CN104499051A - Single crystal corundum production method - Google Patents
Single crystal corundum production method Download PDFInfo
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- CN104499051A CN104499051A CN201410738360.1A CN201410738360A CN104499051A CN 104499051 A CN104499051 A CN 104499051A CN 201410738360 A CN201410738360 A CN 201410738360A CN 104499051 A CN104499051 A CN 104499051A
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- inhibitor
- alpha
- production method
- single alundum
- cooling
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/20—Aluminium oxides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/02—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method without using solvents
Abstract
The invention relates to a single crystal corundum production method, which comprises the following steps: grinding alpha-alumina powder to a median particle size of 1-5mu, then adding an inhibitor, smelting at a temperature of 1500-1700 DEG C after mixing uniformly, keeping stand and cooling for 8-24h after melting fully, and hydrolyzing a mixture subjected to standing and cooling to obtain single crystal corundum, wherein the mass ratio of alpha-alumina powder to inhibitor is 6-25 to 1, and the inhibitor comprises the following components in percentage by mass: 1-3% of titanium oxide, 0-2% of iron oxide and 3-7% of sulfur. The single crystal corundum production method provided by the invention has the beneficial effects that the grain size of the generated single crystal corundum is controlled, and the yield is high.
Description
Technical field
The present invention relates to single alundum technical field, particularly a kind of production method of single alundum.
Background technology
Single alundum, i.e. single crystal electrofusion aluminum oxide (having another name called 32A) abrasive material, be take bauxitic clay as main raw material, with addition of appropriate sulfide, form through high melt.In canescence or shallow khaki color, hardness is high, toughness is large.Employing special process is produced, and each granularity product are that spontaneous nucleation produces, and non-mechanical comminution result.Single alundum is the extraordinary heat-resisting high-grade abrasive substance of a kind of toughness, for making senior cutting and abrasive tool, be applicable to the grinding of the high rigidity such as high-vanadium high-speed steel, austenitic stainless steel, titanium alloy, high-toughness material, especially for dry grinding and the ground finish of yielding easy burn workpiece.
The granularity product that on existing world market, client is maximum to monocrystalline electric smelting aluminium demand mainly concentrate between F60-F120, and its consumption accounts for more than 80% of total amount.And the strong each granularity product of monocrystalline electric smelting aluminium of the good wear resistance of quality are all spontaneous nucleations, not by the method processing that macrobead is pulverized, therefore yield rate is lower.
Summary of the invention
Technical problem to be solved by this invention is: provide that a kind of yield rate is high, the production method of the controllable single alundum of spontaneous nucleation globule size.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is:
A kind of production method of single alundum, alpha-aluminium oxide powder being ground to median particle diameter is 1-5 μ, then inhibitor is added, at 1500-1900 DEG C, melting is carried out after mixing, melt fully and leave standstill cooling, the time of described standing cooling is 8-24h, standing cooled mixture is hydrolyzed, obtain single alundum, the mass ratio 6-25:1 of described alpha-aluminium oxide powder and inhibitor, described inhibitor comprises the component of following mass percent: titanium oxide 1-3%, ferric oxide 0-2% and sulphur 3-7%.
Beneficial effect of the present invention is:
(1) the production method employing median particle diameter of single alundum of the present invention is the alpha-aluminium oxide powder of 1-5 μ is principal phase powder, take inhibitor as second-phase powder, inhibitor under high melt condition can with single alundum in be about about 20% aluminum oxide form aggregate, this aggregate is the material with liquid phase resistance, thus stop aluminum oxide crystal growth, reach the object controlling crystal size size;
(2) by the control of Alpha-alumina Powder Particle Size, its powder granularity under melting condition is made to be tending towards concentrating, being uniformly distributed;
(3) by alpha-aluminium oxide powder and inhibitor (second-phase powder) control of the amount of allocating into and the control of cooling temperature, the single alundum grain size of generation is controlled further.
Embodiment
By describing technology contents of the present invention in detail, being realized object and effect, be explained below in conjunction with embodiment.
The design of most critical of the present invention is: by the design of Alpha-alumina Powder Particle Size, inhibitor composition and the proportioning between them, thus produces the controlled single alundum of grain size.
