CN103205799A - Method for growing C-oriented white stone crystals - Google Patents
Method for growing C-oriented white stone crystals Download PDFInfo
- Publication number
- CN103205799A CN103205799A CN2013101411232A CN201310141123A CN103205799A CN 103205799 A CN103205799 A CN 103205799A CN 2013101411232 A CN2013101411232 A CN 2013101411232A CN 201310141123 A CN201310141123 A CN 201310141123A CN 103205799 A CN103205799 A CN 103205799A
- Authority
- CN
- China
- Prior art keywords
- crystal
- crucible
- white stone
- white
- single crystal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention discloses a method for growing C-oriented white stone crystals, and belongs to the technical field of white stone production. The technical key point of the method comprises the following steps of: (1) in a growing furnace, placing precisely directed C-oriented white stone crystal seeds and aluminum oxide raw materials with the purity of over 99.95% in a flat crucible, wherein the crystal seed direction is C+/-0.5 degrees; (2) adjusting the distances among the crucible, a graphite heating body and a heat field in the growing furnace, wherein the geometric centers of the crucible, the graphite heating body and the heat field in the growing furnace are superposed; (3) sealing the furnace body, heating from room temperature; and meanwhile, starting a heat exchanger to cool the crystal seeds; (4) heating till the aluminum oxide raw materials and white stone crystal seeds are completely melted, maintaining the temperature for 5-10 hours, and then, increasing the helium flow in the heat exchanger to begin to establish the temperature gradient required by the C-oriented white stone crystals, wherein the solid-liquid interface between the molten body and the crystal seeds is propelled slowly from bottom to top in crystal seed part till all the molten bodies are crystallized; and (5) after slowly cooling the temperature in the furnace to room temperature, taking out the C-oriented white stone crystals. The invention aims to provide the method for growing C-oriented white stone crystals, wherein the method is simple to operate, energy-saving and high in work efficiency and is used for production of C-oriented white stone single crystals.
Description
Technical field
The present invention relates to a kind of preparation method of white stone, more particularly, relate in particular to a kind of C of growth to the method for white stone single crystal.
Background technology
White stone (pure alumina single crystal, be white stone again) owing to have high strength, high rigidity, high temperature resistant, wear-resisting wiping, chemical stability is good, ultraviolet-infrared transmittivity height, a series of good physical and chemical performances such as electrical insulation capability is good, so white gem crystal is not only important foundation material such as the epitaxially grown commercialization substrate of GaN of optoelectronic areas, account for market more than 95%, the large-scale integrated circuit substrate, the superconduction substrate, ferroelectric substrate, and be the important optical material of military field such as high-speed missile nose cone, infrared spectrum analyser, night vision equipment, scout instrument and the multispectral wide band window of guidance instrument, the photoelectric nacelle of aircraft, two generation Navsat with spaceborne hydrogen atomic clock white stone microwave resonance cavity material, high-energy laser output window material etc.
White gem crystal belongs to hexagonal system, have tangible anisotropy characteristics, there is evident difference in different directions in physical and chemical performance, optical property that is crystal etc., white gem crystal is uniaxial crystal, upwards there is not birefringent phenomenon in crystal property at C, and this crystal has unique optical axis, therefore compares with other crystal orientation white stones, C has especially laser window element etc. of most important applications such as LED substrate slice, optics to white gem crystal, and these application all need C to white gem crystal.
In sum, white gem crystal has become the indispensable core material of national defense industry, especially develops large size C to high quality white diamond material pressing for of modern national defense construction especially, has important strategic meaning and vast market prospect.
The method growth of white gem crystal has almost covered all artificial crystal growth methods such as flame method, hydrothermal method, falling crucible method, guided mode method, horizontal zone-melting technique, crystal pulling method, warm terraced method, kyropoulos and heat-exchanging method etc.Above-mentioned white gem crystal growth method generally all adopts A to growing technology, and especially the kyropoulos of growing large-size and heat-exchanging method technology also are to adopt A to growing technology.
