CN104528787B - A kind of method preparing fine grain size alumina powder - Google Patents
A kind of method preparing fine grain size alumina powder Download PDFInfo
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- CN104528787B CN104528787B CN201410799593.2A CN201410799593A CN104528787B CN 104528787 B CN104528787 B CN 104528787B CN 201410799593 A CN201410799593 A CN 201410799593A CN 104528787 B CN104528787 B CN 104528787B
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Abstract
The invention provides a kind of method preparing fine grain size alumina powder, belong to powder preparation and size controlling technical field.Technical process is: with industrial aluminium hydroxide or transition aluminas powder for raw material, add crystal seed, dispersion agent, size controlling constituent element and gaseous sources, be pressed into base substrate after raw material powder mixes in raw material powder.Base substrate carries out high-temperature calcination in the atmosphere containing hydrogen halide and size controlling constituent element, and calcining base substrate is broken into powder, carries out low temperature calcination again, obtain particle diameter and be less than 0.14 μm, α-Al after post forming in containing the atmosphere of higher concentration hydrogen halide
2o
3content be 100% submicron order or nano-alumina powder end.This invention temperature of reaction is lower, and the reaction times is shorter, and technique is simple, gained alumina powder favorable dispersity.
Description
Technical field
The invention belongs to powder preparation and size controlling technical field, specifically provide a kind of method preparing fine grain size alumina powder.
Background technology
Fine grain size alumina powder (submicron and nano-alumina powder end) is except the feature such as have that fusing point is high, hardness is large, intensity is high and corrosion-resistant, also there is significant surface effects, small-size effect, quantum effect, macro quanta tunnel effect and high sintering activity, show the electricity of a series of excellence, magnetic, light, mechanics and chemical macroscopic property, have broad application prospects in fields such as abrasive material, cutter, matrix material, microelectronics, chemical industry, aerospace industry, fine ceramics.The preparation of fine grain size alumina powder mainly contains the methods such as solid-phase synthesis, chemical heat solution, Amorphous Crystallization method, sol-gel method, liquid-phase precipitation method.Solid phase method is by aluminium or aluminium salt grinding calcination, after there is solid state reaction, directly obtains fine grain size alumina powder.Vapor phase process, is decomposed and chemical reactive synthesis fine particle aluminum oxide by gas-phase heating for raw material with metal simple-substance, halogenide, hydride or organometallic compound.Liquid-phase precipitation method is under solution state, makes effective constituent in raw material generate precipitation by chemical reaction, more after filtration, washing, dry, thermolysis prepare fine grain size aluminum oxide.There is the problems such as particle diameter and the more difficult control of pattern, complex process, cost be higher in the preparation of fine grain size.
Chinese patent CN1095360A discloses a kind of alpha-alumina powder and production method thereof, calcines under the condition containing crystal seed and/or style control agent with the protective atmosphere of chloride containing hydrogen or halogen, obtains the alumina powder of fine grain size and special construction.The particle diameter of gained fine grain size alumina powder is 0.6 ~ 3.7 μm, the more difficult powder preparing particle diameter more tiny (<0.6 μm).Chinese patent CN1386705A discloses a kind of alpha-alumina fine powder and preparation method thereof, by α-Al
2o
3the mixture of precursor, seed crystal and grain growth inhibitor in 600 ~ 1000 DEG C of dinectly brunings, obtains fine grain size alumina powder, wherein α-Al in the atmosphere containing HCl
2o
3content be greater than 90%.The method calcining temperature is lower, α-Al
2o
3content not high.Chinese patent CN102009993A discloses the method that a kind of two-section roasting (low temperature calcination+high-temperature calcination) prepares submicron order aluminum oxide, first obtain activated alumina 400 ~ 900 DEG C of low temperature calcinations, then 1100 ~ 1400 DEG C of high-temperature calcinations, obtain submicron alumina powder, the particle diameter of alumina powder is 0.4 ~ 0.8 μm.During low temperature (<900 DEG C) calcining, aluminum oxide still exists with the form of transition aluminas, and the phase transformation between transition aluminas belongs to displacement-type phase transformation, does not destroy chemical bond, and intracrystalline defect is few, and activation effect is not remarkable.During high-temperature calcination, aluminum oxide is easily grown up, the nano level alumina powder of more difficult acquisition.The present invention fully utilizes and adds crystal seed and/or style control agent, adopts the sintering atmosphere containing hydrogen halide and/or fluorochemical (aluminum fluoride) of particular design, and carries out twice base and twice calcining (high-temperature calcination+low temperature calcination) to powder.During high-temperature calcination, the phase transformation of particle generation reconstruction formula, granule partial shrinks, and surface forms the defects such as a large amount of fine cracks, and activation effect is remarkable, for fragmentation during low temperature calcination lays the foundation.During low temperature calcination, particle is broken further in the atmosphere containing hydrogen halide.High-temperature calcination+low temperature calcination mode is under above-mentioned mechanism and some other principle still unclear machining function, and crushing effect is better, thus prepares submicron order or nano-alumina powder end that particle diameter is less than 0.14 μm.
