CN1076716C - Process for mfg. non-lumps submicron alpha-Al2O3 powder and microlitic corundum ball - Google Patents
Process for mfg. non-lumps submicron alpha-Al2O3 powder and microlitic corundum ball Download PDFInfo
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- CN1076716C CN1076716C CN97109341A CN97109341A CN1076716C CN 1076716 C CN1076716 C CN 1076716C CN 97109341 A CN97109341 A CN 97109341A CN 97109341 A CN97109341 A CN 97109341A CN 1076716 C CN1076716 C CN 1076716C
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Abstract
The present invention relates to a low-cost method for preparing submicron alpha-Al2O3 powder without agglomeration, and microcrystalline corundum porcelain balls. In the preparation method, 85 to 97 wt% of submicron alpha-Al2O3 powder without agglomeration, and 3 to 15 wt% of flux powder are mixed and perform ball milling for 3 to 5 hours; when the mixture is dried by a spraying machine, the processes of granulation, axial pressurization or cold isostatic compaction, and heat preservation for 1 to 3 hours at a temperature of 1400 to 1580 DEG C are performed. The present invention has the characteristics that cheap raw materials sold in markets are used for preparing the submicron alpha-Al2O3 powder without agglomeration, cheap natural mineral substances are used for manufacturing the flux powder, and the microcrystalline corundum porcelain balls with good performance are rapidly calcined at a low temperature.
Description
The invention belongs to powder preparing and Al
2O
3The pottery preparation.
Alumina-ceramic because of its good electric property, physical strength height, advantage such as hardness is big, thermal expansivity is little, wear-resisting and thermal shock resistance is good, make it become a kind of most widely used pottery.Yet the sintering temperature of corundum porcelain is up to 1600～1700 ℃, and investment is big, energy consumption is high, adds the contradiction between its price and the performance, has limited its widespread use.
In order to address these problems, Chinese scholars had all been carried out number of research projects in recent years.The Japan scholar proposes to make raw material with superfine alumina powder, can prepare the excellent dense base substrate at 1400 ℃ of sintering, but its superfine alumina powder complicated process of preparation, cost is very high; Norton Co adopts sol-gel method to prepare so-called SG material, produces microcrystal fused alumina, and its cost is higher than 6～7 times of traditional methods.Domestic scholars is also being made number of research projects aspect the sintering temperature that reduces alumina-ceramic.But all fundamentally do not solve the price of alumina-ceramic and the contradiction between the performance, the product of using as textile industry and the mill ball in the ceramic glaze fine grinding etc., the use price is 4000～5000 yuans/ton a common raw material, its sintering temperature height, the performance of product particularly wear resisting property do not satisfy user's requirement.And use price is 80000～200000 yuans/ton high pure and ultra-fine raw material, though can reduce sintering temperature and obtain the product of excellent property, its price is that user institute is unacceptable, and external situation is also like this.
Contradiction between the cost/performance ratio that the objective of the invention is to exist at present alumina-ceramic, adopt marketable material, low cost is prepared no reunion submicron alumina powder, select for use the technological process of optimization to make the microcrystal fused alumina porcelain of excellent performance, thereby realize the low-cost industrial preparation of high-performance ceramic.
Below in conjunction with Fig. 1 content of the present invention is specifically described.
Fig. 1. the no reunion submicron alpha-Al of low-cost manufacturing
2O
3The process flow sheet of powder and microcrystal fused alumina porcelain ball
1. there is not reunion submicron alpha-Al2O
3The preparation of powder
With commercially available α-Al2O
3α-Al that powder or modification Bayer process are produced2O
3Powder, add the dispersant (such as one or more of the efficient dispersant such as polyether base, polyhydroxy, many carboxyls) of 0.5～1.5 wt%, conventional method ball milling (material: ball: water=1: 2: 1,24 hours), control the pH value (being generally 6～7) of slip well, adjust and make no reunion submicron alpha-Al by spray-drying2O
3Powder, its particle diameter is 0.1～1 μ m, average grain diameter 0.5 μ m. It is single that these powder can be in an amount of water or organic solvent Disperse, do not have soft-agglomerated attitude, visible isolated particle under the petrographic microscope, it is motion or vibrational state.
