CN104387030B - The preparation method of crystal growth furnace temperature field alumina bubble brick - Google Patents
The preparation method of crystal growth furnace temperature field alumina bubble brick Download PDFInfo
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Abstract
The preparation method that the present invention relates to crystal growth furnace temperature field alumina bubble brick, belongs to technical field of crystal growth.Alumina hollow ball, Alpha-alumina micropowder and yellow starch gum fine powder are sufficiently mixed by it, through overmolding, dry and are fired into product alumina bubble brick.The present invention adopts the alumina hollow ball of different content particle diameter and the Alpha-alumina micropowder of different content particle diameter to be sufficiently mixed, and can form uniform insulation construction, and its thermal conductivity is low, reheating linear shrinkage ratio is low, good thermal shock.Raw materials of the present invention is only aluminium oxide, and yellow starch gum is in high-temperature firing process, substantially can vapor away, other impurity will not be introduced, compare the features such as tradition tungsten, zirconium oxide temperature field have that impurity is few, density is low, thermal conductivity is low, clean environmental protection, deformation rate are low.
Description
Technical field
The preparation method that the present invention relates to crystal growth furnace temperature field alumina bubble brick, belongs to technical field of crystal growth.
Background technology
The technique of kyropoulos growing sapphire, is usually first by fusing after raw alumina heating to fusing point, then makes crystal seed with alumina single crystal rod, touch molten surface, control temperature lower than freezing point simultaneously, make crystal constantly become big；Rotating crystal simultaneously, to improve Temperature Distribution, after liquation is stable with the freezing rate of grain boundary, crystal seed just no longer draws high, also do not rotate, only making crystal down solidify gradually from above controlling cooldown rate mode, final set becomes a whole monocrystalline crystalline substance heavy stone used as an anchor, and this is most widely used at present sapphire crystal growth method.For obtaining higher-quality sapphire crystal, company's independent development top seed temperature gradient technique (TSTGT method), it is that kyropoulos, czochralski method (CZ), heat-exchanging method (HEM), temperature ladder method (TGT) and Bridgman-Stockbarger method are combined, create the special high-temperature vacuum crystal oven at a temperature-adjustable gradient and Wen Chang center, and produce the innovative technology of large scale, high-quality high-temp oxide crystal.In both the above crystal growing technology, insulation material plays a part the temperature difference controlling temperature gradient distribution, isolating between heater and body of heater, and Sapphire Crystal Growth plays critical effect.
In the process of kyropoulos and TSTGT method growing sapphire, the tubular structure that its insulation material is made up of materials such as tungsten, molybdenum, graphite of many layers, it is bushed in together, utilize many lamellar spacings between layers, heater is reduced, thus playing insulation, heat insulation effect to the heat-conducting effect of tweer.The growing environment of sapphire single-crystal can directly affect the quality of sapphire single-crystal, and at high operating temperatures, alumina melt can occur trace to thermally decompose, and discharges O2, the O of these trace2Will react with tungsten and molybdenum crucible, heat-insulation layer isothermal field, thus forming bubble scatterplot so that the yield rate of gem reduces.
2Mo+3O2=2MoO3↑
2W+3O2=2WO3↑
Additionally the density of tungsten and molybdenum material is higher, and the density of tungsten is 19.35g/cm, and molybdenum also has 10.2g/cm, in assembling, cleans in the assembling process of its goods insulation material, often due to its bigger weight and not easily operate.And at high operating temperatures, graphite material goods also can slightly discharge the C of trace, also can with Al2O3There is certain reaction.
2Al2O3+ 3C=Al4O4C+2CO↑
2Al2O3+ C=2Al2O4C+CO↑
Al2O3+ 2C=Al2O+2CO↑
This reaction can promote the formation of bubble in sapphire crystallization process.Carbon monoxide is as a kind of toxic gas, to environment, it addition, evaporate but be not engaged in the C of reaction itself and will also as impurity scatterplot, affects sapphire quality.