Summary of the invention
The object of the present invention is to provide a kind of method preparing fine grain size alumina powder, specifically comprise the steps:
1, raw material mixing: with industrial aluminium hydroxide or transition aluminas powder for raw material, 0.5 ~ 4.5wt.% crystal seed, 0.1 ~ 1.5wt.% dispersion agent, 0.01 ~ 1.2wt.% grain growth inhibitor, 0 ~ 0.5wt.% gaseous sources is added in raw material powder, dry 3 ~ 5 hours at 50 ~ 80 DEG C after adopting the mode of stirring or ball milling to mix, obtain compound;
Described transition aluminas is γ-Al
2o
3, δ-Al
2o
3, ζ-Al
2o
3, η-Al
2o
3, θ-Al
2o
3, κ-Al
2o
3with χ-Al
2o
3in one or more.
Described crystal seed is that median size is less than the aluminium of 30nm, titanium, zirconium, the oxide compound of vanadium, nitride, carbide or carbonitride.
Described grain growth inhibitor is used for the preparation of fine grain size alumina powder, comprises compound and the mixture of the metals such as magnesium, yttrium, zirconium, niobium, as YCl
3, Nb
2o
3, ZrO
2, Mg (OH) Cl, MgO and MgCl
2in one or more.
Described dispersion agent be molecular weight in 120 ~ 600 scopes, the acids containing methyl and phenyl ring or lipid, such as phenylacetate, phenylformic acid, methyl benzoate, n-butylbenzoate etc.
2, a base: add 2.5 ~ 5wt.% dextrin or polyvinyl alcohol in compound after the drying, at the Forming under Pressure of 560 ~ 800MPa, obtain a base substrate;
3, once calcine: one time base substrate carries out high-temperature calcination in the atmosphere containing hydrogen halide and size controlling constituent element, and calcining temperature is 1160 ~ 1300 DEG C, and calcination time is 2 ~ 3 hours, is once calcined base substrate; Described size controlling constituent element is aluminum halide;
The described atmosphere containing hydrogen halide and size controlling constituent element is the mixing gas phase of hydrogen halide, ammonia, aluminum halide, hydrogen, nitrogen and air, and in gas phase, the concentration of hydrogen halide is 0.1 ~ 1.0%, the concentration of ammonia is 1.1 ~ 1.5%, the concentration of aluminum halide is 1 ~ 2%, the concentration of hydrogen is 3 ~ 5%, the concentration of nitrogen is 6-10%, surplus is air.
When once calcining, also halogenation ammonia and halogen compounds can be added in compound in advance, at high temperature decompose and obtain hydrogen halide, ammonia, nitrogen, chlorine or aluminum halide.Halogen compounds is ammoniumper chlorate, hypochlorous acid ammonium, hexafluoro aluminate etc.
For suitability for industrialized production, calcining (comprising a base substrate calcining and the calcining of secondary base substrate) available tunnel furnace, rotary kiln or pusher type furnace carry out in a continuous manner.
4, secondary base: will once calcine base substrate and be broken into powder, and 2.5 ~ 5wt.% dextrin or polyvinyl alcohol is added in broken powder, at the Forming under Pressure of 560 ~ 800MPa, obtain secondary base substrate;
5, secondary clacining: secondary base substrate is carried out low temperature calcination, calcining temperature is 510 ~ 900 DEG C, and calcination time is 2 ~ 5 hours.Obtain secondary clacining base substrate after secondary clacining, obtain particle diameter after the fragmentation of secondary clacining base substrate and be less than 0.14 μm, α-Al
2o
3content be the alumina powder of 100%, the pattern of fine grain size aluminum oxide is as shown in Figure 2.