The production method of a kind of single alundum of the present invention, alpha-aluminium oxide powder being ground to median particle diameter is 1-5 μ, then inhibitor is added, at 1500-1900 DEG C, melting is carried out after mixing, melt fully and leave standstill cooling, the time of described standing cooling is 8-24h, standing cooled mixture is hydrolyzed, obtain single alundum, the mass ratio of described alpha-aluminium oxide powder and inhibitor is 6-25:1, and described inhibitor comprises the component of following mass percent: titanium oxide 1-3%, ferric oxide 0-2% and sulphur 3-7%.
From foregoing description, beneficial effect of the present invention is:
(1) the production method employing median particle diameter of single alundum of the present invention is the alpha-aluminium oxide powder of 1-5 μ is principal phase powder, take inhibitor as second-phase powder, inhibitor forms the material with liquid phase resistance under high melt condition, thus stop aluminum oxide crystal growth, reach the object controlling crystal size size;
(2) by the control of Alpha-alumina Powder Particle Size, its powder granularity under melting condition is made to be tending towards concentrating, being uniformly distributed;
(3) by alpha-aluminium oxide powder and inhibitor (second-phase powder) control of the amount of allocating into and the control of cooling temperature, the single alundum grain size of generation is controlled further.
Further, alpha-aluminium oxide powder being ground to median particle diameter is 1-2 μ, then inhibitor is added, at 1700 DEG C, carry out melting after mixing, melt fully and leave standstill cooling, the time of described standing cooling is 18-24h, standing cooled mixture is hydrolyzed, obtain single alundum, the mass ratio of described alpha-aluminium oxide powder and inhibitor is 7-10:1, and described inhibitor comprises the component of following mass percent: titanium oxide 2-3%, ferric oxide 1-2% and sulphur 6-7%.
Further, alpha-aluminium oxide powder being ground to median particle diameter is 3-5 μ, then inhibitor is added, at 1700 DEG C, carry out melting after mixing, melt fully and leave standstill cooling, the time of described standing cooling is 8-10h, standing cooled mixture is hydrolyzed, obtain single alundum, the mass ratio of described alpha-aluminium oxide powder and inhibitor is 11-24:1, and described inhibitor comprises the component of following mass percent: titanium oxide 1-2%, ferric oxide 0-1% and sulphur 3-5%.
Further, the mixture after melting is put into control mould and carry out leaving standstill cooling, described control mould is plum blossom-shaped, described control mould outer bands heating unit.
Seen from the above description, plum blossom-shaped mould can effectively increase mould specific surface area, homogeneity cooling time of material in further control mould, mixture after melting is put into control mould carry out leave standstill cooling object be: single alundum spontaneous nucleation crystal formation size is relevant to cooling time, crystal formation size was directly proportional to cooling time, cooling time, longer crystal formation was larger, thus controlled crystal formation size further.
Further, the time of described melting is 8-24h.
Embodiments of the invention one are:
The production method of a kind of single alundum of the present embodiment, alpha-aluminium oxide powder being ground to median particle diameter is 1 μ, then inhibitor is added, at 1500 DEG C, carry out melting after mixing, melt fully and leave standstill cooling, the time of described standing cooling is 8h, standing cooled mixture is hydrolyzed, obtain single alundum, the mass ratio of described alpha-aluminium oxide powder and inhibitor is 24:1, and described inhibitor comprises the component of following mass percent: titanium oxide 1% and sulphur 3%.
Embodiments of the invention two are:
The production method of a kind of single alundum of the present embodiment, alpha-aluminium oxide powder being ground to median particle diameter is 5 μ, then inhibitor is added, at 1700 DEG C, melting is carried out after mixing, melt fully and leave standstill cooling, the time of described standing cooling is 24h, standing cooled mixture is hydrolyzed, obtain single alundum, the mass ratio of described alpha-aluminium oxide powder and inhibitor is 7:1, and described inhibitor comprises the component of following mass percent: titanium oxide 3%, ferric oxide 2% and sulphur 7%.
Embodiments of the invention three are:
The production method of a kind of single alundum of the present embodiment: alpha-aluminium oxide powder being ground to median particle diameter is 3 μ, then inhibitor is added, at 1900 DEG C, melting is carried out after mixing, melt fully and leave standstill cooling, the time of described standing cooling is 15h, standing cooled mixture is hydrolyzed, obtain single alundum, the mass ratio of described alpha-aluminium oxide powder and inhibitor is 11:1, and described inhibitor comprises the component of following mass percent: titanium oxide 2%, ferric oxide 1% and sulphur 5%.
