CN103184518A - Treatment method for sapphire raw materials - Google Patents
Treatment method for sapphire raw materials Download PDFInfo
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- CN103184518A CN103184518A CN2011104439584A CN201110443958A CN103184518A CN 103184518 A CN103184518 A CN 103184518A CN 2011104439584 A CN2011104439584 A CN 2011104439584A CN 201110443958 A CN201110443958 A CN 201110443958A CN 103184518 A CN103184518 A CN 103184518A
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Abstract
The invention discloses a treatment method for sapphire raw materials. The treatment method comprises the following steps of: placing alumina powder in a crucible and compacting, fully filling 10-20% of the volume of the crucible by the alumina powder, and then coating the alumina powder by an aluminium sheet; starting a high-frequency generator, heating to melt the aluminium sheet, so as to melt the alumina powder, continuously supplementing the alumina powder, ensuring adequate melting for the added alumina powder, and stopping adding the alumina powder until the melt is slightly higher than an induction coil; and insulating heat to completely fuse, then starting a lowering system, water-cooling the crucible, slowly removing the melt in the crucible out of the coil, starting to solidify and crystallize the melt, finally forming polycrystalline alumina, and mechanically cutting off the impurity-enriched part at the top of the polycrystalline alumina. With the adoption of the treatment method disclosed by the invention, high-purity and high-compactness alumina polycrystalline materials can be obtained, and the existing requirements on raw materials for growing large-size sapphire crystals can be met; and moreover, the treatment method is simple and practicable, low in cost, and capable of being applied in a large scale.
Description
Technical field
The present invention relates to a kind for the treatment of process of sapphire raw material, specifically, relate to a kind of method of utilizing the cold crucible smelting technique to handle the sapphire raw material.
Background technology
The cold crucible smelting technique, be powder stock to be placed on be right after in the copper tube that is arranged in round aecidioid, copper tube places in the ruhmkorff coil, lead to high-frequency current in coil, produce alternating electromagnetic field, alternating electromagnetic field can produce a high-frequency vortex on the raw material surface, and the joule heating that eddy current produces makes the raw material fusing, and the logical water coolant of outer copper tube and base is taken away heat, makes shell form the not molten Al of one deck
2O
3Duricrust is to eliminate crucible to the pollution of melt.
The used raw material of kyropoulos growing sapphire adopts α-Al usually at present
2O
3The crystal block material of powder and flame method growth.Not only the cost high yield is low for the crystal block material of flame method, and size is very big, be difficult to make its compacting, big space has appearred in when filling with substance, usually need to adopt other forms filling spaces therebetween of powder or powder, and impurities may form bubble in the briquetting material that powder and powder are prepared, particulate material in heat-processed, so that influences yield rate and the quality of sapphire raw material.
Sapphire is generally more than the 6N the requirement of material purity, and 6N purity just can reach commercial requirement.Therefore, industry is thirsted for the treatment process of a kind of high-purity alpha-alumina of research and development, and the purity sapphire crystal that grows tall of making a living provides possibility.
Summary of the invention
At the problems referred to above and the demand that prior art exists, the purpose of this invention is to provide a kind for the treatment of process of sapphire raw material, to satisfy the requirement of growth high purity sapphire crystal.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind for the treatment of process of sapphire raw material comprises the steps:
A) aluminum oxide powder is put into crucible and compacting, made its volume that fills up crucible 10～20%, use aluminium flake coated aluminum oxide powder then;
B) ruhmkorff coil that is looped around around the sidewall of crucible is linked to each other with radio-frequency generator, start radio-frequency generator then, heating makes the aluminium flake fusing, so that aluminum oxide powder begins fusing, supplemental aluminium powder continuously, the aluminum oxide powder that assurance is added is fully melted, and stops to add the oxidation aluminium powder during a little more than the ruhmkorff coil height up to melt height;
C) insulation makes complete fusion, starts the decline system then, cold-crucible, melt slowly leaves coil in the crucible, and melt begins solidification and crystallization, finally forms polycrystal alumina, its top impurity enriched part of mechanically cutting namely obtains high purity high-compactness aluminum oxide polycrystal material.
