CN103103604A - Manufacturing method of large-size C-oriented sapphire crystals - Google Patents
Manufacturing method of large-size C-oriented sapphire crystals Download PDFInfo
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- CN103103604A CN103103604A CN2013100262508A CN201310026250A CN103103604A CN 103103604 A CN103103604 A CN 103103604A CN 2013100262508 A CN2013100262508 A CN 2013100262508A CN 201310026250 A CN201310026250 A CN 201310026250A CN 103103604 A CN103103604 A CN 103103604A
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- 239000013078 crystal Substances 0.000 title claims abstract description 112
- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 35
- 239000010980 sapphire Substances 0.000 title claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 title abstract description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000000034 method Methods 0.000 claims abstract description 44
- 239000007788 liquid Substances 0.000 claims abstract description 34
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 32
- 239000010937 tungsten Substances 0.000 claims abstract description 32
- 229910052786 argon Inorganic materials 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000010899 nucleation Methods 0.000 claims abstract description 10
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Abstract
The invention relates to a manufacturing method of large-size C-oriented sapphire crystals. According to the method, an alumina raw material with the high purity of 99.999 wt% is adopted and is heated to be molten and subjected to crystal seeding and crystal growing. A main heater and an assistant heater are adopted, wherein a tungsten rod cylinder-shaped heating body is arranged around a crucible and is used as the main heater; another tungsten disc-shaped heating body is arranged at the bottom of the crucible and is be used as the assistant heater; the power ratio of the main heater to the assistant heater is (20 to 80 KW): (10 to 60 KW). In addition, a tungsten tube is mounted at the top of the crucible, and argon is introduced into the tungsten tube to regulate the temperature of the seed crystal and a liquid surface. As the method is used, the temperature distribution of a longitudinal temperature field in the crucible is improved, so that air bubbles, cracks and other defects are avoided or reduced, i.e., the seed crystal is prevented from being molten at overhigh temperature during the crystal seeding process. Therefore, the generation of a C-oriented long crystal boundary with a small angle is controlled effectively. As a result, the growing C-oriented crystals with the diameter of 14 inches are good in position staggering density and single crystal performance. Consequently, the method provided by the invention reaches the international advanced level.
Description
Technical field
The invention belongs to a kind of manufacture method of sapphire monocrystal, particularly relate to a kind of large size (14 inches of crystal maximum diameters) C to the growth method of sapphire single-crystal.
Background technology
Sapphire has fusing point high (2045 ℃), hardness is high, and (Mohs is 9, be only second to diamond), light transmission is good (has very high transmittance in ultraviolet, visible, infrared band scope, in 3-5 μ m transmitance up to 85%), capability of resistance to radiation is strong, tensile strength is high, anticorrosive, thermal conductivity is high, thermal shock resistance waits well good performance, become most popular Oxide substrate materials, mainly as semiconductor film substrate material, LED chip substrate material, large-scale integrated circuit substrate etc.The good window material of sapphire crystal or infrared military device, guided missile, submarine, satellite spatial technology, detection and high power strong laser etc. in addition, high-end watch dial, mobile phone surface, cell-phone camera head-shield and medical facilities such as use at the high-quality optical material.
the LED illumination is energy-conservation owing to having, brightness is high, the long Core Superiority that waits of life-span, be widely applied rapidly in the whole world, the big area of LED illumination is universal, also driven the fast development of sapphire industry, 2 cun Sapphire Substrate prices were once reaching 35 dollars in 2010, under the ordering about of juice, the investment tide has appearred in domestic sapphire industry, according to incompletely statistics, in two years short, the enterprise of new upper sapphire project is up to family more than 40, greatly aggravated the competition of sapphire industry, 2012, be subjected to that global economy is dispirited to be affected, the sapphire industry is inflicted heavy losses on, 2 cun Sapphire Substrate prices are hovered between the 8-10 dollar, how to reduce production costs, improve competitive edge and be the urgent difficult problem that sapphire enterprise faces.
The growth method of sapphire crystal mainly contains: crystal pulling method (CZ method), kyropoulos (KY method), heat-exchanging method (HEM method), lead embrane method (EFG method), warm terraced method (TGT method) etc.
The A of kyropoulos (KY method) growth is good to crystal mass, but exists large size production qualification rate low, and A is to growth, and C is to drawing rod, the low deficiency that waits of material use efficiency.