Heat-exchanging method is the present unique method of the white gem crystal of stable growth overall dimension and high optical quality in the world, and following advantage is arranged:
1) be not easy to produce bubble and scattering particles in the crystal, bubble position can be controlled in the crystal bottom.
2) crystal stress is little, does not ftracture, so crystal yield rate height.
3) can stablize and produce in batches 110 kilograms of large size white gem crystals, crystal diameter 380mm at present.
4) the white gem crystal profile rule of heat-exchanging method growth, crystal utilization ratio height.
5) the heat-exchanging method growth cycle is shorter than kyropoulos, and power consumption is little, and cost is low.
6) heat-exchanging method growth white gem crystal has good expandability.
Because the special crystal-plane slip crystalline texture of white stone has determined C very difficult to white gem crystal production, lattice defect is many, and internal stress is big, and crystal growth is difficult to control, is difficult to produce the big perfect crystal of diameter.Therefore present nearly all white gem crystal growth all adopts direct growth A to crystal ingot, goes out C to the white stone finished product through directed post-treatment again, and the crystal utilization ratio is very low, and C is to the size-constrained system of crystal product.
The ordinary hot exchange process also be direct growth A to the white stone crystal ingot, its maximum diameter 375mm, can process maximum C is diameter 200mm to the white gem crystal product.The C that can produce in the world at present is 200mm to the white gem crystal maximum diameter.
Summary of the invention
The objective of the invention is at above-mentioned the deficiencies in the prior art, a kind of growth C of easy and simple to handle, energy-conservation and high efficiency is provided the method to the white stone single crystal.
Technical scheme of the present invention is achieved in that a kind of C of growth is to the method for white stone single crystal, wherein this method comprises the steps: that (1) is being in the growth furnace of Heating element with the graphite heater, to place flat crucible bottom central zone for the white stone seed crystal of (0001) direction through accurate pointing, the seed crystal direction requires to be C ± 0.5 degree direction, in the crucible of then the aluminium sesquioxide raw material of purity requirement more than 99.995% being packed into; (2) distance between the thermal field three in adjustment crucible, graphite heater and the growth furnace overlaps the geometric centre of the thermal field in crucible, heating element and the growth furnace; (3) closed furnace body is evacuated to vacuum tightness less than 10mtorr with vacuum in the stove, begins the heating that heats up from room temperature then; The circulated helium that starts simultaneously in the heat exchanger flows with the cooling seed body; (4) be warming up to aluminium sesquioxide raw material and white stone seed crystal all after the fusing, constant temperature 5～10 hours; (5) increase the interior helium gas flow of heat exchanger, set up C to the needed thermograde of white gem crystal; Solid-liquid interface between melt and seed crystal is bottom-up slow propelling from the seed crystal position, finishes until whole melt crystallizations; (6) after melt all crystallizes into white gem crystal, temperature in the stove slowly is down to room temperature after, close heating power supply, open growth furnace, take out C to white gem crystal.
Above-mentioned a kind of C that grows is in the method for white stone single crystal, and the described crucible of step (1) is molybdenum crucible or tungsten crucible or tungsten crucible, and described molybdenum crucible or tungsten crucible or the purity requirement of tungsten crucible are more than 99.5%.
Above-mentioned a kind of C that grows is in the method for white stone single crystal, and the described crucible of step (1) need be in stable vertical position state, can not tilt in the high growth temperature process, and heating element and thermal field should keep the distance of 20～40cm.
Above-mentioned a kind of C that grows after the described relative position with the thermal field in crucible, graphite heater and the growth furnace of step (2) is adjusted, adds a cover molybdenum matter or tungsten matter thermal baffle at crucible in the method for white stone single crystal.
Above-mentioned a kind of C that grows is in the method for white stone single crystal, and the described temperature rise rate of step (3) is 50～200 ℃/hour.
Above-mentioned a kind of C that grows is in the method for white stone single crystal, and the described helium gas flow of step (3) is 50 cubic feet/hour, and helium gas flow fluctuates less than 0.1 cubic feet/hour.