2. the preparation of flux
The chemical composition range of flux is (wt%): CaO 15～30%, and MgO 15～25%, Al
2O
30～5%, SiO
245～70%.It is to be made into by raw mineral materialss such as natural quartz, diopside, rhombspar, Wingdales, and ball milling mixes 5～10 hours, and (material: ball: water=1: 2: 1), 1200～1400 ℃ of insulations 1～3 hour, ball milling was to the ground flux of crossing 300 mesh sieves then.
3. moulding
With the above-mentioned raw material powder that makes by Al
2O
3Powder 85～97wt%, ground flux 3～15wt% batching, ball milling 3～5 hours, spray-dried machine drying-granulating, axial pressure or cold isostatic compaction.
4. burn till
Above-mentioned base substrate was burnt till 1400～1580 ℃ of insulations in 1～3 hour.
Table 1 has been listed 95 porcelain of the present invention's preparation and various main performances and the firing temperature of GB (GB-5593-85) 95 porcelain.
Table 2 has been listed the performance data of 90,95 corundum porcelain balls, commercially available 90,95 porcelain balls and the Japanese import porcelain ball of the present invention's preparation.
Fig. 2 is the grain-size of 90 alumina ceramics that make of the present invention.
Fig. 3 is the grain-size of 95 alumina ceramics that make of the present invention.
95 porcelain of table 1. the present invention preparation and GB 95 porcelain Performance Ratios are
| The present invention prepares 95 porcelain | GB A95 porcelain | |
| Bulk density g/cm3Bending strength MPa linear expansion coefficient (* 10-6/ ℃) 20～500 ℃ of 20～800 ℃ of dielectric loss 1MHz (* 10-4) tangent value 10GHz (* 10-4) dielectric constant 1MHz firing temperature ℃ Al2O 3Content wt% | ＞3.70 377 7.12 7.01 2.3 5.4 3.12 1500 95 | ＞3.60 280 6.2～7.5 6.5～8.0 ≤4 ≤10 9～10 1650 95 |
The main performance index of the porcelain ball that table 2. the present invention makes
| The present invention's preparation | Commercially available | Japan's import | |||
| 90 | 95 | 90 | 95 | ||
| Alumina content wt% microhardness Hm compression strength MPa density g/cm3Wear rate g/kgh water absorption rate % crystallite dimension μ m | 88.75 ＞1800 ＞1500 ＞3.50 ＜0.16 0.23 1～6 | 95 ＞2000 ＞2000 ＞3.70 ＜0.12 0.15 1～6 | 87～90 9.0 (hardness) 〉=1500 〉=3.45 0.8 2.39- | 94～96 9.0 (hardness) 〉=2000 〉=3.60 0.7--- | — 1000 — 3.65 0.17 — 2.6 |
As can be seen from Table 1, the properties of 95 porcelain that the present invention makes reaches or is better than GB, and firing temperature is far below GB In the temperature of regulation, 1500 ℃ of the present invention burn till 95 alumina ceramics, the GB regulation then at 1650 ℃.
The properties of the Corundum Ceramics ball that as can be seen from Table 2, the present invention makes all is better than commercially available porcelain ball, particularly wear rate this generation The key index of table abrading-ball is much better than commercially available abrading-ball especially, even is better than Japanese import abrading-ball, the 90 porcelain mill loss rates that the present invention makes＜0.16g/kgh, 95 porcelain mill loss rate＜0.12g/kgh, commercially available 90 porcelain mill loss rate≤0.8g/kgh, 95 porcelain mill loss rate≤0.7g/kgh, Japan's import Ball wear rate is 0.17g/kgh.
Can find out that from Fig. 2, Fig. 3 with 90,95 porcelain that method of the present invention is prepared, its crystallite dimension is all at 1～6 μ m Between, average grain size is microstructure between 3～4 μ m.
Characteristics of the present invention are:
(1) makes no reunion sub-micron Al with commercially available low-cost raw material2O
3Powder;
(2) produce ground flux with natural minerals with low cost;
(3) low temperature fast firing makes excellent property microcrystal fused alumina porcelain;
(4) to adopt cheap natural mineral and the commercial alumina have a large capacity and a wide range be raw material in the present invention, is particularly suitable for large-scale commercial production;
(5) realize the low cost manufacturing of high-performance ceramic, solved the contradiction between the price and performance during alumina-ceramic is produced.
