CN102011184B - Production method of alpha-aluminum oxide single crystal - Google Patents
Production method of alpha-aluminum oxide single crystal Download PDFInfo
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Abstract
The invention belongs to the technical field of preparation method of synthetic sapphire crystals, particularly relates to a production method of an alpha-aluminum oxide single crystal. The production method of the alpha-aluminum oxide single crystal, producing large-diameter single crystals, specifically comprises steps of adding raw materials, inserting seed crystal and sintering the crystal, the step of sintering the crystal is divided into melting crystal, expanding centre and crystal and growing in constant diameter; the raw material is delta-Al203 or gamma-Al203, the seed crystal for the step of inserting seed crystal is in M axis 90-degree crystal orientation or A axis 75-degree crystal orientation, oxyhydrogen flame proportion for sintering the crystal is 3.7-4.2:1, and flame temperature is 2085-2090 DEG C. outside diameter of the single crystal produced by the method is phi42mm-phi45mm, and total length L thereof is 80mm-95mm, so that the single crystal can be used in the industrial fields of microwave dielectric materials, waveguide lasers, high-precision bearing elements and devices, large-scale integrated electronic circuit board and the like.
Description
Technical field
The invention belongs to preparation method's technical field of synthetic sapphire crystal, particularly the production method of α-aluminum oxide single crystal.
Background technology
The single crystal traditional processing technology is: adopt δ-Al
2O
3Or γ-Al
2O
3Aluminum oxide powder is as raw material, and crystal seed is 90 ° of crystal orientation of M axle or 75 ° of crystal orientation of A axle, oxyhydrogen ratio 2.9~3.6: 1,2030~2080 ℃ of flame temperatures are knocked 45~75 times/min of blanking frequency, single discharge quantity 0.8~1.2g, degrowth speed 8~20mm/h, growth total time 12h.The single crystal growth diameter that adopts this manufacturing process to make is less, and is most of at φ 20mm~φ 40mm, seldom can reach the above large diameter single crystal of φ 42mm.Therefore limiting single crystal in the application in the fields such as industry, national defence, electronics always.
Summary of the invention
Technical problem to be solved by this invention provides a kind of production method of α-aluminum oxide single crystal, and the α that this production method makes-aluminum oxide single crystal diameter is large.
The production method of α-aluminum oxide single crystal of the present invention comprises adding raw material, slotting crystal seed, sintering crystal step that the sintering crystal is divided into the material crystallization, center, crystal are enlarged and isodiametric growth; Described raw material is δ-Al
2O
3Or γ-Al
2O
3, inserting the used crystal seed of crystal seed is 90 ° of crystal orientation of M axle or 75 ° of crystal orientation of A axle, and the oxyhydrogen flame ratio is 3.7~4.2: 1 during the sintering crystal, and flame temperature is 2085~2090 ℃.
Further, raw material is preferably purity more than 99.995%, particle diameter 1.9 μ m~3.0 μ m, density 1.14~1.86g/m
3δ-Al
2O
3Aluminum oxide powder.
Adding the used screen cloth loading hopper of raw material is 140~200 orders.
Insert crystal seed: crystal seed vertically inserts a growth end center, the crown.The molten brilliant termination of crystal seed is just needing four directions four, can not defectiveness.
Sintering crystal: utilize oxyhydrogen flame high temperature melting Al in the sintering burner hearth
2O
3Powder, and crystallization grows single crystal on crystal seed.The major diameter crystal is larger to the heat absorption rate of temperature field, is 3.7~4.2: 1 so the present invention regulates the hydrogen-oxygen ratio of temperature field, and flame temperature is 2085~2090 ℃.
The material crystallization: fusing crystal seed hair is white, shinny, in the blanking crystallization of crystal seed top, knocks 10~25 beats/mins of frequencies, single blanking amount 1.6~2.2g.
To the center: in the material crystallization, crystal seed is aimed at flame and plate cutting center, centering time 8~10 seconds/crystallization kind.
