CN104109904A - Seeding method of sapphire crystal growth kyropoulos method - Google Patents
Seeding method of sapphire crystal growth kyropoulos method Download PDFInfo
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Abstract
The invention discloses a seeding method of a sapphire crystal growth kyropoulos method. The seeding method comprises the following steps of 1, carrying out material melting under electric heating control at a constant power increasing ratio of 4000W/h, and when the heating power is 70000W, sequentially carrying out heating melting at the heating power until the raw material melts, 2, keeping a liquid state of the raw material at a high temperature, and discharging impurities in the raw material by convection, 3, putting seed crystals into the melt material, monitoring seed crystal weight change, and adjusting a crucible temperature so that a seed crystal weight change amount is within +/-1g, 4, dropping the seed crystals under the liquid surface, and carrying out drawing-up crystallization and growth seeding, and 5, carrying out slow seed crystal drawing-up, reducing heating power at a uniform rate, monitoring seed crystal weight, and stopping the automatic seeding when the seed crystal weight is 5kg. The seeding method realizes good product homogeneity and a yield rate more than 80%. Compared with the prior art, the seeding method has obvious advantages and realizes large scale application of the large-size crystal growth kyropoulos method.
Description
Technical field
The present invention relates to crystalline substance and manufacture field, relate in particular to a kind of preparation method of sapphire crystal.
Background technology
α-Al
2o
3monocrystalline claims again sapphire, is commonly called as corundum, is a kind of simple corrdination type oxide crystal.Sapphire crystal has excellent optical property, mechanical property and chemical stability, intensity is high, hardness is large, resistance to erosion, can under the mal-condition that approaches 2000 ℃ of high temperature, work, thereby be widely used in the window material of infrared military installation, satellite spatial technology, high intensity laser beam.Its unique crystalline network, excellent mechanical property, good thermal property make sapphire crystal become the semi-conductor GaN/Al of practical application
2o
3photodiode (LED), the ideal substrate materials such as large-scale integrated circuit SOI and SOS and superconducting nano structural membrane.Low-cost, growing large-size sapphire single-crystal has become the current urgent task facing in high quality.
In prior art, sapphire crystal growth mode can be divided into three kinds of solution growths, melt growth, vapor phase growth, wherein melt growth mode is fast because having growth velocity, the features such as purity height and perfection of crystal are good are the most frequently used crystal growth patterns of preparation large size and specified shape crystal and become.Can be used at present mainly contain flame melt method, crystal pulling method, zone melting method, guided mode method, crucible Mobile Method, heat-exchanging method, temperature gradient method, kyropoulos etc. with the method for melt growth mode Artificial Growth sapphire crystal, and the sapphire crystal of kyropoulos technique growth is about 70% of existing market share.
Kyropoulos (Kyropoulos method, KY method), first be Kyropoulos proposed and for the growth of crystal, in the after this quite a long time, the method is all the preparation for crystal such as large size halogen family crystal, oxyhydroxide and carbonate in nineteen twenty-six.Last century six, the seventies, improved through the Musatov of USSR (Union of Soviet Socialist Republics), this method was applied to the preparation of sapphire single-crystal.The monocrystalline of the method growth, external form is generally pyriform, and crystal diameter can grow into than the size of the little 10～30mm of crucible internal diameter.(Czochralski method) is similar for its principle and Chai Shi crystal pulling method, first heating raw materials is melted to the molten soup of formation to fusing point, again with crystal seed (the Seed Crystal of monocrystalline, claim again seed crystal rod) touch and melt soup surface, in the solid-liquid interface of crystal seed and molten soup, start the monocrystalline of growth and crystal seed same crystal structure, crystal seed with the utmost point slowly speed up draw high, but crystal seed up crystal pulling for some time to form brilliant neck, after the solidification rate at soup fusion and crystal seed interface is stablized, crystal seed just no longer draws high, do not rotate yet, only to control rate of cooling mode, monocrystalline is down solidified gradually from top, final set becomes the brilliant heavy stone used as an anchor of a whole monocrystalline.Kyropoulos is to utilize temperature to control growing crystal, the difference of it and Chai Shi crystal pulling method maximum is only to pull out brilliant neck, brilliant body is partly to grow against temperature variation, lacked the interference that draws high and rotate, relatively good control processing procedure, and in crystal pulling neck, adjust heater power, make the raw material of melting reach the brilliant temperature range of most suitable length, allow the speed of growth reach the most idealized, thereby grow the optimal sapphire single-crystal of quality.
