrial furnace (boiler), infrared radiation heater.
Background technology
Infrared radiant material, because its excellent infrared radiation property is subject to extensive concern, is used widely at aspects such as Energy Saving for Industrial Furnace, raising Infrared heaters thermo-efficiency, spacecraft thermal controls.At present, develop multiple IR Radiation Ceramic Materials both at home and abroad, mainly contained zirconium white system, zircon sand system, silicon carbide system, chromic oxide system, ferric oxide-manganese oxide system etc.
In all kinds of IR Radiation Ceramic Materials, the infrared radiation property of ferric oxide-manganese oxide system transition metal oxide is good, and the temperature stability of its structure and infrared radiation property is better, particularly comes into one's own.But the thermal expansivity of this class infrared radiant material is larger, anti-thermal shock impact property is undesirable.In ferric oxide-manganese oxide system, add the silicate minerals material that thermal expansivity is lower can improve its anti-thermal shock impact property, yet the infrared emittance of silicate minerals material is conventionally lower, add in a large number silicate minerals material when improving anti-thermal shock impact property, can reduce the infrared radiation property of material.And, preparation technology's more complicated of the infrared radiant material of this compound system, often need could obtain through double-firing process, first by a solid phase synthesis, make transition metal oxide form spinel solid solution, then by secondary solid phase synthesis, make spinel solid solution and silicate minerals material form the final product of heterogeneous composite structure.The preparation method of above-mentioned double-firing process needs ball milling mixing, fragmentation, pulverizing and the sintering of twice, and energy consumption is large, and production efficiency is low, and production cost is high.Easy, the high efficiency preparation method of exploring transiting metal oxidation spinel-silicate multiphase composite system infrared radiation ceramic powder have great importance to practical application.
Summary of the invention
Technical problem to be solved by this invention is to propose a kind of short-cut method of preparing the multiphase composite system infrared radiation ceramic powder of spinel-silicate by once-firing for above-mentioned prior art, and its efficiency is high, and production cost is low.
The present invention solves the problems of the technologies described above adopted technical scheme: the preparation method of spinel-silicate multiphase composite system infrared radiation ceramic powder, is characterized in that including following steps:
1) preliminary treatment: first various raw materials are prepared burden to scale, more described batching is carried out to ball milling, mixing, the preliminary treatment that dry and compression moulding is block base substrate; Described raw material comprises the A component of tangible one-tenth spinel type sosoloid, B component and the accelerant C component of formation silicate minerals, and its mass ratio is 100%:20 ~ 300%:0 ~ 15%, and described A component includes Fe
2o
3, MnO
2, CuO, Co
2o
3, Mo
2o
3, NiO, V
2o
5and WO
3, described B component includes Al
2o
3, SiO
2, MgO, BaO, CaO and TiO
2, described accelerant C component includes glass powder and B
2o
3, each component concentration is by percentage to the quality:
Fe
2O
3：0~60%、?MnO
2:?0~60%、Al
2O
3：5~50%、SiO
2：5~50%、CuO：0~12%、
Co
2O
3：0~10%、MgO：0~10%、Mo
2O
3：0~6%、NiO：0~6%、TiO
2：0~6%、
V
2o
5: 0 ~ 5%, WO
3: 0 ~ 5%, BaO:0 ~ 3%, CaO:0 ~ 3%, glass powder: 0 ~ 3%,
B
2O
3：0~3%；
2) burn till preparation: the block base substrate of step 1) gained is carried out to heating and thermal insulation in 800 ~ 980 ℃ of temperature ranges, and the heating and thermal insulation time is 1 ~ 6 hour, forms spinel type sosoloid; Then continue to be warmed up in 1100 ~ 1300 ℃ of temperature ranges and carry out heating and thermal insulation, the heating and thermal insulation time is 2 ~ 8 hours, forms silicate minerals, spinel type sosoloid and silicate minerals is carried out heterogeneous compound, forms the black sintered compact of heterogeneous composite structure;
3) by step 2) the black sintered compact of gained through broken, pulverize and cross 200 ~ 500 mesh sieves, prepare the multiphase composite system infrared radiation ceramic powder that granularity is less than spinel-silicate of 74 μ m.
