CN102011185B - Method for artificially synthesizing sapphire - Google Patents
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Abstract
The invention belongs to the technical field of a preparation method of an artificial crystal material, in particular relating to a method for artificially synthesizing sapphire and aiming to solve the technical problem of providing a preparation method of the artificially synthesized pure white sapphire with stable product quality. The preparation method of artificially synthesizing the sapphire comprises the following steps: adding a raw material; inserting seed crystals; and sintering crystals, wherein, the step of sintering the crystals comprises the procedures of crystallizing chemical materials, centering, expanding the crystals and performing equal-diameter growth; the adopted raw material is aluminum oxide pure white powder, the purity is at least 99.996%, the particle size is 2.1mu m-5.7mu m, and the density is 1.14-1.86g/m<3>; and crystal roots (Phi3-5mm and L5-8mm) grow before expanding the crystals. In the invention, the pure white high-purity superfine aluminum oxide powder is used to replace aluminum oxide powder containing an ammonium ferric sulfate oiling agent and an ammonium fluorotitanate oiling agent to obtain the artificially synthesized pure white sapphire without impurities.
Description
Technical field
The invention belongs to preparation method's technical field of artificial crystal material, particularly a kind of method of artificial synthetic sapphire.
Background technology
One traditional alumina powder be to solve the condition problem of alumina powder in process of production, all can add some chemical impurities (such as ammonium ferric sulfate, ammonium titanium fluoride, methyl red) in alum raw material roasting powder process molten mass.Synthetic sapphire manufacturer all is that the alumina powder of the above-mentioned adding chemical impurity of employing is produced at present.Traditional processing technology comprises and adds raw material, inserts crystal seed, sintering crystal step, and the sintering crystal is divided into the material crystallization, center, the brilliant root of growing, crystal are enlarged and isodiametric growth, and is concrete: as to adopt δ-Al
2O
3Or γ-Al
2O
3Alumina 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 synthetic sapphire of producing partially blue or partially red phenomenon all can occur, thereby affect the quality quality after annealing.Limited synthetic sapphire in the application of microwave dielectric material, waveguide laser, high precision bearing components and parts, industrial circles such as optical mirror slip that light transmittance is higher.
Summary of the invention
Technical problem to be solved by this invention provides a kind of pure white, the preparation method of the artificial synthetic sapphire of constant product quality.
The preparation method of the artificial synthetic sapphire of the present invention, comprise and add raw material, slotting crystal seed, sintering crystal step, the sintering crystal comprises the material crystallization, center, crystal is enlarged and isodiametric growth, raw material is the pure white powder of aluminium oxide, and purity is at least 99.996%, particle diameter 2.1 μ m～5.7 μ m, density 1.14～1.86g/m
3, the brilliant root of growing first before the crystal expansion step, brilliant root ф 3～5mm, L5～8mm.
The pure white powder of aluminium oxide can be α, γ, δ phase Al
2O
3Powder; Be preferably α-Al
2O
3Pure white powder.
Adding the used charging screen cloth of raw material bucket is 80～120 orders.
Slotting crystal seed can adopt the crystal seed in 90 ° of crystal orientation of M axle or 75 ° of crystal orientation of A axle; The present invention is preferably the crystal seed in 90 ° of crystal orientation of M axle.
Crystal is comparatively responsive to the temperature field of oxyhydrogen flame in the sintering furnace, and the numerous appearance fluctuation of warm field frequency can cause crystal sudden contraction, expansion or serious superfusion, thereby affects quality and the profile quality of product.So the flame temperature of a inventive method sintering crystal step setting range is preferably 2020 ℃ at 2000～2030 ℃, the hydrogen-oxygen ratio of flame is 2.2～2.5: 1.
In the production process, for the better crystallization of the melting layer that makes crystalline solid, (single knocks the blanking amount: 0.5～1.0g), and can not knock fast blanking must to control the amount of dropping material.Knock the blanking amount with tradition and compare, single blanking amount reduces.The relative internal stress of pure white material sapphire can increase along with the variation of crystal diameter size, so the diameter of the sapphire crystal of pure white material can not be too large, scope is at 20mm～32mm.
In order to guarantee the formedness of its crystalline texture, the growth decrease speed can not be too quick, otherwise brilliant phenomenon can occur splitting.
For internal soundness and the degree of crystallinity that guarantees its product, every batch of SINTERING PRODUCTION time should be higher than 12 hours.
The material crystallization: dropping material knocks 18～25 beats/mins of frequencies, and single knocks blanking amount 0.5～0.6g;
To the center: in the material crystallization, crystal seed is aimed at flame and plate cutting center.