Embodiments of the invention four are:
The production method of a kind of single alundum of the present embodiment: alpha-aluminium oxide powder being ground to median particle diameter is 1-2 μ, then inhibitor is added, at 1700 DEG C, melting is carried out after mixing, melt fully and leave standstill cooling, the time of described standing cooling is 18-24h, standing cooled mixture is hydrolyzed, obtain single alundum, the mass ratio of described alpha-aluminium oxide powder and inhibitor is 7-10:1, and described inhibitor comprises the component of following mass percent: titanium oxide 2-3%, ferric oxide 1-2% and sulphur 6-7%.
Embodiments of the invention five are:
The production method of a kind of single alundum of the present embodiment: alpha-aluminium oxide powder being ground to median particle diameter is 3-5 μ, then inhibitor is added, at 1700 DEG C, melting is carried out after mixing, melt fully and leave standstill cooling, the time of described standing cooling is 8-10h, standing cooled mixture is hydrolyzed, obtain single alundum, the mass ratio of described alpha-aluminium oxide powder and inhibitor is 10-25:1, and described inhibitor comprises the component of following mass percent: titanium oxide 1-2%, ferric oxide 0-1% and sulphur 3-5%.
Embodiments of the invention six are:
Only described alpha-aluminium oxide powder is that 6:1 is different from the mass ratio of inhibitor, and all the other conditions are that embodiment one is identical.
Embodiments of the invention seven are:
Only described alpha-aluminium oxide powder is that 25:1 is different from the mass ratio of inhibitor, and all the other conditions are that embodiment one is identical.
Experimental analysis
Adopt laser particle analyzer to carry out granularity Detection to the single alundum that embodiment one to seven obtains, and calculate the natural incidence of corresponding granularity.Detected result can the spontaneous nucleation size-grade distribution table of the single alundum prepared by embodiment four shown in reference table 1, and the spontaneous nucleation size-grade distribution table of the single alundum prepared by embodiment five shown in table 2.
The spontaneous nucleation size-grade distribution table of the single alundum of table 1 prepared by embodiment four.
Table 1
| Granularity | Natural incidence % |
| +F24 | ‐ |
| F24 | 0.1 |
| F30 | 1.18 |
| F36 | 2.3 |
| F46 | 4.3 |
| F60 | 6.53 |
| F80 | 21.7 |
| F100 | 27.8 |
| F120 | 22.68 |
| F150 | 11.72 |
| F180 | 0.87 |
| F220 | 0.44 |
| －F220 | 0.38 |
| Close Meter | 100.00 |
As shown in Table 1, can be found out concentrate on effective size of grain F46-F150 in the market by above method gained single alundum major part by above data, crest, at 100 orders, effectively reduces and needs melting again cross coarsness and cross fine granularity per-cent.
The spontaneous nucleation size-grade distribution table of the single alundum of table 2 prepared by embodiment five.
Table 2
| Granularity | Natural incidence % |
| +F24 | 0.01 |
| F24 | 0.3 |
| F30 | 1.18 |
| F36 | 3.3 |
| F46 | 14.53 |
| F60 | 21.7 |
| F80 | 31.8 |
| F100 | 19.68 |
| F120 | 3.89 |
| F150 | 1.92 |
| F180 | 0.87 |
| F220 | 0.44 |
| －F220 | 0.38 |
| Close Meter | 100.00 |
As shown in Table 2, can be found out concentrate on effective size of grain F46-F120 in the market by above method single alundum major part by above data, crest, at 80 orders, effectively reduces and needs melting again cross coarsness and cross fine granularity per-cent.
In sum, the production method of single alundum provided by the invention has the single alundum grain size and the high beneficial effect of yield rate that control to generate.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every equivalents utilizing description of the present invention to do, or be directly or indirectly used in relevant technical field, be all in like manner included in scope of patent protection of the present invention.
Claims (6)
1. the production method of a single alundum, it is characterized in that, alpha-aluminium oxide powder being ground to median particle diameter is 1-5 μ, then inhibitor is added, at 1700 DEG C, melting is carried out after mixing, melt fully and leave standstill cooling, the time of described standing cooling is 8-24h, standing cooled mixture is hydrolyzed, obtain single alundum, the mass ratio of described alpha-aluminium oxide powder and inhibitor is 6-25:1, and described inhibitor comprises the component of following mass percent: titanium oxide 1-3%, ferric oxide 0-2% and sulphur 3-7%.
