CN104264224A - Growth method of large-size square sapphire crystal - Google Patents
Growth method of large-size square sapphire crystal Download PDFInfo
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- CN104264224A CN104264224A CN201410481654.0A CN201410481654A CN104264224A CN 104264224 A CN104264224 A CN 104264224A CN 201410481654 A CN201410481654 A CN 201410481654A CN 104264224 A CN104264224 A CN 104264224A
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- 239000013078 crystal Substances 0.000 title claims abstract description 79
- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 41
- 239000010980 sapphire Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 29
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 17
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 15
- 239000010937 tungsten Substances 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 12
- 230000005540 biological transmission Effects 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 238000012360 testing method Methods 0.000 claims description 5
- 238000002109 crystal growth method Methods 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 238000004854 X-ray topography Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 230000007797 corrosion Effects 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000012774 insulation material Substances 0.000 abstract 2
- MGRWKWACZDFZJT-UHFFFAOYSA-N molybdenum tungsten Chemical compound [Mo].[W] MGRWKWACZDFZJT-UHFFFAOYSA-N 0.000 abstract 2
- 230000007423 decrease Effects 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 238000013461 design Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 235000015895 biscuits Nutrition 0.000 description 1
- 230000036760 body temperature Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/20—Aluminium oxides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a growth method of large-size square sapphire crystal. The maximal side length of the crystal is 320*320mm; 99.999wt% high-purity aluminium oxide is adopted and is put in a tungsten crucible; a tungsten heater and a tungsten-molybdenum thermal insulation material are arranged; the tungsten-molybdenum thermal insulation material is square; the heater is square; and the crucible is square. According to the square sapphire crystal ingot, formed by the method disclosed by the invention, the utilization rate of materials is increased, for example, a square crystal rod for a screen of an iPhone 5S model is hollowed out from 100Kg of sapphire crystal ingot; the utilization rate of the materials can reach 60%-70%; and the production cost is reduced by 20%-30%.
Description
Technical field
The invention belongs to a kind of manufacture method of sapphire monocrystal, particularly relate to the growth method of a kind of large size square (crystal maximal side 320mm × 320mm) sapphire crystal.
Background technology
Sapphire has fusing point high (2045 DEG C), hardness is high, and (Mohs is 9, be only second to diamond), light transmission is good (has very high transmittance within the scope of ultraviolet, visible, infrared band, 3-5 μm of transmitance up to 85%), capability of resistance to radiation is strong, tensile strength is high, anticorrosive, thermal conductivity is high, the performance that thermal shock resistance is well etc. good, become most popular Oxide substrate materials, main as semiconductor film substrate material, LED chip substrate material, large-scale integrated circuit substrate etc.The excellent window material of sapphire crystal or infrared military equipment, guided missile, submarine, satellite spatial technology, detection and high power strong laser etc. in addition, the high-quality optical materials such as high-end watch dial, mobile phone surface, cell-phone camera head-shield and medical facilities use.
Sapphire new opplication is a dark horse; these 2 years; the application of sapphire in consumer electronics has exceeded traditional LED substrate application; except mobile lens protective cover, fingerprint recognition Home key use the circular polished section of sapphire; application on intelligent watch, mobile phone screen also grows with each passing day, and size is increasing.
In the end of the year 2013, apple and GTAT company sign the sapphire order of value 5.78 hundred million dollars, buy out the supply of material of the said firm's next three years, allow sapphire become the market focus of attention at one stroke.In fact, to be applied to mobile phone faceplate long-standing for sapphire.2002, luxurious mobile phone brand VERTU mobile phone selected sapphire as display screen cover plate the earliest.The intelligent watch that Motorola is about to listing also will adopt sapphire OLED display screen, support magneticinduction wireless charging function.This indicates that sapphire starts " entering into common people house ".
Apple will be the hearsay of iPhone of future generation employing sapphire glass screen, and trying to be the first of cell phone manufacturer imitates, and all allow people more and more have an optimistic view of the development prospect of sapphire glass.
Mechanism is had to think, the five-year, the development of smart mobile phone will bring 3,000,000,000 dollars new markets " cake " for sapphire production.2018, the rate of permeation of sapphire in smart mobile phone monitor market will reach 5% ~ 18%.
Sapphire is applied to large size, quadrate future development on intelligent watch and mobile phone screen, and the feature of consumer electronics applications is large usage quantity, but cost must decline to a great extent.
The growth method of sapphire crystal mainly contains: crystal pulling method (CZ method), kyropoulos (KY method), heat-exchanging method (HEM method), warm terraced method (TGT method) etc.