The brilliant root of growing: decrease speed is under the condition of 25～35mm/h, and 4～6 minutes times spent grew ф 3～5mm, the brilliant root of L5～8mm.
Crystal enlarges: the dimension of dripping oxygen speed 3 seconds～10 seconds/; Dropping material knocks frequency: 20～30 beats/mins, single knocks blanking amount 0.5～0.8g; Degrowth speed 5～10mm/h;
Isodiametric growth: degrowth speed: 15～18mm/h; Dropping material knocks frequency: 50～60 beats/mins, and single blanking amount 0.8～1.0g; The dimension of dripping oxygen speed: 14～16 seconds/drip.
The invention has the beneficial effects as follows:
The pure white powder of high-purity ultra-fine alumina any chemical impurity of admixture not in aluminium hydroxide raw material roasting powder process molten mass, the present invention utilizes the pure white powder of high-purity ultra-fine alumina to replace to contain ammonium ferric sulfate and ammonium titanium fluoride that the alumina powder of agent is arranged, that production is made is pure white, without assorted artificial synthetic sapphire, on the technical matters of essence, the change of matter has occured.
The pure white powder particle of high-purity ultra-fine alumina average grain diameter is 3.4 μ m, and the proportion of particle is larger, and particle dispersion is good, and non-agglomerate is " spheroidal " single particle, and the dry sliding that disperses of powder is fine, is not easy to occur the phenomenon of empty powder gas leakage.
The pure white powder of high-purity ultra-fine alumina is purify to produce with aluminium hydroxide, basically do not exist to large natural environment destruction, the content of its impurity can not cause on the quality of artificial synthetic sapphire direct impact.
The pure white powder production of high-purity ultra-fine alumina utilance is 95% in theory, is actually 93%, has improved greatly labor productivity, has reduced production costs.
Embodiment
The technological process of the artificial synthetic sapphire of the pure white preparation of high-purity ultra-fine alumina of the present invention is: add raw material → the insert a crystal seed → oxyhydrogen flame sintering → cleaning sintering furnace → material crystallization → center → brilliant root → crystal expansion → isodiametric growth → blowing out of growing is cooled off → taken out monocrystal, specifically may further comprise the steps:
1, raw material adds: it is inner to purge the charging hopper with air blast, and the pure white powder of high-purity ultra-fine alumina is poured in 80～120 eye mesh screen charging hoppers, adds a cover the isolation dust.Because the pure white powder density of high-purity ultra-fine alumina is larger, so need to add raw material 1 time at every heat;
2, insert crystal seed: at the candlestick top end, vertically insert 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 flame temperature setting range is at 2000 ℃～2030 ℃; Because the variation of flame temperature, the hydrogen-oxygen ratio of regulating flame is 2.2～2.5: 1;
4, cleaning sintering furnace: use dedicated cleaning tool, in inboard wall of burner hearth moving gently on every side, the bonding impurity such as powder are dropped;
5, material crystallization: start electromagnet and knock hammer, knock hopper guide bar and carry out blanking, in the crystallization of crystal seed top; Dropping material knocks 18～25 beats/mins of frequencies, and single knocks blanking amount 0.5～0.6g;
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, the brilliant root of growing: alumina powder melts and drops on the crystallization kind, and decrease speed is under the condition of 30mm/h, grows the brilliant root of growth between 5 minutes times spent, and brilliant root is long to ф 3～5mm, L5～8mm; This kind method can prevent the impact of self internal stress of pure white alumina powder, makes sapphire crystal from the crystallization counterincision; Can also break away from the imperfect tape of crystal seed self to host crystal;
8, 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: 8～12m
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: 3 seconds～10 seconds/drip; Dropping material knocks frequency: 20～30 beats/mins; Single knocks blanking amount 0.5～0.8g; Degrowth speed 5～10mm/h;
9, 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: 15～18mm/h; Dropping material knocks frequency: 50～60 beats/mins; Single blanking amount 0.8～1.0g; The dimension of dripping oxygen speed: 14～16 seconds/drip; Oxygen flow is constant to be about: 11 ± 2m
3/ H
10, blowing out cooling: close the oxyhydrogen valve; Crystal cooling time is 40～60min;
11, take out crystal: without the special process requirement.
Embodiment 1
Prepare: the trial production equipment sintering machine of selecting a better performances; Get ready and test with pure white without agent α-Al
2O
3Powder, purity are 99.996%, and average grain diameter is 3.4 μ m.Make 120 eye mesh screens of charging hopper.
