CN102603273B - 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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- CN102603273B CN102603273B CN 201210061392 CN201210061392A CN102603273B CN 102603273 B CN102603273 B CN 102603273B CN 201210061392 CN201210061392 CN 201210061392 CN 201210061392 A CN201210061392 A CN 201210061392A CN 102603273 B CN102603273 B CN 102603273B
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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 of the sintered compact of the high purity aluminium oxide for Sapphire Crystal Growth.
Background technology
Sapphire main component is aluminum oxide (Al
2o
3), be to be formed with covalent bonds by three Sauerstoffatoms and two aluminium atoms, its crystalline structure is hexagonal lattice structure, it has the characteristics such as the high velocity of sound, high-melting-point (2045 ℃), high temperature resistant, anticorrosive, high rigidity, high light transmittance.And it is very wide that sapphire optics penetrates band, irradiate and all there is good light transmission near ultraviolet light (190nm) to the mid-infrared light line, be widely used on optical element, infrared facility, the radium-shine lens materials of high strength and 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, in crucible, the filler of raw material very little, is difficult to the welding crystal seed, 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, by alumina powder jointed briquetting sintering, the powder initial density of briquetting is 0.3g/cm
2~0.5g/cm
2, after the briquetting sintering, density is 2.7g/cm
2~3.4g/cm
2.But, 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, affect the purity of alumina sintered body; Alumina sintered body purity is inadequate, and foreign matter content is more, and there is lattice imperfection in sapphire crystal, and dislocation is inaccurate, and when causing extension processing, plating gallium arsenide lattice dislocation is inaccurate, and the lattice match rate is low, and after the chip of making, LED is not luminous, or luminosity factor is low.
Disclose a kind of preparation method of the sintered compact of the high purity aluminium oxide for Sapphire Crystal Growth in CN102173756A, it adopts high purity alumina powder, ρ type alumina adhesive, and deionized water and urethane ball grind 5h, compression moulding again after placement 12h; The blank of compression moulding is put in microwave oven and carried out sintering.Its shortcoming is: production efficiency is low, adds ρ type alumina adhesive and deionized water can make alumina sintered body bring secondary pollution, and adopts microwave oven to carry out sintering, and equipment cost is high.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of the sintered compact of the high purity aluminium oxide for Sapphire Crystal Growth, and the method can be avoided secondary pollution, and production efficiency is high, and equipment cost is low; The alumina sintered body made can be supplying raw materials of kyropoulos growing sapphire monocrystalline, can obtain quality high, the sapphire crystal of fabricating low-defect-density.
Technical solution of the present invention is:
A kind of preparation method of the sintered compact of the high purity aluminium oxide for Sapphire Crystal Growth, its concrete steps are:
1, high purity aluminium oxide granulation
Take high purity aluminium oxide as 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%; Preparing particle diameter with tablets press is 1mm~6mm, and 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 made is put in the charge crucible, by the high frequency plasma heating unit, make the alumina particle in crucible be warming up to 1850 ℃~2100 ℃ to the alumina particle sintering, sintering time is 30min~50min, stop 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 sintered compact of the high purity aluminium oxide for Sapphire Crystal Growth, described high purity aluminium oxide granulation and alumina particle sintering are that the dust-free workshop more than 1000 carries out in cleaning requirements, guarantee not introduce other impurity in production process.
The preparation method of the above-mentioned sintered compact of the high purity aluminium oxide for Sapphire Crystal Growth, described charge crucible is placed in 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 sintered compact of the high purity aluminium oxide for Sapphire Crystal Growth, the diameter of described water jacketed copper crucible is 20cm~45cm, is highly 50cm~80cm, 30~65 distinguish, consists of, distinguish is divided into 2~4 zones.
The preparation method of the above-mentioned sintered compact of the high purity aluminium oxide for Sapphire Crystal Growth, the copper coil material of described high frequency plasma heating unit is red copper, the number of turn of copper coil is 1 circle~3 circles.
The preparation method of the above-mentioned sintered compact of the high purity aluminium oxide for Sapphire Crystal Growth, in sintering process, with the cooling copper coil of deionized water of specific conductivity≤1.5 μ S/cm.
The preparation method of the above-mentioned sintered compact of the high purity aluminium oxide for Sapphire Crystal Growth, the high frequency electric source frequency of described high frequency plasma heating unit is 600KHz~800KHz, peak power is 40kw~45kw.
The preparation method of the above-mentioned sintered compact of the high purity aluminium oxide for Sapphire Crystal Growth, the raw material turnover adopts the polyethylene plastic bag packing, prevents from being subject to packing material and extraneous pollution in circular flow.
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, sintering process; do not need to add binding agent, avoided secondary pollution.
2, adopt the high frequency plasma heating unit, equipment cost is low, and production efficiency is high, has avoided the pollution of the volatile matter of the lagging material of body of heater and exothermic material to aluminum oxide.
3, the alumina sintered body tap density made is 3.7g/cm
3~4.1g/cm
3, purity is 99.999%~99.9999%, for kyropoulos growing sapphire monocrystalline, supplies raw materials, and can obtain sapphire crystal high-quality, fabricating low-defect-density.
The accompanying drawing explanation
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.
In figure: 1-copper coil, 2-charge crucible, 3-water jacketed copper crucible, 4-high frequency electric source, 5-plasma generator.
Embodiment
Whole production process is all in cleaning requirements, in the dust-free workshop more than 1000, to carry out.
The 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%) that to get 30kg purity be 99.999%; The high purity aluminium oxide powder is added in 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, the alumina particle that purity is 99.9996%, packed with polyethylene plastic bag.
