CN102603273A - Preparation method of high-purity sintered alumina for monocrystal sapphire growth - Google Patents
Preparation method of high-purity sintered alumina for monocrystal sapphire growth Download PDFInfo
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- CN102603273A CN102603273A CN2012100613923A CN201210061392A CN102603273A CN 102603273 A CN102603273 A CN 102603273A CN 2012100613923 A CN2012100613923 A CN 2012100613923A CN 201210061392 A CN201210061392 A CN 201210061392A CN 102603273 A CN102603273 A CN 102603273A
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Abstract
The invention relates to a preparation method of high-purity sintered alumina for monocrystal sapphire growth, which includes the steps: using high-purity alumina as raw materials to prepare alumina granules with a granulator, placing the alumina granules into a containing crucible, and sintering the alumina granules by means of a high-frequency plasma heating device to obtain the high-purity sintered alumina. The method has the advantages that no other impurity is brought in during granulating and sintering of the high-purity alumina, and adding of binder is not needed, so that secondary pollution is avoided; by means of the high-frequency plasma heating device, equipment cost is low, production efficiency is high, and pollution of the alumina by heat insulation materials of a furnace and volatile matters of heating materials is avoided; and the bulk density of the prepared sintered alumina ranges from 3.7g/cm3 to 4.1g/cm3, the purity of the prepared sintered alumina ranges from 99.999% to 99.9999%, kyropoulos growth of monocrystal sapphires is provided with raw materials, and sapphire crystals with high quality and low defect density can be obtained.
Description
Technical field
The present invention relates to a kind of preparation method who is used for the high purity aluminium oxide sintered compact of Sapphire Crystal Growth.
Background technology
Sapphire staple is aluminum oxide (Al
2O
3), be to form with covalent bonds by three Sauerstoffatoms and two aluminium atoms, its crystalline structure is a hexagonal lattice structure, it has characteristics such as the high velocity of sound, HMP (2045 ℃), high temperature resistant, anticorrosive, high firmness, high light transmittance.And it is very wide that sapphire optics penetrates band, and irradiation all has good light transmission near ultraviolet light (190nm) to the mid-infrared light line, is widely used on optical element, infrared facility, the radium-shine lens materials of HS and the photomask materials.Lattice constant mismatch rate between sapphire C face and III-V and II-VI family deposit film is little, meets resistant to elevated temperatures requirement in gan brilliant (GaN) preparation process of heap of stone simultaneously, makes the sapphire chip become the critical material of making white/indigo plant/green light LED.
When kyropoulos is produced sapphire, use alumina powder, the filler of raw material is difficult to the welding crystal seed very little in the crucible, is unfavorable for the growing large-size crystal, and production efficiency is low; In order to improve the output of sapphire crystal, must improve the aluminum oxide tap density, with alumina powder jointed briquetting sintering, the powder initial density of briquetting is 0.3g/cm
2～0.5g/cm
2, density is 2.7g/cm behind the briquetting sintering
2～3.4g/cm
2But in traditional alumina powder jointed briquetting sintering process, the lagging material of body of heater and the volatile matter of exothermic material can pollute alumina raw material, influence the purity of alumina sintered body; Alumina sintered body purity is not enough, and foreign matter content is more, and there is lattice imperfection in sapphire crystal, and dislocation is inaccurate, and plating gallium arsenide lattice dislocation is inaccurate when causing extension processing, and the lattice match rate is low, and LED is not luminous behind the chip of making, or luminosity factor is low.
Disclose a kind of preparation method who is used for the high purity aluminium oxide sintered compact of Sapphire Crystal Growth among the CN102173756A, it adopts high purity alumina powder, ρ type alumina adhesive, and deionized water and urethane ball grind 5h, compression moulding again behind the placement 12h; The blank of compression moulding put into carry out sintering in the microwave oven.Its shortcoming is: production efficiency is low, adds ρ type alumina adhesive and deionized water and can make alumina sintered body bring secondary pollution, and adopt microwave oven to carry out sintering, and equipment cost is high.
Summary of the invention
The technical problem that the present invention will solve provides a kind of preparation method who is used for the high purity aluminium oxide sintered compact of Sapphire Crystal Growth, and this method can be avoided secondary pollution, and production efficiency is high, and equipment cost is low; The alumina sintered body that makes can be supplying raw materials of kyropoulos growing sapphire monocrystalline, can obtain the quality height, the sapphire crystal of fabricating low-defect-density.
