CN103101949A - Preparation method of alpha-AL2O3 polishing powder - Google Patents
Preparation method of alpha-AL2O3 polishing powder Download PDFInfo
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- CN103101949A CN103101949A CN2011103569010A CN201110356901A CN103101949A CN 103101949 A CN103101949 A CN 103101949A CN 2011103569010 A CN2011103569010 A CN 2011103569010A CN 201110356901 A CN201110356901 A CN 201110356901A CN 103101949 A CN103101949 A CN 103101949A
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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 the manufacture method of a kind of α-AL2O3 polishing powder, be specifically related to the manufacture method of a kind of α for craft and half mechanical polishing polishing-AL2O3 polishing powder.
Background technology
The existing α in market-AL2O3 polishing powder average crystal size fluctuation range is bigger than normal, and is in the powder granule coacervate, intergranular sticking excessively strong.Bigger than normal between the mean sizes wave zone, in the time of can causing polishing grinding, 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, during especially manual or half mechanical type polishing, above-mentioned weakness can make the polishing fluid dispersion stabilization poor, and quality of finish and efficient fluctuation are excessive.
Need a kind of α-AL2O3 polishing powder, coacervate is loose for this reason, can constantly disperse through simple manual stirring in water, 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, dispersion stabilization is good in water, forms stable suspension, the manufacture method of the little α of quality of finish and polishing efficiency fluctuation-AL2O3 polishing powder.
For achieving the above object, technical scheme of the present invention is as follows: the manufacture method of a kind of α-AL2O3 polishing powder has the following step:
(a). adopt supersaturation rapid crystallization method to carry out crystallization raw material A L (OH) 3 powders, the mean sizes of AL (OH) 3 crystallizations is controlled, guarantee that its mean sizes is not more than 0.15 μ m;
(b). described AL (OH) 3 crystallizations are carried out ball milling, to AL(OH after ball milling after taking off sodium and processing) the coacervate mean sizes of 3 particles controls, and guarantees that its mean sizes is not more than 17 μ m;
(c). described AL(OH) in the container of packing into of 3 loose particles;
(d). described container interval is positioned in the box type heater of oxidizing atmosphere;
(e). described process furnace is warming up to 180-220 ℃, is incubated 1-2 hour; Then with the average heating speed less than 30 ℃/hour, furnace temperature is risen to 600 ± 30 ℃; With the average heating speed less than 40 ℃/hour, furnace temperature is risen to 700 ± 30 ℃; With the average heating speed less than 50 ℃/hour, furnace temperature is risen to 1290 ± 30 ℃, 1290 ± 30 ℃ of insulations 1-5 hour, obtain α-AL2O3 crystal grain;
(f). insulation passes into cold wind after finishing, and furnace temperature is down to rear slow cooling below 1200 ℃;
(g). come out of the stove after cooling, described α-AL2O3 coacervate particle is sieved, controlling its mean sizes is 0.14-0.25 μ m, and the α that then mistake is sieved-AL2O3 coacervate particle is packed.
Preferably, the described sodium that takes off is treated to AL (OH) 3 slurries is put into whizzer, repeatedly rushes filter with clear water, 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 of described container interval placement is not less than 25 ㎜.
Adopt the beneficial effect of the technical program to be: α-AL2O3 polishing powder coacervate is loose, and dispersion stabilization is good in water, forms stable suspension, and quality of finish and polishing efficiency fluctuation are little.
Embodiment
The below is clearly and completely described the technical scheme in the embodiment of the present invention, and 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 belong to the scope of protection of the invention not making the every other embodiment that obtains under the creative work prerequisite.