Above-mentioned a kind of C that grows is in the method for white stone single crystal, and the described increase helium gas flow of step (5) is specially: helium gas flow was increased to 600 cubic feet/hour from 50 cubic feet/hour in 200～260 hours.
Above-mentioned a kind of C that grows is in the method for white stone single crystal, and the described helium gas flow fluctuation of step (5) is less than 0.1 cubic feet/hour.Helium gas flow fluctuation is excessive, can make the lattice defect of production many, has a lot of dislocations, and stress is big, crystal even can ftracture when serious.
Above-mentioned a kind of C that grows is in the method for white stone single crystal, and the described C of step (6) is 100 kilograms to white gem crystal weight, and diameter is 15 inches.
After the present invention adopts aforesaid method, cooperate flat crucible that crystal is carried out melting crystal by adopting graphite heater, and the position relation between the thermal field three in strict control crucible, graphite heater and the growth furnace, to guarantee the normal growth of crystal.Simultaneously, thus further guarantee the formation of crystal by the fluctuation of strictness control helium gas flow.
Pass through the inventive method, successfully produced diameter 375mm C to white gem crystal, weigh 100 kilograms, maximum can process the C of diameter 370mm to white gem crystal such as various types of substrates sheet, laser window material etc., this technological breakthrough the C that grows in the world to the difficult problem of white gem crystal, also be at present in the world the C of overall dimension, maximum weight to the growing technology of white gem crystal.
1) can provide the C of maximum diameter to the white stone substrate material.As 8 inches-15 inches of diameters.The white stone substrate of main flow is 2 inches and 4 inches in the world at present.
2) can provide the C of 15 inches of maximum diameters to white stone light laser and optical window material.
3) can provide the C of special military use to white gem crystal.
4) A with identical weight (100Kg is example) compares to the white stone crystal ingot, is to do under the situation of substrate material equally, and C can multi-processing go out 80% product to the white stone crystal ingot, and namely crystal is worth increases by 80%, has very high economical efficiency.
5) white gem crystal of same size, C generally is higher than A to white stone product price 80%-100% to price.
So this invention technology not only can directly promote the value of white gem crystal that heat-exchanging method is produced, and can provide the above C of direct 200mm to the white gem crystal goods in batches, have very strong novelty, have strategic value and good economic benefits.
Embodiment
Below involutory specific embodiment the present invention is further illustrated, but do not constitute any limitation of the invention.
Embodiment 1
A kind of C that grows of the present invention is to the method for white stone single crystal, and this method comprises the steps:
(1) be in the growth furnace of Heating element with the graphite heater, to place the flat molybdenum crucible bottom centre zone of diameter 380 mm through accurate pointing for the high quality white jewel seed crystal of (0001) direction, then 100kg high purity aluminium oxide raw material is packed in the molybdenum crucible, the aluminium sesquioxide material purity is more than 99.995%, and the molybdenum crucible purity requirement is more than 99.5%;
(2) distance between the thermal field three in adjustment crucible, graphite heater and the growth furnace, the geometric centre that guarantees the thermal field in crucible, heating element and the growth furnace overlaps, crucible need be in stable vertical position state, in the high growth temperature process, can not tilt, in order to avoid contact with graphite heater, heating element and thermal field should keep the distance of 20cm, in order to avoid the contact back produces electric arc;
(3) after the relative position adjustment with the thermal field in crucible, graphite heater and the growth furnace, in order to reduce the volatilization of aluminium sesquioxide raw material under the high-temperature fusant state, add a cover molybdenum matter thermal baffle at crucible; Closed furnace body is evacuated to vacuum tightness 1mtorr with vacuum in the stove, begins the heating that heats up from room temperature, and temperature rise rate is 50 ℃/hour, and the too fast meeting of temperature rise rate causes crystal cleavage; The circulated helium that starts simultaneously in the heat exchanger flows with the cooling seed body, and 50 cubic feet/hour of flow sets prevent that seed crystal from ftractureing and melt in the body of heater temperature-rise period; The helium gas flow fluctuation is less than 0.1 cubic feet/hour; Helium gas flow fluctuation is excessive, can make the lattice defect of production many, has a lot of dislocations, and stress is big, crystal even can ftracture when serious;
