CN103101949B - Preparation method of alpha-AL2O3 polishing powder - Google Patents
Preparation method of alpha-AL2O3 polishing powder Download PDFInfo
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- CN103101949B CN103101949B CN201110356901.0A CN201110356901A CN103101949B CN 103101949 B CN103101949 B CN 103101949B CN 201110356901 A CN201110356901 A CN 201110356901A CN 103101949 B CN103101949 B CN 103101949B
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- powder
- polishing powder
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- coacervate
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Abstract
The invention discloses a preparation method of alpha-Al2O3 polishing powder. The method comprises: (a) crystallizing raw material Al(OH)3 powder by using an oversaturation and rapid crystallization method, and controlling an average size of the Al(OH)3 crystal so as to ensure the average size of the crystal is not more than 0.15 [mu]m; (b) removing sodium for the AL(OH)3 crystal, ball milling, and controlling average size of aggregates of the Al(OH)3 particles so as to ensure the average size of the aggregates is not more than 17 [mu]m; (c) loosely filling the Al(OH)3 particles into containers; and (d) putting the containers into a box heating furnace with an oxidation atmosphere at intervals. The method is beneficial in that the aggregates of the alpha-Al2O3 polishing powder are loose, good in dispersion stability in water, small in fluctuation of polishing quality and polishing efficiency, and can form stabile suspensions.
Description
Technical field
The present invention relates to a kind of α-Al
2o
3the manufacture method of polishing powder, is specifically related to a kind of α-Al for craft and half mechanical polishing polishing
2o
3the manufacture method of polishing powder.
Background technology
Existing α-the Al in market
2o
3polishing powder average crystal size fluctuation range is bigger than normal, in powder granule coacervate, intergranular sticky excessively strong.Bigger than normal between mean sizes wave zone, can cause polishing grinding time, the fluctuation of different work batch, period, polishing efficiency and quality of finish.In coacervate, adhesive power is excessively strong, can cause the erratic scratch of polished surface.Adopting wet polishing, when especially manual or half mechanical type polishing, above-mentioned weakness can make polishing fluid dispersion stabilization poor, and quality of finish and efficiency fluctuation are excessive.
Need a kind of α-Al for this reason
2o
3polishing powder, coacervate is loose, can in water, can constantly disperse through simple manual stirring, forms stable suspension.
Summary of the invention
For solving the problems of the technologies described above, the object of the present invention is to provide a kind of coacervate loose, in water, dispersion stabilization is good, forms stable suspension, quality of finish and the polishing efficiency little α-Al that fluctuates
2o
3the manufacture method of polishing powder.
For achieving the above object, technical scheme of the present invention is as follows: a kind of α-Al
2o
3the manufacture method of polishing powder, has the following step:
(a). by raw material A l (OH)
3powder adopts supersaturation rapid crystallization method to carry out crystallization, to Al (OH)
3the mean sizes of crystallization is controlled, and guarantees that its mean sizes is not more than 0.15 μ m;
(b). described Al (OH)
3crystallization, after de-sodium is processed, is carried out ball milling, to Al after ball milling (OH)
3the coacervate mean sizes of particle is controlled, and guarantees that its mean sizes is not more than 17 μ m;
(c). described Al (OH)
3packing in container of loose particles;
(d). described container interval is positioned in the box type heater of oxidizing atmosphere;
(e). described box type heater is warming up to 180-220 ℃, insulation 1-2 hour; Then with the average heating speed that is less than 30 ℃/h, furnace temperature is risen to 600 ± 30 ℃; With the average heating speed that is less than 40 ℃/h, furnace temperature is risen to 700 ± 30 ℃; With the average heating speed that is less than 50 ℃/h, furnace temperature is risen to 1290 ± 30 ℃, at 1290 ± 30 ℃ of insulation 1-5 hour, obtain α-Al
2o
3crystal grain;
(f). after insulation finishes, pass into cold wind, furnace temperature is down to 1200 ℃ of following rear Slow coolings;
(g). come out of the stove after cooling, by described α-Al
2o
3coacervate particle sieves, and controlling its mean sizes is 0.14-0.25 μ m, then will cross the α-Al being sieved
2o
3coacervate particle is packed.
Preferably, described de-sodium is treated to by Al (OH)
3slurry is put into whizzer, by clear water washing and filtering repeatedly, until sodium content is down to below 0.1%wt.