Embodiment 1:
(1) no reunion submicron alpha-Al
2O
3The preparation of powder
With commercially available α-Al
2O
3α-Al that powder or modification bayer's process are produced
2O
3Powder adds compound many carboxyls high molecular polymer (PAA: NH of 1wt%
4PAA=1: 1) dispersion agent, (material: ball: water=1: 2: 1) 24 hours, the pH value of regulating slip was between 6～7 to ball milling, and spraying drying makes no reunion submicron alpha-Al then
2O
3Powder.
(2) preparation of flux
(wt%) composed as follows of flux: diopside 89.4%, natural quartz 0.2% is from marble 10.4%.With above-mentioned raw materials earlier respectively ball milling cross mixing behind 200 mesh sieves, in the corundum crucible of packing into, 1200 ℃ of calcinings 1 hour, ball milling was to the ground flux of crossing 300 mesh sieves then.
(3) easy fired
Ceramic formula is (wt%): no reunion submicron alpha-Al
2O
3Powder 85%, ground flux 15%, ball milling (material: ball: water=1: 2: 1) 3 hours mixings, slip send the spray-drier drying-granulating, and cold isostatic compaction is sent into low temperature fast firing in the Si-Mo rod stove then, and 1400 ℃ of insulations promptly made the porcelain ball in 1 hour.
Embodiment 2:
(1) no reunion submicron alpha-Al
2O
3Powder, preparation method thereof is identical with embodiment one;
(2) preparation method of flux is identical with embodiment one;
(3) easy fired
Ceramic formula is (wt%): no reunion submicron alpha-Al
2O
3Powder 90%, ground flux 10%.Manufacturing process is identical with embodiment one, and firing temperature is 1450 ℃, is incubated 1 hour and makes the porcelain ball.
(4) salient features of the porcelain ball of Huo Deing
Microhardness Hm:2081
Ultimate compression strength MPa:＞1500
Density g/cm
3: 3.52
Wear rate g/kgh:0.159
Water-intake rate %:0.23
Grain-size μ m:1～6 embodiment 3:
(1) no reunion submicron alpha-Al
2O
3Powder, preparation method thereof is identical with embodiment one;
(2) preparation method of flux is identical with embodiment one;
(3) easy fired
Ceramic formula is (wt%): no reunion submicron alpha-Al
2O
3Powder 95%, ground flux 5%.Manufacturing process is identical with embodiment one, and firing temperature is 1500 ℃, is incubated 1 hour and makes the porcelain ball.
(4) salient features of the porcelain ball of Huo Deing
Microhardness Hm:2254
Ultimate compression strength MPa:＞2000
Density g/cm
3: 3.74
Wear rate g/kgh:0.113
Water-intake rate %:0.15
Grain-size μ m:1～6
Claims (1)
1. the preparation method of an alumina-ceramic uses no reunion submicron alpha-Al
2O
3Powder 85～97wt%, ground flux 3～15wt% proportioning, ball milling 3～5 hours, spray-dried granulation, axial pressure or cold isostatic compaction, 1400～1580 ℃ of insulations were burnt till in 1～3 hour, wherein: with α-Al
2O
3α-Al that powder or modification bayer's process are produced
2O
3Powder adds the dispersion agent of 0.5～1.5wt%, material: ball: water=1: 2: 1 ball milling 24 hours, and the pH value of slip is 6～7, drying makes no reunion submicron alpha-Al
2O
3Powder, its particle diameter are 0.1～1 micron, 0.5 micron of median size, and the chemical composition range of flux is: CaO
215～30wt%, MgO15～25wt%, Al
2O
30～5wt%, SiO
245～70wt%: it is by natural quartz, diopside, and rhombspar, the limestone mine raw material is made into, material: ball: water=ball milling mixed 5～10 hours in 1: 2: 1, and 1200～1400 ℃ of insulations 1～3 hour, ball milling made to crossing 300 mesh sieves then.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97109341A CN1076716C (en) | 1997-12-16 | 1997-12-16 | Process for mfg. non-lumps submicron alpha-Al2O3 powder and microlitic corundum ball |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97109341A CN1076716C (en) | 1997-12-16 | 1997-12-16 | Process for mfg. non-lumps submicron alpha-Al2O3 powder and microlitic corundum ball |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1189475A CN1189475A (en) | 1998-08-05 |