Take CZ method and falling crucible method etc. as main C to long brilliant method, level of automation is high, C is to growth, C is to drawing rod, and material use efficiency is high, but exists crystal dislocation density high, be prone to the low angle boundary defective, size be difficult to do greatly (generally can only accomplish at present diameter below 8 inches (weight 30Kg is following) both at home and abroad, iridium crucible is with high costs, production efficiency is low wait not enough.
The developing direction in sapphire crystal future is high-quality, large size, direct growth C to, improve material use efficiency, reduce costs.
But the lattice deformability degree of growth C during to sapphire single-crystal is obviously greater than other direction, and due to the anisotropy of sapphire single-crystal, any heterogeneous nucleation all easily causes the cracking of sapphire single-crystal.Therefore, direct growth large size, high-quality C are higher to the sapphire crystal difficulty.
Summary of the invention
The present invention is directed to existing KY method and C to the deficiency of long brilliant method, provide a kind of novel large size C to the sapphire growth technology, not only size can be accomplished 14 inches (weight 80Kg), realize that C is to growth, also make the indexs such as dislocation desity, monocrystalline reach the level of KY method crystal, also avoided preferably in addition the generation of low angle boundary defective.
The technical solution used in the present invention is:
First aspect, large size C provided by the invention is to growth method of sapphire single crystal, adopt the high purity aluminium oxide of 99.999wt%, be placed in tungsten crucible, tungsten well heater and tungsten lagging material are installed, install temperature thermocouple, the sealing furnace chamber also installs camera, starts watch-dog and registering instrument, and heating schedule is set in automatic control program, vacuumize, vacuum tightness reaches 10
-4Pa, temperature rise rate are 200 ℃/h; Intensification is melted alumina raw material, by means of infrared thermometer, the liquid level temperature is controlled between 2050 ℃～2070 ℃, and the liquid level flow line is clear evenly, and reaches steady state; With the seed crystal slow decreasing, the Touch liquid level; Rapid lifting growth neck; Slow pulling growth shoulder; The isometrical section of little pulling growth, extremely long crystalline substance is completed; Lower the temperature, take out crystal; With crystal processing in flakes, use the KOH corrosion, adopt dislocation desity, light transmission and the monocrystalline of X ray TOPO GRAPHY, microscope, scanning electron microscope and spectrophotometer test crystal; It is characterized in that: described tungsten well heater is major and minor double-heater, wherein adopting tungsten bar round shape heating element in the crucible surrounding is primary heater, adopting tungsten disc heating element in crucible bottom is secondary heater, by adjusting the power ratio of major and minor well heater, form the thermograde of stable suitable growing high quality crystal.
As preferably, the ratio of described major and minor heater power is 20～80KW: 10～60KW.
As further preferred, the ratio of described major and minor heater power is 40～60KW: 20～40KW.
Second aspect, large size C provided by the invention is to growth method of sapphire single crystal, adopt the high purity aluminium oxide of 99.999wt%, be placed in tungsten crucible, tungsten well heater and tungsten lagging material are installed, install temperature thermocouple, the sealing furnace chamber also installs camera, starts watch-dog and registering instrument, and heating schedule is set in automatic control program, vacuumize, vacuum tightness reaches 10
-4Pa, temperature rise rate are 200 ℃/h; Intensification is melted alumina raw material, by means of infrared thermometer, the liquid level temperature is controlled between 2050 ℃～2070 ℃, and the liquid level flow line is clear evenly, and reaches steady state; With the seed crystal slow decreasing, the Touch liquid level; Rapid lifting growth neck; Slow pulling growth shoulder; The isometrical section of little pulling growth, extremely long crystalline substance is completed; Lower the temperature, take out crystal; With crystal processing in flakes, use the KOH corrosion, adopt X ray TOPO GRAPHY
,Dislocation desity, light transmission and the monocrystalline of microscope, scanning electron microscope and spectrophotometer test crystal; It is characterized in that: described tungsten well heater is major and minor double-heater, wherein adopting tungsten bar round shape heating element in the crucible surrounding is primary heater, adopting tungsten disc heating element in crucible bottom is secondary heater, by adjusting the power ratio of major and minor well heater, form the thermograde of stable suitable growing high quality crystal; And, at the crucible top, apart from liquid levels 30～60mm place, the tungsten pipe is installed, and logical argon gas, be used for regulating the temperature of seed crystal when seeding, prevent because of excess Temperature, the situation of fusing appears in seed crystal, and is used for regulating the speed of crystal growth when shouldering, form rational thermograde, the cracking from growing large-size C to crystal and the low angle boundary problem that are prone to when solving.