Technical solution of the present invention is:
A kind of preparation method who is used for the high purity aluminium oxide sintered compact of Sapphire Crystal Growth, its concrete steps are:
1, high purity aluminium oxide granulation
With the high purity aluminium oxide is raw material, described high purity aluminium oxide purity>=99.999%, the content F e of impurity＜0.0006%, Si＜0.0005%, Zr＜0.0001%, Cu＜0.0001%, K＜0.0001%, Na＜0.0001%; Use tablets press to prepare particle diameter and be 1mm～6mm, density is 2.0g/cm
3～3.0g/cm
3Alumina particle, described tablets press and raw material contact component all adopt 99.99% alumina sintering ceramic structure or the outer 99.99% aluminum oxide coating layer structure that applies of steel core;
2, alumina particle sintering
The ceramic crucible of the alumina sintering with 99.99% or the crucible that applies 99.99% aluminum oxide coating layer are as the charge crucible; The alumina particle that makes is put in the charge crucible; Make the alumina particle in the crucible be warming up to 1850 ℃～2100 ℃ to the alumina particle sintering through the high frequency plasma heating unit, sintering time is 30min～50min, stops heating; The crucible naturally cooling, obtaining purity is 99.999%～99.9999% high purity aluminium oxide sintered compact.
The preparation method of the above-mentioned high purity aluminium oxide sintered compact that is used for Sapphire Crystal Growth, described high purity aluminium oxide granulation and alumina particle sintering are to carry out at the dust-free workshop of cleaning requirements more than 1000, guarantee not introduce other impurity in the production process.
The preparation method of the above-mentioned high purity aluminium oxide sintered compact that is used for Sapphire Crystal Growth, described charge crucible is placed in the water jacketed copper crucible, and the copper coil of high frequency plasma heating unit is equipped with in the water jacketed copper crucible top.
The preparation method of the above-mentioned high purity aluminium oxide sintered compact that is used for Sapphire Crystal Growth, the diameter of described water jacketed copper crucible is 20cm～45cm, highly is 50cm～80cm, is made up of 30～65 distinguish, distinguish is divided into 2～4 zones.
The preparation method of the above-mentioned high purity aluminium oxide sintered compact that is used for Sapphire Crystal Growth, the copper coil material of said high frequency plasma heating unit is a red copper, the number of turn of copper coil is 1 circle～3 circles.
The preparation method of the above-mentioned high purity aluminium oxide sintered compact that is used for Sapphire Crystal Growth is in sintering process, with the deionized water cooling copper coil of specific conductivity≤1.5 μ S/cm.
The preparation method of the above-mentioned high purity aluminium oxide sintered compact that is used for Sapphire Crystal Growth, the high frequency electric source frequency of said high frequency plasma heating unit is 600KHz～800KHz, peak power is 40kw～45kw.
The preparation method of the above-mentioned high purity aluminium oxide sintered compact that is used for Sapphire Crystal Growth, the polyethylene plastic bag packing is adopted in the raw material turnover, prevents in circular flow, to receive packing material and external pollution.
The invention has the beneficial effects as follows:
1, tablets press and raw material contact component, charge crucible all adopt 99.99% alumina sintering ceramic structure or the outer 99.99% aluminum oxide coating layer structure that applies of steel core; Guarantee not introduce other impurity in granulation, the sintering process; Need not add sticker, avoid secondary pollution.
2, adopt the high frequency plasma heating unit, equipment cost is low, and production efficiency is high, and the volatile matter of lagging material and exothermic material of having avoided body of heater is to the pollution of aluminum oxide.
3, the alumina sintered body tap density that makes is 3.7g/cm
3～4.1g/cm
3, purity is 99.999%～99.9999%, supplies raw materials for kyropoulos growing sapphire monocrystalline, can obtain sapphire crystal high-quality, fabricating low-defect-density.
Description of drawings
Fig. 1 is the scheme of installation of the present invention the charge crucible, cold-crucible and the high frequency plasma heating unit copper coil that use;
Fig. 2 is the schematic circuit diagram of high frequency plasma heating unit.
Among the figure: 1-copper coil, 2-charge crucible, 3-water jacketed copper crucible, 4-high frequency electric source, 5-plasma generator.
Embodiment
Whole process of production is all in the dust-free workshop of cleaning requirements more than 1000, to carry out.
