CN110256058A - A kind of preparation method of crystalline ceramics high purity alumina powder - Google Patents
A kind of preparation method of crystalline ceramics high purity alumina powder Download PDFInfo
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C04B35/115—Translucent or transparent products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/62655—Drying, e.g. freeze-drying, spray-drying, microwave or supercritical drying
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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Abstract
The invention discloses a kind of preparation methods of crystalline ceramics high purity alumina powder, the preparation method include the following steps: using purity for 99.99%-99.999% high purity aluminium oxide as raw material, be equipped with the ground slurry that 20%-40% contains admittedly with high purity water, spray drying, air-flow crushing obtain crystalline ceramics high purity alumina powder.The present invention solves the problems, such as the purity, intensity, light transmittance of crystalline ceramics, improves yield rate, the high-purity for processing efficiency, reducing cost, keeping product, the intensity for increasing product, the light transmittance for improving product.
Description
Technical field
The present invention relates to a kind of high-purity, high transparency, high intensity novel nano structure ceramics alumina powder.
Background technique
Currently, preparing high purity aluminium oxide method both at home and abroad has alum pyrolysismethod, aluminium carbonate ammonium pyrolysismethod, improvement Bayer
Method, pyrohydrolytic method etc..The advantages of alum method, has raw material inexpensively and mother liquor can recycle, and technology maturation is easy to work
Industry production；Stabilization easy to operate, product purity are high；Product is reunited less, and in preparation ceramics extrusion forming, density is lower, and initial stage burns
Knot slowly, is easy to get to Even Sintering tissue.And the shortcomings that this technique is that a large amount of ammonia and sulfur trioxide are generated in decomposable process,
It is be easy to cause environmental pollution, although can meet environmental requirements by vent gas treatment, causes that the production cost increases；Pass through recrystallization
It can remove Na+、Mg2+、Ca2+Equal metal impurities ion, but K+, the more difficult removal of impurity such as halogen, separation is difficult, and mistake
Journey is complicated, and the period is longer；There is thermal melting phenomenon in separation process, and volume expansion is serious, and product apparent density is caused to reduce.
Aluminium carbonate ammonium pyrolysismethod is the improvement of alum pyrolysismethod, and this method can avoid lacking for alum production technology
Point；Epigranular, partial size is thin and is evenly distributed；Exhaust gas is easy recycling, and sintered density is high.Although this method reduce exhaust gas
Discharge, but aggravated waste liquid [such as (NH4)2SO4] pollution, the problems such as production cycle is longer, requirement of process control is stringent.
The advantages of improveing Bayer process is that raw material sources are wide, and at low cost, process is pollution-free.But this method production technology is relatively
Complexity, production efficiency is lower, and product sintered density is low, and sintering temperature is higher, is restricted in industrial application.
What my company used is pyrohydrolytic method, and this method is since using aluminium and water as raw material, by-product is hydrogen gas and water, oxygen
Changing aluminium is product, and production process does not pollute environment, and at low cost, and low energy consumption, meets " green industry " advocated now.
Current ceramic field, it is stringent that crystalline ceramics is that high-purity, high-compactness, high transparency, technique require, and performance
It is required that harsh a kind of new structure ceramic material.Be used to prepare alumina transparent ceramic original powder require high-purity, small particle,
Monocrystalline type.High-purity requires purity to reach 99.99%-99.999%, and small particle requires biggish bulk density, good fluidity,
Surface is smooth, and dispersion performance is good, and adsorption capacity is strong, and thermal stability is good, high mechanical strength, and crystal form is α phase.
Crystalline ceramics and surface preventing material for preparing using high purity alumina powder as raw material etc. have high temperature resistant, high-strength
The features such as degree, high rigidity, high transparency.The product is for alum method or aluminium carbonate ammonium method, in production process
The use cost of less pollution, the discharge of no exhaust gas, waste water, client is relatively low.