(4) rise to 2045 when spending when temperature in the stove, aluminium sesquioxide raw material and white stone seed crystal begin fusing, after aluminium sesquioxide raw material and the whole fusings of white stone seed crystal, constant temperature 10 hours, increase the helium gas flow in the heat exchanger then, in 260 hours, be increased to 600 cubic feet/hour from 50 cubic feet/hour, begin to set up C to the needed thermograde of white gem crystal, the helium gas flow fluctuation is less than 0.1 cubic feet/hour, increase along with helium gas flow, the heat that goes out to take away from seed body also increases, and the temperature at seed body place also descends, and it is low that melt can produce temperature of lower, the phenomenon that upper temp is high, be that the temperature of different zones is inequality in the melt, i.e. thermograde, this is the most basic motivating force of growing crystal; Solid-liquid interface between melt and seed crystal is bottom-up slow propelling from the seed crystal position, finishes until whole melt crystallizations;
(5) after melt all crystallizes into white gem crystal, temperature in the stove slowly is down to room temperature after, close heating power supply, open growth furnace, take out C to white gem crystal.Crystal is very complete, transparent height, the diffraction 2q angle that adopts X-ray diffractometer to measure the white gem crystal of producing be 41 ° 40 ', be defined as C to white gem crystal.White gem crystal weight is 100 kilograms, and diameter is 15 inches.
Embodiment 2
A kind of C that grows of the present invention is to the method for white stone single crystal, and this method comprises the steps:
(1) be in the growth furnace of Heating element with the graphite heater, to place the flat tungsten crucible bottom centre zone of diameter 350mm through accurate pointing for the high quality white jewel seed crystal of (0001) direction, then 100kg high purity aluminium oxide raw material is packed in the tungsten crucible, the aluminium sesquioxide material purity is more than 99.995%, and the tungsten crucible purity requirement is more than 99.5%;
(2) distance between the thermal field three in adjustment crucible, graphite heater and the growth furnace, the geometric centre that guarantees the thermal field in tungsten crucible, heating element and the growth furnace overlaps, crucible need be in stable vertical position state, in the high growth temperature process, can not tilt, in order to avoid contact with graphite heater, heating element and thermal field should keep the distance of 30cm, in order to avoid the contact back produces electric arc;
(3) after the relative position adjustment with the thermal field in crucible, graphite heater and the growth furnace, in order to reduce the volatilization of aluminium sesquioxide raw material under the high-temperature fusant state, add a cover tungsten matter thermal baffle at tungsten crucible; Closed furnace body is evacuated to vacuum tightness 8mtorr with vacuum in the stove, begins the heating that heats up from room temperature, and temperature rise rate is 100 ℃/hour; The circulated helium that starts simultaneously in the heat exchanger flows with the cooling seed body, and 50 cubic feet/hour of flow sets prevent that seed crystal from ftractureing and melt in the body of heater temperature-rise period; The helium gas flow fluctuation is less than 0.1 cubic feet/hour;
(4) rise to 2045 when spending when temperature in the stove, aluminium sesquioxide raw material and white stone seed crystal begin fusing, after aluminium sesquioxide raw material and the whole fusings of white stone seed crystal, constant temperature 8 hours, increase the helium gas flow in the heat exchanger then, be increased to 600 cubic feet/hour from 50 cubic feet/hour in 230 hours, begin to set up C to the needed thermograde of white gem crystal, helium gas flow fluctuates less than 0.1 cubic feet/hour; Solid-liquid interface between melt and seed crystal is bottom-up slow propelling from the seed crystal position, finishes until whole melt crystallizations;
(5) after melt all crystallizes into white gem crystal, temperature in the stove slowly is down to room temperature after, close heating power supply, open growth furnace, take out C to white gem crystal.Crystal is very complete, transparent height, the diffraction 2q angle that adopts X-ray diffractometer to measure the white gem crystal of producing be 41 ° 50 ', be defined as C to white gem crystal.White gem crystal weight is 100 kilograms, and diameter is 350mm.