Press such scheme, each component concentration of described raw material is preferably 20%Fe by percentage to the quality
2o
3, 12%MnO
2, 2.4%CuO, 2.4%Mo
2o
3, 2%V
2o
5, 1.2%WO
3, 20%Al
2o
3, 25.1%SiO
2, 10%MgO, 1.5%BaO, 1.4%CaO, 1% glass powder and 1%B
2o
3.
Press such scheme, each component concentration of described raw material is preferably 11%MnO by percentage to the quality
2, 10%Co
2o
3, 3%NiO, 5%WO
3, 50%Al
2o
3, 9%SiO
2, 6%TiO
2, 3%CaO and 3% glass powder.
Press such scheme, each component concentration of described raw material is preferably 6%Fe by percentage to the quality
2o
3, 12%CuO, 4%Mo
2o
3, 5%V
2o
5, 14%Al
2o
3, 50%SiO
2, 3%MgO, 3%BaO and 3%B
2o
3.
Press such scheme, each component concentration of described raw material is preferably 60%Fe by percentage to the quality
2o
3, 8%MnO
2, 4%CuO, 3%Co
2o
3, 6%Mo
2o
3, 2%WO
3, 5%Al
2o
3, 10%SiO
2, 1%MgO and 1%BaO.
Press such scheme, each component concentration of described raw material is preferably 60%MnO by percentage to the quality
2, 4%CuO, 2%Mo
2o
3, 3%V
2o
5, 6%NiO, 11%Al
2o
3, 5%SiO
2, 3%TiO
2, 2%BaO, 2% glass powder and 2%B
2o
3.
Press such scheme, each component concentration of described raw material is preferably in mass ratio by percentage to the quality: 11%Fe
2o
3, 30%MnO
2, 3%CuO, 2%Mo
2o
3, 2%V
2o
5, 1%WO
3, 33%Al
2o
3, 14%SiO
2, 3%CaO and 1% glass powder.
Press such scheme, each component concentration of described raw material is preferably in mass ratio by percentage to the quality: 24%Fe
2o
3, 40%MnO
2, 7%Co
2o
3, 3%Mo
2o
3, 2%NiO, 14%Al
2o
3, 6%SiO
2, 1%MgO, 1%BaO, 1%CaO and 1%B
2o
3.
Press such scheme, each component concentration of described raw material is preferably 30%Fe by percentage to the quality
2o
3, 21%MnO
2, 10%CuO, 1%WO
3, 10%Al
2o
3, 23%SiO
2, 2%BaO and 3%MgO.
Press such scheme, described glass powder is formed by the raw material configuration of following quality percentage composition: SiO
2: 65%, Al
2o
3: 15%, CaO:5%, BaO:3%, MgO:8%, TiO
2: 2%, ZnO:2%.
Primitive reaction principle of the present invention is: by sintering temperature system, control solid phase synthesis, the formation solid phase synthesis of silicate minerals and the heterogeneous complex reaction of spinel type sosoloid and silicate minerals that spinel type sosoloid occurs to form various raw materials substep under differing temps, and utilize promotor to improve the solid phase synthesis of spinel type sosoloid and the solid phase synthesis of silicate minerals.