Adopt during secondary clacining containing the atmosphere of higher concentration hydrogen halide, wherein the concentration of hydrogen halide is 1.6 ~ 2.0%, the concentration of ammonia is 2.3 ~ 3%, the concentration of hydrogen is 8 ~ 10%, the concentration of nitrogen is 11 ~ 13%, surplus is air.
During secondary clacining, also halogenation ammonia, ammoniumper chlorate or hypochlorous acid ammonium can be added in compound in advance, at high temperature decompose and obtain hydrogen halide, ammonia, nitrogen or chlorine.
Aluminium hydroxide or transition alumina powder are carried out high temperature+low temperature two benches calcining by the present invention in the atmosphere containing halogen and halogen compounds gas.In high-temperature burning process, halide molecule destroys the regularly arranged of former alpha-alumina crystals interior atoms, forms Al
3+ionic vacancies, accelerates Al
3+the velocity of diffusion of ion and Al
2o
3crystal transition.In phase transition process, morphology control agent participates in phase transformation reaction, and the gas phase compounds intermediate product of generation promotes atomic migration, is conducive to crystal transition and crystal growth.In low temperature calcination process, the alumina powder with greater activity and more defect in the atmosphere of the halide gas phase containing higher concentration after calcining by further refinement, obtain dispersed fine grain size alumina powder preferably.Preforming controls the tightness degree of Powder Particles Packing by changing pressing pressure, play vital effect to augmenting response substrate concentration and raising chemical reaction rate.In atmosphere, introduce the action time that halogenide extends halogenide and raw material powder, improve the degree of uniformity of reaction.The introducing of halogen reduces calcining temperature, accelerating oxidation aluminium transformation of crystal, can realize the refinement of alumina powder at a lower temperature.The advantage of this invention is: the crystal formation of alumina powder, granularity and morphology controllable, and powder uniformity coefficient is high, and reaction process is easy to control, and side reaction is few, and technique is simple, easily realizes suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention
Fig. 2 is the pattern of fine grain size aluminum oxide
Embodiment
Embodiment 1: be that fine grain size alumina powder prepared by raw material with aluminium hydroxide
With industrial aluminium hydroxide powder for raw material, 0.5wt.% crystal seed (α-TiNC of 20nm), 0.1wt.% dispersion agent (phenylformic acid), 0.015wt.% grain growth inhibitor (Mg (OH) Cl) is added in raw material powder, dry 8 hours at 50 DEG C after adopting the mode of stirring or ball milling to mix, obtain compound.Add 1wt.% dextrin or polyvinyl alcohol in compound after the drying, at the Forming under Pressure of 600MPa, obtain a base substrate; One time base substrate carries out high-temperature calcination, and calcining temperature is 1160 DEG C, and calcination time is 8 hours.In a calcination atmosphere, hydrofluoric concentration is 0.1%, the concentration of ammonia is 1.1%, the concentration of aluminum fluoride is 1%, the concentration of hydrogen is 4%, the concentration of nitrogen is 6%, surplus is air.Once once calcined base substrate after calcining; To once calcine base substrate and be broken into powder, and add 0.5wt.% dextrin or polyvinyl alcohol in broken powder, at the Forming under Pressure of 560MPa, obtain secondary base substrate; Secondary base substrate is carried out low temperature calcination, and calcining temperature is 510 DEG C, and calcination time is 2 hours.In secondary clacining atmosphere, hydrofluoric concentration is 1.6%, the concentration of ammonia is 2.3%, the concentration of hydrogen is 9%, the concentration of nitrogen is 11%, surplus is air.Obtain secondary clacining base substrate after secondary clacining, after the fragmentation of secondary clacining base substrate, obtain fine grain size alumina powder.The median size of gained alumina powder is 0.09 μm, α-Al
2o
3content be 100%.