Embodiment 3
A kind of C that grows of the present invention is to the method for white stone single crystal, and this method comprises the steps:
(1) be in the growth furnace of Heating element with the graphite heater, to place the flat tungsten crucible bottom central zone of diameter 375mm through accurate pointing for the high quality white jewel seed crystal of (0001) direction, then 100kg high purity aluminium oxide raw material is packed in the molybdenum crucible, the aluminium sesquioxide material purity is more than 99.995%, and the purity requirement of tungsten crucible is more than 99.5%;
(2) distance between the thermal field three in adjustment tungsten crucible, graphite heater and the growth furnace, the geometric centre that guarantees tungsten crucible, heating element and thermal field overlaps, the tungsten crucible need be in stable vertical position state, in the high growth temperature process, can not tilt, in order to avoid contact with graphite heater, heating element and thermal field should keep the distance of 40cm, in order to avoid the contact back produces electric arc;
(3) after the relative position adjustment with the thermal field in tungsten crucible, graphite heater and the growth furnace, in order to reduce the volatilization of aluminium sesquioxide raw material under the high-temperature fusant state, add a cover molybdenum matter thermal baffle at the tungsten crucible; Closed furnace body is evacuated to vacuum tightness 10mtorr with vacuum in the stove, begins the heating that heats up from room temperature, and temperature rise rate is 200 ℃/hour; The circulated helium that starts simultaneously in the heat exchanger flows with the cooling seed body, and 50 cubic feet/hour of flow sets prevent that seed crystal from ftractureing and melt in the body of heater temperature-rise period; The helium gas flow fluctuation is less than 0.1 cubic feet/hour;
(4) rise to 2045 when spending when temperature in the stove, aluminium sesquioxide raw material and white stone seed crystal begin fusing, after aluminium sesquioxide raw material and the whole fusings of white stone seed crystal, constant temperature 5 hours, increase the helium gas flow in the heat exchanger then, be increased to 600 cubic feet/hour from 50 cubic feet/hour in 200 hours, begin to set up C to the needed thermograde of white gem crystal, helium gas flow fluctuates less than 0.1 cubic feet/hour; Solid-liquid interface between melt and seed crystal is bottom-up slow propelling from the seed crystal position, finishes until whole melt crystallizations;
(5) after melt all crystallizes into white gem crystal, temperature in the stove slowly is down to room temperature after, close heating power supply, open growth furnace, take out C to white gem crystal.Crystal is very complete, transparent height, the diffraction 2q angle that adopts X-ray diffractometer to measure the white gem crystal of producing be 41 ° 46 ', be defined as C to white gem crystal.White gem crystal weight is 100 kilograms, and diameter is 375mm.
Claims (9)
1. the method for C to the white stone single crystal of growing, it is characterized in that, this method comprises the steps: that (1) is being in the growth furnace of Heating element with the graphite heater, to place flat crucible bottom central zone for the white stone seed crystal of (0001) direction through accurate pointing, the seed crystal direction requires to be C ± 0.5 degree direction, in the crucible of then the aluminium sesquioxide raw material of purity requirement more than 99.995% being packed into; (2) distance between the thermal field three in adjustment crucible, graphite heater and the growth furnace overlaps the geometric centre of the thermal field in crucible, heating element and the growth furnace; (3) closed furnace body is evacuated to 1～10mtorr with vacuum in the stove, begins the heating that heats up from room temperature then; The circulated helium that starts simultaneously in the heat exchanger flows with the cooling seed body; (4) be warming up to aluminium sesquioxide raw material and white stone seed crystal all after the fusing, constant temperature 5～10 hours; (5) increase the interior helium gas flow of heat exchanger, set up C to the needed thermograde of white gem crystal; Solid-liquid interface between melt and seed crystal is bottom-up slow propelling from the seed crystal position, finishes until whole melt crystallizations; (6) after melt all crystallizes into white gem crystal, temperature in the stove slowly is down to room temperature after, close heating power supply, open growth furnace, take out C to white gem crystal.