As preferably, the ratio of described major and minor heater power is 20～80KW: 10～60KW.
As further preferred, the ratio of described major and minor heater power is 40～60KW: 20～40KW.
As preferably, in seeding and shouldering process, described argon flow amount is 1～20L/min.
As further preferred, in seeding and shouldering process, described argon flow amount is 5～15L/min.
In the present invention, described Rapid lifting growth neck is the pull rate growth neck with 1mm/h～3mm/h; Slowly the pulling growth shoulder is the pull rate growth shoulder with 0.5mm/h～2mm/h; The isometrical section of little pulling growth is the isometrical section of pull rate growth with 0.2mm/h～1mm/h.
Research is found, adopts double-heater in Sapphire Crystal Growth process of the present invention, regulates seed temperature and liquid level temperature by argon gas, has following beneficial effect.
(1) improve the temperature distribution of longitudinal temperature field in crucible, avoid or reduce the generation of the defectives such as bubble, cracking.
traditional KY method is long brilliant, the general birdcage well heater that adopts more, this type of heating can only be used for growth small size crystal (50Kg is following), because (generally below 260mm) is less for crucible diameter, the longitudinal temperature distribution that laterally reaches in crucible is easily controlled, thermograde is less, the crystal mass of growth is better, if but the larger sized crystal of growing (14 inches of diameters), the diameter of crucible just must be greater than 430mm so, if so large crucible still uses single birdcage heating element, in crucible laterally and the longitudinal temperature field be difficult to control, and thermograde is very large, especially crucible inner melt core temperature point is very low, when long brilliant longitudinally the speed of growth far above horizontal growth, easily long brilliant failure, even long brilliant success, crystal also is easy to produce bubble, polycrystalline, cracking, the defectives such as dislocation.As long as sapphire exists radial symmetry gradient and longitudinal temperature gradient in long brilliant process, in melt, thermal motion will appear, cause solid-liquid interface place crystal to exist thermal stresses, the critical stress that surpasses crystalline material, make the crystals particle arrange slippage mutually between distortion, former sub-queue, no longer meet the Methodistic arrangement of ideal lattice and form the defective of wire, will produce dislocation in crystal.
In addition due to C to the natural growing direction that is not crystal, so growth C is more much bigger to the crystal difficulty than growth A to crystal, must design more reasonably laterally reach thermograde longitudinally, adopt double-heater can effectively solve this outstanding problem, the crucible surrounding adopts the drum type brake well heater, crucible bottom is used the disc well heater, and two well heaters form rational power ratio, can reach the purpose of longitudinal temperature field and transverse temperature field in reasonable control crucible.
(2) regulate seed crystal and liquid level temperature, when guaranteeing seeding, seed crystal can not melt because of excess Temperature, in addition by the adjusting of argon flow amount, can adjust long brilliant needed rational temperature spot.
Traditional A to long crystalline substance be generally seed crystal Touch after liquid level, just begin slowly long brilliantly, temperature spot is lower than the fusing point of seed crystal, so the situation that general seed crystal can not occur fusing.
C to long brilliant when the Touch to the requirement of temperature spot than A to long brilliant strict many, Touch point temperature must be accurate control, reach the solid-liquid stagnation point, seed crystal cannot not reach moltenly not long good order and condition, after 1～3h in liquid, and then slow cooling, begin longly brilliant, this growth C must strictly control well during to crystal, otherwise the defectives such as polycrystalline, cracking can appear in crystal.
Owing to there is no steady in a long-termly accurately to measure the thermopair of 2050 ℃, so reasonably long brilliant temperature spot is controlled substantially and judged according to the fusing situation of seed crystal by accurate weighing system (being accurate to 1g), reduce again certain power after the little fusing of general requirement seed crystal and reach C to long brilliant rational temperature spot.But in actual seeding process, seed crystal is fusing fully usually, causes the seeding failure.