Preferably, described container is thin-walled alumina porcelain container with lid, and its volume is 1.5L, and its diameter is less than 150 ㎜.
Preferably, the spacing that place at described container interval is not less than 25 ㎜.
Adopt the beneficial effect of the technical program to be: α-Al
2o
3polishing powder coacervate is loose, and in water, dispersion stabilization is good, forms stable suspension, and quality of finish and polishing efficiency fluctuation are little.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, rather than whole embodiment.Based on the embodiment in the present invention, those of ordinary skills, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
A kind of α-Al
2o
3the manufacture method of polishing powder, has the following step:
(a). by raw material A l (OH)
3powder adopts supersaturation rapid crystallization method to carry out crystallization, to Al (OH)
3the mean sizes of crystallization is controlled, and guarantees that its mean sizes is not more than 0.15 μ m;
(b). described Al (OH)
3crystallization, after de-sodium is processed, is carried out ball milling, to Al after ball milling (OH)
3the coacervate mean sizes of particle is controlled, and guarantees that its mean sizes is not more than 17 μ m;
(c). described Al (OH)
3packing in container of loose particles;
(d). described container interval is positioned in the box type heater of oxidizing atmosphere;
(e). described box type heater is warming up to 180-220 ℃, insulation 1-2 hour, holding temperature is too high easily causes dehydration violent, causes powder to spray in container; Then with the average heating speed that is less than 30 ℃/h, furnace temperature is risen to 600 ± 30 ℃, with the average heating speed that is less than 40 ℃/h, furnace temperature is risen to 700 ± 30 ℃, this stage intensification is too fast to be caused equally powder to spray in container and may cause container to destroy; With the average heating speed that is less than 50 ℃/h, furnace temperature is risen to 1290 ± 30 ℃, at 1290 ± 30 ℃ of insulation 1-5 hour, obtain α-Al
2o
3crystal grain;
(f). after insulation finishes, pass into cold wind, furnace temperature is down to 1200 ℃ of following rear Slow coolings;
(g). come out of the stove after cooling, by described α-Al
2o
3coacervate particle sieves, and controls its Water-borne paint and is not more than 75 μ m, and average crystalline size is 0.14-0.25 μ m, then will cross the α-Al being sieved
2o
3coacervate particle is packed.
In aforesaid method, de-sodium is treated to by Al (OH)
3slurry is put into whizzer, by clear water washing and filtering repeatedly, until sodium content is down to below 0.1%wt.
In aforesaid method, container is thin-walled alumina porcelain container with lid, and its volume is 1.5L, and its diameter is less than 150 ㎜.The spacing that place at container interval is not less than 25 ㎜.
In aforesaid method, the visual batch of soaking time, charging mode and container vary in size and change, minimum should guarantee all materials all reach holding temperature and again this temperature stop more than 30 minutes.
Check raw material A l (OH)
3powder mean sizes and Al (OH)
3the method of the coacervate mean sizes of particle, random sampling product a little, point is put on slide glass, drip a small amount of glycerol dispersant, with spicule stir loose after in 40 ~ 100 × test under microscope distribution of sizes, with second slide glass by after on slide glass, liquid rolls, 1000 × microscopic examination crystalline size, have or not excessive particle.
Table 1 is the α-Al under different holding temperatures and different soaking time
2o
3:
Embodiment 1
Holding temperature is 1290 ℃, and soaking time is 5 hours, α-Al
2o
3mean sizes be 0.18 ㎜, bonding without crystal.
Embodiment 2
As shown in table 1, holding temperature is 1300 ℃, and soaking time is 30 minutes, α-Al
2o
3mean sizes be 0.1646 ㎜, bonding without crystal.
Embodiment 3
As shown in table 1, holding temperature is 1300 ℃, and soaking time is 1 hour, α-Al
2o
3mean sizes be 0.2058 ㎜, bonding without crystal.
Embodiment 4
As shown in table 1, holding temperature is 1300 ℃, and soaking time is 2 hours, α-Al
2o
3mean sizes be 0.1926 ㎜, bonding without crystal.
Embodiment 5
As shown in table 1, holding temperature is 1300 ℃, and soaking time is 3 hours, α-Al
2o
3mean sizes be 0.1968 ㎜, bonding without crystal.