2. a kind of C that grows according to claim 1 is characterized in that to the method for white stone single crystal the described crucible of step (1) is molybdenum crucible or tungsten crucible or tungsten crucible, and described molybdenum crucible or tungsten crucible or the purity requirement of tungsten crucible are more than 99.5%.
3. a kind of method of C to the white stone single crystal of growing according to claim 1, it is characterized in that, the described crucible of step (1) need be in stable vertical position state, can not tilt in the high growth temperature process, and heating element and thermal field should keep the distance of 20～40cm.
4. a kind of C that grows according to claim 1 is characterized in that to the method for white stone single crystal, after the described relative position with the thermal field in crucible, graphite heater and the growth furnace of step (2) is adjusted, adds a cover molybdenum matter or tungsten matter thermal baffle at crucible.
5. a kind of C that grows according to claim 1 is characterized in that to the method for white stone single crystal the described temperature rise rate of step (3) is 50～200 ℃/hour.
6. a kind of C that grows according to claim 1 is characterized in that to the method for white stone single crystal the described helium gas flow of step (3) is 50 cubic feet/hour, and helium gas flow fluctuates less than 0.1 cubic feet/hour.
7. a kind of method of C to the white stone single crystal of growing according to claim 1, it is characterized in that the described increase helium gas flow of step (5) is specially: helium gas flow was increased to 600 cubic feet/hour from 50 cubic feet/hour in 200～260 hours.
According to claim 1 or 7 described a kind of C that grow to the method for white stone single crystal, it is characterized in that the described helium gas flow fluctuation of step (5) is less than 0.1 cubic feet/hour.
9. a kind of C that grows according to claim 1 is characterized in that to the method for white stone single crystal the described C of step (6) is 100 kilograms to white gem crystal weight, and diameter is 15 inches.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101411232A CN103205799A (en) | 2013-04-23 | 2013-04-23 | Method for growing C-oriented white stone crystals |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101411232A CN103205799A (en) | 2013-04-23 | 2013-04-23 | Method for growing C-oriented white stone crystals |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103205799A true CN103205799A (en) | 2013-07-17 |
Family
ID=48753200
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2013101411232A Pending CN103205799A (en) | 2013-04-23 | 2013-04-23 | Method for growing C-oriented white stone crystals |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103205799A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103695995A (en) * | 2013-12-26 | 2014-04-02 | 贵州省高新光电材料及器件研究院有限公司 | Growing method of carbon-doped sapphire crystals |
| CN105369345A (en) * | 2015-12-03 | 2016-03-02 | 洛阳西格马炉业股份有限公司 | Crucible and preparation method for preparing sapphire single crystals |
| CN105401215A (en) * | 2015-12-03 | 2016-03-16 | 洛阳西格马炉业股份有限公司 | Device and method for preparing large-flake sapphire single crystals |
| CN106987903A (en) * | 2017-03-27 | 2017-07-28 | 宁夏佳晶科技有限公司 | A kind of improved large scale synthetic sapphire production technology |
| CN107130289A (en) * | 2017-06-13 | 2017-09-05 | 江苏吉星新材料有限公司 | A kind of growing method for improving heat exchange large size sapphire crystal |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3898051A (en) * | 1973-12-28 | 1975-08-05 | Crystal Syst | Crystal growing |
| CN102713027A (en) * | 2009-10-22 | 2012-10-03 | 先进再生能源有限责任公司 | Crystal growth methods and systems |
-
2013
- 2013-04-23 CN CN2013101411232A patent/CN103205799A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3898051A (en) * | 1973-12-28 | 1975-08-05 | Crystal Syst | Crystal growing |
| CN102713027A (en) * | 2009-10-22 | 2012-10-03 | 先进再生能源有限责任公司 | Crystal growth methods and systems |