Crystal enlarges: need control to drip and tie up oxygen speed, strengthen oxygen flow, according to the crystal growth conditions, the control discharge quantity cooperates with the effective of degrowth speed, and crystal diameter is grown up.Preferably, drip dimension oxygen speed 0.5~10 second/drip; Dropping material knocks frequency: 40~50 times/min, and single blanking amount 1.6~2.2g; Degrowth speed 2~5mm/h.
During isodiametric growth, dropping material knocks 55~80 times/min of frequency, single blanking amount 1.6~2.2g, degrowth speed 5~10mm/h, the dimension of dripping oxygen speed: 16~20 seconds/drip.The control speed of growth and blanking amount make crystal upwards be the parallel upright growth.
The blowing out cooling: close blanking system, descending system, oxyhydrogen flame, crystal leaves standstill cooling in stove; Cooling 90~120min.The caloric receptivity of major diameter crystal is larger, and the present invention has prolonged the cooling time of crystal.
Take out crystal after the cooling without the special process requirement.
The crystal that the present invention obtains is complete single structure, belongs to hexagonal system, and symmetry class is heavy trilateral scalenohedron crystal, and its lattice is comprised of the oxonium ion of divalence and the Chrome ion of trivalent.α-aluminum oxide single crystal that the present invention obtains, its outside diameter: φ 42mm~φ 45mm, total length L=80mm~95mm.Increase the Application Areas of synthetic sapphire, can be applied to the industrial circles such as microwave dielectric material, waveguide laser, high degree of accuracy bearing components and parts, large-scale integrated electronic circuit board, guided missile and satellite reception window.
Embodiment
Flame method of the present invention prepares major diameter α-Al
2O
3The technical process of single crystal is: add raw material → insert a crystal seed → oxyhydrogen flame sintering → cleaning sintering oven → material crystallization → center → crystal expansion → isodiametric growth → blowing out is cooled off → taken out single crystal, specifically may further comprise the steps:
1, raw material adds: purge the charging hopper with gas blower inner, Al
2O
3Powder is poured in 140~200 eye mesh screen loading hoppers, adds a cover the isolation dust.
2, insert crystal seed: the crystal seed in 90 ° of crystal orientation of M axle or 75 ° of crystal orientation of A axle;
3, some oxyhydrogen flame: light oxyhydrogen flame, the hydrogen-oxygen ratio of regulating flame is 3.7~4.2: 1,2085~2090 ℃ of flame temperatures;
4, cleaning sintering oven: use dedicated cleaning tool, in inboard wall of burner hearth moving gently on every side, bonding impurity is dropped;
5, material crystallization: start electro-magnet and knock hammer, knock hopper guide bar and carry out blanking, in the crystallization of crystal seed top; Dropping material knocks 15~20 beats/mins of frequencies, single discharge quantity: 1.6~2.2g;
6, to the center: mainly be that crystal seed is aimed at flame and plate cutting center; Centering time 8~10 seconds/crystallization kind;
7, crystal enlarges: control is dripped and is tieed up oxygen speed, strengthens oxygen flow, 10 growths of sintering unit head, and oxygen flow is total up to: 15~25m
3/ H.According to the crystal growth conditions, the control discharge quantity cooperates with the effective of degrowth speed; The dimension of dripping oxygen speed is from fast to slow: 0.5~10 second/drip; Dropping material knocks frequency: 40~50 beats/mins; Degrowth speed 2~5mm/h;
8, isodiametric growth: mainly be that degrowth speed, dropping material are knocked frequency, drip and tie up the control of oxygen speed; Crystal is normal when isometrical, degrowth speed: 5~10mm/h; Dropping material knocks frequency: 55~80 beats/mins of (single blanking amounts 1.6~2.2g); The dimension of dripping oxygen speed: 16~20 seconds/drip; Oxygen flow is constant to be about: 25 ± 1m
3/ H;
9, blowing out cooling: close the oxyhydrogen valve; Crystal cooling time is 90~120min;
10, take out crystal: without the special process requirement.