As shown in Figure 1 and Figure 2, 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 crucible by 99.99% alumina sintering, charge crucible 2 is placed in water jacketed copper crucible 3, 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 comprised of high frequency electric source 4, plasma generator 5 and copper coil 1, wherein, the material of copper coil 1 is red copper, the number of turn is 3 circles, adopts the cooling copper coil 1 of deionized water that specific conductivity is 1.4 μ S/cm; The diameter of water jacketed copper crucible 3 is 30cm, is highly 70cm, 65 distinguish, consists of, and is divided into four zones, and there are respectively a water-in and a water outlet in each zone, and each distinguish is by inwall one side water inlet, 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, obtain 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 raw material, uses the long crystalline substance of kyropoulos single crystal growing furnace, obtains 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 production process is all in cleaning requirements, in the dust-free workshop more than 1000, to carry out.
The 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%) that to get 30kg purity be 99.999%; The high purity aluminium oxide powder is added to granulation in tablets press, and making particle diameter is 1mm~6mm, and density is 2.0g/cm
3, the alumina particle that purity is 99.9993%, packed 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 water jacketed copper crucible 3, 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 comprised of high frequency electric source 4, plasma generator 5 and copper coil 1, wherein, the material of copper coil 1 is red copper, the number of turn of copper coil 1 is 2 circles, adopts the cooling copper coil 1 of deionized water that specific conductivity is 1.3 μ S/cm; The diameter of water jacketed copper crucible 3 is 30cm, is highly 70cm, 48 distinguish, consists of, and is divided into three zones, and there are respectively a water-in and a water outlet in each zone, and each distinguish is by inwall one side water inlet, 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 raw material, uses the long crystalline substance of kyropoulos single crystal growing furnace, obtains 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 production process is all in cleaning requirements, in the dust-free workshop more than 1000, to carry out.
The 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%) that to get 30kg purity be 99.999%; The high purity aluminium oxide powder is added in tablets press, and making particle diameter is 1mm~6mm, and density is 3.0g/cm
3, the alumina particle that purity is 99.9997%, packed 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 water jacketed copper crucible 3, 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 comprised of high frequency electric source 4, plasma generator 5, copper coil 1, wherein, the material of copper coil 1 is red copper, the number of turn of copper coil 1 is 1 circle, adopts the cooling copper coil 1 of deionized water that specific conductivity is 1.2 μ S/cm; The diameter of water jacketed copper crucible 3 is 45cm, is highly 80cm, 30 distinguish, consists of, and is divided into Two Areas, and there are respectively a water-in and a water outlet in each zone, and each distinguish is by inwall one side water inlet, 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 raw material, uses the long crystalline substance of kyropoulos single crystal growing furnace, obtains 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 the other the same as in Example 1~embodiment 3.
Claims (3)
1. the preparation method of the sintered compact of the high purity aluminium oxide for Sapphire Crystal Growth is characterized in that:
1.1 high purity aluminium oxide granulation
Take high purity aluminium oxide as 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%; Preparing particle diameter with tablets press is 1mm~6mm, and 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 made is put in the charge crucible, described charge crucible is placed in water jacketed copper crucible, and the copper coil of high frequency plasma heating unit is equipped with in described water jacketed copper crucible top; The diameter of described water jacketed copper crucible is 20cm~45cm, is highly 50cm~80cm, 30~65 distinguish, consists of, and distinguish is divided into 2~4 zones; By the high frequency plasma heating unit, make the alumina particle in crucible be warming up to 1850 ℃~2100 ℃ to the alumina particle sintering, the high frequency electric source frequency of described high frequency plasma heating unit is 600kHz~800kHz, peak power is 40kW~45kW, sintering time is 30min~50min, stop heating, the crucible naturally cooling, obtaining purity is 99.999%~99.9999% high purity aluminium oxide sintered compact.
2. the preparation method of the sintered compact of the high purity aluminium oxide for Sapphire Crystal Growth according to claim 1, it is characterized in that: the copper coil material of described high frequency plasma heating unit is red copper, the number of turn of copper coil is 1 circle~3 circles.
3. the preparation method of the sintered compact of the high purity aluminium oxide for 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.
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JP2013245149A (en) * | 2012-05-28 | 2013-12-09 | Sumitomo Chemical Co Ltd | Raw material alumina for producing sapphire single crystal and method for producing the sapphire single crystal |
CN103643290B (en) * | 2013-12-02 | 2016-03-30 | 昆明理工大学 | Method for purifying high-purity alumina for sapphire crystals |
CN103691948B (en) * | 2013-12-25 | 2015-06-17 | 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 |
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 |
CN110592671B (en) * | 2019-10-15 | 2022-09-27 | 赵伟轩 | Preparation method of film-coating-grade alpha-high-purity alumina polycrystalline particles |
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CN101205628A (en) * | 2006-12-18 | 2008-06-25 | 庄育丰 | Sapphire crystal growth method |
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 |
CN102173756A (en) * | 2011-01-30 | 2011-09-07 | 河北恒博精细陶瓷材料有限公司 | Preparation method of high-purity aluminum oxide sintered body for growing sapphire crystal |
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RU2554196C2 (en) * | 2010-03-09 | 2015-06-27 | Сумитомо Кемикал Компани, Лимитед | ALUMINIUM α-OXIDE FOR OBTAINING SAPPHIRE MONOCRYSTAL AND METHOD OF OBTAINING THEREOF |
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CN101205628A (en) * | 2006-12-18 | 2008-06-25 | 庄育丰 | Sapphire crystal growth method |
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 |
CN102173756A (en) * | 2011-01-30 | 2011-09-07 | 河北恒博精细陶瓷材料有限公司 | Preparation method of high-purity aluminum oxide sintered body for growing sapphire crystal |
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