The crystal of long crystal method growth all presents circle above, circular crystal bar is got if drawn, get roundlet in great circle, adopt close-packed to draw bar mode, material use efficiency can be accomplished that 30% ~ 50%(draws and be got different size crystal bar material use efficiency difference), if but draw and get square crystal rod, get square products in great circle, remaining brilliant shell scrap stock can be more, and material use efficiency is lower, can only 20% ~ 40% be accomplished, as Fig. 1.
Summary of the invention
The present invention is directed to existing growth circular sapphire crystal to draw and get square crystal rod, make mobile phone screen, the problem that material use efficiency is low, there is provided a kind of large size square sapphire crystal growth technology, crystal ingot can be accomplished square, the crystal ingot length of side reaches 320mm × 320mm(weight 100Kg), draw and get 5 inch box panel crystal bar (apple 5S screen sizes, 121.7mm × 56.5mm), material use efficiency is up to 60% ~ 70%, significantly improve material use efficiency, reduce cost, also achieve in addition A to and C to growth, dislocation desity, the index such as monocrystalline reaches the level of KY method crystal.
The technical solution used in the present invention is: the square sapphire crystal growth method of a kind of large size, 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, close furnace chamber and install camera, start watch-dog and registering instrument, in automatic control program, arrange heating schedule, vacuumize, vacuum tightness reaches 10
-4pa, temperature rise rate is 200 DEG C/h; Heat up and melt alumina raw material, by means of infrared thermometer, liquid level temperature controlled between 2050 DEG C ~ 2070 DEG C, liquid level flow line is evenly clear, and reaches steady state; Seed crystal is slowly declined, Touch liquid level; Rapid lifting growth neck; Slow pulling growth shoulder; The isometrical portion of micro-pulling growth, completes to long crystalline substance; Lower the temperature, take out crystal; Crystal pro cessing is in blocks, use KOH corrosion, adopt the dislocation desity of X-ray TOPO GRAPHY, microscope, scanning electron microscope and spectrophotometer test crystal, light transmission and monocrystalline; It is characterized in that: described tungsten lagging material shape is square, and well heater is square, and crucible is square.
As preferably, the interior length of side of described square tungsten lagging material is 850mm ~ 950mm.
As preferably, the interior length of side of described square heater is 650mm ~ 750mm.
As preferably, the outer length of side of described square crucible is 200mm ~ 500mm.
As further preferred, the outer length of side of described square crucible is 300mm ~ 400mm.
Due to the design of heating arrangement and temperature of thermal field gradient, crystal presents up big and down small shape, in order to promote material use efficiency further, takes the mode of cutting in half up and down, below because the length of side is larger, draws that to get mobile phone screen square rod more.
Research finds, the present invention grows square sapphire crystal ingot, has following beneficial effect.
, improve material use efficiency
Circular crystal ingot, makes LED substrate crystal bar, and adopt close-packed mode to draw rod, material use efficiency can reach 30% ~ 50%, but gets the square mobile phone screen of large size if drawn in circular crystal ingot, then utilization ratio is very low, only has 20% ~ 40%, and scrap stock waste is surprising.
Draw in square crystal ingot and get square mobile phone screen crystal bar, can material use efficiency be increased substantially, in order to obtain larger material use efficiency, can according to the size of the size design crystal ingot of mobile phone screen, just right satisfied of crystal ingot size draws the needs getting mobile phone screen size, reduces the waste of scrap stock.
Test proves, 100Kg level sapphire crystal ingot is drawn and got apple 5S type screen square crystal rod, and material use efficiency can reach 60% ~ 70%.
, cost is lower
Growth 100Kg level crystal ingot, square identical with the circle long brilliant time, raw and auxiliary material used is identical, power drain is identical, and the cost of whole crystal ingot is basically identical, but if the material use efficiency of square crystal ingot is higher, also just mean that cost is lower, the sapphire prerequisites of intelligent terminal large-area applications such as mobile phone are that cost must lower, and just can exchange the larger market space for, and grow square sapphire crystal ingot cost and can decline 20% ~ 30%.
Accompanying drawing explanation
Fig. 1 is that the circular crystal ingot of 100Kg level is drawn and got 5 inch box (apple 5S type) mobile phone screen schematic diagram.
Fig. 2 is that the square crystal ingot of 100Kg level is drawn and got 5 inch box (apple 5S type) mobile phone screen schematic diagram.
Fig. 3 makes a living the square crucible schematic diagram of rectangle sapphire crystal ingot.
Embodiment
(1) main composition batching, adopts square biscuit and the part irregularly shaped particles of the high purity aluminium oxide diameter 50mm × 50mm of 99.999wt% shown in table 1;
(2) filler: the alumina raw material weighed up is put into the square crucible that the outer length of side shown in Fig. 3 is 400 × 400mm, close-packed is put, intersects between levels and puts, liquid splash when preventing from melting, and fills irregularly shaped particles;
(3) adjustment installs well heater and thermal field: adjustment installs tungsten double-heater and tungsten thermal field, close furnace chamber and install camera, install A to and C to the square seed crystal of 25mm × 25mm, and adjust position (according to Theoretical Calculation, seed crystal is rested on ullage distance liquid level 200mm place), start watch-dog and registering instrument.