Compare with the preparation method of existing spinel-silicate multiphase composite system infrared radiation ceramic powder, feature of the present invention is:
(1) in 800 ~ 980 ℃ of temperature ranges, Fe
2o
3, MnO
2, CuO, Co
2o
3, Mo
2o
3, NiO, V
2o
5and WO
3etc. multiple transition metal oxide, by solid state reaction, form spinel type sosoloid.Owing to being distributed with the multiple transition metal ion of different sorts and valence state in the crystalline structure at spinel type sosoloid, strengthened its ir radiation ability, compare with current ferric oxide-manganese oxide system material, there is better infrared radiation property;
(2) at 1100 ~ 1300 ℃ of temperature ranges, Al
2o
3, SiO
2, MgO, BaO, CaO, TiO
2deng oxide compound, by solid state reaction, form silicate minerals, transition metal ion in a small amount of spinel type sosoloid can enter in the lattice of formed silicate phase in solid solution, thereby improved the infrared radiation property of silicate minerals, overcome the lower deficiency of conventional silicate minerals material infrared emittance;
(3) by control, heat up and heat preservation method system, make the solid phase synthesis of spinel type sosoloid, heterogeneous being compounded in once-firing process of the solid phase synthesis of silicate minerals and spinel type sosoloid and silicate minerals completes successively, simplified production process, shortened the production cycle, enhance productivity, reduce manufacturing cost;
(4) add a small amount of glass powder and B
2o
3deng low melting component, promote completing successively of the solid phase synthesis of spinel type sosoloid and the solid phase synthesis of silicate minerals;
The raw materials used common raw material that is of the present invention, preparation method is simple, the Stability Analysis of Structures of the heterogeneous compound system material of spinel-silicate is good, infrared radiation property is good, and be easy to regulate by controlling composition structure and the performance of material, application prospect is extensive, is specially adapted to the product such as infrared radiative energy-saving coating, infrared radiation heater of high-temperature industrial furnace (boiler).
Accompanying drawing explanation
Fig. 1 is the XRD figure of the heterogeneous compound system ceramic powder of embodiment 1 spinel-silicate.
Embodiment
Below in conjunction with embodiment, the present invention is further detailed explanation, but this explanation can not be construed as limiting the invention:
Embodiment 1
In mass ratio: 20%Fe
2o
3, 12%MnO
2, 2.4%CuO, 2.4%Mo
2o
3, 2%V
2o
5, 1.2%WO
3, 20%Al
2o
3, 25.1%SiO
2, 10%MgO, 1.5%BaO, 1.4%CaO, 1% glass powder and 1%B
2o
3prepare burden, the raw material of described glass powder consists of: 65%SiO
2, 15%Al
2o
3, 5%CaO, 3%BaO, 8%MgO, 2%TiO
2, 2%ZnO, by above-mentioned batching carry out ball milling, mixing, dry and compression moulding is block base substrate; Burning till in preparation process of above-mentioned block base substrate, first be heated to 950 ℃ of insulations 4 hours, form spinel type sosoloid, then continue to be warmed up to 1200 ℃ of insulations 2 hours, form silicate minerals, spinel type sosoloid and silicate minerals are carried out heterogeneous compound, form the black sintered compact of heterogeneous composite structure; Through broken and pulverizing, cross 320 mesh sieves again, prepare the heterogeneous compound system ceramic powder of spinel-silicate that granularity is less than 47 μ m.
The normal direction all wave band radiant ratio of the heterogeneous compound system ceramic powder of spinel-silicate of gained is that the radiant ratio of 0.91,8 μ m ~ 25 mu m waveband is that the radiant ratio of 0.93,8 μ m ~ 14 mu m waveband is that the radiant ratio of 0.94,14 μ m ~ 25 mu m waveband is 0.95.
Fig. 1 is multiple transition metal oxide and Al in embodiment 1
2o
3, SiO
2, oxide compound synthetic product that forms after Primary batching system and secondary substep high temperature solid state reaction such as MgO, BaO, CaO XRD figure compose, be mainly the diffraction peak of spinel type sosoloid and trichroite, in addition the diffraction honeybee that also has a small amount of magnesium-aluminium spinel, illustrate that synthetic product has heterogeneous composite structure, mainly spinel type sosoloid and trichroite, consist of, wherein multiple transition metal oxide forms the sosoloid of spinel structure.
Embodiment 2
In mass ratio: 11%MnO
2, 10%Co
2o
3, 3%NiO, 5%WO
3, 50%Al
2o
3, 9%SiO
2, 6%TiO
2, 3%CaO, 3% glass powder prepare burden, wherein the raw material of glass powder consists of 65%SiO
2, 15%Al
2o
3, 5%CaO, 3%BaO, 8%MgO, 2%TiO
2, 2%ZnO, by above-mentioned batching carry out ball milling, mixing, dry and compression moulding is block base substrate; Burning till in preparation process of above-mentioned base substrate, be first heated to 800 ℃ of insulations 6 hours, then continue to be warmed up to 1300 ℃ of insulations 6 hours; Through broken and pulverizing, cross 200 mesh sieves again, prepare the heterogeneous compound system ceramic powder of spinel-silicate that granularity is less than 74 μ m.