The manufacture method of a kind of α-AL2O3 polishing powder has the following step:
(a). adopt supersaturation rapid crystallization method to carry out crystallization raw material A L (OH) 3 powders, the mean sizes of AL (OH) 3 crystallizations is controlled, guarantee that its mean sizes is not more than 0.15 μ m;
(b). described AL (OH) 3 crystallizations are carried out ball milling, to AL(OH after ball milling after taking off sodium and processing) the coacervate mean sizes of 3 particles controls, and guarantees that its mean sizes is not more than 17 μ m;
(c). described AL(OH) in the container of packing into of 3 loose particles;
(d). described container interval is positioned in the box type heater of oxidizing atmosphere;
(e). described process furnace is warming up to 180-220 ℃, is incubated 1-2 hour, and holding temperature is too high easily causes dehydration violent, causes powder to spray in container; Then with the average heating speed less than 30 ℃/hour, furnace temperature is risen to 600 ± 30 ℃, with the average heating speed less than 40 ℃/hour, 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 less than 50 ℃/hour, furnace temperature is risen to 1290 ± 30 ℃, 1290 ± 30 ℃ of insulations 1-5 hour, obtain α-AL2O3 crystal grain;
(f). insulation passes into cold wind after finishing, and furnace temperature is down to rear slow cooling below 1200 ℃;
(g). come out of the stove after cooling, described α-AL2O3 coacervate particle is sieved, control its Water-borne paint and be not more than 75 μ m, average crystalline size is 0.14-0.25 μ m, and the α that then mistake is sieved-AL2O3 coacervate particle is packed.
In aforesaid method, take off sodium and be treated to AL (OH) 3 slurries are put into whizzer, repeatedly rush filter with clear water, 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 the 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) 3 powder mean sizes and AL(OH) method of the coacervate mean sizes of 3 particles, the 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 * the test under microscope distribution of sizes, with second slide glass with after on slide glass, liquid rolls, 1000 * the microscopic examination crystalline size, have or not excessive particle.
Table 1 is the α-AL2O3 under different holding temperatures and different soaking time:
| 1 ℃ of holding temperature | 2 ℃ of holding temperatures | Soaking time ∑ min | Crystal formation | Average crystalline size (micron) | Crystal is bonding |
| 1000 | - | 60 | κ-AL2O3θ-AL2O3α-AL2O3 | - | Nothing |
| 1100 | - | 30 | κ-AL2O3θ-AL2O3α-AL2O3 | - | Nothing |
| 1150 | - | 30 | θ-AL2O3α-AL2O3 | 0.1078 | Nothing |
| 1150 | 1200 | 60 | θ-AL2O3α-AL2O3 | 0.1275 | Nothing |
| 1250 | - | 30 | α-AL2O3 | 0.1428 | Nothing |
| 1300 | - | 30 | α-AL2O3 | 0.1646 | Nothing |
| 1300 | - | 60 | α-AL2O3 | 0.2058 | Nothing |
| 1300 | - | 120 | α-AL2O3 | 0.1926 | Nothing |
| 1300 | - | 180 | α-AL2O3 | 0.1968 | Nothing |
| 1300 | - | 240 | α-AL2O3 | 0.1708 | Nothing |
| 1300 | - | 300 | α-AL2O3 | 0.1775 | Nothing |
| 1350 | - | 60 | α-AL2O3 | 0.1851 | Little |
| 1400 | - | 60 | α-AL2O3 | 0.1927 | Obviously |
Embodiment 1
Holding temperature is 1290 ℃, and soaking time is 5 hours, and the mean sizes of α-AL2O3 is 0.18 ㎜, and is bonding without crystal.
Embodiment 2
As shown in table 1, holding temperature is 1300 ℃, and soaking time is 30 minutes, and the mean sizes of α-AL2O3 is 0.1646 ㎜, and is bonding without crystal.
Embodiment 3
As shown in table 1, holding temperature is 1300 ℃, and soaking time is 1 hour, and the mean sizes of α-AL2O3 is 0.2058 ㎜, and is bonding without crystal.
Embodiment 4
As shown in table 1, holding temperature is 1300 ℃, and soaking time is 2 hours, and the mean sizes of α-AL2O3 is 0.1926 ㎜, and is bonding without crystal.
Embodiment 5
As shown in table 1, holding temperature is 1300 ℃, and soaking time is 3 hours, and the mean sizes of α-AL2O3 is 0.1968 ㎜, and is bonding without crystal.
Embodiment 6
As shown in table 1, holding temperature is 1300 ℃, and soaking time is 4 hours, and the mean sizes of α-AL2O3 is 0.1708 ㎜, and is bonding without crystal.
Embodiment 7
As shown in table 1, holding temperature is 1300 ℃, and soaking time is 5 hours, and the mean sizes of α-AL2O3 is 0.1775 ㎜, and is bonding without crystal.