Get 30kg purity and be 99.999% high purity aluminium oxide (the content F e of impurity＜0.0006%, Si0.0005%, Zr＜0.0001%, Cu＜0.0001%, K＜0.0001%, Na＜0.0001%); The high purity aluminium oxide powder is added in the tablets press, and tablets press is all adopting the ceramic structure of 99.99% alumina sintering with the raw material contact component, and making particle diameter is between 1mm～6mm, and density is 2.6g/cm
3, purity is 99.9996% alumina particle, packs with polyethylene plastic bag.
Like Fig. 1, shown in Figure 2; Get the alumina particle that 3kg makes and be put in the charge crucible 2 that internal diameter is 225mm * 340mm, charge crucible 2 is that charge crucible 2 is placed in the water jacketed copper crucible 3 by the ceramic crucible of 99.99% alumina sintering; The copper coil 1 of high frequency plasma heating unit is housed on water jacketed copper crucible 3; The high frequency plasma heating unit is made up of high frequency electric source 4, plasma generator 5 and copper coil 1, and wherein, the material of copper coil 1 is a red copper; The number of turn is 3 circles, and adopting specific conductivity is the deionized water cooling copper coil 1 of 1.4 μ S/cm; The diameter of water jacketed copper crucible 3 is 30cm, highly is 70cm, is made up of 65 distinguish, is divided into four zones, and each zone has a water-in and a water outlet respectively, and each distinguish all is by the water inlet of inwall one side, outer wall one side water outlet; Fill up alumina particle, build bell, connect high frequency electric source 4; The frequency of high frequency electric source 4 is 600KHz, power is transferred to 45kw alumina particle is heated, when temperature is 1850 ℃; Constant temperature 30min carries out the alumina particle sintering, closes high frequency electric source 4, the crucible naturally cooling; Get the high purity aluminium oxide sintered compact, density is 3.9g/cm
3, the purity that adopts laser ablation and ICP-MS coupling to detect alumina sintered body is 99.9996%.
The high purity aluminium oxide sintered compact that employing makes is a raw material, uses the long crystalline substance of kyropoulos single crystal growing furnace, gets the water white transparency sapphire crystal, and the dislocation density of lattice is 574/cm
2, the index of products obtained therefrom meets the technological standard of LED substrate slice.
Embodiment 2
Whole process of production is all in the dust-free workshop of cleaning requirements more than 1000, to carry out.
Get 30kg purity and be 99.999% high purity aluminium oxide (the content F e of impurity＜0.0006%, Si0.0005%, Zr＜0.0001%, Cu＜0.0001%, K＜0.0001%, Na＜0.0001%); The high purity aluminium oxide powder is added granulation in the tablets press, and making particle diameter is 1mm～6mm, and density is 2.0g/cm
3, purity is 99.9993% alumina particle, packs with polyethylene plastic bag.
Getting the alumina particle that 3kg makes is put in the charge crucible 2 that internal diameter is 225mm * 340mm; Charge crucible 2 is the ceramic crucibles by 99.99% alumina sintering; Charge crucible 2 is placed in the water jacketed copper crucible 3, and the copper coil 1 of high frequency plasma heating unit is housed on water jacketed copper crucible 3, and the high frequency plasma heating unit is made up of high frequency electric source 4, plasma generator 5 and copper coil 1; Wherein, The material of copper coil 1 is a red copper, and the number of turn of copper coil 1 is 2 circles, and adopting specific conductivity is the deionized water cooling copper coil 1 of 1.3 μ S/cm; The diameter of water jacketed copper crucible 3 is 30cm, highly is 70cm, is made up of 48 distinguish, is divided into three zones, and each zone has a water-in and a water outlet respectively, and each distinguish all is by the water inlet of inwall one side, outer wall one side water outlet; Fill up alumina particle, build bell, connect high frequency electric source 4; The frequency of high frequency electric source 4 is 700KHz, power is transferred to 42kw alumina particle is heated, when temperature is 2000 ℃; Constant temperature 40min carries out the alumina particle sintering, closes high frequency electric source 4, the crucible naturally cooling; Obtain the high purity aluminium oxide sintered compact, density is 3.7g/cm
3, the purity that adopts laser ablation and ICP-MS coupling to detect alumina sintered body is 99.9993%.
The high purity aluminium oxide sintered compact that employing makes is a raw material, uses the long crystalline substance of kyropoulos single crystal growing furnace, gets the water white transparency sapphire crystal, and the dislocation density of lattice is 604/cm
2, the index of products obtained therefrom meets the technological standard of LED substrate slice.