In recent years, plant illumination field is one of faster agriculture lighting area of development, and LED illumination has luminous efficiency
Height, little power consumption, it is small in size, the service life is long many advantages, such as, substantially increase yield, reduce costs, plant lamp also with
LED lighting technology it is increasingly mature, enterprise fights in different parts plant illumination field from general illumination market one after another, and plant illumination possesses wide
Prospect, the market of crystalline ceramics is considerable, and the demand of high purity aluminium oxide will be substantially improved, this will necessarily make high-purity alumina powder
The technology of preparing of body turns to low cost, scale.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of crystalline ceramics high purity alumina powder, the preparation sides
Method solves the problems, such as the purity, intensity, light transmittance of crystalline ceramics, improves yield rate, processing efficiency, reduces cost, keeps product
High-purity, the intensity for increasing product, the light transmittance for improving product.
In order to achieve the above objectives, present invention employs the following technical solutions:
A kind of preparation method of crystalline ceramics high purity alumina powder, the preparation method include the following steps:
Using purity for 99.99%-99.999% high purity aluminium oxide as raw material, it is solid to be equipped with 20%-40% with high purity water
The slurry contained is ground, be spray-dried, air-flow crushing obtains crystalline ceramics high purity alumina powder.
Preferably, the high purity aluminium oxide that purity is 99.99%-99.999% is prepared using following methods:
It using the aluminium of 99.99%-99.999% and water as raw material, is atomized through 600-700 DEG C, then is hydrolyzed through 80-90 DEG C, reaction
High purity aluminium hydroxide is generated, then is calcined through 1000-1380 DEG C, moisture is removed, obtains the height that purity is 99.99%-99.999%
Pure α-Al2O3。
Preferably, the grinding specifically:
The slurry that 20%-40% contains admittedly is in sand mill, and grinding revolving speed is that 900r/h-1200r/h is ground, slurry
2 μm of D50 < of material, it is 1.0-1.2mm zirconium oxide combined oxidation aluminium ball that grinding mill, which is situated between,.
Preferably, the slurry qualified to grinding is spray-dried, and 300 DEG C of drying temperature <.
Preferably, the air-flow crushing, crushes pressure < 15MPa, and crushing frequency is 50Hz-65Hz.
According to a preferred embodiment of the present invention, a kind of preparation method of crystalline ceramics high purity alumina powder raw material,
The preparation method comprises the following steps:
1, it using the aluminium of 99.99%-99.999% and water as raw material, through pyrohydrolysis, is atomized through 650 DEG C, then through 85 DEG C of water
Solution, reaction generate high purity aluminium hydroxide.It is calcined again through 1000-1380 DEG C, removes moisture, finished product is high-purity α-Al2O3
(99.99%-99.999%).
2, to calcine by 1000-1380 DEG C, the high purity aluminium oxide that purity is 99.99%-99.999% is used as raw material
Pure water as solvent, for the slurry that outfit 20%-40% contains admittedly in sand mill, grinding revolving speed is that 900r/h-1200r/h is ground
Mill, 2 μm of grinding slurry D50 <, it is 1.0-1.2mm zirconium oxide combined oxidation aluminium ball that grinding mill, which is situated between,.The slurry qualified to grinding into
Row spray drying, using air-flow crushing, crushes pressure < 15MPa, crushing frequency is 50Hz- by 300 DEG C of drying temperature <
65Hz, it is ensured that process product finally obtain 2.5 μm of median particle diameter D50 < without agglomeration, and the crystalline ceramics that purity is >=99.995% is used
High purity alumina powder.Alumina powder carries out weighing packaging to material by automatic measuring packing device after crushing.
The high purity water (High purity water) that the present invention uses controls, one according to the control standard in industry
As when referring to 25 DEG C conductivity less than 0.1 μ s/cm and residual salt content be less than 0.3mg/L, and eliminate the micro of non-dielectric
The water of the impurity such as bacterium, microorganism, particle.Preparation method has distillation, UF membrane, ion exchange and sterilizing.
The crystalline ceramics pipe that the present invention is produced using high purity alumina powder as raw material has high-purity, high intensity, high light transmission
The uniform feature of rate, particle size distribution.Cost is relatively low for opposite similar product.
Detailed description of the invention
Fig. 1 is that embodiment 1 prepares crystalline ceramics high purity alumina powder raw material grain of sand degree distribution map；
Fig. 2 is that embodiment 1 prepares particle size distribution figure after crystalline ceramics high purity alumina powder raw material powder.