The normal direction all wave band radiant ratio of the heterogeneous compound system ceramic powder of spinel-silicate is that the radiant ratio of 0.90,8 μ m ~ 25 mu m waveband is that the radiant ratio of 0.94,8 μ m ~ 14 mu m waveband is that the radiant ratio of 0.92,14 μ m ~ 25 mu m waveband is 0.94.
Embodiment 3
In mass ratio: 6%Fe
2o
3, 12%CuO, 4%Mo
2o
3, 5%V
2o
5, 14%Al
2o
3, 50%SiO
2, 3%MgO, 3%BaO, 3%B
2o
3prepare burden, by above-mentioned batching carry out ball milling, mixing, dry and compression moulding is block base substrate; Burning till in preparation process of above-mentioned base substrate, be first heated to 950 ℃ of insulations 2 hours, then continue to be heated to 1200 ℃ of insulations 8 hours; Through broken and pulverizing, cross 400 mesh sieves again, prepare the heterogeneous compound system ceramic powder of spinel-silicate that granularity is less than 38 μ m.
The normal direction all wave band radiant ratio of the heterogeneous compound system ceramic powder of spinel-silicate is that the radiant ratio of 0.89,8 μ m ~ 25 mu m waveband is that the radiant ratio of 0.90,8 μ m ~ 14 mu m waveband is that the radiant ratio of 0.90,14 μ m ~ 25 mu m waveband is 0.93.
Embodiment 4
In mass ratio: 60%Fe
2o
3, 8%MnO
2, 4%CuO, 3%Co
2o
3, 6%Mo
2o
3, 2%WO
3, 5%Al
2o
3, 10%SiO
2, 1%MgO, 1%BaO prepare burden, by above-mentioned batching carry out ball milling, mixing, dry and compression moulding is block base substrate; Burning till in preparation process of above-mentioned base substrate, be first heated to 980 ℃ of insulations 3 hours, 1250 ℃ of insulations 2 hours then continue to heat up; Through broken and pulverizing, cross 500 mesh sieves again, prepare the heterogeneous compound system ceramic powder of spinel-silicate that granularity is less than 26 μ m.
The normal direction all wave band radiant ratio of the heterogeneous compound system ceramic powder of spinel-silicate is that the radiant ratio of 0.91,8 μ m ~ 25 mu m waveband is that the radiant ratio of 0.93,8 μ m ~ 14 mu m waveband is that the radiant ratio of 0.92,14 μ m ~ 25 mu m waveband is 0.94.
Embodiment 5
In mass ratio: 60%MnO
2, 4%CuO, 2%Mo
2o
3, 3%V
2o
5, 6%NiO, 11%Al
2o
3, 5%SiO
2, 3%TiO
2, 2%BaO, 2% glass powder, 2%B
2o
3prepare burden, wherein the raw material of glass powder consists of: 65%SiO
2, 15%Al
2o
3, 5%CaO, 3%BaO, 8%MgO, 2%TiO
2, 2%ZnO, by above-mentioned batching carry out ball milling, mixing, dry and compression moulding is block base substrate; Burning till in preparation process of above-mentioned base substrate, be first heated to 850 ℃ of insulations 5 hours, then continue to be warmed up to 1100 ℃ of insulations 8 hours; Through broken and pulverizing, cross 230 mesh sieves again, prepare the heterogeneous compound system ceramic powder of spinel-silicate that granularity is less than 61 μ m.
The normal direction all wave band radiant ratio of the heterogeneous compound system ceramic powder of spinel-silicate is that the radiant ratio of 0.91,8 μ m ~ 25 mu m waveband is that the radiant ratio of 0.92,8 μ m ~ 14 mu m waveband is that the radiant ratio of 0.95,14 μ m ~ 25 mu m waveband is 0.96.
