CN103910368A - Preparation method of axiolitic, approximate hexagonal plate sheet-shaped, or drum-shaped primary particles or alpha-aluminum oxide powder composed of aggregate of approximate hexagonal plate sheet-shaped, or drum-shaped primary particles - Google Patents
Preparation method of axiolitic, approximate hexagonal plate sheet-shaped, or drum-shaped primary particles or alpha-aluminum oxide powder composed of aggregate of approximate hexagonal plate sheet-shaped, or drum-shaped primary particles Download PDFInfo
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- CN103910368A CN103910368A CN201410090500.9A CN201410090500A CN103910368A CN 103910368 A CN103910368 A CN 103910368A CN 201410090500 A CN201410090500 A CN 201410090500A CN 103910368 A CN103910368 A CN 103910368A
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Abstract
The invention discloses a preparation method of axiolitic, approximate hexagonal plate sheet-shaped, or drum-shaped primary particles or alpha-aluminum oxide powder composed of an aggregate of the approximate hexagonal plate sheet-shaped, or drum-shaped primary particles. The preparation method comprises following steps: a small amount of a fluorine-containing compound and a small amount of a liquid disperse medium are added into aluminium raw material; an obtained mixture is subjected to mineralization pretreatment, is dried, and is subjected to high-temperature mineralization heat treatment or roasting so as to obtain the axiolitic, approximate hexagonal plate sheet-shaped, or drum-shaped primary particles or the alpha-aluminum oxide powder composed of the aggregate of the approximate hexagonal plate sheet-shaped, or drum-shaped primary particles. Particle size ranges from tens of nanometers (nm) to hundreds of micrometers (mum). Beneficial effects of the preparation method are that: purity of the aluminium raw material is not reduced, and particle morphology of the alpha-aluminum oxide powder can be controlled effectively by changing preparation conditions.
Description
Technical field
The present invention relates to a kind of alumina powder jointed preparation method, particularly the preparation method of the alpha-alumina powder of a kind of ellipsoid shape, nearly hexagonal plate sheet or the former grade particles of drum type or its coacervate composition.
Background technology
Nano-powder technology of preparing is one of at present domestic and international chemical engineering and field of new technology of greatest concern, and the pattern of powder granule has become one of important factor of the material property that affects powder characteristic and develop take powder as raw material.From root, the rise, growth, maturation, application and following development that depend on the material preparation technology of powder granule pattern all will be decided by generation and the development of powder granule pattern technology of preparing, also by the application development that promotes them in inorganic chemical engineering and field of new.
It is mainly by Mechanical Crushing and grinding that traditional method is prepared powder body material, and the pattern of powder granule depends primarily on the character of material itself and the feature of the equipment of use, and the overwhelming majority is irregular polyhedron and sheet; Grain graininess depends primarily on equipment characteristic and ability and processing method.The appearance of artificial Preparation Technique of Powders and wet chemistry method is that people become possibility according to oneself wish and the desirable pattern that designs powder granule, as powder granule pattern can be made spherical or subsphaeroidal, hollow ball, needle-like, bar-shaped, whisker etc.Nowadays people even can prepare the CNT (carbon nano-tube) with property according to wish.That is to say, can accomplish powder granule pattern to carry out autotelic control by some method people---enter the powder granule morphology control technology of preparing stage.For example alumina powder jointed, prepare transparent alumina polycrystalline ceramics, leave single dispersion, spherical, ultra-fine, high-purity alumina powder jointed be almost impossible.
The implication of former grade particles: be defined as standard in " powder technology and equipment " (Tao Zhendong, Zheng Shaohua chief editor, the August in 2003 the 1st edition) of publishing with Chemical Industry Press.Be again former grade particles, basic granules or primary particle (English is generally Primary Particles); refer to the particulate matter that determines, forms at first by character and the system character of material itself under certain condition; as the deposit seeds in colloidal solid, precipitation system in colloidal dispersion (colloidal sol or gel) and they are heat-treated the particle of rear formation, the solid granule forming in thermal decomposition process etc.Former grade particles may only comprise a crystal grain, also may comprise multiple crystal grain.The shape of the former grade particles that present method relates to, is mainly ellipsoid shape, nearly hexagonal plate sheet, is secondly drum type, is take six side's en plaques as basic coacervate etc. again.Be commonly referred to as second particle (particle) by many former grade particles by physical adsorption, chemisorption, physical and chemical adsorption or the various liquid bridge power particle swarm forming of reuniting, be again cluster of grains aggressiveness or coacervate particle (English is generally Secondary Particles).