In the step a) mass ratio of the aluminum oxide powder of used aluminium flake and coating be recommended as 0.03: 1～0.045: 1.
Described crucible is recommended as copper crucible.
The power of described radio-frequency generator is recommended as 100～500KW, frequency is recommended as 0.5～10MHz.
The present invention adopts the three-phase alternating current electrical network to supply with voltage 380V, frequency 50Hz.By powder heating, fusing, constant temperature and the directional freeze crystallization of ruhmkorff coil to needing fusion that has induction heating function.Need fusing by the original powder that defines much amounts, select size, the frequency generator of crucible, weight and ruhmkorff coil and the bath surface position etc. of the metal that ignites, to reach best heat condition.
Al
2O
3The powder fusion needs about 2323K, produces high like this temperature, and only heating means are the higher frequency electromagnetic field heating that utilize radio-frequency generator to produce.But only work to electrical conductor in the higher frequency electromagnetic field, and Al
2O
3Powder is dielectric substance at normal temperatures, only just is transformed into electrical conductor under molten state.As long as at Al
2O
3The temperature that occurs a point in the powder surpasses 2323K, therefore at Al
2O
3Add the amount of metallic aluminum sheet in the powder, the melting process of metallic aluminium be to finish by the energy of absorbing high-frequency field.Higher frequency electromagnetic field heating of metal aluminium reaches temperature of fusion, and this temperature can make the Al around the metallic aluminium
2O
3Powder surpasses the 2323K fusing and forms electrical conductor, these Al
2O
3At once by the higher frequency electromagnetic field heat temperature raising and make around Al
2O
3Powder becomes electrical conductor, just can make all Al thus
2O
3The pruinescence fusing.
Be K, Na, Si, the Ca with big segregation coefficient because of the major impurity element in the aluminum oxide powder, therefore, compared with prior art, the present invention adopts the cold crucible smelting technique, utilize unidirectional solidification/segregation purification principle, have positive effect, can obtain high purity high-compactness aluminum oxide polycrystal material, can satisfy present growing large-size sapphire crystal to the requirement of raw material; And treatment process is simple, cost is low, but mass-producing is used.
Embodiment
The present invention is described in further detail and completely below in conjunction with embodiment.
Embodiment 1
A) aluminum oxide powder of 8Kg is put into the copper crucible compacting that diameter is 400mm, made its volume that fills up crucible 10～20%, with the aluminium flake coated aluminum oxide powder of 250g;
B) radio-frequency generator that to make the ruhmkorff coil that is looped around around the sidewall of crucible be 500KW with power, be operated in 0.9MHz links to each other, start radio-frequency generator then, heating makes the aluminium flake fusing, so that aluminum oxide powder begins fusing, supplemental aluminium powder continuously, the aluminum oxide powder that assurance is added is fully melted, and stops to add the oxidation aluminium powder during a little more than the ruhmkorff coil height up to melt height;
C) insulation makes complete fusion, starts the decline system then, and melt slowly leaves coil in the cold-crucible, crucible, and melt begins solidification and crystallization, finally forms polycrystal alumina, and its top impurity enriched part of mechanically cutting namely obtains high purity high dense aluminum oxide polycrystal material.
The analysis showed that purity＞99.996% of the aluminum oxide polycrystal material after the processing, density＞3.7g/cm
3
Embodiment 2
A) aluminum oxide powder of 10Kg is put into the copper crucible compacting that diameter is 500mm, made its volume that fills up crucible 10～20%, with the aluminium flake coated aluminum oxide powder of 300g;
B) radio-frequency generator that to make the ruhmkorff coil that is looped around around the sidewall of crucible be 300KW with power, be operated in 1.2MHz links to each other, start radio-frequency generator then, heating makes the aluminium flake fusing, so that aluminum oxide powder begins fusing, supplemental aluminium powder continuously, the aluminum oxide powder that assurance is added is fully melted, and stops to add the oxidation aluminium powder during near the ruhmkorff coil height up to melt height;
C) insulation makes complete fusion, starts the decline system then, and melt slowly leaves coil in the cold-crucible, crucible, and melt begins solidification and crystallization, finally forms polycrystal alumina, and its top impurity enriched part of mechanically cutting namely obtains high purity high dense aluminum oxide polycrystal material.