Embodiment 1
Prepare: a growth head selecting sinter machine; Get test δ-Al ready
2O
3Powder, median size are 2.1 μ m.Make 180 eye mesh screens of charging hopper.
Cleaning: purge the charging hopper with gas blower inner.
Charging: δ-Al
2O
3Powder is poured in the 180 eye mesh screen loading hoppers, adds a cover the isolation dust.
Insert crystal seed: the crystal seed in 75 ° of crystal orientation of A axle is vertically inserted a growth top end; When selecting crystal seed, the molten brilliant termination of crystal seed just is being required to be four directions four, the crystal orientation defective can not be arranged, otherwise can exert an influence to its light refraction.
1), igniting, regulating the qi flowing in the channels sintering crystal:: light oxyhydrogen flame, regulate the ratio 3.7: 1 of oxyhydrogen gas just commonly used, 2085 ℃ of flame temperatures.
2), material crystallization: start electro-magnet and knock hammer, knock hopper guide bar and carry out blanking, in the crystallization of crystal seed top; The dropping material that slows down knocks frequency: 20 times/min, and single discharge quantity: 1.6~2.2g.Concentrate at the center of blanking, and single blanking amount is normal.
3), to center (flame kernel, powder center): in blanking simultaneously, slight, a quick travel growth head is aimed at its flame kernel, plate cutting center, so that powder is in the crystallization of crystal seed upper end.
4), crystal enlarges: 10 growths of sintering unit head, oxygen flow is total up to: 15m
3/ H.Afterwards, the dimension oxygen speed of dripping becomes: 0.5~10 second/drip; Dropping material knocks frequency: 40~50 beats/mins, and single discharge quantity: 1.6~2.2g; Degrowth speed 2~5mm/h; Crystal has the sign of obvious expansion, and crystal edge is outwards upheld.Whole crystal expansion process required time is 80~90min.
5), isodiametric growth: the slowing down dimension oxygen speed to 16~20 seconds/drip of dripping, improve dropping material and knock frequency to 60 time/min, single discharge quantity: 1.6~2.2g accelerates degrowth speed to 5~8mm/h; Make crystal upwards be the parallel upright growth.2085 ℃ of oxyhydrogen flame kernel temperature.Whole isodiametric growth process required time is 8~9h.
6), blowing out cooling: stop blanking, close the oxyhydrogen valve, stop to descend; Take out crystal behind the non-shock chilling.
The crystal that obtains does not have split across, and is excellent, diameter ф 42mm, total length 75mm.
The appraising datum of crystal is as follows:
Fusing point: the crystal melting temperature is 2085 ℃; Boiling point: the crystal gasification temperature is 3500 ℃; Density: 3.98g/cm
3Hardness of crystals: 9 grades of Mohs;
Crystal color: be micro white (near transparent), average transmittance can reach more than 92%;
Resistance: in the time of 1231 ℃, be 1 megaohm; Resistivity: in the time of 500 ℃, 10
11Ohm/cm; In the time of 1000 ℃, 10
6Ohm/cm; In the time of 2000 ℃, 10
3Ohm/cm.
Embodiment 2
Prepare: a growth head selecting sinter machine; Get test δ-Al ready
2O
3Powder, median size are 2.1 μ m.Make 180 eye mesh screens of charging hopper.
Cleaning: purge the charging hopper with gas blower inner.
Charging: δ-Al
2O
3Powder is poured in the 180 eye mesh screen loading hoppers, adds a cover the isolation dust.
Insert crystal seed: the crystal seed in 75 ° of crystal orientation of A axle is vertically inserted a growth top end; When selecting crystal seed, the molten brilliant termination of crystal seed just is being required to be four directions four, the crystal orientation defective can not be arranged, otherwise can exert an influence to its light refraction.
1), igniting, regulating the qi flowing in the channels sintering crystal:: light oxyhydrogen flame, regulate the ratio 3.9: 1 of oxyhydrogen gas just commonly used, 2085 ℃ of flame temperatures.