Processing and control to powder granule pattern have diverse ways.What have achieves the goal according to the character of material and the feature of equipment, as prepares the platy shaped particle that sticking power is stronger, utilizes the joint of material itself and reactive force that equipment applies material and realizes; The purposes according to preparation technology's feature and powder body material having realizes, as prepared, sintered density approaches theoretical density to greatest extent single disperses, spheroidal particle, the method adopting have particulate in liquid phase method forming core, grow up mechanism and realize, or adopt prilling process to be achieved.Along with development and the progress of material preparation technology, prepare high performance material more and more higher to the requirement of raw material.Such as, powder raw material is not only required to high purity, ultrafine, sometimes also powder granule pattern is had to special requirement, to realize the more high-performance optimization of material.
Summary of the invention
In order to meet, simple granule-morphology is carried out to the autotelic strict demand of effectively controlling, the embodiment of the present invention provides the preparation method of the alpha-alumina powder of a kind of ellipsoid shape, nearly hexagonal plate sheet or the former grade particles of drum type or its coacervate composition.
In order to realize foregoing invention object; the invention provides the preparation method of the alpha-alumina powder of a kind of ellipsoid shape, nearly hexagonal plate sheet or the former grade particles of drum type or its coacervate composition; to utilize fluorochemicals as mineralizer or additive; the auxiliary control that realizes the former grade particles of alpha-alumina powder to generating with suitable technological process; make the former grade particles of its individual particle or composition coacervate generate the pattern of ellipsoid shape, nearly hexagonal plate sheet or drum type or its coacervate, comprise the following steps:
(1) take aluminum-containing raw material A;
(2) account for the fluorochemicals that aluminum-containing raw material A quality percentage composition is 0.5%～10% and obtain a kind of mixture B to adding in raw material A,
Under described fluorochemicals effect, carry out the mixture meal that the pre-treatment of dry method mineralising obtains and be called presoma first, the pre-treatment of described dry method mineralising comprises mixing, stirring, grinds;
Or add the additive that accounts for mixture B quality percentage composition 10% in mixture B, described additive is liquid dispersion medium or pH value conditioning agent or precipitation agent, under fluorochemicals effect, carry out the pre-treatment of wet method mineralising and obtain product C, the pre-treatment of described wet method mineralising comprises stirring, dispersion, mixing, hydrolysis, solvent thermal, precipitation or recrystallization; By the dry product C presoma second that obtains;
(3) by presoma first or the mineralising thermal treatment at a certain temperature of presoma second; obtain simple granule-morphology substantially take ellipsoid shape, nearly hexagonal plate sheet or drum type as main; or the alpha-alumina powder of its coacervate, obtaining former grade particles or its Water-borne paint scope is that (μ is m) to hundreds of microns for tens nanometer (nm).
Described aluminum-containing raw material A is one or more the mixture in the inorganic acid salt of aluminum oxide, hydrated aluminum oxide, aluminium hydroxide, aluminium-alcohol salt and hydrolysate thereof, aluminium and the organic acid salt of aluminium.
Fluorochemicals in described step (2) is that aluminum fluoride, Neutral ammonium fluoride, hydrogen fluoride, hexafluoro close one or several the mixture in sodium aluminate and their hydrate.
Described liquid dispersion medium refers to the mixture of a kind of of water, alcohol or two kinds.
Described water is distilled water, deionized water or ion exchanged water; Described alcohol is fatty alcohol nontoxic, pollution-free, that carbon atoms number is 2～8 or low-carbon alcohol, and described alcohol is ethanol, n-propyl alcohol, Virahol, propyl carbinol, isopropylcarbinol, the trimethyl carbinol, primary alconol, secondary alcohol or the tertiary alcohol.
The described pretreated time of dry method mineralising is 0.1～12 hour; The described pretreated time of wet method mineralising is 0.1～12 hour; The heat treated time of described mineralising is 0.1～12 hour.