Embodiment 6
In mass ratio: 11%Fe
2o
3, 30%MnO
2, 3%CuO, 2%Mo
2o
3, 2%V
2o
5, 1%WO
3, 33%Al
2o
3, 14%SiO
2, 3%CaO, 1% glass powder prepare burden, wherein the raw material of glass powder consists of: 65%SiO
2, 15%Al
2o
3, 5%CaO, 3%BaO, 8%MgO, 2%TiO
2, 2%ZnO, by above-mentioned batching carry out ball milling, mixing, dry and compression moulding is block base substrate; Burning till in preparation process of above-mentioned base substrate, be first heated to 900 ℃ of insulations 2 hours, then continue to be warmed up to 1150 ℃ of insulations 6 hours; Through broken and pulverizing, cross 400 mesh sieves again, prepare the heterogeneous compound system ceramic powder of spinel-silicate that granularity is less than 38 μ m.
The normal direction all wave band radiant ratio of the heterogeneous compound system ceramic powder of spinel-silicate is that the radiant ratio of 0.92,8 μ m ~ 25 mu m waveband is that the radiant ratio of 0.94,8 μ m ~ 14 mu m waveband is that the radiant ratio of 0.93,14 μ m ~ 25 mu m waveband is 0.95.
Embodiment 7
In mass ratio: 24%Fe
2o
3, 40%MnO
2, 7%Co
2o
3, 3%Mo
2o
3, 2%NiO, 14%Al
2o
3, 6%SiO
2, 1%MgO, 1%BaO, 1%CaO, 1%B
2o
3prepare burden, by above-mentioned batching carry out ball milling, mixing, dry and compression moulding is block base substrate; Burning till in preparation process of above-mentioned base substrate, be first heated to 850 ℃ of insulations 3 hours, then continue to be warmed up to 1130 ℃ of insulations 5 hours; Through broken and pulverizing, cross 200 mesh sieves again, prepare the heterogeneous compound system ceramic powder of spinel-silicate that granularity is less than 74 μ m.
The normal direction all wave band radiant ratio of the heterogeneous compound system ceramic powder of spinel-silicate is that the radiant ratio of 0.90,8 μ m ~ 25 mu m waveband is that the radiant ratio of 0.93,8 μ m ~ 14 mu m waveband is that the radiant ratio of 0.92,14 μ m ~ 25 mu m waveband is 0.92.
Embodiment 8
In mass ratio: 30%Fe
2o
3, 21%MnO
2, 10%CuO, 1%WO
3, 10%Al
2o
3, 23%SiO
2, 2%BaO, 3%MgO prepare burden, by above-mentioned batching carry out ball milling, mixing, dry and compression moulding is block base substrate; Burning till in preparation process of above-mentioned base substrate, be first heated to 950 ℃ of insulations 4 hours, then continue to be warmed up to 1250 ℃ of insulations 7 hours; Through broken and pulverizing, cross 325 mesh sieves again, prepare the heterogeneous compound system ceramic powder of spinel-silicate that granularity is less than 44 μ m.
The normal direction all wave band radiant ratio of the heterogeneous compound system ceramic powder of spinel-silicate is that the radiant ratio of 0.89,8 μ m ~ 25 mu m waveband is that the radiant ratio of 0.92,8 μ m ~ 14 mu m waveband is that the radiant ratio of 0.92,14 μ m ~ 25 mu m waveband is 0.93.
Through ir radiation test proof, the heterogeneous compound system ceramic powder of spinel-silicate prepared by the present invention has good infrared radiation property, its normal direction all wave band radiant ratio is 0.89 ~ 0.92, the radiant ratio of 8 μ m ~ 25 mu m wavebands is 0.90 ~ 0.94, the radiant ratio of 8 μ m ~ 14 mu m wavebands is that the radiant ratio of 0.89 ~ 0.95,14 μ m ~ 25 mu m wavebands is 0.92 ~ 0.96.
The raw materials used common raw material that is wide material sources of preparation method of the present invention, the Stability Analysis of Structures of the heterogeneous compound system material of spinel-silicate is good, infrared radiation property is good, this preparation method is simple, with short production cycle, low cost of manufacture, significant for applying of the heterogeneous compound system material of spinel-silicate.