Specific embodiment
Any feature is disclosed to obtain in this specification, it unless specifically stated, can be equivalent or with similar purpose by other
Alternative features are replaced.Unless specifically stated, each feature is an example in a series of equivalent or similar characteristics
?.It is described to understand the present invention just for the sake of help, it should not be considered as to concrete restriction of the invention.
With the drawings and specific embodiments, the present invention is described in further detail below.
Embodiment one:
1, it using the aluminium of 99.99%-99.999% and water as raw material, is atomized through 650 DEG C, then is hydrolyzed through 85 DEG C, reaction generates
High purity aluminium hydroxide.It is calcined again through 1020 DEG C, removes moisture, finished product is high-purity α-Al2O3(99.993%).
2, with by 1020 DEG C of calcinings, purity is the high purity aluminium oxide of 99.99%-99.999% as raw material, pure water is used
Make solvent, the slurry that outfit 20% contains admittedly is in sand mill, and grinding revolving speed is that 900r/h is ground, and grinding slurry D50 is 1.0
μm, it can be seen that the median particle diameter D50 of slurry is 1.0 μm from the size distribution of Fig. 1, it is that 1.0-1.2mm is aoxidized that grinding mill, which is situated between,
Zirconium composite oxide aluminium ball.To grinding, qualified slurry is spray-dried, and 250 DEG C of drying temperature, using air-flow crushing, is crushed
Pressure 4MPa, crushing frequency are 52Hz, it is ensured that process product finally obtain the transparent pottery that median particle diameter D50 is 1.17 μm without agglomeration
Porcelain high purity alumina powder, the median particle diameter D50 after it can be seen that powder in the size distribution of Fig. 2 are 1.17 μm.After crushing
Alumina powder carries out weighing packaging to material by automatic measuring packing device.Every bag of 25 ± 0.02kg.Powder obtained by the process
Body purity is 99.995%, and finished product crystalline ceramics pipe compression strength is 287N/m, and light transmittance reaches 87.3%.
Embodiment two:
1, it using the aluminium of 99.99%-99.999% and water as raw material, is atomized through 600 DEG C, then is hydrolyzed through 80 DEG C, reaction generates
High purity aluminium hydroxide.It is calcined again through 1150 DEG C, removes moisture, finished product is high-purity α-Al2O3(99.993%).
2, with by 1150 DEG C of calcinings, purity is the high purity aluminium oxide of 99.99%-99.999% as raw material, pure water is used
Make solvent, the slurry that outfit 30% contains admittedly is in sand mill, and grinding revolving speed is that 1050r/h is ground, and grinding slurry D50 is
1.2 μm, it is 1.0-1.2mm zirconium oxide combined oxidation aluminium ball that grinding mill, which is situated between,.To grinding, qualified slurry is spray-dried, dry
240 DEG C of temperature, using air-flow crushing, pressure 6MPa is crushed, crushing frequency is 55Hz, it is ensured that process product are finally obtained without agglomeration
The crystalline ceramics high purity alumina powder for being 1.17 μm to median particle diameter D50.Alumina powder passes through automatic gauge after crushing
Packing device carries out weighing packaging to material.Every bag of 25 ± 0.02kg.Powder purity obtained by the process is 99.995%, and finished product is saturating
Bright ceramic tube compression strength is 293N/m, and light transmittance reaches 95.2%.
Embodiment three:
1, it using the aluminium of 99.99%-99.999% and water as raw material, is atomized through 700 DEG C, then is hydrolyzed through 90 DEG C, reaction generates
High purity aluminium hydroxide.It is calcined again through 1350 DEG C, removes moisture, finished product is high-purity α-Al2O3(99.993%).
