CN102826579A - Preparation method of ultrahigh-purity and superfine aluminium oxide powder - Google Patents

Preparation method of ultrahigh-purity and superfine aluminium oxide powder Download PDF

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Publication number
CN102826579A
CN102826579A CN2012103501760A CN201210350176A CN102826579A CN 102826579 A CN102826579 A CN 102826579A CN 2012103501760 A CN2012103501760 A CN 2012103501760A CN 201210350176 A CN201210350176 A CN 201210350176A CN 102826579 A CN102826579 A CN 102826579A
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aluminium
purity
virahol
preparation
reactions
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王保奎
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DALIAN HILAND PHOTOELECTRIC MATERIAL Co Ltd
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DALIAN HILAND PHOTOELECTRIC MATERIAL Co Ltd
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Abstract

The invention relates to a preparation method of ultrahigh-purity and superfine alumina powder. The preparation method comprises the following process steps of: (1) injecting a high-purity aluminium sheet, isopropanol and a catalyst into a synthetic reaction tower to generate gaseous aluminium isopropoxide; cooling gaseous aluminium isopropoxide into liquid aluminium isopropoxide by virtue of a condenser; (2) injecting liquid aluminium isopropoxide into a reduced pressure distillation purification tank for evaporating to form steam, injecting the steam to a material receiving tank to become liquid ultrahigh-purity aluminium isopropoxide; (3) adding ultrahigh-purity aluminium isopropoxide into a vacuum stirring and drying machine, injecting high-purity water, and carrying out hydrolysis reaction under the circulating water cooling condition, so as to obtain ultrahigh-purity aluminium hydroxide and isopropanol aqueous solution; and drying in a vacuum stirring and drying machine; and (4) placing ultrahigh-purity aluminium hydroxide powder into a corundum crucible, and calcining in an electrically pushed slab kiln until the aluminium hydroxide powder is changed into alpha-Al2O3 powder, thus preparation is completed.