The foregoing is only embodiments of the invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (4)
1. the preparation method of spinel-silicate multiphase composite system infrared radiation ceramic powder, is characterized in that including following steps:
1) preliminary treatment: first various raw materials are prepared burden to scale, more described batching is carried out to ball milling, mixing, the preliminary treatment that dry and compression moulding is block base substrate; Described raw material comprises the A component of tangible one-tenth spinel type sosoloid, B component and the accelerant C component of formation silicate minerals, and its mass ratio is 100%:20 ~ 300%:0 ~ 15%, and described A component includes Fe
2o
3, MnO
2, CuO, Mo
2o
3, V
2o
5and WO
3, described B component includes Al
2o
3, SiO
2, MgO, BaO and CaO, described accelerant C component includes glass powder and B
2o
3, each component concentration is by percentage to the quality:
20%Fe
2o
3, 12%MnO
2, 2.4%CuO, 2.4%Mo
2o
3, 2%V
2o
5, 1.2%WO
3, 20%Al
2o
3, 25.1%SiO
2, 10%MgO, 1.5%BaO, 1.4%CaO, 1% glass powder and 1%B
2o
3, described glass powder is formed by the raw material configuration of following quality percentage composition: SiO
2: 65%, Al
2o
3: 15%, CaO:5%, BaO:3%, MgO:8%, TiO
2: 2%, ZnO:2%;
2) burn till preparation: the block base substrate of step 1) gained is carried out to heating and thermal insulation in 800 ~ 980 ℃ of temperature ranges, and the heating and thermal insulation time is 1 ~ 6 hour, forms spinel type sosoloid; Then continue to be warmed up in 1100 ~ 1300 ℃ of temperature ranges and carry out heating and thermal insulation, the heating and thermal insulation time is 2 ~ 8 hours, forms silicate minerals, spinel type sosoloid and silicate minerals is carried out heterogeneous compound, forms the black sintered compact of heterogeneous composite structure;
3) by step 2) the black sintered compact of gained through broken, pulverize and cross 200 ~ 500 mesh sieves, prepare the multiphase composite system infrared radiation ceramic powder that granularity is less than spinel-silicate of 74 μ m.
2. the preparation method of spinel-silicate multiphase composite system infrared radiation ceramic powder, is characterized in that including following steps:
1) preliminary treatment: first various raw materials are prepared burden to scale, more described batching is carried out to ball milling, mixing, the preliminary treatment that dry and compression moulding is block base substrate; Described raw material comprises the A component of tangible one-tenth spinel type sosoloid, B component and the accelerant C component of formation silicate minerals, and its mass ratio is 100%:20 ~ 300%:0 ~ 15%, and described A component includes MnO
2, Co
2o
3, NiO and WO
3, described B component includes Al
2o
3, SiO
2, CaO and TiO
2, described accelerant C component includes glass powder, and each component concentration is by percentage to the quality:
11%MnO
2, 10%Co
2o
3, 3%NiO, 5%WO
3, 50%Al
2o
3, 9%SiO
2, 6%TiO
2, 3%CaO and 3% glass powder, described glass powder is formed by the raw material configuration of following quality percentage composition: SiO
2: 65%, Al
2o
3: 15%, CaO:5%, BaO:3%, MgO:8%, TiO
2: 2%, ZnO:2%;
2) burn till preparation: the block base substrate of step 1) gained is carried out to heating and thermal insulation in 800 ~ 980 ℃ of temperature ranges, and the heating and thermal insulation time is 1 ~ 6 hour, forms spinel type sosoloid; Then continue to be warmed up in 1100 ~ 1300 ℃ of temperature ranges and carry out heating and thermal insulation, the heating and thermal insulation time is 2 ~ 8 hours, forms silicate minerals, spinel type sosoloid and silicate minerals is carried out heterogeneous compound, forms the black sintered compact of heterogeneous composite structure;
3) by step 2) the black sintered compact of gained through broken, pulverize and cross 200 ~ 500 mesh sieves, prepare the multiphase composite system infrared radiation ceramic powder that granularity is less than spinel-silicate of 74 μ m.