| CN1076716C true CN1076716C (en) | 2001-12-26 |
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|---|---|---|---|
| CN97109341A Expired - Fee Related CN1076716C (en) | 1997-12-16 | 1997-12-16 | Process for mfg. non-lumps submicron alpha-Al2O3 powder and microlitic corundum ball |
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Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1303180C (en) * | 2003-11-08 | 2007-03-07 | 桂林工学院 | Process for producing grinding media |
| CN1328209C (en) * | 2005-10-12 | 2007-07-25 | 中国铝业股份有限公司 | Prepn of microcrystalline alumina ceramic grain |
| CN100378002C (en) * | 2006-01-13 | 2008-04-02 | 中国科学院上海硅酸盐研究所 | Plate-like aluminum oxide granule preparation method |
| CN100374371C (en) * | 2006-09-07 | 2008-03-12 | 郑州华硕精密陶瓷有限公司 | Method of spraying granulation for preparing miropowder of silicon carbide in submicro level |
| CN100411693C (en) * | 2006-10-17 | 2008-08-20 | 山东大学 | Hydroxy apatite-base composite bioceramic material, and its preparing process |
| CA2673769C (en) | 2007-01-15 | 2012-08-21 | Saint-Gobain Ceramics & Plastics, Inc. | Ceramic particulate material and processes for forming same |
| CN101704680B (en) * | 2009-11-18 | 2012-09-05 | 中国地质大学（北京） | Submicron alumina ceramic material and preparation method thereof |
| CN101817685B (en) * | 2010-03-16 | 2013-03-06 | 山东鲲鹏新材料科技股份有限公司 | Composite precursor sol preparation method |
| CN102070165A (en) * | 2010-12-07 | 2011-05-25 | 邹平金刚新材料有限公司 | High temperature production process of alpha-aluminum oxide |
| CN102145993B (en) * | 2011-05-12 | 2013-04-24 | 安徽理工大学 | Low-temperature quick sintered high-strength aluminum oxide ceramic and preparation method thereof |
| CN103216683B (en) * | 2012-01-18 | 2016-12-21 | 醴陵科泰工程陶瓷有限公司 | A kind of production technology of FRP composite corindon earthenware and products thereof |
| CN107098367B (en) * | 2017-06-26 | 2018-06-26 | 东北林业大学 | A kind of preparation method of alumina hollow ball for vibration damping and noise reducing |
| CN109336564B (en) * | 2018-11-08 | 2020-02-11 | 娄底市安地亚斯电子陶瓷有限公司 | Preparation method of high-alumina ceramic and high-alumina ceramic prepared by using same |
| CN110642608A (en) * | 2019-10-21 | 2020-01-03 | 河南科技学院 | Wear-resistant microcrystalline alumina ceramic powder, wear-resistant microcrystalline alumina ceramic, and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1073931A (en) * | 1912-09-20 | 1913-09-23 | Grover C Royse | Concrete reinforcement. |
| US5376606A (en) * | 1993-12-30 | 1994-12-27 | Korea Institute Of Science And Technology | Light-transmissive polycrystalline alumina ceramics |
| US5382556A (en) * | 1992-04-22 | 1995-01-17 | Sumitomo Chemical Company, Limited | Translucent polycrystalline alumina and process for producing the same |
| CN1103381A (en) * | 1993-07-27 | 1995-06-07 | 住友化学工业株式会社 | Alumina composition, alumina molded article, alumina ceramics, and process for producing ceramics |
-
1997
- 1997-12-16 CN CN97109341A patent/CN1076716C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1073931A (en) * | 1912-09-20 | 1913-09-23 | Grover C Royse | Concrete reinforcement. |
| US5382556A (en) * | 1992-04-22 | 1995-01-17 | Sumitomo Chemical Company, Limited | Translucent polycrystalline alumina and process for producing the same |
| CN1103381A (en) * | 1993-07-27 | 1995-06-07 | 住友化学工业株式会社 | Alumina composition, alumina molded article, alumina ceramics, and process for producing ceramics |
| US5376606A (en) * | 1993-12-30 | 1994-12-27 | Korea Institute Of Science And Technology | Light-transmissive polycrystalline alumina ceramics |
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|---|---|
| CN1189475A (en) | 1998-08-05 |
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