Zirconium oxide, due to its heat-resisting quantity, corrosion resistance, non-oxidizability and low heat conductivity, also tends to use as insulation material.Zirconium oxide has three kinds of crystal structure forms, can produce the change of structure when variations in temperature.
In transition process, zirconium oxide can produce corresponding change in volume, and when raising temperature, monoclinic phase can to tetragonal phase converting, volume contraction 5%, and when reducing temperature, Tetragonal can be changed into monoclinic phase, and volume can expand 8%.As a result of which so that zirconium oxide is the efflorescence because of the change of phase variable volume in repeatedly cooling procedure, so, zirconia material does not accommodate the insulation material as kyropoulos and TSTGT method growing sapphire yet.
Summary of the invention
It is an object of the invention to overcome above-mentioned weak point, the preparation method that a kind of alumina bubble brick being exclusively used in crystal growth furnace temperature field is provided, the alumina bubble brick prepared by the method, compared with common heat-barrier material, has that impurity is few, density is low, thermal conductivity is low, a feature such as clean environmental protection, deformation rate are low.
According to technical scheme provided by the invention, the preparation method of crystal growth furnace temperature field alumina bubble brick, step is by weight:
(1) batch mixing: take the alumina hollow ball of 60-70 part, 25-35 part Alpha-alumina micropowder, 5-15 part yellow starch gum fine powder, with batch mixer first by alumina hollow ball mix homogeneously, it is subsequently adding Alpha-alumina micropowder and yellow starch gum fine powder, spray process is adopted to add water after being dry mixed 4-5min, the ratio of water and material is 1:3-5, wet mixing 8-10min；
(2) molding: according to self body of heater size, shape, temperature field requirement, design dividing plate mould, above-mentioned compound is weighed corresponding weight, add in dividing plate mould, adopt vibrations pressurization molding, briquetting pressure 10-15MPa, 4-10 time/s of frequency of vibration, then the demoulding, obtains alumina bubble brick first product；
(3) dry: the alumina bubble brick first product after the demoulding to be dried at 100-150 DEG C 35-50h, removes moisture therein；
(4) burning till: by dry alumina bubble brick first product loading of kiln, loading of kiln is highly 0.3-0.6m；First being warming up to 300-450 DEG C with 4-6h, then constant temperature fires 1-2h, is then warming up to 1000-1100 DEG C with 3-4h, finally being warming up to 1750 DEG C with 6-9h, constant temperature stops heating after firing 5-8h, utilizes the remaining temperature of kiln to keep high temperature, and Temperature fall, obtain alumina bubble brick.
Temperature rise period at initial stage makes yellow starch gum fully to vapor away slowly, and the interstage prevents aluminium oxide deformation so quickly excessive, and the phase III forms by a firing and needs slow intensification.
The Al of described alumina hollow ball2O3Content is more than 99%, and grain size specification is Φ 2-3mm, 1-2mm, 0.5-1mm respectively, and three's ratio by weight is followed successively by 50-60 part, 25-35 part, 10-20 part.These three kinds of specifications can ensure the abundant combination of hollow ball and powder, forms uniform insulation construction.
Al in described Alpha-alumina micropowder2O3Content, more than 99.99%, is divided into 325 orders and less than two kinds of specifications of 150 order, both by weight ratio be followed successively by 60-70 part, 30-40 part.The micropowder of 325 orders, for the filling in gap between hollow ball, can reduce the reheating linear shrinkage ratio of goods less than the micropowder of 150 orders, increases thermal shock resistance.
The particle diameter of described yellow starch gum fine powder is less than 325 orders.Yellow starch gum is easy in the moulding before sintering of hollow ball brick, and to preventing from subsiding, conformal guarantor is stupefied good effect, and in high-temperature firing process, yellow starch gum substantially can vapor away, thus the purity of the aluminium oxide of goods can be improved.