Embodiment 8
As shown in table 1, holding temperature is 1400 ℃, and soaking time is 1 hour, and the mean sizes of α-AL2O3 is 0.1927 ㎜, has obvious crystal bonding.
By the data of table 1,1250 ℃ of following temperature calcinings of temperature, the conversion of κ-AL2O3 → θ-AL2O3 → α-AL2O3 is incomplete.Temperature was calcined more than 30 minutes (to contain 1250 ℃) more than 1250 ℃, transformed fully.1250-1300 ℃ of temperature calcining, soaking time is within 30 minutes-5 hour periods, α-AL2O3 crystalline size does not produce considerable change with the variation of soaking time, powder in water through hand mixing, can form stable suspension, coacervate does not have obvious visible rapid subsidence, and the hand polishing glass surface occurs without the 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, the stability of suspension variation to this powder amplifying observation under Electronic Speculum, has produced more sticking between visible crystals.
Determine that thus available holding temperature should be limited between 1250 ℃-1350 ℃.The size ranges of α-AL2O3 crystal grain is 0.14 ~ 0.25 μ m, optimum size 0.18 μ m, coacervate is loose, can can constantly disperse through simple manual stirring in water, form stable suspension, coacervate does not have obvious visible rapid subsidence, hand polishing glass surface, occur without the scratch phenomenon, quality of finish and efficient fluctuation are little.
Adopt the beneficial effect of the technical program to be: α-AL2O3 polishing powder coacervate is loose, and dispersion stabilization is good in water, forms stable suspension, and quality of finish and polishing efficiency fluctuation are little.
To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be apparent concerning those skilled in the art, and General Principle as defined herein can be in the situation that do not break away from the spirit or scope of the present invention, realization 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 (4)
1. the manufacture method of α-AL2O3 polishing powder is characterized in that having the following step:
(a). adopt supersaturation rapid crystallization method to carry out crystallization raw material A L (OH) 3 powders, the mean sizes of AL (OH) 3 crystallizations is controlled, guarantee that its mean sizes is not more than 0.15 μ m;
(b). described AL (OH) 3 crystallizations are carried out ball milling, to AL(OH after ball milling after taking off sodium and processing) the coacervate mean sizes of 3 particles controls, and guarantees that its mean sizes is not more than 17 μ m;
(c). described AL(OH) in the container of packing into of 3 loose particles;
(d). described container interval is positioned in the box type heater of oxidizing atmosphere;
(e). described process furnace is warming up to 180-220 ℃, is incubated 1-2 hour; Then with the average heating speed less than 30 ℃/hour, furnace temperature is risen to 600 ± 30 ℃, with the average heating speed less than 40 ℃/hour, furnace temperature is risen to 700 ± 30 ℃; With the average heating speed less than 50 ℃/hour, furnace temperature is risen to 1290 ± 30 ℃, 1290 ± 30 ℃ of insulations 1-5 hour, obtain α-AL2O3 crystal grain;
(f). insulation passes into cold wind after finishing, and furnace temperature is down to rear slow cooling below 1200 ℃;
(g). come out of the stove after cooling, described α-AL2O3 crystal coacervate particle is sieved, control coacervate particle size≤75 μ m.α-AL2O3 average crystalline size is 0.14-0.25 μ m, and the α that then mistake is sieved-AL2O3 coacervate particle is packed.
2. the manufacture method of a kind of α according to claim 1-AL2O3 polishing powder, is characterized in that, the described sodium that takes off is treated to AL (OH) 3 slurries is put into whizzer, repeatedly rushes filter with clear water, until sodium content is down to below 0.1%wt.
3. the manufacture method of a kind of α according to claim 1 and 2-AL2O3 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. the manufacture method of a kind of α according to claim 1 and 2-AL2O3 polishing powder, is characterized in that, the spacing of described container interval placement is not less than 25 ㎜.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106698489A (en) * | 2017-01-04 | 2017-05-24 | 杭州智华杰科技有限公司 | Preparation method of high-cutting and high-brightness alumina 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 |
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Patent Citations (4)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106698489A (en) * | 2017-01-04 | 2017-05-24 | 杭州智华杰科技有限公司 | Preparation method of high-cutting and high-brightness alumina 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 |
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