3. the preparation method of spinel-silicate multiphase composite system infrared radiation ceramic powder, is characterized in that including following steps:
1) preliminary treatment: first various raw materials are prepared burden to scale, more described batching is carried out to ball milling, mixing, the preliminary treatment that dry and compression moulding is block base substrate; Described raw material comprises the A component of tangible one-tenth spinel type sosoloid, B component and the accelerant C component of formation silicate minerals, and its mass ratio is 100%:20 ~ 300%:0 ~ 15%, and described A component includes MnO
2, CuO, Mo
2o
3, NiO and V
2o
5, described B component includes Al
2o
3, SiO
2, BaO and TiO
2, described accelerant C component includes glass powder and B
2o
3, each component concentration is by percentage to the quality:
60%MnO
2, 4%CuO, 2%Mo
2o
3, 3%V
2o
5, 6%NiO, 11%Al
2o
3, 5%SiO
2, 3%TiO
2, 2%BaO, 2% glass powder and 2%B
2o
3, described glass powder is formed by the raw material configuration of following quality percentage composition: SiO
2: 65%, Al
2o
3: 15%, CaO:5%, BaO:3%, MgO:8%, TiO
2: 2%, ZnO:2%;
2) burn till preparation: the block base substrate of step 1) gained is carried out to heating and thermal insulation in 800 ~ 980 ℃ of temperature ranges, and the heating and thermal insulation time is 1 ~ 6 hour, forms spinel type sosoloid; Then continue to be warmed up in 1100 ~ 1300 ℃ of temperature ranges and carry out heating and thermal insulation, the heating and thermal insulation time is 2 ~ 8 hours, forms silicate minerals, spinel type sosoloid and silicate minerals is carried out heterogeneous compound, forms the black sintered compact of heterogeneous composite structure;
3) by step 2) the black sintered compact of gained through broken, pulverize and cross 200 ~ 500 mesh sieves, prepare the multiphase composite system infrared radiation ceramic powder that granularity is less than spinel-silicate of 74 μ m.
4. the preparation method of spinel-silicate multiphase composite system infrared radiation ceramic powder, is characterized in that including following steps:
1) preliminary treatment: first various raw materials are prepared burden to scale, more described batching is carried out to ball milling, mixing, the preliminary treatment that dry and compression moulding is block base substrate; Described raw material comprises the A component of tangible one-tenth spinel type sosoloid, B component and the accelerant C component of formation silicate minerals, and its mass ratio is 100%:20 ~ 300%:0 ~ 15%, and described A component includes Fe
2o
3, MnO
2, CuO, Mo
2o
3, V
2o
5and WO
3, described B component includes Al
2o
3, SiO
2and CaO, described accelerant C component includes glass powder, and each component concentration is by percentage to the quality:
11%Fe
2o
3, 30%MnO
2, 3%CuO, 2%Mo
2o
3, 2%V
2o
5, 1%WO
3, 33%Al
2o
3, 14%SiO
2, 3%CaO and 1% glass powder, described glass powder is formed by the raw material configuration of following quality percentage composition: SiO
2: 65%, Al
2o
3: 15%, CaO:5%, BaO:3%, MgO:8%, TiO
2: 2%, ZnO:2%;
2) burn till preparation: the block base substrate of step 1) gained is carried out to heating and thermal insulation in 800 ~ 980 ℃ of temperature ranges, and the heating and thermal insulation time is 1 ~ 6 hour, forms spinel type sosoloid; Then continue to be warmed up in 1100 ~ 1300 ℃ of temperature ranges and carry out heating and thermal insulation, the heating and thermal insulation time is 2 ~ 8 hours, forms silicate minerals, spinel type sosoloid and silicate minerals is carried out heterogeneous compound, forms the black sintered compact of heterogeneous composite structure;
3) by step 2) the black sintered compact of gained through broken, pulverize and cross 200 ~ 500 mesh sieves, prepare the multiphase composite system infrared radiation ceramic powder that granularity is less than spinel-silicate of 74 μ m.
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