Embodiment 3
Whole process of production is all in the dust-free workshop of cleaning requirements more than 1000, to carry out.
Get 30kg purity and be 99.999% high purity aluminium oxide (the content F e of impurity＜0.0006%, Si0.0005%, Zr＜0.0001%, Cu＜0.0001%, K＜0.0001%, Na＜0.0001%); The high purity aluminium oxide powder is added in the tablets press, and making particle diameter is 1mm～6mm, and density is 3.0g/cm
3, purity is 99.9997% alumina particle, packs with polyethylene plastic bag.
The alumina particle that 3kg is made is put in the charge crucible 2 that internal diameter is 225mm * 340mm; Charge crucible 2 is the ceramic crucibles by 99.99% alumina sintering; Charge crucible 2 is placed in the water jacketed copper crucible 3, and the copper coil 1 of high frequency plasma heating unit is housed on water jacketed copper crucible 3, and the high frequency plasma heating unit is made up of high frequency electric source 4, plasma generator 5, copper coil 1; Wherein, The material of copper coil 1 is a red copper, and the number of turn of copper coil 1 is 1 circle, and adopting specific conductivity is the deionized water cooling copper coil 1 of 1.2 μ S/cm; The diameter of water jacketed copper crucible 3 is 45cm, highly is 80cm, is made up of 30 distinguish, is divided into two zones, and each zone has a water-in and a water outlet respectively, and each distinguish all is by the water inlet of inwall one side, outer wall one side water outlet; Fill up alumina particle, build bell, connect high frequency electric source 4; The frequency of high frequency electric source 4 is 800KHz, power is transferred to 40kw alumina particle is heated, when temperature is 2100 ℃; Constant temperature 50min carries out the alumina particle sintering, closes high frequency electric source 4, the crucible naturally cooling; Obtain the high purity aluminium oxide sintered compact, density is 4.0g/cm
3, the purity that adopts laser ablation and ICP-MS coupling to detect alumina sintered body is 99.9997%.
The high purity aluminium oxide sintered compact that employing makes is a raw material, uses the long crystalline substance of kyropoulos single crystal growing furnace, gets the water white transparency sapphire crystal, and the dislocation density of lattice is 524/cm
2, the index of products obtained therefrom meets the technological standard of LED substrate slice.
The charge crucible is the quartz crucible of surface-coated 99.99% aluminum oxide coating layer, and other is with embodiment 1～embodiment 3.
Claims (8)
1. preparation method who is used for the high purity aluminium oxide sintered compact of Sapphire Crystal Growth is characterized in that:
1.1 high purity aluminium oxide granulation
With the high purity aluminium oxide is raw material, described high purity aluminium oxide purity>=99.999%, the content F e of impurity＜0.0006%, Si＜0.0005%, Zr＜0.0001%, Cu＜0.0001%, K＜0.0001%, Na＜0.0001%; Use tablets press to prepare particle diameter and be 1mm～6mm, density is 2.0g/cm
3～3.0g/cm
3Alumina particle, described tablets press and raw material contact component all adopt 99.99% alumina sintering ceramic structure or the outer 99.99% aluminum oxide coating layer structure that applies of steel core;
1.2 alumina particle sintering
The ceramic crucible of the alumina sintering with 99.99% or the crucible that applies 99.99% aluminum oxide coating layer are as the charge crucible; The alumina particle that makes is put in the charge crucible; Make the alumina particle in the crucible be warming up to 1850 ℃～2100 ℃ to the alumina particle sintering through the high frequency plasma heating unit, sintering time is 30min～50min, stops heating; The crucible naturally cooling, obtaining purity is 99.999%～99.9999% high purity aluminium oxide sintered compact.
2. the preparation method who is used for the high purity aluminium oxide sintered compact of Sapphire Crystal Growth according to claim 1; It is characterized in that: described high purity aluminium oxide granulation and alumina particle sintering are to carry out at the dust-free workshop of cleaning requirements more than 1000, to guarantee not introduce other impurity in the production process.
3. the preparation method who is used for the high purity aluminium oxide sintered compact of Sapphire Crystal Growth according to claim 1; It is characterized in that: described charge crucible is placed in the water jacketed copper crucible, and the copper coil of high frequency plasma heating unit is equipped with in described water jacketed copper crucible top.
4. the preparation method who is used for the high purity aluminium oxide sintered compact of Sapphire Crystal Growth according to claim 1; It is characterized in that: the diameter of described water jacketed copper crucible is 20cm～45cm; Highly be 50cm～80cm, form that distinguish is divided into 2～4 zones by 30～65 distinguish.