The crystal mass of kyropoulos depends primarily on the design of temperature field and the quality of seeding.In the situation that a temperature design is at present increasingly rationalized, the quality of seeding quality becomes crystal mass most critical factor.Meanwhile, the human factor that how to reduce seeding also becomes the problem that kyropoulos large-scale application must solve.
Summary of the invention
Because the above-mentioned defect of prior art, technical problem to be solved by this invention is to provide a kind of automatic seeding method of kyropoulos sapphire crystal growth, to obtain high-quality seeding result.
For solving the problems of the technologies described above, the invention provides a kind of seeding method that kyropoulos is prepared sapphire crystal, comprise the steps:
1) raw material melts
Material process is by electric heating control, and increased power value is fixed as 4000W/ hour, and final heating power is increased to 70000W, maintains heating power to raw material and has melted;
2) row's bubble
At high temperature maintain the liquid state of raw material, by convection current, discharge the impurity in raw material;
3) examination temperature
Put into seed crystal, and monitor seed crystal changes in weight, adjust crucible temperature, make seed crystal changes in weight in ± 1g;
4) sow
Seed crystal is dropped to below liquid level, lift crystallization, growth seeding;
5) shouldering
Lift at a slow speed seed crystal, at the uniform velocity reduce heating power, monitoring seed crystal weight, after seed crystal weight arrives 5 kilograms, automatic seeding end of processing.
Preferably, step 1) in, in raw material thaw process, maintain furnace chamber vacuum tightness 10
-3more than Pa; In temperature-rise period, monitoring burner hearth vacuum tightness, when lower than 10
-3during Pa, suspend and heat up, treat that vacuum reaches 10
-3after Pa is above, continue to heat up, vacuum is lower than 1 * 10 again
-2during Pa, end heating.
Preferably, in other embodiments, step 1) in, increased power value is fixed as 4000W/ hour, and heating power is increased to 70000W; Now in stove, temperature is 2000 ± 50 ℃, continue to maintain heating power and remain unchanged 4 to 8 hours, in stove, temperature rises to 2140 ± 20 ℃ gradually, and temperature in stove being detected a larger decline process (20 to 30 ℃), now complete material process, enter next step.
Preferably, step 2) in, crucible temperature is maintained to 2140 ℃, the time is 8-12 hour, then in 4 hours, the speed with 10 ℃/h is cooled to 2100 ℃, enters next stage.
Preferably, step 3) in, seed crystal from liquid level top 10mm fast-descending to liquid level under 30mm place, then fast lifting is to 10mm place, liquid level top, contrasts front and back seed crystal changes in weight, adjustment crucible temperature makes seed crystal changes in weight in ± 1g.
Preferably, step 3) in, reducing at a slow speed seed rod to 20mm place, liquid level top, monitoring seed crystal weight, when appearanceization seed crystal phenomenon, illustrates excess Temperature, according to material speed, Modulating Power; Nothingization seed crystal phenomenon, try temperature:
The first round, drops to seed crystal 30-40mm under liquid level fast, and then rises to 10mm place, liquid level top, monitoring seed crystal weight, if weight rises, illustrate that temperature is too low, produce crystallization, if weight declines, excess Temperature is described, dissolves seed crystal, according to changes in weight Modulating Power, re-start examination temperature, until seed crystal changes in weight is in 1g;
Second takes turns, and fast seed crystal is dropped to 30-40mm under liquid level, waits for for 10 seconds, then rise to 10mm place, liquid level top, monitoring seed crystal weight, if weight rises, illustrate that temperature is too low, produce crystallization, if weight declines, excess Temperature is described, dissolve seed crystal, according to changes in weight Modulating Power, re-start examination temperature, until changes in weight, in 1g, enters the stage of sowing.