Non-Patent Citations (2)
| Title |
|---|
| CHANDRA P. KHATTAK 等: "GROWTH OF NEAR-NET-SHAPED SAPPHIRE DOMES USING THE HEAT EXCHANGER METHOD", 《MATERIALS LETTERS》, vol. 7, no. 910, 31 January 1989 (1989-01-31), pages 318 - 321 * |
| 张雪平: "蓝宝石晶体生长与LED应用研究", 《中国优秀硕士学位论文全文数据库 信息科技辑》, no. 2, 15 February 2013 (2013-02-15) * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103695995A (en) * | 2013-12-26 | 2014-04-02 | 贵州省高新光电材料及器件研究院有限公司 | Growing method of carbon-doped sapphire crystals |
| CN103695995B (en) * | 2013-12-26 | 2015-11-25 | 贵州省高新光电材料及器件研究院有限公司 | A kind of growth method of carbon-doped sapphire crystal |
| CN105369345A (en) * | 2015-12-03 | 2016-03-02 | 洛阳西格马炉业股份有限公司 | Crucible and preparation method for preparing sapphire single crystals |
| CN105401215A (en) * | 2015-12-03 | 2016-03-16 | 洛阳西格马炉业股份有限公司 | Device and method for preparing large-flake sapphire single crystals |
| CN105401215B (en) * | 2015-12-03 | 2017-09-29 | 河南西格马晶体科技有限公司 | A kind of device and method for being used to prepare big sheet sapphire monocrystal |
| CN105369345B (en) * | 2015-12-03 | 2018-01-26 | 河南西格马晶体科技有限公司 | A kind of crucible and preparation method for being used to prepare sapphire monocrystal |
| CN106987903A (en) * | 2017-03-27 | 2017-07-28 | 宁夏佳晶科技有限公司 | A kind of improved large scale synthetic sapphire production technology |
| CN107130289A (en) * | 2017-06-13 | 2017-09-05 | 江苏吉星新材料有限公司 | A kind of growing method for improving heat exchange large size sapphire crystal |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102758249B (en) | A kind of preparation method of colourless boule monocrystal | |
| CN102628184B (en) | Method for growing gem crystals by way of vacuum induction heating and device realizing method | |
| CN101962798B (en) | Method and equipment for producing sapphire single crystal | |
| CN102289235B (en) | Heating control system and method based on top separated control polycrystalline silicon ingot casting furnace | |
| CN101935869B (en) | Crucible and substrate slice for growing and casting monocrystalline silicon | |
| CN103205799A (en) | Method for growing C-oriented white stone crystals | |
| CN101913636A (en) | Method for producing high-purity high-density alumina block material for sapphire single crystals | |
| CN102877117A (en) | Ingot furnace thermal field structure based on multi-heater and operation method | |
| CN104651935B (en) | A kind of method that crucible rise method prepares high-quality sapphire crystal | |
| CN103556223B (en) | A kind of method of growing large-size and square sapphire single-crystal | |
| CN103789835A (en) | Improved gradient freeze GaAs single crystal growing method | |
| US7972439B2 (en) | Method of growing single crystals from melt | |
| CN202989351U (en) | Ingot furnace thermal field structure based on multiple heaters | |
| CN102877129A (en) | Crystalline silicon and preparation method thereof | |
| CN103710741A (en) | Single crystal growth device and method | |
| CN102978694A (en) | Improved kyropoulos method for sapphire crystal growth | |
| CN102965727B (en) | Polycrystalline silicon ingot and casting method thereof | |
| CN103132142B (en) | Polycrystal silicon ingot and manufacture method thereof | |
| CN102758244A (en) | Compound heating-type Czochralski polycrystalline silicon or monocrystal silicon preparation technology | |
| CN103243380A (en) | Horizontally directional zone-melting crystallization preparation method for large-size Re:YAG series of laser crystals | |
| CN104073875A (en) | Preparation method of large-size sapphire crystal dynamic temperature field | |
| CN104120488A (en) | Dynamic-temperature-field preparation method for large-size C-axis sapphire crystal | |
| CN101597787A (en) | Under nitrogen, cast the method for the controlled doped monocrystalline silicon of nitrogen concentration | |
| CN103422163A (en) | Device and method for growing sapphire single crystals | |
| CN203530480U (en) | Equipment for growing sapphire single crystals |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130717 |