We pass through at the crucible top, apart from liquid levels 30～60mm place, the tungsten pipe is installed, and the mode of logical argon gas is come the regulating liquid surface temperature, before Touch, the seed crystal slow decreasing is extremely apart from liquid level 10～30mm place, and argon flow amount is 1～20L/min, observe the changes in weight of seed crystal this moment, if seed crystal weight is constant, slowly turn argon flow amount down, if the seed crystal fusing, strengthen argon flow amount, and minimizing power, after 1～3h, then turn argon flow amount down, repeatable operation like this is until adjust the brilliant temperature spot of rational length.
(3) can effectively control C to the generation of long brilliant low angle boundary.
C is low angle boundary to the most incidental defective of long crystalline substance, from A to long brilliant (low angle boundary can disappear) different be that low angle boundary not only can not disappear, and can enlarge gradually in case produce, and affect the excellent rate that gets of crystal.
Crystal is grown too fast or excessively slow when growth neck and shoulder, all the polycrystalline defective can occur, must control the speed of growth in certain scope, at this moment, can regulate long brilliant speed by increase and decrease power, but because melt in crucible is more, thermal capacity is larger, the increase and decrease power temperature of trace needs long time just can display, can not in time control flexibly, at this moment, by adjusting the flow of argon gas, the generation of low angle boundary is effectively avoided and reduced to the brilliant speed of the length of can rectifying a deviation timely.
Compare to long brilliant method (take the CZ method with falling crucible method as representative) growing sapphire single crystal technology with original KY method and C, the present invention has high, with short production cycle, the long brilliant good stability of level of automation, qualification rate advantages of higher, and the sapphire crystal of the present invention's preparation has that size large (14 inches of crystal maximum diameters), weight large (80Kg), bubble are few, the low (≤1000ps/cm of dislocation desity
2), the characteristics such as monocrystalline good (≤15 second of arc), can satisfy preferably the requirement of MOCVD extension LED chip, C to long brilliant, adopts and vertically draws rod in addition, gets excellent rate high, has lower cost, possesses core competitive.
Description of drawings
Fig. 1 is crystal monocrystalline property testing figure (＜15 second of arc).
Fig. 2 is crystal dislocation density measurement figure (＜1000ps/cm
2).
Fig. 3 is crystal TOPO GRAPHY surface reflection figure.
Embodiment
(1) main composition batching, cake and the part irregularly shaped particles of the high purity aluminium oxide diameter 50mm of 99.999wt% shown in employing table 1;
(2) filler: the alumina raw material that weighs up is put into crucible, intersect between cake and put, liquid splash when preventing from melting, and fill irregularly shaped particles;
(3) adjustment installs well heater and thermal field: adjust and install tungsten double-heater and tungsten thermal field, the sealing furnace chamber also installs camera, C is installed to 30 * 30mm seed crystal, and adjust the position (according to Theoretical Calculation, seed crystal is rested on liquid level top apart from liquid level 200mm place), startup watch-dog and registering instrument.
(4) heating: heating schedule is set in automatic control program, primary heater power is set between 20KW～80KW, secondary heater power is set between 10KW～60KW, 200 ℃/h of heat-up rate vacuumizes in stove, and vacuum tightness reaches 10
-4Pa.
(5) raw material melts: adopt the heating schedule that sets, intensification is melted alumina raw material, can experience to melt → solidify in melting process → melt repeatedly, finally reaches complete melted state.
(6) adjust the liquid level temperature: by Modulating Power, the liquid level temperature is adjusted, by means of infrared thermometer, the liquid level temperature is controlled between 2050 ℃～2060 ℃, the liquid level flow line is clear evenly, and reaches steady state.
(7) transfer seed crystal: with the speed slow decreasing of seed crystal according to 40mm/h～60mm/h, drop to the place apart from liquid level 10mm-30mm, by increase and decrease power, above adjusting crucible, (1L/min～20L/min) adjust crucible central liquid temperature point reaches 2050 ℃～2060 ℃ to the tungsten pipe high-purity argon gas amount of being filled with.
(8) seed crystal touches liquid level: seed crystal is touched liquid level according to the speed of 1mm/min～3mm/min, touch after liquid level the changes in weight by high-precision weighing systematic observation seed crystal, according to the program adjustment increase and decrease power of growth or fusing with adjust the crucible top tungsten pipe high-purity argon gas amount of being filled with (1L/min～20L/min), until reach stable, seed crystal cannot not be in moltenly not long state, after 1～3h, beginning slow decreasing power begins long brilliant.