Embodiment 2: with γ-Al
2o
3for fine grain size alumina powder prepared by raw material
With γ-Al
2o
3for raw material, in raw material powder, add the 1wt.% crystal seed (V of 15nm
2o
5), 0.6wt.% dispersion agent (phenylacetate), 1.2wt.% grain growth inhibitor (MgO) and 0.4wt.% gaseous sources (hypochlorous acid ammonium), dry 3 hours at 80 DEG C after adopting the mode of stirring or ball milling to mix, obtain compound.Add 2.6wt.% dextrin or polyvinyl alcohol in compound after the drying, at the Forming under Pressure of 700MPa, obtain a base substrate; One time base substrate carries out high-temperature calcination, and calcining temperature is 1300 DEG C, and calcination time is 3 hours.In a calcination atmosphere, the concentration of hydrogenchloride is 1.0%, the concentration of ammonia is 1.5%, the concentration of aluminum fluoride is 2%, the concentration of hydrogen is 5%, the concentration of nitrogen is 10%, surplus is air.Once once calcined base substrate after calcining; To once calcine base substrate and be broken into powder, and add 2wt.% dextrin or polyvinyl alcohol in broken powder, at the Forming under Pressure of 700MPa, obtain secondary base substrate; Secondary base substrate is carried out low temperature calcination, and calcining temperature is 700 DEG C, and calcination time is 3 hours.In secondary clacining atmosphere, the concentration of hydrogenchloride is 2%, the concentration of ammonia is 2.5%, the concentration of hydrogen is 8%, the concentration of nitrogen is 12%, surplus is air.Obtain secondary clacining base substrate after secondary clacining, after the fragmentation of secondary clacining base substrate, obtain fine grain size alumina powder.The median size of gained alumina powder is 0.13 μm, α-Al
2o
3content be 100%.
Embodiment 3: with aluminium hydroxide and NH
4f is that fine grain size alumina powder prepared by raw material
With θ-Al
2o
3powder is raw material, adds the 0.8wt.% crystal seed (α-TiO of 15nm in raw material powder
2), 1.0wt.% dispersion agent (methyl benzoate), 0.06wt.% grain growth inhibitor (MgCl
2), 0.5wt.% gaseous sources (NH
4cl), dry 4 hours at 60 DEG C after adopting the mode of stirring or ball milling to mix, obtain compound.Add 3wt.% dextrin or polyvinyl alcohol in compound after the drying, at the Forming under Pressure of 580MPa, obtain a base substrate; One time base substrate carries out high-temperature calcination, and calcining temperature is 1200 DEG C, and calcination time is 6 hours.In a calcination atmosphere, the concentration of hydrogen bromide is 0.5%, the concentration of ammonia is 1.2%, the concentration of aluminum fluoride is 2%, the concentration of hydrogen is 3%, the concentration of nitrogen is 8%, surplus is air.Once once calcined base substrate after calcining; To once calcine base substrate and be broken into powder, and add 3wt.% dextrin or polyvinyl alcohol in broken powder, at the Forming under Pressure of 600MPa, obtain secondary base substrate; Secondary base substrate is carried out low temperature calcination, and calcining temperature is 900 DEG C, and calcination time is 12 hours.In secondary clacining atmosphere, the concentration of hydrogen bromide is 1.8%, the concentration of ammonia is 3%, the concentration of hydrogen is 10%, the concentration of nitrogen is 13%, surplus is air.Obtain secondary clacining base substrate after secondary clacining, after the fragmentation of secondary clacining base substrate, obtain fine grain size alumina powder.The median size of gained alumina powder is 0.14 μm, α-Al
2o
3content be 100%.
Embodiment 4: with aluminium hydroxide and NH
4cl is raw material, and 700MPa is shaped and prepares fine grain size alumina powder
With industrial aluminium hydroxide powder for raw material, in raw material powder, add the 4.5wt.% crystal seed (α-Al of 30nm
2o
3), 1.5wt.% dispersion agent (phenylformic acid), 0.08wt.% grain growth inhibitor (Nb
2o
3), 0.15wt.% gaseous sources (ammoniumper chlorate), dries 5 hours at 70 DEG C after adopting the mode of stirring or ball milling to mix, obtains compound.Add 2.9wt.% dextrin or polyvinyl alcohol in compound after the drying, at the Forming under Pressure of 800MPa, obtain a base substrate; One time base substrate carries out high-temperature calcination, and calcining temperature is 1200 DEG C, and calcination time is 2 hours.In a calcination atmosphere, the concentration of hydrogenchloride is 0.8%, the concentration of ammonia is 1.3%, the concentration of aluminum fluoride is 1.5%, the concentration of hydrogen is 4.5%, the concentration of nitrogen is 9.0%, surplus is air.Once once calcined base substrate after calcining; To once calcine base substrate and be broken into powder, and add 1wt.% dextrin or polyvinyl alcohol in broken powder, at the Forming under Pressure of 800MPa, obtain secondary base substrate; Secondary base substrate is carried out low temperature calcination, and calcining temperature is 600 DEG C, and calcination time is 10 hours.In secondary clacining atmosphere, the concentration of hydrogenchloride is 1.7%, the concentration of ammonia is 2.3%, the concentration of hydrogen is 9%, the concentration of nitrogen is 12%, surplus is air.Obtain secondary clacining base substrate after secondary clacining, after the fragmentation of secondary clacining base substrate, obtain fine grain size alumina powder.The median size of gained alumina powder is 0.03 μm, α-Al
2o
3content be 100%.