2), material crystallization: start electro-magnet and knock hammer, knock hopper guide bar and carry out blanking, in the crystallization of crystal seed top; The dropping material that slows down knocks frequency: 20 times/min, and single discharge quantity: 1.6~2.2g.Concentrate at the center of blanking, and single blanking amount is normal.
3), to center (flame kernel, powder center): in blanking simultaneously, slight, a quick travel growth head is aimed at its flame kernel, plate cutting center, so that powder is in the crystallization of crystal seed upper end.
4), crystal enlarges: 10 growths of sintering unit head, oxygen flow is total up to: 15m
3/ H.Afterwards, the dimension oxygen speed of dripping is: 0.5~10 second/drip; Dropping material knocks frequency: 40~50 beats/mins, and single discharge quantity: 1.6~2.2g; Degrowth speed 2~5mm/h; Crystal has the sign of obvious expansion, and crystal edge is outwards upheld.Whole crystal expansion process required time is 85~95min.
5), isodiametric growth: the slowing down dimension oxygen speed to 16~20 seconds/drip of dripping, improve dropping material and knock frequency to 65 time/min, single discharge quantity: 1.6~2.2g accelerates degrowth speed to 5~7mm/h; Make crystal upwards be the parallel upright growth.2085 ℃ of oxyhydrogen flame kernel temperature.Whole isodiametric growth process required time is 10~11h.
6), blowing out cooling: stop blanking, close the oxyhydrogen valve, stop to descend; Take out crystal behind the non-shock chilling.
The crystal that obtains does not have split across, and is excellent, diameter ф 43mm, total length 85mm.
The appraising datum of crystal is as follows:
Fusing point: the crystal melting temperature is 2085 ℃; Boiling point: the crystal gasification temperature is 3500 ℃; Density: 3.98g/cm
3Hardness of crystals: 9 grades of Mohs;
Crystal color: be micro white (near transparent), average transmittance can reach more than 92%;
Resistance: in the time of 1231 ℃, be 1 megaohm; Resistivity: in the time of 500 ℃, 10
11Ohm/cm; In the time of 1000 ℃, 10
6Ohm/cm; In the time of 2000 ℃, 10
3Ohm/cm.
Embodiment 3
Prepare: a growth head selecting sinter machine; Get test δ-Al ready
2O
3Powder, median size are 2.1 μ m.Make 180 eye mesh screens of charging hopper.
Cleaning: purge the charging hopper with gas blower inner.
Charging: δ-Al
2O
3Powder is poured in the 180 eye mesh screen loading hoppers, adds a cover the isolation dust.
Insert crystal seed: the crystal seed in 75 ° of crystal orientation of A axle is vertically inserted a growth top end; When selecting crystal seed, the molten brilliant termination of crystal seed just is being required to be four directions four, the crystal orientation defective can not be arranged, otherwise can exert an influence to its light refraction.
1), igniting, regulating the qi flowing in the channels sintering crystal:: light oxyhydrogen flame, regulate the ratio 4.1: 1 of oxyhydrogen gas just commonly used, 2090 ℃ of flame temperatures.
2), material crystallization: start electro-magnet and knock hammer, knock hopper guide bar and carry out blanking, in the crystallization of crystal seed top; The dropping material that slows down knocks frequency: 20 times/min, and single discharge quantity: 1.6~2.2g.Concentrate at the center of blanking, and single blanking amount is normal.
3), to center (flame kernel, powder center): in blanking simultaneously, slight, a quick travel growth head is aimed at its flame kernel, plate cutting center, so that powder is in the crystallization of crystal seed upper end.
4), crystal enlarges: 10 growths of sintering unit head, oxygen flow is total up to: 15m
3/ H.Afterwards, the dimension oxygen speed of dripping is: 0.5~10 second/drip; Dropping material knocks frequency: 40~50 beats/mins, and single discharge quantity: 1.6~2.2g; Degrowth speed 2~5mm/h; Crystal has the sign of obvious expansion, and crystal edge is outwards upheld.Whole crystal expansion process required time is 110~140min.