Preferably, step 3) in, described is 30cm/min fast.
Preferably, step 4) in, seed crystal is dropped to the following 2mm of liquid level, first draw high at a slow speed, monitoring seed crystal weight, when seed crystal weight reaches after 10g, carries out soon, circulates and lift at a slow speed;
The described method of pulling up that circulates at a slow speed is soon: first lift at a slow speed 30 minutes, then Rapid lifting is 5 minutes, and circulation lifts, and after the seeding length that arrival arranges, enters the shouldering stage.
Preferably, step 4) in, the speed that draws high is at a slow speed 0.5mm/h, and Rapid lifting speed is 100mm/h, and the seeding length of setting is 60mm～80mm.
Preferably, step 5) in, lift at a slow speed seed crystal, at the uniform velocity reduce heating power, monitoring seed crystal weight, keeps seed crystal weight rate of rise in 30g/h, after arriving 5 kilograms, automatic seeding end of processing;
Wherein, the described speed that lifts at a slow speed seed crystal is 0.5mm/h, and the described speed that at the uniform velocity reduces heating power is 50W/h.
Technique effect
1, use method of the present invention to improve significantly the homogeneity of product.
2, more than having improved yield to 80% significantly.
3, the large-scale application of kyropoulos large-size crystals growth can be realized.
To the technique effect of design of the present invention, concrete structure and generation be described further below, to understand fully object of the present invention, feature and effect.
Embodiment
A kind of seeding method that the invention provides kyropoulos sapphire crystal growth, comprises the steps:
1) raw material melts
Raw material thaw process is by electric heating control, and increased power value is fixed as 4000W/ hour, and heating power is increased to 70000W; Now in stove, temperature is 2000 ± 50 ℃, continue to maintain heating power and remain unchanged 4 to 8 hours, in stove, temperature rises to 2140 ± 20 ℃ gradually, and temperature in stove being detected a larger decline process (20 to 30 ℃), now complete material process, enter next step.
2) row's bubble
At high temperature maintain the liquid state of raw material, by convection current, discharge the impurity in raw material, in order to avoid produce bubble in follow-up crystallisation process; Slowly adjust the power of heating, make solution temperature reach gradually the temperature of sowing.
Be embodied in crucible temperature is maintained to 2140 ℃, the time is 8 to 12 hours, then in 4 hours with 10 degree/hour speed be cooled to 2100 ℃, enter next stage.
3) examination temperature
Seed crystal from liquid level top 10mm fast-descending to liquid level under 30mm place, then fast lifting is to 10mm place, liquid level top, contrasts front and back seed crystal changes in weight, repeatedly adjusts crucible temperature, makes seed crystal changes in weight in ± 1g;
4) sow
Seed crystal is dropped to below liquid level, and the fast jogging speed by setting, alternately lifts crystallization, growth seeding;
5) shouldering
Lift at a slow speed seed crystal, at the uniform velocity reduce heating power, monitoring seed crystal weight, after seed crystal weight arrives 5 kilograms, automatic seeding end of processing.
Below in conjunction with embodiment, method of the present invention is described the JY85K-KY type optical crystal growth furnace that the equipment using in embodiment is produced for Shanghai Jia Yu Information Technology Co., Ltd.
Embodiment 1
The seeding method of the kyropoulos sapphire crystal growth of the present embodiment, comprises the steps:
1) raw material melts
Maintain furnace chamber vacuum tightness 10
-3more than Pa, start the heat-up rate with 4KW/h, heating power supply power is risen to 70KW; In temperature-rise period, monitoring burner hearth vacuum tightness, when lower than 10
-3during Pa, suspend and heat up, treat that vacuum reaches 10
-3after Pa is above, continue to heat up, vacuum is lower than 1 * 10 again
-2during Pa, end heating;
2) row's bubble
Be embodied in crucible temperature is maintained to 2140 ℃, the time is 8 to 12 hours, then in 4 hours with 10 degree/hour speed be cooled to 2100 ℃, enter next stage.