(9) neck growth: with the pull rate of 1mm/h～3mm/h, the neck of the speed growing crystal of 10g/h～30g/h is if long brilliant speed departs from, by adjusting the crucible top tungsten pipe high-purity argon gas amount of being filled with (1L/min～20L/min) rectify a deviation.
(10) shoulder growth: with the pull rate of 0.5mm/h～2mm/h, slow decreasing power, shoulder with the speed growing crystal of 50g/h～150g/h, if long brilliant speed departs from, (1L/min～20L/min) rectify a deviation is when the shoulder growth is completed by the tungsten pipe high-purity argon gas amount of being filled with above adjusting crucible, guaranteeing in long brilliant speed 100g/h～600g/h situation, progressively turn down the high-purity argon gas amount of being filled with, until flow is down to 0, stop being filled with of argon gas.
(11) isometrical growth: with the pull rate of 0.2mm/h～1mm/h, slow decreasing power carries out the growth of the isometrical section of crystal, until long crystalline substance is completed.
(12) cooling: major and minor well heater cooling process is set, is cooled to 1600 ℃ with the cooling rate of 20 ℃/h～40 ℃/h, then be cooled to room temperature with the cooling rate of 60 ℃/h～120 ℃/h, and power descend complete after, be filled with argon gas and carry out cooling fast.
(13) get crystal: close heating power supply, close argon gas, open stove, take out crystal.
(14) crystal detects: detect the light transmission rate of crystal with the printing opacity instrument, with crystal processing in flakes, and use the KOH corrosion, adopt X ray TOPO GRAPHY
,Dislocation desity, light transmission and the monocrystalline of microscope, scanning electron microscope and spectrophotometer test crystal.
The purity requirement of table 1 alumina raw material
| Sequence number | Project | Content (weight) |
| 1 | Al 2O 3，% | ≥99.999 |
| 2 | Si，ppm | ≤2 |
| 3 | Fe，ppm | ≤2 |
| 4 | Mg，ppm | ≤1 |
| 5 | Na，ppm | ≤3 |
| 6 | Ca，ppm | ≤1 |
The equipment of growing sapphire crystal is resistance heading furnace, and its composition can be divided into following nine parts:
(1) power cabinet: for resistive heating provides power supply.
(2) body of heater: comprise well heater, crucible, crucible supporting system, tungsten thermal field and annex and lift weighing system.
(3) housing: comprise accurately controlling of voltage, electric current, heating and rate of cooling, long brilliant speed.
(4) lift weighing device: control pull rate, can accurately measure in real time the weight of crystal growth, lift the weighing system precision and reach 1g.
(5) cooling water system: utilize water-cooling pattern to control the stability of furnace body temperature, temperature remains on 23 ℃～28 ℃.
(6) system of supervision: high-definition camera and professional watch-dog can monitor the convection current situation of liquid level and grow brilliant situation.
(7) Research on Automatic Measuring System of Temperature: adopt infrared thermometer, in time test fluid surface temperature.
(8) thermopair: be placed in crucible bottom and crucible sidepiece, can show the temperature curve in raw material fusing and long brilliant process.
(9) registering instrument: heating power curve, crystal weight change curve and electric thermo-couple temperature curve record can be got off.
Experiment shows, large size C provided by the invention is to growth method of sapphire single crystal, the C of the diameter 14 inches (80Kg) that grows out is to crystal, the key indexs such as the dislocation desity of crystal, monocrystalline are better, reached international most advanced level, the index test result of crystal such as Fig. 1, Fig. 2 and shown in Figure 3.