Description

Ultra-pure, superfine alumina powder preparation method
Technical field
The present invention relates to prepare the high purity alumina powder method with the high-purity aluminium ingot of purity>99.99%, particularly suitable prepares alumina content >=99.999%, the primary particle median size aluminum oxide powder body method at 0.2~0.4 μ m.
Background technology
The method for preparing at present high purity alumina powder comprises spark-discharge method, organoaluminum decomposition method, choline method etc. in exsiccated ammonium alum thermal decomposition method, aluminium carbonate ammonium thermal decomposition method, Bayer improved method, the aluminium powder water.Wherein the aluminium-alcohol salt hydrolysis method is to prepare high-purity, the state-of-the-art method of ultra-fine alumina at present.The aluminium-alcohol salt hydrolysis method is a kind of employing organic chemistry method production inorganic materials novel method; Be very different with conventional production methods; Use a large amount of organic solvent Virahols as raw material, thereby strict in the production technique, harsh requirement arranged fire-proof and explosion-proof to safety requirements; Armamentarium must have fire-proof and explosion-proof function; To the also strict evaluation of surrounding environment, manufacturing enterprise must possess relevant qualification, equipment design manufacturer, pressurized vessel manufacturer will possess relevant qualification, thereby facility investment is bigger.And Production Check Equipment, instrument are expensive, and it is well educated to require the testing staff to possess simultaneously, so expense is also very big.
The method of other various production high purity aluminium oxides, purity all can not reach 5N purity, and growth LED wafer must reach more than the 5N ultra-high purity with the Sapphire Substrate aluminum oxide.Because the sapphire crystal substrate dislocation desity of the ultra-pure oxidation aluminum feedstock growth of 5N just in time is complementary with gallium arsenide wafer number of dislocations lattice less than 300/ square centimeter, just can obtain the high-power and high-luminance LED wafer.
Summary of the invention
For solving 5N ultra-high purity, ultra-fine alumina powdered material, we initiate and adopt the aluminum isopropylate hydrolysis method to produce ultra-pure oxidation aluminium.
Preparing method of the present invention is:
1, with 99.99% or higher high-purity aluminium flake and the Virahol of purity, is injected in the stainless steel building-up reactions tower of forming by lower heating reaction kettle and top condensing surface, adds the catalyzer post-heating, Virahol and aluminium generation building-up reactions, generation gaseous state aluminum isopropylate.The gaseous state aluminum isopropylate gets into condensing surface, after condensing surface is cooled to liquid aluminum isopropylate, is back in the building-up reactions tower; Building-up reactions is accomplished in so ceaselessly evaporation-condensation-backflow, and final aluminium flake and Virahol generate liquid aluminum isopropylate fully.
Its chemical equation is:
2Al+6C 3H 7OH=2Al(C 3H 7O) 3+3H 2
2, liquid aluminum isopropylate is injected stainless steel underpressure distillation purification jar; Liquid high puring aluminium isopropoxide flashes to steam in jar is purified in underpressure distillation; Liquefy ultra-high purity isopropanol aluminium behind the entering splice jug, and impurity element is stayed the purification pot bottom, thus accomplish the aluminum isopropylate purification process.
3, liquid ultra-high purity isopropanol aluminium is added in the stainless steel vacuum stirring drying machine, inject high purity water, hydrolytic reactions under recirculated water cooling condition obtains ultra-pure white lake and isopropanol water solution.
Its reaction equation is:
Al(C 3H 7O) 3+3H 2O=Al(OH) 3+3C 3H 7OH
After hydrolysis reaction is accomplished, in the vacuum stirring drying machine, proceed oven dry, liquid Virahol becomes the gaseous state Virahol, and by vacuum system suction condenser system, the liquefy Virahol is discharged.And ultra-pure white lake is stayed in the hydrolysis drying machine tank body with the solid state powder form.
4, ultra-pure aluminium-hydroxide powder is packed in the high-purity corundum crucible, in electric pushed bat kiln, calcine.Aluminium-hydroxide powder is sloughed crystal water, accomplishes crystal conversion, becomes α-Al 2O 3Powder, preparation is accomplished.
But the inside and outside sapphire producer that produces of product supply country of the present invention is used to produce LED wafer, LED light fixture, high-performance ceramic etc.
Embodiment
Its preparation method:
1, with 99.99% or higher high-purity aluminium flake and the Virahol of purity, is injected in the stainless steel building-up reactions tower of forming by lower heating reaction kettle and top condensing surface, adds catalyzer mercury chloride; Its weight part is: aluminium flake 50-60, Virahol 350-360, mercury chloride 0.001-0.002.When Heating temperature reaches 84 ℃-120 ℃, Virahol and aluminium generation building-up reactions generate the gaseous state aluminum isopropylate.The gaseous state aluminum isopropylate gets into condensing surface, and 20 ℃ of-30 ℃ of cooled liquid aluminum isopropylates of cooling temperature are back in the building-up reactions tower; So ceaselessly evaporation-condensation-backflow, through 5-6 hour, reflux course finished, and accomplished building-up reactions, and final aluminium flake and Virahol generate liquid aluminum isopropylate fully.
Its chemical equation is:
2Al+6C 3H 7OH=2Al(C 3H 7O) 3+3H 2
2, liquid aluminum isopropylate is injected stainless steel underpressure distillation purification jar; Under vacuum tightness 1-20mmHg condition; Temperature reaches 150 ℃-200 ℃, and liquid high puring aluminium isopropoxide flashes to steam in the underpressure distillation purification jar, liquefy ultra-high purity isopropanol aluminium behind the entering splice jug; And impurity element is stayed the purification pot bottom, thereby accomplishes the aluminum isopropylate purification process.
3, liquid ultra-high purity isopropanol aluminium is added in the stainless steel vacuum stirring drying machine; Inject resistivity 10-18 megaohm high purity water; Its weight is the 30%-35% of pure aluminum isopropylate; Hydrolytic reactions under 20 ℃-30 ℃ recirculated water cooling condition obtains ultra-pure white lake and isopropanol water solution.
Its reaction equation is:
Al(C 3H 7O) 3+3H 2O=Al(OH) 3+3C 3H 7OH
After hydrolysis reaction is accomplished, in the vacuum stirring drying machine, proceed oven dry, after Heating temperature to 80 ℃-99 ℃, liquid Virahol becomes the gaseous state Virahol, and by vacuum system suction condenser system, the liquefy Virahol is discharged under 25 ℃ of-30 ℃ of temperature.And ultra-pure white lake is stayed in the hydrolysis drying machine tank body with the solid state powder form.
4, ultra-pure aluminium-hydroxide powder is packed in the high-purity corundum crucible, in electric pushed bat kiln, calcine.Through calcining in 5-6 hour, aluminium-hydroxide powder was sloughed crystal water under 1180 ℃ of-1250 ℃ of temperature, accomplished crystal conversion, became α-Al 2O 3Powder, preparation is accomplished.
Its reaction equation is:
2Al(OH) 3=Al 2O 3+3H 2O
At last to product A l 2O 3Powder is tested:
(1), adopts ICP-OES; Be the plasma Atomic Emission SpectrometerAES, product is carried out impurities analysis, detect for a long time through domestic and international authoritative feeler mechanism; The result shows impurity element Fe<3ppm, Si<2ppm, Ca<1ppm, Na<1ppm, Mg<1ppm, Cr<1ppm, Al 2O 3Content>=99.999% reaches ultra-pure standard.
(2), adopt X-ray diffractometer, to Al 2O 3Powder carries out the crystal formation analysis.
(3), adopt observation sample granule-morphology in the scanning electron microscopy, α-Al 2O 3Primary particle is subsphaeroidal.
(4), adopt laser particle analyzer that sample is carried out check and analysis, α-Al 2O 3Granularity is less, D 50Be 0.2~0.4 μ m, reach ultra-fine standard.