5), isodiametric growth: the slowing down dimension oxygen speed to 16~20 seconds/drip of dripping, improve dropping material and knock frequency to 75 time/min, single discharge quantity: 1.6~2.2g accelerates degrowth speed to 5~6mm/h; Make crystal upwards be the parallel upright growth.2085 ℃ of oxyhydrogen flame kernel temperature.Whole isodiametric growth process required time is 12~13h.
6), blowing out cooling: stop blanking, close the oxyhydrogen valve, stop to descend; Take out crystal behind the non-shock chilling.
The crystal that obtains does not have split across, and is excellent, diameter ф 45mm, total length 90mm.
The appraising datum of crystal is as follows:
Fusing point: the crystal melting temperature is 2090 ℃; Boiling point: the crystal gasification temperature is 3500 ℃; Density: 3.98g/cm
3Hardness of crystals: 9 grades of Mohs;
Crystal color: be micro white (near transparent), average transmittance can reach more than 93%;
Resistance: in the time of 1231 ℃, be 1 megaohm; Resistivity: in the time of 500 ℃, 10
11Ohm/cm; In the time of 1000 ℃, 10
6Ohm/cm; In the time of 2000 ℃, 10
3Ohm/cm.
Embodiment 4
Prepare: a growth head selecting sinter machine; Get test δ-Al ready
2O
3Powder, median size are 2.1 μ m.Make 180 eye mesh screens of charging hopper.
Cleaning: purge the charging hopper with gas blower inner.
Charging: δ-Al
2O
3Powder is poured in the 180 eye mesh screen loading hoppers, adds a cover the isolation dust.
Insert crystal seed: the crystal seed in 75 ° of crystal orientation of A axle is vertically inserted a growth top end; When selecting crystal seed, the molten brilliant termination of crystal seed just is being required to be four directions four, the crystal orientation defective can not be arranged, otherwise can exert an influence to its light refraction.
1), igniting, regulating the qi flowing in the channels sintering crystal:: light oxyhydrogen flame, regulate the ratio 4.2: 1 of oxyhydrogen gas just commonly used, 2090 ℃ of flame temperatures.
2), material crystallization: start electro-magnet and knock hammer, knock hopper guide bar and carry out blanking, in the crystallization of crystal seed top; The dropping material that slows down knocks frequency: 20 times/min, and single discharge quantity: 1.6~2.2g.Concentrate at the center of blanking, and single blanking amount is normal.
3), to center (flame kernel, powder center): in blanking simultaneously, slight, a quick travel growth head is aimed at its flame kernel, plate cutting center, so that powder is in the crystallization of crystal seed upper end.
4), crystal enlarges: 10 growths of sintering unit head, oxygen flow is total up to: 15m3/H.Afterwards, the dimension oxygen speed of dripping is: 0.5~10 second/drip; Dropping material knocks frequency: 40~50 beats/mins, and single discharge quantity: 1.6~2.2g; Degrowth speed 2~5mm/h; Crystal has the sign of obvious expansion, and crystal edge is outwards upheld.Whole crystal expansion process required time is 110~140min.
5), isodiametric growth: the slowing down dimension oxygen speed to 16~20 seconds/drip of dripping, improve dropping material and knock frequency to 80 time/min, single discharge quantity: 1.6~2.2g accelerates degrowth speed to 5~6mm/h; Make crystal upwards be the parallel upright growth.2085 ℃ of oxyhydrogen flame kernel temperature.Whole isodiametric growth process required time is 13~14h.
6), blowing out cooling: stop blanking, close the oxyhydrogen valve, stop to descend; Take out crystal behind the non-shock chilling.
The crystal that obtains does not have split across, and is excellent, diameter ф 45mm, total length 95mm.