Described pH adjusting agent is one or several the mixture in ammoniacal liquor, urea or organic amine; Precipitation agent is one or several the mixture in ammoniacal liquor, urea, carbonic acid, carbonic acid gas or oxalic acid.
Described in described step (2), dry mode is convection current, radiation or thermal conduction, and drying temperature is 120 ℃～180 ℃.
The heat treated treatment temp of mineralising described in described step (3) is 1000 ℃～1400 ℃, and the treatment time is 0.5～6 hour.
Described aluminum oxide purity >=95%.
, there is following chemical reaction in high-temperature roasting in presoma first or presoma second:
The chemical reaction that water-soluble aluminum salt hydrolytic precipitation process occurs:
Al
3++ OH
-→ AlOOH ↓ or Al
3++ 3OH
-→ Al (OH)
3↓
The chemical reaction occurring in hydrolytic sol gelation process is as follows:
Al(OR)
3+3H
2O→Al(OH)
3↓+3HOR
The beneficial effect that the technical scheme that the embodiment of the present invention provides is brought is: do not reduce the purity of aluminum-containing raw material, and effectively control the granule-morphology of alpha-alumina powder by changing preparation condition.
Accompanying drawing explanation
Fig. 1, for the ellipsoid shape particulate scan electromicroscopic photograph that the embodiment of the present invention 1 produces, amplifies 1000 times.
Fig. 2, for the ellipsoid shape particulate scan electromicroscopic photograph that the embodiment of the present invention 1 produces, amplifies 5000 times.
The drum type particulate scan electromicroscopic photograph that Fig. 3 produces for the embodiment of the present invention 2, amplifies 5000 times.
The hexagonal flake particulate scan electromicroscopic photograph that Fig. 4 produces for the embodiment of the present invention 3, amplifies 1000 times.
The hexagonal flake particulate scan electromicroscopic photograph that Fig. 5 produces for the embodiment of the present invention 3, amplifies 5000.
Fig. 6, for the hexagonal flake particulate scan electromicroscopic photograph that the embodiment of the present invention 3 produces, amplifies 10000 times.
The coacervate stereoscan photograph of the little hexagonal flake granulometric composition that Fig. 7 produces for the embodiment of the present invention 4, amplifies 1000 times.
The coacervate stereoscan photograph of the little hexagonal flake granulometric composition that Fig. 8 produces for the embodiment of the present invention 4, amplifies 5000 times.
Embodiment
Often can introduce impurity for the existing method of preparing alpha-alumina crystals, and can not effectively control the problem of crystal morphology, the invention provides the preparation method of the alpha-alumina powder of a kind of ellipsoid shape, nearly hexagonal plate sheet or the former grade particles of drum type or its coacervate composition; Comprise the following steps:
(1) take aluminum-containing raw material A;
(2) account for the fluorochemicals that aluminum-containing raw material A quality percentage composition is 0.5%～10% and obtain a kind of mixture B to adding in raw material A,
Under fluorochemicals effect, carry out the mixture meal that the pre-treatment of dry method mineralising obtains and be called presoma first, the pre-treatment of dry method mineralising comprises mixing, stirring, grinds;
Or add the additive that accounts for mixture B quality percentage composition 10% in mixture B, additive is liquid dispersion medium or pH value conditioning agent or precipitation agent, under fluorochemicals effect, carry out the pre-treatment of wet method mineralising and obtain product C, the pre-treatment of wet method mineralising comprises stirring, dispersion, mixing, hydrolysis, solvent thermal, precipitation or recrystallization; By the dry product C presoma second that obtains;
(3) by presoma first or the mineralising thermal treatment at a certain temperature of presoma second; obtain simple granule-morphology substantially take ellipsoid shape, nearly hexagonal plate sheet or drum type as main; or the alpha-alumina powder of its coacervate, obtaining former grade particles or its Water-borne paint scope is that (μ is m) to hundreds of microns for tens nanometer (nm).
Embodiment 1:
(1) take Al (OH)
350 grams are placed in pottery mortar;
(2) add 0.25 gram of AlF
33.5H
2o, in pottery mortar, is ground to and obtains loose meal and obtain presoma first;
(3) presoma first is incubated to 6 hours in High Temperature Furnaces Heating Apparatus at 1000 ℃ and carries out mineralising thermal treatment, obtaining former grade particles is axiolitic alpha-alumina powder, as shown in Fig. 1～2.