Claims (9)

1. ultra-pure, superfine alumina powder preparation method, its process step is:
(1), with 99.99% or higher high-purity aluminium flake and the Virahol of purity; Be injected in the stainless steel building-up reactions tower of forming by lower heating reaction kettle and top condensing surface; Add the catalyzer post-heating, Virahol and aluminium generation building-up reactions generate the gaseous state aluminum isopropylate; The gaseous state aluminum isopropylate gets into condensing surface, after condensing surface is cooled to liquid aluminum isopropylate, is back in the building-up reactions tower, and building-up reactions is accomplished in so ceaselessly evaporation-condensation-backflow, and final aluminium flake and Virahol generate liquid aluminum isopropylate fully;
Its chemical equation is:
2Al+6C 3H 7OH=2Al(C 3H 7O) 3+3H 2
(2), liquid aluminum isopropylate is injected stainless steel underpressure distillation purification jar; Liquid high puring aluminium isopropoxide flashes to steam in jar is purified in underpressure distillation; Liquefy ultra-high purity isopropanol aluminium behind the entering splice jug, and impurity element is stayed the purification pot bottom, thus accomplish the aluminum isopropylate purification process;
(3), liquid ultra-high purity isopropanol aluminium is added in the stainless steel vacuum stirring drying machine, inject high purity water, hydrolytic reactions under recirculated water cooling condition obtains ultra-pure white lake and isopropanol water solution;
Its reaction equation is:
Al(C 3H 7O) 3+3H 2O=Al(OH) 3+3C 3H 7OH
After hydrolysis reaction is accomplished, in the vacuum stirring drying machine, proceed oven dry, liquid Virahol becomes the gaseous state Virahol, and by vacuum system suction condenser system, the liquefy Virahol is discharged; And ultra-pure white lake is stayed in the hydrolysis drying machine tank body with the solid state powder form.
(4), ultra-pure aluminium-hydroxide powder is packed in the high-purity corundum crucible, in electric pushed bat kiln, calcine, aluminium-hydroxide powder is sloughed crystal water, accomplishes crystal conversion, becomes α-Al 2O 3Powder, preparation is accomplished.
2. preparation method according to claim 1, in said step (1), adding catalyzer in the stainless steel building-up reactions tower is mercury chloride.
3. preparation method according to claim 2, in described step (1), the weight part of aluminium flake, Virahol and the mercury chloride that adds in the stainless steel building-up reactions tower is: aluminium flake 50-60, Virahol 350-360, mercury chloride 0.001-0.002.
4. according to claim 1,3 described preparing methods, in described step (1), Heating temperature reaches 84 ℃-120 ℃, and Virahol and aluminium generation building-up reactions generate the gaseous state aluminum isopropylate.
5. preparation method according to claim 4, in described step (1), cooling temperature is 20 ℃-30 ℃ in condensing surface, and cooled liquid aluminum isopropylate is back in the building-up reactions tower; Through ceaselessly evaporation-condensation-backflow in 5-6 hour, reflux course finished, and accomplished building-up reactions.
6. according to claim 1 or 5 described preparing methods, in described step (2), the vacuum tightness 1-20mmHg during the stainless steel underpressure distillation is purified jar, temperature reaches 150 ℃-200 ℃.
7. according to claim 1 or 5 described preparing methods, in described step (3), inject resistivity 10-18 megaohm high purity water, its weight is the 30%-35% of pure aluminum isopropylate, and cooling temperature of circulating water is 20 ℃-30 ℃.
8. according to claim 1 or 5 described preparing methods, in described step (3), after hydrolysis reaction was accomplished, Heating temperature to 80 was ℃-99 ℃ in the vacuum stirring drying machine; Gaseous state Virahol liquefy Virahol under 25 ℃ of-30 ℃ of temperature of condenser system is discharged.
9. according to claim 1 or 8 described preparing methods, in described step (4), calcining temperature is 1180 ℃-1250 ℃ in the electric pushed bat kiln, calcination time 5-6 hour.
CN2012103501760A 2012-09-05 2012-09-05 Preparation method of ultrahigh-purity and superfine aluminium oxide powder Pending CN102826579A (en)