3) examination temperature
In row's bubble later stage, (10mm/h) reduces seed rod to 10mm place, liquid level top at a slow speed, and monitoring seed crystal weight, when appearanceization seed crystal phenomenon, illustrates excess Temperature, according to material speed, Modulating Power; Nothingization seed crystal phenomenon, can try temperature:
The first round, fast (30cm/min) is by seed crystal decline 40mm and then rising 40mm, monitoring seed crystal weight, if weight rises, illustrate that temperature is too low, produce crystallization, if weight declines, excess Temperature is described, dissolves seed crystal, according to changes in weight Modulating Power, re-start examination temperature, until seed crystal changes in weight is in 1g;
Second takes turns, and fast (30cm/min), by the seed crystal 40mm that declines, waited for for 10 seconds, and then rising 40mm, monitoring seed crystal weight, if weight rises, illustrate that temperature is too low, produce crystallization, if weight declines, excess Temperature is described, dissolve seed crystal, according to changes in weight Modulating Power, re-start examination temperature, until changes in weight, in 1g, enters the stage of sowing.
4) sow
Seed crystal is dropped to the following 2mm of liquid level, first draw high at a slow speed (0.5mm/h), monitoring seed crystal weight, when seed crystal weight reaches after 10g, carries out soon, circulates and lift at a slow speed;
The described method of pulling up that circulates at a slow speed is soon: first (0.5mm/h) lifts 30 minutes at a slow speed, and then Rapid lifting (100mm/h) is 5 minutes, and circulation lifts, and after the seeding length (60mm～80mm) that arrival arranges, enters the shouldering stage.
5) shouldering
(0.5mm/h) lifts seed crystal at a slow speed, with the speed of 50W/h, at the uniform velocity reduces heating power, and monitoring seed crystal weight keeps seed crystal weight rate of rise in 30g/h, after arriving 5 kilograms, and automatic seeding end of processing.
After testing, the present embodiment products obtained therefrom yield has reached 90%.
Adopt in the seeding process of present method enforcement, product homogeneity is good, and yield can reach more than at least 80%, compared with prior art has obvious technical superiority, has realized the large-scale application of kyropoulos large-size crystals growth.Meanwhile, above step can be by software control, reduces artificial interference factor, saves manpower, also the stability of keep-process at utmost.
More than describe preferred embodiment of the present invention in detail.Should be appreciated that those of ordinary skill in the art just can design according to the present invention make many modifications and variations without creative work.Therefore, all technician in the art, all should be in the determined protection domain by claims under this invention's idea on the basis of existing technology by the available technical scheme of logical analysis, reasoning, or a limited experiment.
Claims (10)
1. kyropoulos is prepared a seeding method for sapphire crystal, comprises the steps:
1) raw material melts
Material process is by electric heating control, and increased power value is fixed as 4000W/ hour, and final heating power is increased to 70000W, maintains heating power to raw material and has melted;
2) row's bubble
At high temperature maintain the liquid state of raw material, by convection current, discharge the impurity in raw material;
3) examination temperature
Put into seed crystal, and monitor seed crystal changes in weight, adjust crucible temperature, make seed crystal changes in weight in ± 1g;
4) sow
Seed crystal is dropped to below liquid level, lift crystallization, growth seeding;
5) shouldering
Lift at a slow speed seed crystal, at the uniform velocity reduce heating power, monitoring seed crystal weight, after seed crystal weight arrives 5 kilograms, automatic seeding end of processing.
2., the method for claim 1, wherein step 1), in raw material thaw process, maintain furnace chamber vacuum tightness 10
-3more than Pa; In temperature-rise period, monitoring burner hearth vacuum tightness, when lower than 10
-3during Pa, suspend and heat up, treat that vacuum reaches 10
-3after Pa is above, continue to heat up, vacuum is lower than 1 * 10 again
-2during Pa, end heating.
3. the method for claim 1, wherein step 1), increased power value is fixed as 4000W/ hour, and heating power is increased to 70000W; Now in stove, temperature is 2000 ± 50 ℃, continue to maintain heating power and remain unchanged 4 to 8 hours, in stove, temperature rises to 2140 ± 20 ℃ gradually, and temperature in stove being detected a larger decline process (20 to 30 ℃), now complete material process, enter next step.