2, with by 1350 DEG C of calcinings, purity is the high purity aluminium oxide of 99.99%-99.999% as raw material, pure water is used
Make solvent, the slurry that outfit 40% contains admittedly is in sand mill, and grinding revolving speed is that 1200r/h is ground, and grinding slurry D50 is
1.4 μm, it is 1.0-1.2mm zirconium oxide combined oxidation aluminium ball that grinding mill, which is situated between,.To grinding, qualified slurry is spray-dried, dry
260 DEG C of temperature, using air-flow crushing, pressure 8MPa is crushed, crushing frequency is 58Hz, it is ensured that process product are finally obtained without agglomeration
The crystalline ceramics high purity alumina powder for being 1.17 μm to median particle diameter D50.Alumina powder passes through automatic gauge after crushing
Packing device carries out weighing packaging to material.Every bag of 25 ± 0.02kg.Powder purity obtained by the process is 99.995%, and finished product is saturating
Bright ceramic tube compression strength is 298N/m, and light transmittance reaches 91.8%.
Crystalline ceramics pipe light transmittance made of crystalline ceramics high-purity alumina powder produced by the invention reaches customer requirement
95% or more, shrinking percentage reaches the 22.0%-23.5% range of customer requirement, and purity is relative to France, Japanese pottery powder
It is higher, up to 99.995% or more.
Technological parameter (such as temperature, time) section bound value of the invention and interval value can realize this law,
Embodiment numerous to list herein.
Ordinary skill in the art knowledge can be used in the unspecified content of the present invention.
It should be noted last that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting.Although ginseng
It is described the invention in detail according to embodiment, it will be apparent to an ordinarily skilled person in the art that technical side of the invention
Case is modified or replaced equivalently, and without departure from the spirit and scope of technical solution of the present invention, should all be covered in the present invention
Scope of the claims in.
Claims (5)
1. a kind of preparation method of crystalline ceramics high purity alumina powder, the preparation method include the following steps:
Using purity for 99.99%-99.999% high purity aluminium oxide as raw material, be equipped with what 20%-40% contained admittedly with high purity water
Slurry is ground, be spray-dried, air-flow crushing obtains crystalline ceramics high purity alumina powder.
2. preparation method according to claim 1, which is characterized in that purity is the high pure zirconia of 99.99%-99.999%
Aluminium is prepared using following methods:
It using the aluminium of 99.99%-99.999% and water as raw material, is atomized through 600-700 DEG C, then is hydrolyzed through 80-90 DEG C, reaction generates
High purity aluminium hydroxide, then calcined through 1000-1380 DEG C, moisture is removed, high-purity α-that purity is 99.99%-99.999% is obtained
Al2O3。
3. preparation method according to claim 1, which is characterized in that the grinding specifically:
The slurry that 20%-40% contains admittedly is in sand mill, and grinding revolving speed is that 900r/h-1200r/h is ground, grinding slurry
2 μm of D50 <, it is 1.0-1.2mm zirconium oxide combined oxidation aluminium ball that grinding mill, which is situated between,.
4. preparation method according to claim 1, which is characterized in that grinding, qualified slurry is spray-dried, and is done
300 DEG C of dry temperature <.
5. preparation method according to claim 1, which is characterized in that the air-flow crushing crushes pressure < 15MPa, powder
Broken frequency is 50Hz-65Hz.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111704813A (en) * | 2020-06-03 | 2020-09-25 | 上海大学 | Wet grinding preparation method of aluminum oxide powder |
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| CN104787787A (en) * | 2015-02-16 | 2015-07-22 | 青海圣诺光电科技有限公司 | Method for preparing ultra-micro alumina powder by using mechanical crushing |
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| JPH01141817A (en) * | 1987-11-26 | 1989-06-02 | Mitsubishi Mining & Cement Co Ltd | Production of translucent alumina material powder |
| CN1394807A (en) * | 2002-07-09 | 2003-02-05 | 刘明 | Preparation method of high-purity superfine alumina powder body |
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| CN102491392A (en) * | 2011-12-13 | 2012-06-13 | 大连交通大学 | Preparation method for aluminium oxide |
| CN104787787A (en) * | 2015-02-16 | 2015-07-22 | 青海圣诺光电科技有限公司 | Method for preparing ultra-micro alumina powder by using mechanical crushing |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111704813A (en) * | 2020-06-03 | 2020-09-25 | 上海大学 | Wet grinding preparation method of aluminum oxide powder |
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Application publication date: 20190920 |