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Cited By (10)

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Publication number Priority date Publication date Assignee Title
CN104230662A (en) * 2014-09-23 2014-12-24 成都冠禹科技有限公司 Preparation method of high-purity 5N aluminum isopropoxide
CN104261447A (en) * 2014-09-23 2015-01-07 成都冠禹科技有限公司 Production method of 5N high-purity alpha alumina powder
RU2538606C1 (en) * 2013-12-30 2015-01-10 Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Национальный исследовательский технологический университет "МИСиС" Method of producing highly pure aluminium oxide by electrolysis
CN105293548A (en) * 2015-11-30 2016-02-03 成都乐氏化工工程有限公司 Gas-phase nanometer aluminium oxide
CN105948090A (en) * 2016-06-14 2016-09-21 袁伟昊 Ultra-pure nano-alumina green synthesis method and industrialization device
CN109264680A (en) * 2018-11-09 2019-01-25 厦门钜瓷科技有限公司 The method for preparing high-purity ultra-fine aluminum nitride powder based on aluminium alcoholates Hydrolyze method
CN112250452A (en) * 2020-09-25 2021-01-22 新疆众和股份有限公司 Alumina water-based coating material, preparation method thereof and crucible coating method
CN112939045A (en) * 2021-02-03 2021-06-11 浙江爱科新材料有限公司 Preparation method of superfine high-purity gamma-alumina
CN113072087A (en) * 2021-04-20 2021-07-06 江西宝弘纳米科技有限公司 Preparation method of high-purity alumina
CN117963962A (en) * 2023-12-22 2024-05-03 江苏容导半导体科技有限公司 Preparation process of alumina

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2538606C1 (en) * 2013-12-30 2015-01-10 Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Национальный исследовательский технологический университет "МИСиС" Method of producing highly pure aluminium oxide by electrolysis
CN104230662A (en) * 2014-09-23 2014-12-24 成都冠禹科技有限公司 Preparation method of high-purity 5N aluminum isopropoxide
CN104261447A (en) * 2014-09-23 2015-01-07 成都冠禹科技有限公司 Production method of 5N high-purity alpha alumina powder
CN104230662B (en) * 2014-09-23 2015-12-02 成都冠禹科技有限公司 A kind of preparation method of high-purity 5N aluminum isopropylate
CN105293548A (en) * 2015-11-30 2016-02-03 成都乐氏化工工程有限公司 Gas-phase nanometer aluminium oxide
CN105948090A (en) * 2016-06-14 2016-09-21 袁伟昊 Ultra-pure nano-alumina green synthesis method and industrialization device
CN109264680A (en) * 2018-11-09 2019-01-25 厦门钜瓷科技有限公司 The method for preparing high-purity ultra-fine aluminum nitride powder based on aluminium alcoholates Hydrolyze method
CN112250452A (en) * 2020-09-25 2021-01-22 新疆众和股份有限公司 Alumina water-based coating material, preparation method thereof and crucible coating method
CN112939045A (en) * 2021-02-03 2021-06-11 浙江爱科新材料有限公司 Preparation method of superfine high-purity gamma-alumina
CN113072087A (en) * 2021-04-20 2021-07-06 江西宝弘纳米科技有限公司 Preparation method of high-purity alumina
CN117963962A (en) * 2023-12-22 2024-05-03 江苏容导半导体科技有限公司 Preparation process of alumina

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Application publication date: 20121219