Embodiment 5: with aluminium hydroxide and NH
4cl is raw material, and 500MPa is shaped and prepares fine grain size alumina powder
Except the pressing pressure in a base process is 650MPa, the pressing pressure in secondary base process is outside 650MPa, prepares fine grain size alumina powder according to the method identical with embodiment 4, and the median size of gained alumina powder is 0.08 μm, α-Al
2o
3content be 100%.
Embodiment 6: with aluminium hydroxide and NH
4cl is raw material, and 300MPa is shaped and prepares fine grain size alumina powder
Except the pressing pressure in a base process is 560MPa, the pressing pressure in secondary base process is outside 560MPa, prepares fine grain size alumina powder according to the method identical with embodiment 4, and the median size of gained alumina powder is 0.10 μm, α-Al
2o
3content be 100%.
Comparative example 1: adopt and prepare fine grain size alumina powder without the technique of press forming
Except a nothing base and secondary preforming, prepare fine grain size alumina powder according to the method identical with embodiment 4, the median size of gained alumina powder is 0.82 μm, α-Al
2o
3content be 100%.
Comparative example 2: adopt low temperature calcination+high-temperature calcination technique to prepare fine grain size alumina powder
Except changing the temperature of once calcining into 480 DEG C, the temperature of secondary clacining changes into outside 1180 DEG C, prepares fine grain size alumina powder according to the method identical with embodiment 4, and the median size of gained alumina powder is 37 μm, α-Al
2o
3content be 99%.
Comparative example 3: adopt air calcination technique to prepare fine grain size alumina powder
Except once calcining and all carrying out in air atmosphere with secondary clacining, prepare fine grain size alumina powder according to the method identical with embodiment 4, the median size of gained alumina powder will be 2.5 μm, α-Al
2o
3content be 98%.
Following table is the data synopsis of embodiment 1-6 and comparative example 1-3:
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. prepare a method for fine grain size alumina powder, it is characterized in that:
Step one, with industrial aluminium hydroxide or transition aluminas powder for raw material, in raw material powder, add a certain amount of batching, adopt stir or the mode of ball milling mix after dry 3 ~ 5 hours at 50 ~ 80 DEG C, obtain compound,
Step 2, compound after the drying obtain a base substrate after press forming;
Step 3, a base substrate are carrying out high-temperature calcination, and calcining temperature is 1000 ~ 1150 DEG C, and calcination time is 3.5 ~ 8 hours, is once calcined base substrate after high-temperature calcination;
Step 4, will once calcine base substrate and be broken into powder, after press forming, obtain secondary base substrate;
Step 5, secondary base substrate is carried out low temperature calcination, calcining temperature is 510 ~ 900 DEG C, calcination time is 2 ~ 5 hours, secondary clacining base substrate is obtained after low temperature calcination, fine grain size alumina powder is obtained after the fragmentation of secondary clacining base substrate, wherein, described batching comprises 0.5 ~ 4.5wt.% crystal seed, 0.1 ~ 1.5wt.% dispersion agent, 0.01 ~ 1.2wt.% grain growth inhibitor, 0 ~ 0.5wt.% gaseous sources; A base substrate calcining carries out in the atmosphere containing hydrogen halide and size controlling constituent element, and described size controlling constituent element is aluminum halide; The calcining of secondary base substrate carries out in containing the atmosphere of hydrogen halide.
2. a kind of method preparing fine grain size alumina powder as claimed in claim 1, is characterized in that: described transition aluminas is γ-Al
2o
3, δ-Al
2o
3, ζ-Al
2o
3, η-Al
2o
3, θ-Al
2o
3, κ-Al
2o
3with χ-Al
2o
3in one or more.