Cleaning: it is inner to purge the charging hopper with air blast.
The charging: pure white without agent α-Al
2O
3Powder is poured in the 120 eye mesh screen charging hoppers, adds a cover the isolation dust.
Insert crystal seed: the crystal seed in 90 ° of crystal orientation of M 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 2.4: 1 of oxyhydrogen gas just commonly used, 2020 ℃ of flame temperatures.
2), material crystallization: start electromagnet 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, single knocks blanking amount 0.5～0.6g.
3), to center (flame kernel, powder center): in blanking simultaneously, slight, a fast moving growth head is aimed at its flame kernel, plate cutting center, so that powder is in the crystallization of crystal seed upper end.
4), the brilliant root of growing: the alumina powder thawing drops on the crystallization kind, is not increasing oxygen and is speeding under the condition that decrease speed is 30mm/h, grows the brilliant root of growth between 5 minutes times spent, and brilliant root is long to ф 3～5mm, L5～8mm.
5), crystal enlarges: 1 second 2 the dimension oxygen speed of dripping, carry out oxygenation and enlarge.10 growths of sintering unit head, oxygen flow is total up to: 10m
3/ H.Afterwards, the dimension oxygen speed of dripping becomes: 3 seconds～10 seconds/drip; Dropping material knocks frequency: 30 times/min, single knocks blanking amount 0.5～0.8g; Degrowth speed 5～8mm/h; Crystal has the sign of obvious expansion, and crystal edge is outwards upheld.Whole crystal expansion process required time is 1h.
6), isodiametric growth: the slowing down dimension oxygen speed to 14～16 seconds/drip of dripping, improve dropping material and knock frequency to 50～60 time/min, single blanking amount 0.8～1.0g; Accelerate degrowth speed to 15～18mm/h; Make crystal upwards be the parallel upright growth.2020 ℃ of oxyhydrogen flame kernel temperature.Whole isodiametric growth process required time is 10h.
7), blowing out cooling: stop blanking, close the oxyhydrogen valve, stop to descend; Take out crystal after the static cooling.Crystal cooling time is 40min.
The crystal that obtains does not split, and is excellent, diameter ф 22mm, total length 137mm.
The appraising datum of crystal is as follows:
Fusing point: the crystal melting temperature is 2030 ℃; Boiling point: the crystal gasification temperature is 3500 ℃; Density: 3.98g/cm
3Hardness of crystals: 9 grades of Mohs;
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.
Crystal color: be pure white Transparent color, invariably molten impurity; Average transmittance can reach more than 96%;
The crystal mass index: qualification rate is more than 96%.
Embodiment 2
Prepare: the trial production equipment sintering machine of selecting a better performances; Get ready and test with pure white without agent α-Al
2O
3Powder, purity are 99.996%, and average grain diameter is 3.4 μ m.Make 120 eye mesh screens of charging hopper.
Cleaning: it is inner to purge the charging hopper with air blast.
The charging: pure white without agent α-Al
2O
3Powder is poured in the 120 eye mesh screen charging hoppers, adds a cover the isolation dust.
Insert crystal seed: the crystal seed in 90 ° of crystal orientation of M 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 2.4: 1 of oxyhydrogen gas just commonly used, 2020 ℃ of flame temperatures.
2), material crystallization: start electromagnet and knock hammer, knock hopper guide bar and carry out blanking, in the end crystallization of crystal seed top; The dropping material that slows down knocks frequency: 20 times/min, single knocks blanking amount 0.5～0.6g.Concentrate at the center of blanking, and single blanking amount is normal.
3), to center (flame kernel, powder center): in blanking simultaneously, slight, a fast moving growth head is aimed at its flame kernel, plate cutting center, so that powder is in the crystallization of crystal seed upper end.
4), the brilliant root of growing: the alumina powder thawing drops on the crystallization kind, is not increasing oxygen and is speeding under the condition that decrease speed is 30mm/h, grows the brilliant root of growth between 5 minutes times spent, and brilliant root is long to ф 3～5mm, L5～8mm.
5), crystal enlarges: 1 second 2 the dimension oxygen speed of dripping, carry out oxygenation and enlarge.10 growths of sintering unit head, oxygen flow is total up to: 11m
3/ H.Afterwards, the dimension oxygen speed of dripping is from fast to slow: 3 seconds～10 seconds/drip; Dropping material knocks frequency: 30 times/min, single knocks blanking amount 0.5～0.8g; Degrowth speed 5～8mm/h; Crystal has the sign of obvious expansion, and crystal edge is outwards upheld.Whole crystal expansion process required time is 1.5h.