Embodiment 2
(1) take Al
2o
3xH
2o50 gram is placed in pottery mortar;
(2) be that 10% ethanol is dispersion medium by adding mass percent, process through the pre-mineralising of wet method of the processes such as mixing, grinding and oven dry the loose powder obtaining for 10 hours and obtain presoma second;
(3) by presoma second, in High Temperature Furnaces Heating Apparatus, at 1400 ℃, be incubated 1 hour, obtain the alpha-alumina powder that former grade particles is drum type, as shown in Figure 3.
Embodiment 3:
(1) take γ-Al
2o
350 grams are placed in pottery mortar,
(2) add 1.0 grams of NH
4f, in pottery mortar, is ground to and obtains loose meal and obtain presoma first;
(3) by presoma first, in High Temperature Furnaces Heating Apparatus, at 1200 ℃, be incubated 3 hours, obtain the alpha-alumina powder that former grade particles is six side's en plaques, as shown in Fig. 4～6.
Embodiment 4:
(1) take the Tai-Ace S 150 Al of 167.6 grams
2(SO
4)
3be placed in pottery mortar;
(2) add 2.0 grams of AlF
33.5H
2o and NH
4the mixture of F in pottery mortar, wherein AlF
33.5H
2o and NH
4f mass ratio is 1:3; Then adding mass percent is that 10% ethanol is dispersion medium, the loose powder presoma second obtaining through the pre-mineralising processing of wet method of the processes such as mixing, grinding and oven dry;
(3) by presoma second, in High Temperature Furnaces Heating Apparatus, at 1300 ℃, be incubated 6 hours, obtain particle take the coacervate of six side's en plaques as main alpha-alumina powder, as shown in Fig. 7～8.
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. a preparation method for the alpha-alumina powder of ellipsoid shape, nearly hexagonal plate sheet or the former grade particles of drum type or its coacervate composition, is characterized in that, comprises the following steps:
(1) take aluminum-containing raw material A;
(2) account for the fluorochemicals that aluminum-containing raw material A quality percentage composition is 0.5%～10% and obtain a kind of mixture B to adding in raw material A,
Under described fluorochemicals effect, carry out the mixture meal that the pre-treatment of dry method mineralising obtains and be called presoma first, the pre-treatment of described dry method mineralising comprises mixing, stirring, grinds;
Or add the additive that accounts for mixture B quality percentage composition 10% in mixture B, described additive is liquid dispersion medium or pH value conditioning agent or precipitation agent, under fluorochemicals effect, carry out the pre-treatment of wet method mineralising and obtain product C, the pre-treatment of described wet method mineralising comprises stirring, dispersion, mixing, hydrolysis, solvent thermal, precipitation or recrystallization; By the dry product C presoma second that obtains;
(3) by described presoma first or the mineralising thermal treatment at a certain temperature of described presoma second; obtain simple granule-morphology substantially take ellipsoid shape, nearly hexagonal plate sheet or drum type as main; or the alpha-alumina powder of its coacervate, obtaining former grade particles or its Water-borne paint scope is that (μ is m) to hundreds of microns for tens nanometer (nm).
2. preparation method according to claim 1, is characterized in that, described aluminum-containing raw material A is one or more the mixture in the inorganic acid salt of aluminum oxide, hydrated aluminum oxide, aluminium hydroxide, aluminium-alcohol salt and hydrolysate thereof, aluminium and the organic acid salt of aluminium.
3. preparation method according to claim 1, is characterized in that, the fluorochemicals in described step (2) is that aluminum fluoride, Neutral ammonium fluoride, hydrogen fluoride, hexafluoro close one or several the mixture in sodium aluminate and their hydrate.
4. preparation method according to claim 1, is characterized in that, described liquid dispersion medium refers to the mixture of a kind of of water, alcohol or two kinds.
5. preparation method according to claim 4, is characterized in that, described water is distilled water, deionized water or ion exchanged water; Described alcohol is fatty alcohol nontoxic, pollution-free, that carbon atoms number is 2～8 or low-carbon alcohol, and described alcohol is ethanol, n-propyl alcohol, Virahol, propyl carbinol, isopropylcarbinol, the trimethyl carbinol, primary alconol, secondary alcohol or the tertiary alcohol.