2. the production method of single alundum according to claim 1, it is characterized in that, alpha-aluminium oxide powder being ground to median particle diameter is 1-2 μ, then inhibitor is added, at 1700 DEG C, melting is carried out after mixing, melt fully and leave standstill cooling, the time of described standing cooling is 18-24h, standing cooled mixture is hydrolyzed, obtain single alundum, the mass ratio of described alpha-aluminium oxide powder and inhibitor is 7-10:1, and described inhibitor comprises the component of following mass percent: titanium oxide 2-3%, ferric oxide 1-2% and sulphur 6-7%.
3. the production method of single alundum according to claim 1, it is characterized in that, alpha-aluminium oxide powder being ground to median particle diameter is 3-5 μ, then inhibitor is added, at 1700 DEG C, melting is carried out after mixing, melt fully and leave standstill cooling, the time of described standing cooling is 8-10h, standing cooled mixture is hydrolyzed, obtain single alundum, the mass ratio of described alpha-aluminium oxide powder and inhibitor is 11-24:1, and described inhibitor comprises the component of following mass percent: titanium oxide 1-2%, ferric oxide 0-1% and sulphur 3-5%.
4. the production method of single alundum according to claim 1, is characterized in that, the mixture after melting is put into control mould and carries out leaving standstill cooling.
5. the production method of single alundum according to claim 1, is characterized in that, described control mould is plum blossom-shaped, described control mould outer bands heating unit.
6. the production method of single alundum according to claim 1, is characterized in that, the time of described melting is 8-24h.
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| CN201410738360.1A CN104499051B (en) | 2014-12-05 | 2014-12-05 | Single crystal corundum production method |
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| CN201410738360.1A CN104499051B (en) | 2014-12-05 | 2014-12-05 | Single crystal corundum production method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110241458A (en) * | 2019-05-24 | 2019-09-17 | 淅川正弘单晶刚玉厂 | The production method of canescence single alundum |
| CN114408954A (en) * | 2022-01-26 | 2022-04-29 | 株洲科能新材料股份有限公司 | Preparation method of single crystal alumina micro powder |
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| JPS60112700A (en) * | 1983-11-21 | 1985-06-19 | Seiko Epson Corp | Synthesizing method of corundum |
| JPS60226497A (en) * | 1984-04-19 | 1985-11-11 | Seiko Epson Corp | Production of star sapphire single crystal |
| CN1113269A (en) * | 1995-01-29 | 1995-12-13 | 陈秋生 | Method for production of single alundum |
| CN1114642A (en) * | 1994-07-08 | 1996-01-10 | 董杰 | Method for producing high-purity micro-crystal white alundum |
| CN101748486A (en) * | 2008-12-05 | 2010-06-23 | 西峡县正弘单晶刚玉厂 | Production method for blue SA (single alundum) |
| CN101906663A (en) * | 2010-08-09 | 2010-12-08 | 西峡县正弘单晶刚玉有限责任公司 | Blue ssuperindividual corundum and preparation method thereof |
| CN103359763A (en) * | 2013-07-04 | 2013-10-23 | 鸿福晶体科技(安徽)有限公司 | Chemical preparation method for spherical hollow alumina powder for producing gemstone by using flame fusion method |
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2014
- 2014-12-05 CN CN201410738360.1A patent/CN104499051B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60112700A (en) * | 1983-11-21 | 1985-06-19 | Seiko Epson Corp | Synthesizing method of corundum |
| JPS60226497A (en) * | 1984-04-19 | 1985-11-11 | Seiko Epson Corp | Production of star sapphire single crystal |
| CN1114642A (en) * | 1994-07-08 | 1996-01-10 | 董杰 | Method for producing high-purity micro-crystal white alundum |
| CN1113269A (en) * | 1995-01-29 | 1995-12-13 | 陈秋生 | Method for production of single alundum |
| CN101748486A (en) * | 2008-12-05 | 2010-06-23 | 西峡县正弘单晶刚玉厂 | Production method for blue SA (single alundum) |
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| CN103359763A (en) * | 2013-07-04 | 2013-10-23 | 鸿福晶体科技(安徽)有限公司 | Chemical preparation method for spherical hollow alumina powder for producing gemstone by using flame fusion method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110241458A (en) * | 2019-05-24 | 2019-09-17 | 淅川正弘单晶刚玉厂 | The production method of canescence single alundum |
| CN114408954A (en) * | 2022-01-26 | 2022-04-29 | 株洲科能新材料股份有限公司 | Preparation method of single crystal alumina micro powder |
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