Embodiment 6
As shown in table 1, holding temperature is 1300 ℃, and soaking time is 4 hours, α-Al
2o
3mean sizes be 0.1708 ㎜, bonding without crystal.
Embodiment 7
As shown in table 1, holding temperature is 1300 ℃, and soaking time is 5 hours, α-Al
2o
3mean sizes be 0.1775 ㎜, bonding without crystal.
Embodiment 8
As shown in table 1, holding temperature is 1400 ℃, and soaking time is 1 hour, α-Al
2o
3mean sizes be 0.1927 ㎜, have obvious crystal bonding.
By the data of table 1, at 1250 ℃ of following temperature calcinings of temperature, κ-Al
2o
3→ θ-Al
2o
3→ α-Al
2o
3conversion incomplete.1250 ℃ of above (containing 1250 ℃) temperature are calcined more than 30 minutes, transform completely.In the calcining of 1250-1300 ℃ of temperature, soaking time within 30 minutes-5 hour periods, α-Al
2o
3crystalline size does not produce considerable change with the variation of soaking time, and powder through hand mixing, can form stable suspension in water, and coacervate does not have obvious visible rapid subsidence, and hand polishing glass surface occurs without scratch phenomenon.Firing temperature is increased to 1350 ℃-1400 ℃, and crystalline size is grown up not obvious.But at 1350 ℃, the existing fast phenomenon of coacervate settling velocity when powder is dispersed in water; Produce obvious rapid subsidence at 1400 ℃ of coacervates, stability of suspension variation, to this powder amplifying observation under Electronic Speculum, has produced more sticky between visible crystals.
Determine that thus available holding temperature should be limited between 1250 ℃-1350 ℃.α-Al
2o
3the size ranges of crystal grain is 0.14 ~ 0.25 μ m, optimum size 0.18 μ m, coacervate is loose, can in water, can constantly disperse through simple manual stirring, form stable suspension, coacervate does not have obvious visible rapid subsidence, hand polishing glass surface, occur without scratch phenomenon, quality of finish and efficiency fluctuation are little.
Adopt the beneficial effect of the technical program to be: α-Al
2o
3polishing powder coacervate is loose, and in water, dispersion stabilization is good, forms stable suspension, and quality of finish and polishing efficiency fluctuation are little.
To the above-mentioned explanation of the disclosed embodiments, make professional and technical personnel in the field can realize or use the present invention.To be apparent for those skilled in the art to the multiple modification of these embodiment, General Principle as defined herein can, in the situation that not departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (1)
1. a α-Al
2o
3the manufacture method of polishing powder, is characterized in that, has the following step:
(a). by raw material A l (OH)
3powder adopts supersaturation rapid crystallization method to carry out crystallization, to Al (OH)
3the mean sizes of crystallization is controlled, and guarantees that its mean sizes is not more than 0.15 μ m;
(b). described Al (OH)
3crystallization, after de-sodium is processed, is carried out ball milling, to Al after ball milling (OH)
3the coacervate mean sizes of particle is controlled, and guarantees that its mean sizes is not more than 17 μ m;
(c). described Al (OH)
3packing in container of loose particles;
(d). described container interval is positioned in the box type heater of oxidizing atmosphere;
(e). described box type heater is warming up to 180-220 ℃, insulation 1-2 hour; Then with the average heating speed that is less than 30 ℃/h, furnace temperature is risen to 600 ± 30 ℃, with the average heating speed that is less than 40 ℃/h, furnace temperature is risen to 700 ± 30 ℃; With the average heating speed that is less than 50 ℃/h, furnace temperature is risen to 1290 ± 30 ℃, at 1290 ± 30 ℃ of insulation 1-5 hour, obtain α-Al
2o
3crystal grain;
(f). after insulation finishes, pass into cold wind, furnace temperature is down to 1200 ℃ of following rear Slow coolings;
(g). come out of the stove after cooling, by described α-Al
2o
3crystal coacervate particle sieves, and controls coacervate particle size≤75 μ m, α-Al
2o
3average crystalline size is 0.14-0.25 μ m, then will cross the α-Al being sieved
2o
3coacervate particle is packed.
2. a kind of α-Al according to claim 1
2o
3the manufacture method of polishing powder, is characterized in that, described de-sodium is treated to by Al (OH)
3slurry is put into whizzer, by clear water washing and filtering repeatedly, until sodium content is down to below 0.1%wt.