5. the preparation method who is used for the high purity aluminium oxide sintered compact of Sapphire Crystal Growth according to claim 1 is characterized in that: the copper coil material of said high frequency plasma heating unit is a red copper, and the number of turn of copper coil is 1 circle～3 circles.
6. the preparation method who is used for the high purity aluminium oxide sintered compact of Sapphire Crystal Growth according to claim 1 is characterized in that: in sintering process, with the deionized water cooling copper coil of specific conductivity below 1.5 μ S/cm.
7. the preparation method who is used for the high purity aluminium oxide sintered compact of Sapphire Crystal Growth according to claim 1 is characterized in that: the high frequency electric source frequency of said high frequency plasma heating unit is 600KHz～800KHz, and peak power is 40kw～45kw.
8. the preparation method who is used for the high purity aluminium oxide sintered compact of Sapphire Crystal Growth according to claim 1 is characterized in that: the polyethylene plastic bag packing is adopted in the raw material turnover, prevents in circular flow, to receive packing material and external pollution.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103643290A (en) * | 2013-12-02 | 2014-03-19 | 昆明理工大学 | Method for purifying high-purity alumina for sapphire crystals |
| CN103691948A (en) * | 2013-12-25 | 2014-04-02 | 山东晶鑫晶体科技有限公司 | Device and method for machining high-density aluminum oxide by plasma |
| 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 |
| CN104321472A (en) * | 2012-05-28 | 2015-01-28 | 住友化学株式会社 | Starting material alumina for production of sapphire single crystal and method for producing sapphire single crystal |
| CN104651936A (en) * | 2015-02-06 | 2015-05-27 | 蚌埠诺德科技有限公司 | Raw material formula of dopant sapphire crystal |
| CN105777079A (en) * | 2016-01-28 | 2016-07-20 | 深圳市商德先进陶瓷有限公司 | Plasma etching resistant ceramic body and manufacturing method thereof, and plasma etching device |
| CN107324816A (en) * | 2017-07-25 | 2017-11-07 | 云南省科学技术院 | The preparation method and Preparation equipment of a kind of high temperature resistant high purity aluminium oxide cotton |
| CN107829132A (en) * | 2017-10-10 | 2018-03-23 | 上海应用技术大学 | A kind of method for preparing alumina single crystal |
| CN110592671A (en) * | 2019-10-15 | 2019-12-20 | 赵伟轩 | Preparation method of film-coating-grade alpha-high-purity alumina polycrystalline particles |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104321472A (en) * | 2012-05-28 | 2015-01-28 | 住友化学株式会社 | Starting material alumina for production of sapphire single crystal and method for producing sapphire single crystal |
| CN103643290A (en) * | 2013-12-02 | 2014-03-19 | 昆明理工大学 | Method for purifying high-purity alumina for sapphire crystals |
| CN103643290B (en) * | 2013-12-02 | 2016-03-30 | 昆明理工大学 | Method for purifying high-purity alumina for sapphire crystals |
| CN103691948A (en) * | 2013-12-25 | 2014-04-02 | 山东晶鑫晶体科技有限公司 | Device and method for machining high-density aluminum oxide by plasma |
| 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 |
| CN104651936A (en) * | 2015-02-06 | 2015-05-27 | 蚌埠诺德科技有限公司 | Raw material formula of dopant sapphire crystal |
| CN105777079A (en) * | 2016-01-28 | 2016-07-20 | 深圳市商德先进陶瓷有限公司 | Plasma etching resistant ceramic body and manufacturing method thereof, and plasma etching device |
| CN105777079B (en) * | 2016-01-28 | 2019-02-01 | 深圳市商德先进陶瓷股份有限公司 | Resistant to plasma etches ceramic body and its manufacturing method, plasma etching equipment |
| CN107324816A (en) * | 2017-07-25 | 2017-11-07 | 云南省科学技术院 | The preparation method and Preparation equipment of a kind of high temperature resistant high purity aluminium oxide cotton |
| CN107829132A (en) * | 2017-10-10 | 2018-03-23 | 上海应用技术大学 | A kind of method for preparing alumina single crystal |
| CN110592671A (en) * | 2019-10-15 | 2019-12-20 | 赵伟轩 | Preparation method of film-coating-grade alpha-high-purity alumina polycrystalline particles |
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