Beneficial effects of the present invention: the present invention adopts the alumina hollow ball of different content particle diameter and the Alpha-alumina micropowder of different content particle diameter to be sufficiently mixed, and can form uniform insulation construction, and its thermal conductivity is low, reheating linear shrinkage ratio is low, good thermal shock.Raw materials of the present invention is only aluminium oxide, and yellow starch gum is in high-temperature firing process, substantially can vapor away, other impurity will not be introduced, compare the features such as tradition tungsten, zirconium oxide temperature field have that impurity is few, density is low, thermal conductivity is low, clean environmental protection, deformation rate are low.
Detailed description of the invention
Embodiment 1
The preparation method of crystal growth furnace temperature field alumina bubble brick, step is by weight:
(1) batch mixing: take the alumina hollow ball of 60 parts, 25 parts of Alpha-alumina micropowders, 5 parts of yellow starch gum fine powders, with batch mixer first by alumina hollow ball mix homogeneously, it is subsequently adding Alpha-alumina micropowder and yellow starch gum fine powder, spray process is adopted to add water after being dry mixed 4min, the ratio of water and material is 1:3, wet mixing 8min；
(2) molding: added by step (1) gained mixture in dividing plate mould, adopts vibrations pressurization molding, the then demoulding, briquetting pressure 10MPa, 10 times/s of frequency of vibration, obtains alumina bubble brick first product；
(3) dry: the alumina bubble brick first product after the demoulding to be dried at 100 DEG C 50h, removes moisture therein；
(4) burning till: by dry alumina bubble brick first product loading of kiln, loading of kiln is highly 0.3-0.6m；First being warming up to 300 DEG C with 4h, then constant temperature fires 1h, is then warming up to 1000 DEG C with 3h, is finally warming up to 1750 DEG C with 6-9h, and constant temperature stops heating after firing 5h, utilizes the remaining temperature of kiln to keep high temperature Temperature fall, obtains alumina bubble brick.
The Al of described alumina hollow ball2O3Content is more than 99%, and grain size specification is Φ 2-3mm, 1-2mm, 0.5-1mm respectively, and three's ratio by weight is followed successively by 50 parts, 35 parts, 15 parts.
Al in described Alpha-alumina micropowder2O3Content, more than 99.99%, is divided into 325 orders and less than two kinds of specifications of 150 order, both by weight ratio be followed successively by 60 parts, 40 parts.
The particle diameter of described yellow starch gum fine powder is less than 325 orders.
Embodiment 2
The preparation method of crystal growth furnace temperature field alumina bubble brick, step is by weight:
(1) batch mixing: take the alumina hollow ball of 70 parts, 35 parts of Alpha-alumina micropowders, 15 parts of yellow starch gum fine powders, with batch mixer first by alumina hollow ball mix homogeneously, it is subsequently adding Alpha-alumina micropowder and yellow starch gum fine powder, spray process is adopted to add water after being dry mixed 5min, the ratio of water and material is 1:5, wet mixing 10min；
(2) molding: added by step (1) gained mixture in dividing plate mould, adopts vibrations pressurization molding, briquetting pressure 15MPa, 4 times/s of frequency of vibration, the then demoulding, obtains alumina bubble brick first product；
(3) dry: the alumina bubble brick first product after the demoulding to be dried at 150 DEG C 50h, removes moisture therein；
(4) burning till: by dry alumina bubble brick first product loading of kiln, loading of kiln is highly 0.6m；First being warming up to 450 DEG C with 6h, then constant temperature fires 2h, is then warming up to 1100 DEG C with 4h, is finally warming up to 1750 DEG C with 9h, and constant temperature stops heating after firing 8h, utilizes the remaining temperature of kiln to keep high temperature Temperature fall, obtains alumina bubble brick.
The Al of described alumina hollow ball2O3Content is more than 99%, and grain size specification is Φ 2-3mm, 1-2mm, 0.5-1mm respectively, and three's ratio by weight is followed successively by 60 parts, 25 parts, 15 parts.