The appraising datum of crystal is as follows:
Fusing point: the crystal melting temperature is 2090 ℃; Boiling point: the crystal gasification temperature is 3500 ℃; Density: 3.98g/cm
3Hardness of crystals: 9 grades of Mohs;
Crystal color: be micro white (near transparent), average transmittance can reach more than 93%;
Resistance: in the time of 1231 ℃, be 1 megaohm; Resistivity: in the time of 500 ℃, 10
11Ohm/cm; In the time of 1000 ℃, 10
6Ohm/cm; In the time of 2000 ℃, 10
3Ohm/cm.
Claims (2)
1. the production method of α-aluminum oxide single crystal comprises adding raw material, slotting crystal seed, sintering crystal step, and the sintering crystal is divided into the material crystallization, center, crystal are enlarged and isodiametric growth; Described raw material is δ-Al
2O
3Or γ-Al
2O
3, inserting the used crystal seed of crystal seed is 90 ° of crystal orientation of M axle or 75 ° of crystal orientation of A axle, and it is characterized in that: the oxyhydrogen flame ratio is 3.7~4.2:1 during the sintering crystal, and flame temperature is 2085~2090 ℃;
Described δ-Al
2O
3Aluminum oxide powder material purity more than 99.995%, particle diameter 1.9 μ m ~ 3.0 μ m, density 1.14~1.86g/m
3
10~25 beats/mins of frequencies are knocked in the material crystallization, single blanking amount 1.6~2.2g;
The dimension oxygen speed of dripping that crystal enlarges 0.5~10 second/; Dropping material knocks frequency: 40~50 times/min, and single blanking amount 1.6~2.2g; Degrowth speed 2~5mm/h;
During isodiametric growth, dropping material knocks 55~80 times/min of frequency, single blanking amount 1.6~2.2g, degrowth speed 5~10mm/h, the dimension of dripping oxygen speed: 16~20 seconds/drip.
2. the production method of α-aluminum oxide single crystal according to claim 1, it is characterized in that: adding the used screen cloth loading hopper of raw material is 140~200 orders.
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CN102503104A (en) * | 2011-10-27 | 2012-06-20 | 扬州高能新材料有限公司 | Alpha-aluminum oxide quasi-fusion cake microwave sintering method |
CN103014855A (en) * | 2012-12-25 | 2013-04-03 | 福建鑫磊晶体有限公司 | Preparation method and equipment for preparing alpha-Al2O3 single crystal through gamma-Al2O3 |
CN107557863B (en) * | 2014-11-26 | 2020-10-27 | 三祥新材股份有限公司 | Production method of monocrystal electric melting alumina |
CN104562182B (en) * | 2015-01-29 | 2017-04-19 | 常州焱晶科技有限公司 | Synthesis method of sapphire crystal |
CN106544730A (en) * | 2017-01-22 | 2017-03-29 | 四川省久宝晶体科技有限公司 | A kind of ruby preparation method of synthetic major diameter |
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CN101024898A (en) * | 2007-01-17 | 2007-08-29 | 上海晶生实业有限公司 | Blue-jewel-crystal multi-crucible melt growth technolgoy |
CN101054723A (en) * | 2007-02-07 | 2007-10-17 | 深圳市淼浩高新科技开发有限公司 | Method for growing R-surface sapphire crystal |
CN101205628A (en) * | 2006-12-18 | 2008-06-25 | 庄育丰 | Sapphire crystal growth method |
CN101280458A (en) * | 2007-12-28 | 2008-10-08 | 中国科学院上海光学精密机械研究所 | Method for growing carbon-doped sapphire crystal by using guided mode method |
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CN101205628A (en) * | 2006-12-18 | 2008-06-25 | 庄育丰 | Sapphire crystal growth method |
CN101024898A (en) * | 2007-01-17 | 2007-08-29 | 上海晶生实业有限公司 | Blue-jewel-crystal multi-crucible melt growth technolgoy |
CN101054723A (en) * | 2007-02-07 | 2007-10-17 | 深圳市淼浩高新科技开发有限公司 | Method for growing R-surface sapphire crystal |
CN101280458A (en) * | 2007-12-28 | 2008-10-08 | 中国科学院上海光学精密机械研究所 | Method for growing carbon-doped sapphire crystal by using guided mode method |
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