6. according to the arbitrary described preparation method of claim 1-5, it is characterized in that, the described pretreated time of dry method mineralising is 0.1～12 hour; The described pretreated time of wet method mineralising is 0.1～12 hour; The heat treated time of described mineralising is 0.1～12 hour.
7. preparation method according to claim 1, is characterized in that, described pH adjusting agent is one or several the mixture in ammoniacal liquor, urea or organic amine; Precipitation agent is one or several the mixture in ammoniacal liquor, urea, carbonic acid, carbonic acid gas or oxalic acid.
8. preparation method according to claim 1, is characterized in that, described in described step (2), dry mode is convection current, radiation or thermal conduction, and drying temperature is 120 ℃～180 ℃.
9. preparation method according to claim 1, is characterized in that, the heat treated treatment temp of mineralising described in described step (3) is 1000 ℃～1400 ℃, and the treatment time is 0.5～6 hour.
10. preparation method according to claim 2, is characterized in that described aluminum oxide purity >=95%.
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| CN201410090500.9A CN103910368A (en) | 2014-03-12 | 2014-03-12 | Preparation method of axiolitic, approximate hexagonal plate sheet-shaped, or drum-shaped primary particles or alpha-aluminum oxide powder composed of aggregate of approximate hexagonal plate sheet-shaped, or drum-shaped primary particles |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104556167A (en) * | 2014-12-19 | 2015-04-29 | 贵州天合国润高新材料科技有限公司 | Method for preparing flaky alumina powder |
| CN104724741A (en) * | 2015-03-23 | 2015-06-24 | 北京科技大学 | Preparation method of flaky alumina |
| CN104891540A (en) * | 2015-06-18 | 2015-09-09 | 成都华泽晶体材料有限公司 | Preparation method of micrometer-scale sphere-like alpha-aluminium oxide powder |
| CN108910927A (en) * | 2018-07-09 | 2018-11-30 | 郑州大学 | A kind of method of low temperature preparation polyhedral nano-alpha aluminium oxide powder |
| CN110563010A (en) * | 2019-09-19 | 2019-12-13 | 中国计量大学 | preparation method of low-sodium regular hexagonal flaky alpha-alumina micro powder |
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| CN101607726A (en) * | 2008-06-20 | 2009-12-23 | 大连交通大学 | Former grade particles is the manufacture method of the alpha-alumina powder of nearly hexagonal plate sheet or drum type |
| CN103553096A (en) * | 2013-10-28 | 2014-02-05 | 郑州玉发精瓷科技有限公司 | Preparation method of tabular corundum phase aluminum oxide powder for electronic material polishing |
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2014
- 2014-03-12 CN CN201410090500.9A patent/CN103910368A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101607726A (en) * | 2008-06-20 | 2009-12-23 | 大连交通大学 | Former grade particles is the manufacture method of the alpha-alumina powder of nearly hexagonal plate sheet or drum type |
| CN103553096A (en) * | 2013-10-28 | 2014-02-05 | 郑州玉发精瓷科技有限公司 | Preparation method of tabular corundum phase aluminum oxide powder for electronic material polishing |
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|---|
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104556167A (en) * | 2014-12-19 | 2015-04-29 | 贵州天合国润高新材料科技有限公司 | Method for preparing flaky alumina powder |
| CN104724741A (en) * | 2015-03-23 | 2015-06-24 | 北京科技大学 | Preparation method of flaky alumina |
| CN104891540A (en) * | 2015-06-18 | 2015-09-09 | 成都华泽晶体材料有限公司 | Preparation method of micrometer-scale sphere-like alpha-aluminium oxide powder |
| CN108910927A (en) * | 2018-07-09 | 2018-11-30 | 郑州大学 | A kind of method of low temperature preparation polyhedral nano-alpha aluminium oxide powder |
| CN110563010A (en) * | 2019-09-19 | 2019-12-13 | 中国计量大学 | preparation method of low-sodium regular hexagonal flaky alpha-alumina micro powder |
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Application publication date: 20140709 |