4. the method for claim 1, wherein step 2), crucible temperature is maintained to 2140 ℃, the time is 8-12 hour, and then in 4 hours, the speed with 10 ℃/h is cooled to 2100 ℃, enters next stage.
5. the method for claim 1, wherein step 3), seed crystal from liquid level top 10mm fast-descending to liquid level under 30mm place, then fast lifting is to 10mm place, liquid level top, contrasts front and back seed crystal changes in weight, adjust crucible temperature, make seed crystal changes in weight in ± 1g.
6. the method for claim 1, wherein step 3), reduce at a slow speed seed rod to 20mm place, liquid level top, monitor seed crystal weight, when appearanceization seed crystal phenomenon, excess Temperature is described, according to material speed, Modulating Power; Nothingization seed crystal phenomenon, try temperature:
The first round, drops to seed crystal 30-40mm under liquid level fast, and then rises to 10mm place, liquid level top, monitoring seed crystal weight, if weight rises, illustrate that temperature is too low, produce crystallization, if weight declines, excess Temperature is described, dissolves seed crystal, according to changes in weight Modulating Power, re-start examination temperature, until seed crystal changes in weight is in 1g;
Second takes turns, and fast seed crystal is dropped to 30-40mm under liquid level, waits for for 10 seconds, then rise to 10mm place, liquid level top, monitoring seed crystal weight, if weight rises, illustrate that temperature is too low, produce crystallization, if weight declines, excess Temperature is described, dissolve seed crystal, according to changes in weight Modulating Power, re-start examination temperature, until changes in weight, in 1g, enters the stage of sowing.
7. method as claimed in claim 6, wherein, step 3) in, described is 30cm/min fast.
8. the method for claim 1, wherein step 4), seed crystal is dropped to the following 2mm of liquid level, first draw high at a slow speed, monitoring seed crystal weight, when seed crystal weight reaches after 10g, carries out soon, circulation lifts at a slow speed;
The described method of pulling up that circulates at a slow speed is soon: first lift at a slow speed 30 minutes, then Rapid lifting is 5 minutes, and circulation lifts, and after the seeding length that arrival arranges, enters the shouldering stage.
9. method as claimed in claim 8, wherein, step 4) in, the speed that draws high is at a slow speed 0.5mm/h, and Rapid lifting speed is 100mm/h, and the seeding length of setting is 60mm～80mm.
10. the method for claim 1, wherein step 5), lift at a slow speed seed crystal, at the uniform velocity reduce heating power, monitoring seed crystal weight, keeps seed crystal weight rate of rise in 30g/h, after arriving 5 kilograms, and automatic seeding end of processing
Wherein, the described speed that lifts at a slow speed seed crystal is 0.5mm/h, and the described speed that at the uniform velocity reduces heating power is 50W/h.