6), isodiametric growth: the slowing down dimension oxygen speed to 14～16 seconds/drip of dripping, improve dropping material and knock frequency to 50～60 time/min, single blanking amount 0.8～1.0g; Accelerate degrowth speed to 15～18mm/h; Make crystal upwards be the parallel upright growth.2020 ℃ of oxyhydrogen flame kernel temperature.Whole isodiametric growth process required time is 10.5h.
7), blowing out cooling: stop blanking, close the oxyhydrogen valve, stop to descend; Take out crystal after the static cooling.Crystal cooling time is 50min.
The crystal that obtains does not split, and is excellent, diameter ф 26mm, total length 134mm.
The appraising datum of crystal is as follows:
Fusing point: the crystal melting temperature is 2030 ℃; Boiling point: the crystal gasification temperature is 3500 ℃; Density: 3.98g/cm
3Hardness of crystals: 9 grades of Mohs;
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.
Crystal color: be pure white Transparent color, invariably molten impurity; Average transmittance can reach more than 96%;
The crystal mass index: qualification rate is more than 96%.
Embodiment 3
Prepare: the trial production equipment sintering machine of selecting a better performances; Get ready and test with pure white without agent α-Al
2O
3Powder, purity are 99.996%, and average grain diameter is 3.4 μ m.Make 120 eye mesh screens of charging hopper.
Cleaning: it is inner to purge the charging hopper with air blast.
The charging: pure white without agent α-Al
2O
3Powder is poured in the 120 eye mesh screen charging hoppers, adds a cover the isolation dust.
Insert crystal seed: the crystal seed in 90 ° of crystal orientation of M 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 2.4: 1 of oxyhydrogen gas just commonly used, 2020 ℃ of flame temperatures.
2), material crystallization: start electromagnet and knock hammer, knock hopper guide bar and carry out blanking, in the end crystallization of crystal seed top; The dropping material that slows down knocks frequency: 15 times/min, single knocks blanking amount 0.5～0.6g.Concentrate at the center of blanking, and single blanking amount is normal.
3), to center (flame kernel, powder center): in blanking simultaneously, slight, a fast moving growth head is aimed at its flame kernel, plate cutting center, so that powder is in the crystallization of crystal seed upper end.
4), the brilliant root of growing: the alumina powder thawing drops on the crystallization kind, is not increasing oxygen and is speeding under the condition that decrease speed is 30mm/h, grows the brilliant root of growth between 5 minutes times spent, and brilliant root is long to ф 3～5mm, L5～8mm.
5), crystal enlarges: 1 second 2 the dimension oxygen speed of dripping, carry out oxygenation and enlarge.10 growths of sintering unit head, oxygen flow is total up to: 12m
3/ H.Afterwards, the dimension oxygen speed of dripping is from fast to slow: 3 seconds～10 seconds/drip; Dropping material knocks frequency: 30 times/min, single knocks blanking amount 0.5～0.8g; Degrowth speed 5～8mm/h; Crystal has the sign of obvious expansion, and crystal edge is outwards upheld.Whole crystal expansion process required time is 100min.
6), isodiametric growth: the slowing down dimension oxygen speed to 14～16 seconds/drip of dripping, improve dropping material and knock frequency to 50～60 time/min, single blanking amount 0.8～1.0g; Accelerate degrowth speed to 15～18mm/h; Make crystal upwards be the parallel upright growth.2020 ℃ of oxyhydrogen flame kernel temperature.Whole isodiametric growth process required time is 10.5h.
7), blowing out cooling: stop blanking, close the oxyhydrogen valve, stop to descend; Take out crystal after the static cooling.Crystal cooling time is 55min.
The crystal that obtains does not split, and is excellent, diameter ф 30mm, total length 126mm.
The appraising datum of crystal is as follows:
Fusing point: the crystal melting temperature is 2030 ℃; Boiling point: the crystal gasification temperature is 3500 ℃; Density: 3.98g/cm
3Hardness of crystals: 9 grades of Mohs;
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.
Crystal color: be pure white Transparent color, invariably molten impurity; Average transmittance can reach more than 96%;
The crystal mass index: qualification rate is more than 96%.
Embodiment 4
Prepare: the trial production equipment sintering machine of selecting a better performances; Get ready and test with pure white without agent α-Al
2O
3Powder, purity are 99.996%, and average grain diameter is 3.4 μ m.Make 120 eye mesh screens of charging hopper.
Cleaning: it is inner to purge the charging hopper with air blast.