The analysis showed that purity＞99.996% of the aluminum oxide polycrystal material after the processing, density＞3.7g/cm
3
In sum as seen, the present invention adopts the cold crucible smelting technique, utilizes unidirectional solidification/segregation purification principle, has positive effect, can obtain high purity high-compactness aluminum oxide polycrystal material, can satisfy present growing large-size sapphire crystal to the requirement of raw material; And treatment process is simple, cost is low, but mass-producing is used.
Be necessary at last to be pointed out that at this: above content only is used for the present invention is described in further detail; can not be interpreted as limiting the scope of the invention, some nonessential improvement and adjustment that those skilled in the art makes according to foregoing all belong to protection scope of the present invention.
Claims (4)
1. the treatment process of a sapphire raw material is characterized in that, comprises the steps:
A) aluminum oxide powder is put into crucible and compacting, made its volume that fills up crucible 10～20%, use aluminium flake coated aluminum oxide powder then;
B) ruhmkorff coil that is looped around around the sidewall of crucible is linked to each other with radio-frequency generator, start radio-frequency generator then, heating makes the aluminium flake fusing, so that aluminum oxide powder begins fusing, supplemental aluminium powder continuously, the aluminum oxide powder that assurance is added is fully melted, and stops to add the oxidation aluminium powder during a little more than the ruhmkorff coil height up to melt height;
C) insulation makes complete fusion, starts the decline system then, cold-crucible, melt slowly leaves coil in the crucible, and melt begins solidification and crystallization, finally forms polycrystal alumina, its top impurity enriched part of mechanically cutting namely obtains high purity high-compactness aluminum oxide polycrystal material.
2. the treatment process of sapphire raw material according to claim 1 is characterized in that: the mass ratio of the aluminum oxide powder of used aluminium flake and coating is 0.03: 1～0.045: 1 in the step a).
3. the treatment process of sapphire raw material according to claim 1, it is characterized in that: described crucible is copper crucible.
4. the treatment process of sapphire raw material according to claim 1, it is characterized in that: the power of described radio-frequency generator is 100～500KW, frequency 0.5～10MHz.
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| CN2011104439584A CN103184518A (en) | 2011-12-27 | 2011-12-27 | Treatment method for sapphire raw materials |
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| CN2011104439584A CN103184518A (en) | 2011-12-27 | 2011-12-27 | Treatment method for sapphire raw materials |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103614774A (en) * | 2013-12-13 | 2014-03-05 | 东莞市精研粉体科技有限公司 | Preparation method of doping raw material used for growing sapphire single crystal through pulling method or edge-defined film-fed method |
| CN103628130A (en) * | 2013-12-13 | 2014-03-12 | 东莞市精研粉体科技有限公司 | Cold crucible smelting device capable of realizing continuous crystal pulling |
| CN104195630A (en) * | 2014-09-23 | 2014-12-10 | 成都冠禹科技有限公司 | Production method of high-purity alumina polycrystalline |
| CN104790034A (en) * | 2015-02-16 | 2015-07-22 | 青海圣诺光电科技有限公司 | Alumina polycrystal preparation method |
| CN106676624A (en) * | 2017-03-31 | 2017-05-17 | 宁夏佳晶科技有限公司 | Guide mode processing method for flaky sapphire |
| CN107502951A (en) * | 2017-10-18 | 2017-12-22 | 睿为电子材料（天津）有限公司 | The process of the floated cold crucible high purity aluminum oxide polycrystal body of graphite |