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| CN104695010A (en) * | 2014-12-26 | 2015-06-10 | 浙江东海蓝玉光电科技有限公司 | Improved Kyropulos method for quickly preparing large-size sapphire crystals |
| CN104711676A (en) * | 2015-03-16 | 2015-06-17 | 内蒙古京晶光电科技有限公司 | Gem single crystal growth method |
| CN105506738A (en) * | 2015-11-06 | 2016-04-20 | 浙江露通机电有限公司 | Seeding process for manufacturing sapphire crystal from sapphire fragments |
| CN105568369A (en) * | 2016-01-26 | 2016-05-11 | 中山大学 | Crystal feeding method for Czochralski method crystal growth and automatic crystal feeding equipment |
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| CN107653489A (en) * | 2017-09-15 | 2018-02-02 | 福建晶安光电有限公司 | A kind of growing method of crystal |
| CN107743531A (en) * | 2015-09-07 | 2018-02-27 | 韩国生产技术研究院 | The island position detecting device and method of melting furnace |
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| CN113699585A (en) * | 2021-09-03 | 2021-11-26 | 福建晶安光电有限公司 | Sapphire crystal growth process |
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| CN104695010B (en) * | 2014-12-26 | 2017-05-03 | 江西东海蓝玉光电科技有限公司 | Improved Kyropulos method for quickly preparing large-size sapphire crystals |
| CN104695010A (en) * | 2014-12-26 | 2015-06-10 | 浙江东海蓝玉光电科技有限公司 | Improved Kyropulos method for quickly preparing large-size sapphire crystals |
| CN104711676B (en) * | 2015-03-16 | 2017-05-24 | 内蒙古京晶光电科技有限公司 | Gem single crystal growth method |
| CN104711676A (en) * | 2015-03-16 | 2015-06-17 | 内蒙古京晶光电科技有限公司 | Gem single crystal growth method |
| CN107743531A (en) * | 2015-09-07 | 2018-02-27 | 韩国生产技术研究院 | The island position detecting device and method of melting furnace |
| CN105506738A (en) * | 2015-11-06 | 2016-04-20 | 浙江露通机电有限公司 | Seeding process for manufacturing sapphire crystal from sapphire fragments |
| CN105648529A (en) * | 2016-01-25 | 2016-06-08 | 福建福晶科技股份有限公司 | Simple seed crystal reinforcing method |
| CN105648521A (en) * | 2016-01-26 | 2016-06-08 | 中山大学 | Crystal growth method and device |
| CN105568369A (en) * | 2016-01-26 | 2016-05-11 | 中山大学 | Crystal feeding method for Czochralski method crystal growth and automatic crystal feeding equipment |
| CN105603512A (en) * | 2016-01-26 | 2016-05-25 | 中山大学 | Seeding temperature capturing method for crystal growth adopting czochralski method and automatic capturing equipment |
| CN105603512B (en) * | 2016-01-26 | 2018-10-16 | 中山大学 | A kind of lower brilliant temperature catching method and automatic capture equipment of method of crystal growth by crystal pulling |
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| CN105648521B (en) * | 2016-01-26 | 2018-10-30 | 中山大学 | A kind of growing method and equipment |
| CN107099839A (en) * | 2017-05-16 | 2017-08-29 | 内蒙古恒嘉晶体材料有限公司 | A kind of M is to the preparation technology and M of monocrystalline sapphire to monocrystalline sapphire |
| US11486054B2 (en) | 2017-09-15 | 2022-11-01 | Fujian Jing'an Optoelectronics Co., Ltd. | Method for growing crystal boule |
| CN107653489A (en) * | 2017-09-15 | 2018-02-02 | 福建晶安光电有限公司 | A kind of growing method of crystal |
| WO2019052210A1 (en) * | 2017-09-15 | 2019-03-21 | 福建晶安光电有限公司 | Crystal growing method |
| CN107653489B (en) * | 2017-09-15 | 2020-06-09 | 福建晶安光电有限公司 | Crystal growth method |
| CN108411361A (en) * | 2018-04-20 | 2018-08-17 | 何熠岑 | Storage medium, growing method and its system |
| CN108411361B (en) * | 2018-04-20 | 2023-01-06 | 何熠岑 | Storage medium, crystal growth method and system thereof |
| CN113699585B (en) * | 2021-09-03 | 2022-04-29 | 福建晶安光电有限公司 | Sapphire crystal growth process |
| CN113699585A (en) * | 2021-09-03 | 2021-11-26 | 福建晶安光电有限公司 | Sapphire crystal growth process |
| CN114318533A (en) * | 2021-12-28 | 2022-04-12 | 安徽科瑞思创晶体材料有限责任公司 | Intelligent control system for crystal growth |
| CN114775057A (en) * | 2022-06-23 | 2022-07-22 | 天通控股股份有限公司 | Method for growing 6-inch lithium tantalate crystal |
| CN114775057B (en) * | 2022-06-23 | 2022-09-23 | 天通控股股份有限公司 | Method for growing 6-inch lithium tantalate crystal |
| CN116411338A (en) * | 2023-06-12 | 2023-07-11 | 内蒙古晶环电子材料有限公司 | Material boiling process for producing sapphire single crystal |
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