CN102011184A - Production method of alpha-aluminum oxide single crystal - Google Patents
Production method of alpha-aluminum oxide single crystal Download PDFInfo
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- CN102011184A CN102011184A CN 201010612217 CN201010612217A CN102011184A CN 102011184 A CN102011184 A CN 102011184A CN 201010612217 CN201010612217 CN 201010612217 CN 201010612217 A CN201010612217 A CN 201010612217A CN 102011184 A CN102011184 A CN 102011184A
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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 synthetic sapphire crystalline preparation method technical field, particularly the production method of α-aluminium sesquioxide 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 blanking amount 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 the application of single crystal in fields such as industry, national defence, electronics always.
Summary of the invention
Technical problem to be solved by this invention provides the production method of a kind of α-aluminium sesquioxide single crystal, and the α that this production method makes-aluminium sesquioxide single crystal diameter is big.
The production method of α of the present invention-aluminium sesquioxide single crystal, comprise add raw material, insert crystal seed, sintering crystal step, being divided into of sintering crystal material crystallization, to center, crystal expansion 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 bigger 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 ℃.
Change the material crystallization: fusing crystal seed hair is white, shinny, in the blanking crystallization of crystal seed top, knocks frequency 10～25 times/minute, single blanking amount 1.6～2.2g.
To the center: changing the material crystalline simultaneously, crystal seed is aimed at flame and blanking 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 state, control blanking amount cooperates with the effective of degrowth speed, and crystal diameter is grown up.Preferably, drip dimension oxygen speed 0.5～10 second/drip; Following blanking knocks frequency: 40～50 times/min, and single blanking amount 1.6～2.2g; Degrowth speed 2～5mm/h.
During isodiametric growth, following blanking 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.Control growing speed and blanking amount make crystal upwards be the parallel upright growth.
The blowing out cooling: close blanking system, decline system, oxyhydrogen flame, crystal leaves standstill cooling in stove; Cooling 90～120min.Major diameter crystalline caloric receptivity is bigger, and the present invention has prolonged crystalline cooling time.
Crystal is taken out in the cooling back does not have 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 made up of the oxonium ion of divalence and the Chrome ion of trivalent.The α that the present invention obtains-aluminium sesquioxide single crystal, its outside diameter: φ 42mm～φ 45mm, total length L=80mm～95mm.Increase the Application Areas of synthetic sapphire, can be applied to industrial circles such as microwave dielectric material, waveguide laser, high degree of accuracy bearing components and parts, extensive integrated electronic wiring board, guided missile and satellite receive 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 → change material crystallization → to center → crystal expansion → isodiametric growth → blowing out cooling → taking-up single crystal, specifically may further comprise the steps:
1, raw material adds: purge charging hopper inside with gas blower, 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 special-purpose cleaning tool,, bonding impurity is dropped in inboard wall of burner hearth moving gently on every side;
5, change the material crystallization: start electro-magnet and knock hammer, knock hopper guide bar and carry out blanking, in the crystallization of crystal seed top; Following blanking knocks frequency 15～20 times/minute, single blanking amount: 1.6～2.2g;
6, to the center: mainly be that crystal seed is aimed at flame and blanking 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 state, control blanking amount cooperates with the effective of degrowth speed; The dimension of dripping oxygen speed is by slack-off soon: 0.5～10 second/drip; Following blanking knocks frequency: 40～50 times/minute; Degrowth speed 2～5mm/h;
8, isodiametric growth: mainly be that degrowth speed, following blanking are knocked frequency, drip and tie up the control of oxygen speed; Crystal is normal when isometrical, degrowth speed: 5～10mm/h; Following blanking knocks frequency: 55～80 times/minute (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: no 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 charging hopper inside with gas blower.
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 for use, 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), change the material crystallization: start electro-magnet and knock hammer, knock hopper guide bar and carry out blanking, in the crystallization of crystal seed top; Slowing down down, blanking knocks frequency: 20 times/min, and single blanking amount: 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, blanking 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; Following blanking knocks frequency: 40～50 times/minute, and single blanking amount: 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 down blanking and knock frequency to 60 time/min, single blanking amount: 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 crystalline appraising datum 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 charging hopper inside with gas blower.
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 for use, 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), change the material crystallization: start electro-magnet and knock hammer, knock hopper guide bar and carry out blanking, in the crystallization of crystal seed top; Slowing down down, blanking knocks frequency: 20 times/min, and single blanking amount: 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, blanking 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; Following blanking knocks frequency: 40～50 times/minute, and single blanking amount: 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 down blanking and knock frequency to 65 time/min, single blanking amount: 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 crystalline appraising datum 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 charging hopper inside with gas blower.
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 for use, 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), change the material crystallization: start electro-magnet and knock hammer, knock hopper guide bar and carry out blanking, in the crystallization of crystal seed top; Slowing down down, blanking knocks frequency: 20 times/min, and single blanking amount: 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, blanking 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; Following blanking knocks frequency: 40～50 times/minute, and single blanking amount: 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 down blanking and knock frequency to 75 time/min, single blanking amount: 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 crystalline appraising datum 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 charging hopper inside with gas blower.
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 for use, 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), change the material crystallization: start electro-magnet and knock hammer, knock hopper guide bar and carry out blanking, in the crystallization of crystal seed top; Slowing down down, blanking knocks frequency: 20 times/min, and single blanking amount: 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, blanking 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; Following blanking knocks frequency: 40～50 times/minute, and single blanking amount: 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 down blanking and knock frequency to 80 time/min, single blanking amount: 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 crystalline appraising datum 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 (6)
1. the production method of α-aluminium sesquioxide single crystal comprises adding raw material, inserting crystal seed, sintering crystal step, being divided into of sintering crystal material crystallization, to center, crystal expansion 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 ℃.
2. the production method of α according to claim 1-aluminium sesquioxide single crystal is characterized in that: raw material is 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.
3. the production method of α according to claim 1 and 2-aluminium sesquioxide single crystal is characterized in that: adding the used screen cloth loading hopper of raw material is 140～200 orders.
4. the production method of α according to claim 1-aluminium sesquioxide single crystal is characterized in that: change the material crystallization and knock frequency 10～25 times/minute, single blanking amount 1.6～2.2g.
5. the production method of α according to claim 1-aluminium sesquioxide single crystal is characterized in that: the dimension oxygen speed of dripping that crystal enlarges 0.5～10 second/; Following blanking knocks frequency: 40～50 times/min, and single blanking amount 1.6～2.2g; Degrowth speed 2～5mm/h.
6. the production method of α according to claim 1-aluminium sesquioxide single crystal, it is characterized in that: during isodiametric growth, following blanking 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.
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Cited By (5)
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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 |
| CN104562182A (en) * | 2015-01-29 | 2015-04-29 | 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 |
| CN107557863A (en) * | 2014-11-26 | 2018-01-09 | 三祥新材股份有限公司 | A kind of production method of single crystal electrofusion aluminum oxide |
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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 |
| CN107557863A (en) * | 2014-11-26 | 2018-01-09 | 三祥新材股份有限公司 | A kind of production method of single crystal electrofusion aluminum oxide |
| CN104562182A (en) * | 2015-01-29 | 2015-04-29 | 常州焱晶科技有限公司 | Synthesis method of sapphire crystal |
| 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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|---|---|
| CN102011184B (en) | 2013-04-10 |
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