Al in described Alpha-alumina micropowder2O3Content, more than 99.99%, is divided into 325 orders and less than two kinds of specifications of 150 order, both by weight ratio be followed successively by 70 parts, 30 parts.
The particle diameter of described yellow starch gum fine powder is less than 325 orders.
Embodiment 3
The preparation method of crystal growth furnace temperature field alumina bubble brick, step is by weight:
(1) batch mixing: take the alumina hollow ball of 65 parts, 30 parts of Alpha-alumina micropowders, 10 parts of yellow starch gum fine powders, with batch mixer first by alumina hollow ball mix homogeneously, it is subsequently adding Alpha-alumina micropowder and yellow starch gum fine powder, spray process is adopted to add water after being dry mixed 4min, the ratio of water and material is 1:4, wet mixing 9min；
(2) molding: added by step (1) gained mixture in dividing plate mould, adopts vibrations pressurization molding, briquetting pressure 12MPa, 6 times/s of frequency of vibration, the then demoulding, obtains alumina bubble brick first product；
(3) dry: the alumina bubble brick first product after the demoulding to be dried at 125 DEG C 40h, removes moisture therein；
(4) burning till: by dry alumina bubble brick first product loading of kiln, loading of kiln is highly 0.5m；First being warming up to 400 DEG C with 5h, then constant temperature fires 1h, is then warming up to 1050 DEG C with 4h, is finally warming up to 1750 DEG C with 8h, and constant temperature stops heating after firing 6h, utilizes the remaining temperature of kiln to keep high temperature Temperature fall, obtains alumina bubble brick.
The Al of described alumina hollow ball2O3Content is more than 99%, and grain size specification is Φ 2-3mm, 1-2mm, 0.5-1mm respectively, and three's ratio by weight is followed successively by 55 parts, 30 parts, 20 parts.
Al in described Alpha-alumina micropowder2O3Content, more than 99.99%, is divided into 325 orders and less than two kinds of specifications of 150 order, both by weight ratio be followed successively by 65 parts, 35 parts.
The particle diameter of described yellow starch gum fine powder is less than 325 orders.
Claims (1)
1. the preparation method of crystal growth furnace temperature field alumina bubble brick, is characterized in that: step is by weight:
(1) batch mixing: take the alumina hollow ball of 60-70 part, 25-35 part Alpha-alumina micropowder, 5-15 part yellow starch gum fine powder, with batch mixer first by alumina hollow ball mix homogeneously, it is subsequently adding Alpha-alumina micropowder and yellow starch gum fine powder, spray process is adopted to add water after being dry mixed 4-5min, the ratio of water and material is 1:3-5, wet mixing 8-10min；
(2) molding: added by step (1) gained mixture in dividing plate mould, adopts vibrations pressurization room temperature extrusion forming, briquetting pressure 10-15MPa, 4-10 time/s of frequency of vibration, obtains alumina bubble brick first product after the demoulding；
(3) dry: the alumina bubble brick first product after the demoulding to be dried at 100-150 DEG C 35-50h, removes moisture therein；
(4) burning till: by dry alumina bubble brick first product loading of kiln, loading of kiln is highly 0.3-0.6m；First being warming up to 300-450 DEG C with 4-6h, then constant temperature fires 1-2h, is then warming up to 1000-1100 DEG C with 3-4h, finally being warming up to 1750 DEG C with 6-9h, constant temperature stops heating after firing 5-8h, utilizes the remaining temperature of kiln to keep high temperature, and Temperature fall, obtain alumina bubble brick；
The Al of described alumina hollow ball2O3Content is more than 99%, and grain size specification is Φ 2-3mm, 1-2mm, 0.5-1mm respectively, and three's ratio by weight is followed successively by 50-60 part, 25-35 part, 10-20 part；
Al in described Alpha-alumina micropowder2O3Content, more than 99.99%, is divided into 325 orders and less than two kinds of specifications of 150 order, both by weight ratio be followed successively by 60-70 part, 30-40 part；
The particle diameter of described yellow starch gum fine powder is less than 325 orders.
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