| CN107557857A (en) * | 2017-10-18 | 2018-01-09 | 睿为电子材料（天津）有限公司 | The sloping casting system and method for high purity aluminium oxide polycrystalline ingot are prepared for cold crucible |
| CN107747127A (en) * | 2017-10-31 | 2018-03-02 | 鄂尔多斯市达瑞祥光电科技有限公司 | A kind of large scale Al2O3The preparation method of polycrystal |
| CN112126985A (en) * | 2020-07-10 | 2020-12-25 | 新疆三锐佰德新材料有限公司 | Method and device for physically purifying high-purity aluminum oxide material for sapphire |
| CN117904707A (en) * | 2024-03-15 | 2024-04-19 | 北京铭镓半导体有限公司 | Crystal growth method for reducing gallium oxide Luan Jing quantity |
Citations (1)
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| CN101913636A (en) * | 2010-08-20 | 2010-12-15 | 李振亚 | Method for producing high-purity high-density alumina block material for sapphire single crystals |
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Patent Citations (1)
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| CN101913636A (en) * | 2010-08-20 | 2010-12-15 | 李振亚 | Method for producing high-purity high-density alumina block material for sapphire single crystals |
Non-Patent Citations (1)
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| 何雪梅等: "《宝石人工合成技术》", 31 January 2005, article "冷坩埚熔壳法合成立方氧化锆晶体工艺", pages: 153 - 3 * |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103628130A (en) * | 2013-12-13 | 2014-03-12 | 东莞市精研粉体科技有限公司 | Cold crucible smelting device capable of realizing continuous crystal pulling |
| CN103628130B (en) * | 2013-12-13 | 2015-12-02 | 东莞市精研粉体科技有限公司 | A kind of Cold Crucible Melting device realizing continuous crystal-pulling |
| CN103614774B (en) * | 2013-12-13 | 2016-06-15 | 东莞市精研粉体科技有限公司 | The preparation method growing the doped raw material of gem monocrystalline for czochralski method or EFG technique |
| CN103614774A (en) * | 2013-12-13 | 2014-03-05 | 东莞市精研粉体科技有限公司 | Preparation method of doping raw material used for growing sapphire single crystal through pulling method or edge-defined film-fed method |
| CN104195630A (en) * | 2014-09-23 | 2014-12-10 | 成都冠禹科技有限公司 | Production method of high-purity alumina polycrystalline |
| CN104790034B (en) * | 2015-02-16 | 2017-10-31 | 刘冠华 | A kind of method for preparing aluminum oxide polycrystal body |
| CN104790034A (en) * | 2015-02-16 | 2015-07-22 | 青海圣诺光电科技有限公司 | Alumina polycrystal preparation method |
| CN106676624A (en) * | 2017-03-31 | 2017-05-17 | 宁夏佳晶科技有限公司 | Guide mode processing method for flaky sapphire |
| CN106676624B (en) * | 2017-03-31 | 2019-01-29 | 宁夏佳晶科技有限公司 | A kind of guided mode processing method of flaky sapphire |
| CN107502951A (en) * | 2017-10-18 | 2017-12-22 | 睿为电子材料（天津）有限公司 | The process of the floated cold crucible high purity aluminum oxide polycrystal body of graphite |
| CN107557857A (en) * | 2017-10-18 | 2018-01-09 | 睿为电子材料（天津）有限公司 | The sloping casting system and method for high purity aluminium oxide polycrystalline ingot are prepared for cold crucible |
| CN107557857B (en) * | 2017-10-18 | 2024-04-19 | 睿为电子材料（天津）有限公司 | Oblique casting system and method for preparing high-purity alumina polycrystalline ingot by using cold crucible |
| CN107747127A (en) * | 2017-10-31 | 2018-03-02 | 鄂尔多斯市达瑞祥光电科技有限公司 | A kind of large scale Al2O3The preparation method of polycrystal |
| CN112126985A (en) * | 2020-07-10 | 2020-12-25 | 新疆三锐佰德新材料有限公司 | Method and device for physically purifying high-purity aluminum oxide material for sapphire |
| CN117904707A (en) * | 2024-03-15 | 2024-04-19 | 北京铭镓半导体有限公司 | Crystal growth method for reducing gallium oxide Luan Jing quantity |
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Application publication date: 20130703 |