The charging: pure white without agent α-Al
2O
3Powder is poured in the 120 eye mesh screen charging 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 2.5: 1 of oxyhydrogen gas just commonly used, 2030 ℃ of flame temperatures.
2), material crystallization: start electromagnet and knock hammer, knock hopper guide bar and carry out blanking, in the end crystallization of crystal seed top; The dropping material that slows down knocks frequency: 15 times/min, single knocks blanking amount 0.5～0.6g.Concentrate at the center of blanking, and single blanking amount is normal.
3), to center (flame kernel, powder center): in blanking simultaneously, slight, a fast moving growth head is aimed at its flame kernel, plate cutting center, so that powder is in the crystallization of crystal seed upper end.
4), the brilliant root of growing: the alumina powder thawing drops on the crystallization kind, is not increasing oxygen and is speeding under the condition that decrease speed is 30mm/h, grows the brilliant root of growth between 5 minutes times spent, and brilliant root is long to ф 3～5mm, L5～8mm.
5), crystal enlarges: 1 second 2 the dimension oxygen speed of dripping, carry out oxygenation and enlarge.10 growths of sintering unit head, oxygen flow is total up to: 12m
3/ H.Afterwards, the dimension oxygen speed of dripping is from fast to slow: 3 seconds～10 seconds/drip; Dropping material knocks frequency: 30 times/min, single knocks blanking amount 0.5～0.8g; Degrowth speed 5～8mm/h; Crystal has the sign of obvious expansion, and crystal edge is outwards upheld.Whole crystal expansion process required time is 120min.
6), isodiametric growth: the slowing down dimension oxygen speed to 14～16 seconds/drip of dripping, improve dropping material and knock frequency to 50～60 time/min, single blanking amount 0.8～1.0g; Accelerate degrowth speed to 15～18mm/h; Make crystal upwards be the parallel upright growth.2030 ℃ of oxyhydrogen flame kernel temperature.Whole isodiametric growth process required time is 10h.
7), blowing out cooling: stop blanking, close the oxyhydrogen valve, stop to descend; Take out crystal after the static cooling.Crystal cooling time is 60min.
The crystal that obtains does not split, and is excellent, diameter ф 30mm, total length 118mm.
The appraising datum of crystal is as follows:
Fusing point: the crystal melting temperature is 2030 ℃; Boiling point: the crystal gasification temperature is 3500 ℃; Density: 3.98g/cm
3Hardness of crystals: 9 grades of Mohs;
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.
Crystal color: be pure white Transparent color, invariably molten impurity; Average transmittance can reach more than 96%;
The crystal mass index: qualification rate is more than 96%.
Claims (2)
1. the preparation method of artificial synthetic sapphire, comprise and add raw material, slotting crystal seed, sintering crystal step, the sintering crystal comprises the material crystallization, center, crystal is enlarged and isodiametric growth, it is characterized in that: raw material is the pure white powder of aluminium oxide, and purity is at least 99.996%, particle diameter 2.1 μ m～5.7 μ m, density 1.14～1.86g/m
3, the brilliant root of growing first before the crystal expansion step, brilliant root ф 3～5mm, L5～8mm;
Described slotting crystal seed adopts the crystal seed in 90 ° of crystal orientation of M axle or 75 ° of crystal orientation of A axle;
2000～2030 ℃ of the flame temperatures of described sintering crystal, the hydrogen-oxygen ratio of flame is 2.2～2.5:1;
Single knocks the blanking amount and is during described sintering crystal: 0.5～1.0g, sintering time are higher than 12 hours;
Dropping material knocks 18～25 beats/mins of frequencies in the described material crystallisation step, and single knocks blanking amount 0.5～0.6g;
Decrease speed is 25～35mm/h during the brilliant root of described growth, 4～6 minutes times spent;
In the described crystal expansion step: the dimension of dripping oxygen speed 3 seconds～10 seconds/; Dropping material knocks frequency: 20～30 beats/mins, single knocks blanking amount 0.5～0.8g; Degrowth speed 5～10mm/h;
In the described isodiametric growth step: degrowth speed: 15～18mm/h; Dropping material knocks frequency: 50～60 beats/mins, and single blanking amount 0.8～1.0g; The dimension of dripping oxygen speed: 14～16 seconds/drip.
2. the preparation method of artificial synthetic sapphire according to claim 1, it is characterized in that: the pure white powder of aluminium oxide is α-Al
2O
3Pure white powder.
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| CN1544712A (en) * | 2003-11-18 | 2004-11-10 | 陈迎春 | Integrated melt method for crystal growth |
| 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 |
| 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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