3. a kind of method preparing fine grain size alumina powder as claimed in claim 2, is characterized in that: described crystal seed is oxide compound, nitride, carbide or the carbonitride that median size one of to be less than in the aluminium of 30nm, titanium, zirconium, vanadium four kinds of elements; Described grain growth inhibitor is YCl
3, Nb
2o
3, ZrO
2, Mg (OH) Cl, MgO and MgCl
2in one or more.
4. a kind of method preparing fine grain size alumina powder as claimed in claim 2, is characterized in that: described dispersion agent be molecular weight in 120 ~ 600 scopes, the acids containing methyl and phenyl ring or lipid.
5. a kind of method preparing fine grain size alumina powder as claimed in claim 1, it is characterized in that: the compound after oven dry and the powder that once calcining base is broken into all once will be calcined and secondary clacining after press forming again, the binder dextrin added or the content of polyvinyl alcohol are 2.5 ~ 5wt.%, and compacting pressure is 560 ~ 800MPa.
6. a kind of method preparing fine grain size alumina powder as claimed in claim 1, is characterized in that: in the atmosphere of contained hydrogen halide and size controlling constituent element, the concentration of hydrogen halide is 0.1 ~ 1.0%, the concentration of ammonia is 1.1 ~ 1.5%, the concentration of aluminum halide is 1 ~ 2%, the concentration of hydrogen is 3 ~ 5%, the concentration of nitrogen is 6-10%, surplus is air.
7. a kind of method preparing fine grain size alumina powder as claimed in claim 1, it is characterized in that: adopt containing the atmosphere of higher concentration hydrogen halide during secondary clacining, wherein the concentration of hydrogen halide is 1.6 ~ 2.0%, the concentration of ammonia is 2.3 ~ 3%, the concentration of hydrogen is 8 ~ 10%, the concentration of nitrogen is 11 ~ 13%, surplus is air.
8. a kind of method preparing fine grain size alumina powder as claimed in claim 1, it is characterized in that: for suitability for industrialized production, calcining tunnel furnace, rotary kiln or pusher type furnace carry out in a continuous manner.
9. a kind of method preparing fine grain size alumina powder as claimed in claim 1, is characterized in that: the particle diameter of fine grain size alumina powder is less than 0.14 μm, α-Al
2o
3content be 100%.
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| CN109530721A (en) * | 2018-12-11 | 2019-03-29 | 湖南金昊新材料科技股份有限公司 | A kind of sub-micron aluminium powder and acieral powder preparation method |
| CN109607584A (en) * | 2019-01-31 | 2019-04-12 | 东北大学 | A kind of preparation method of the ultralow sodium alumina powder material of high temperature |
| CN110625109A (en) * | 2019-09-30 | 2019-12-31 | 中南大学 | Preparation method of submicron aluminum-based alloy powder |
| CN111205070A (en) * | 2020-03-11 | 2020-05-29 | 苏州贝尔德新材料科技有限公司 | Preparation method of easily-sintered high-purity alumina |
| CN114835164B (en) * | 2022-03-21 | 2023-11-28 | 厦门钨业股份有限公司 | Method for treating tungsten oxide oversize material |
| CN114988886B (en) * | 2022-06-01 | 2023-05-12 | 洛阳中超新材料股份有限公司 | Preparation method of high-purity alpha-alumina powder capable of being sintered at low temperature |
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| CN1095360A (en) * | 1993-04-13 | 1994-11-23 | 住友化学工业株式会社 | Alpha-alumina powder and production method thereof |
| CN1108215A (en) * | 1993-11-25 | 1995-09-13 | 住友化学工业株式会社 | Method for producing alpha-alumina powder |
| CN1386705A (en) * | 2001-05-21 | 2002-12-25 | 住友化学工业株式会社 | Alpha-alumina fine powder and method for producing same |
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| US4019914A (en) * | 1973-06-27 | 1977-04-26 | Robert Bosch G.M.B.H. | Method of manufacturing α-alumina |
| CN1095360A (en) * | 1993-04-13 | 1994-11-23 | 住友化学工业株式会社 | Alpha-alumina powder and production method thereof |
| CN1108215A (en) * | 1993-11-25 | 1995-09-13 | 住友化学工业株式会社 | Method for producing alpha-alumina powder |
| CN1386705A (en) * | 2001-05-21 | 2002-12-25 | 住友化学工业株式会社 | Alpha-alumina fine powder and method for producing same |
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| C06 | Publication | ||
| PB01 | Publication | ||
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