Claims (6)
1. a large size C is to growth method of sapphire single crystal, adopt the high purity aluminium oxide of 99.999wt%, be placed in tungsten crucible, tungsten well heater and tungsten lagging material are installed, are installed temperature thermocouple, the sealing furnace chamber also installs camera, start watch-dog and registering instrument, heating schedule is set in automatic control program, vacuumizes, vacuum tightness reaches 10
-4Pa, temperature rise rate are 200 ℃/h; Intensification is melted alumina raw material, by means of infrared thermometer, the liquid level temperature is controlled between 2050 ℃～2070 ℃, and the liquid level flow line is clear evenly, and reaches steady state; With the seed crystal slow decreasing, the Touch liquid level; Rapid lifting growth neck; Slow pulling growth shoulder; The isometrical section of little pulling growth, extremely long crystalline substance is completed; Lower the temperature, take out crystal; With crystal processing in flakes, use the KOH corrosion, adopt X ray
TOPO GRAPHY,Dislocation desity, light transmission and the monocrystalline of microscope, scanning electron microscope and spectrophotometer test crystal; It is characterized in that: described tungsten well heater is major and minor double-heater, wherein adopting tungsten bar round shape heating element in the crucible surrounding is primary heater, adopting tungsten disc heating element in crucible bottom is secondary heater, by adjusting the power ratio of major and minor well heater, form the thermograde of stable suitable growing high quality crystal.
2. large size C according to claim 1 to growth method of sapphire single crystal, is characterized in that: the ratio of described major and minor heater power is 20～80KW: 10～60KW.
3. large size C according to claim 2 to growth method of sapphire single crystal, is characterized in that: the ratio of described major and minor heater power is 40～60KW: 20～40KW.
4. large size C according to claim 1 is to growth method of sapphire single crystal, it is characterized in that: at the crucible top, apart from liquid levels 30～60mm place, the tungsten pipe is installed, and logical argon gas, be used for regulating the temperature of seed crystal when seeding, prevent because of excess Temperature, the situation of fusing appears in seed crystal, and the speed that is used for regulating crystal during shouldering, form rational thermograde, the cracking from growing large-size C to crystal and the low angle boundary problem that are prone to when solving.
5. large size C according to claim 4 to growth method of sapphire single crystal, is characterized in that: described argon flow amount is 1～20L/min.
6. large size C according to claim 5 to growth method of sapphire single crystal, is characterized in that: described argon flow amount is 5～15L/min.
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| CN104775152A (en) * | 2015-03-16 | 2015-07-15 | 内蒙古京晶光电科技有限公司 | Automatic growth control method of sapphire (80-150 kg) monocrystalline |
| CN105160286A (en) * | 2015-06-18 | 2015-12-16 | 江苏苏创光学器材有限公司 | Preparation method of sapphire fingerprint identification panel |
| CN105154968A (en) * | 2015-06-18 | 2015-12-16 | 江苏苏创光学器材有限公司 | Preparation method for sapphire LED filament substrate |
| CN105183206A (en) * | 2015-06-18 | 2015-12-23 | 江苏苏创光学器材有限公司 | Production method of sapphire fingerprint identification panel |
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| CN105401211A (en) * | 2014-08-08 | 2016-03-16 | 上海超硅半导体有限公司 | Crystal growing furnace and method for drawing C-axis sapphire single crystal |
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| CN104775152B (en) * | 2015-03-16 | 2017-06-30 | 内蒙古京晶光电科技有限公司 | A kind of automatic growth control method of 80 150kg jewel monocrystalline |
| 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 |
| CN105154968A (en) * | 2015-06-18 | 2015-12-16 | 江苏苏创光学器材有限公司 | Preparation method for sapphire LED filament substrate |
| CN105183207A (en) * | 2015-06-18 | 2015-12-23 | 江苏苏创光学器材有限公司 | Manufacturing method of sapphire borderless touch screen panel |
| CN105183206A (en) * | 2015-06-18 | 2015-12-23 | 江苏苏创光学器材有限公司 | Production method of sapphire fingerprint identification panel |
| CN105160286A (en) * | 2015-06-18 | 2015-12-16 | 江苏苏创光学器材有限公司 | Preparation method of sapphire fingerprint identification panel |
| 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 |
| CN109112631A (en) * | 2018-10-29 | 2019-01-01 | 浙江昀丰新材料科技股份有限公司 | A kind of sapphire C is to long crystal method |
| CN114318494A (en) * | 2021-11-30 | 2022-04-12 | 江苏吉星新材料有限公司 | Method for reducing crystal growth defects of sapphire crystal and sapphire crystal growth furnace |
| CN114318494B (en) * | 2021-11-30 | 2023-09-19 | 江苏吉星新材料有限公司 | Method for reducing sapphire crystal growth defect and sapphire crystal growth furnace |
| CN115446671A (en) * | 2022-11-10 | 2022-12-09 | 天通控股股份有限公司 | Preparation method of sapphire spherical crystal |
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