3. a kind of α-Al according to claim 1 and 2
2o
3the manufacture method of polishing powder, is characterized in that, described container is thin-walled alumina porcelain container with lid, and its volume is 1-1.5L, and its diameter is less than 150 ㎜.
4. a kind of α-Al according to claim 1 and 2
2o
3the manufacture method of polishing powder, is characterized in that, the spacing that place at described container interval is not less than 25 ㎜.
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|---|---|---|---|
| CN201110356901.0A CN103101949B (en) | 2011-11-11 | 2011-11-11 | Preparation method of alpha-AL2O3 polishing powder |
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|---|---|---|---|
| CN201110356901.0A CN103101949B (en) | 2011-11-11 | 2011-11-11 | Preparation method of alpha-AL2O3 polishing powder |
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| CN103101949A CN103101949A (en) | 2013-05-15 |
| CN103101949B true CN103101949B (en) | 2014-06-04 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106698489B (en) * | 2017-01-04 | 2019-03-01 | 杭州智华杰科技有限公司 | A kind of preparation method of high cutting high brightness aluminum oxide polishing powder |
| CN109439283A (en) * | 2018-11-02 | 2019-03-08 | 长沙县新光特种陶瓷有限公司 | A kind of polishing preparation method of alumina powder |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4407296A1 (en) * | 1994-03-04 | 1995-09-07 | Inst Neue Mat Gemein Gmbh | Preparation of sintered alpha alumina having microcrystalline structure |
| CN101289206A (en) * | 2008-06-12 | 2008-10-22 | 中国铝业股份有限公司 | Method for preparing thermal spraying alumina powder |
| CN101824279A (en) * | 2010-05-10 | 2010-09-08 | 上海高纳粉体技术有限公司 | High accuracy aluminum oxide polishing powder and production method thereof |
| CN102093843A (en) * | 2010-12-09 | 2011-06-15 | 中国铝业股份有限公司 | Preparation method of alpha-alumina polishing powder |
-
2011
- 2011-11-11 CN CN201110356901.0A patent/CN103101949B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4407296A1 (en) * | 1994-03-04 | 1995-09-07 | Inst Neue Mat Gemein Gmbh | Preparation of sintered alpha alumina having microcrystalline structure |
| CN101289206A (en) * | 2008-06-12 | 2008-10-22 | 中国铝业股份有限公司 | Method for preparing thermal spraying alumina powder |
| CN101824279A (en) * | 2010-05-10 | 2010-09-08 | 上海高纳粉体技术有限公司 | High accuracy aluminum oxide polishing powder and production method thereof |
| CN102093843A (en) * | 2010-12-09 | 2011-06-15 | 中国铝业股份有限公司 | Preparation method of alpha-alumina polishing powder |
Non-Patent Citations (9)
| Title |
|---|
| A.H. Heuer.Oxygen and aluminum diffusion in α-Al2O3: How much we really understand?.《Journal of the European Ceramic Society》.2008,第28卷第1459-1507页. |
| Oxygen and aluminum diffusion in α-Al2O3: How much we really understand?;A.H. Heuer;《Journal of the European Ceramic Society》;20080201;第28卷;第1459-1507页 * |
| 吴光进等.工业氢氧化铝制备高纯超细氧化铝.《贵州大学学报(自然科学版)》.2009,第26卷(第4期),第95-96页. * |
| 固相法制备片状α-Al2O3粉体及其影响因素的研究;黎少华等;《中国稀土学报》;20061031;第24卷;第310-313页 * |
| 崔香枝等.氢氧化铝热分解制备α-Al2O3纳米粉体.《耐火材料》.2006,第40卷(第5期),第353-357页. |
| 工业级氢氧化铝制备高韧性氧化铝陶瓷及机理分析;张新霓等;《人工晶体学报》;20081231;第37卷(第6期);第1425-1429页 * |
| 张新霓等.工业级氢氧化铝制备高韧性氧化铝陶瓷及机理分析.《人工晶体学报》.2008,第37卷(第6期),第1425-1429页. |
| 氢氧化铝热分解制备α-Al2O3纳米粉体;崔香枝等;《耐火材料》;20060531;第40卷(第5期);第353-357页 * |
| 黎少华等.固相法制备片状α-Al2O3粉体及其影响因素的研究.《中国稀土学报》.2006,第24卷第310-313页. |
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