(4) heat: in automatic control program, arrange heating schedule, heat-up rate 120 DEG C/h, vacuumize in stove, vacuum tightness reaches 10
-4pa.
(5) melting sources: adopt the heating schedule that sets, heats up and to melt alumina raw material, can experience to melt → solidify in melting process → fusing repeatedly, finally reach complete melted state.
(6) liquid level temperature is adjusted: adjusted liquid level temperature by Modulating Power, by means of infrared thermometer, liquid level temperature controlled between 2050 DEG C ~ 2070 DEG C, liquid level flow line is evenly clear, and reaches steady state.
(7) transfer seed crystal: the speed of seed crystal according to 40mm/h ~ 60mm/h slowly declined, drop to distance liquid level 10mm ~ 30mm place, by increase and decrease power adjustment crucible central liquid surface temperature point, reach 2050 DEG C ~ 2070 DEG C.
(8) seed crystal touches liquid level: seed crystal is touched liquid level according to the speed of 1mm/min ~ 3mm/min, touch the changes in weight by high-precision weighing systematic observation seed crystal after liquid level, temperature control is carried out by adjustment heating power, until reach stable, seed crystal cannot not be in moltenly not long state, after 1h ~ 3h, start slowly to decline power, start long brilliant.
(9) neck growth: with the pull rate of 1mm/h ~ 3mm/h, the neck of the growth rate crystal of 10g/h ~ 30g/h, if long brilliant speed departs from, is rectified a deviation by adjustment heating power.
(10) shoulder growth: with the pull rate of 0.5mm/h ~ 2mm/h, slow decline power, with the shoulder of the growth rate crystal of 50g/h ~ 150g/h, if long brilliant speed departs from, rectified a deviation by adjustment heating power, when shoulder has grown, the long brilliant speed of adjustment has been 300g/h ~ 600g/h.
(11) isometrical portion growth: with the pull rate of 0.2mm/h ~ 1mm/h, slowly decline power, carries out the growth in the isometrical portion of crystal, until long crystalline substance completes.
(12) lower the temperature: major and minor well heater cooling process is set, be cooled to 1600 DEG C with the cooling rate of 20 DEG C/h ~ 40 DEG C/h, then be cooled to room temperature with the cooling rate of 60 DEG C/h ~ 120 DEG C/h, and after power drop completes, be filled with argon gas and cool fast.
(13) get crystal: close heating power supply, close argon gas, open stove, take out crystal.
(14) crystal detects: the light transmission rate detecting crystal with printing opacity instrument, and crystal pro cessing is in blocks, and uses KOH to corrode, and adopts X-ray TOPO GRAPHY
,microscope, scanning electron microscope and the spectrophotometer test dislocation desity of crystal, light transmission and monocrystalline.
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 voltage, electric current, heating and rate of cooling, grow accurately controlling of brilliant speed.
(4) weighing device is lifted: control pull rate, can the weight of real―time precision measurment crystal growth, lift weighing system precision reaches 1g.
(5) cooling water system: utilize water-cooling pattern to control the stability of furnace body temperature, temperature remains on 23 DEG C ~ 28 DEG C.
(6) system of supervision: high-definition camera and professional watch-dog, can monitor the convection current situation of liquid level and long brilliant situation.
(7) Research on Automatic Measuring System of Temperature: adopt infrared thermometer, can test fluid surface temperature in time.
(8) thermopair: be placed in crucible bottom and crucible sidepiece, can show the temperature curve in melting sources 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, the square sapphire crystal growth method of large size provided by the invention, and well heater, thermal field structure and crucible design are reasonable, homogeneous temperature in crucible, be beneficial to the growth of crystal, the square sapphire crystal ingot regular shape grown out, under equal processing condition, only need change A to and C to seed crystal, can carry out A to and C to the growth of sapphire crystal ingot, crystal bottom sides reaches 320mm × 320mm, draws that to get apple 5S mobile phone screen crystal bar material use efficiency high, reach 60% ~ 70%, as Fig. 2.
Claims (5)
1. the square sapphire crystal growth method of large size, 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, close furnace chamber and install camera, start watch-dog and registering instrument, in automatic control program, arrange heating schedule, vacuumize, vacuum tightness reaches 10
-4pa, temperature rise rate is 200 DEG C/h; Heat up and melt alumina raw material, by means of infrared thermometer, liquid level temperature controlled between 2050 DEG C ~ 2070 DEG C, liquid level flow line is evenly clear, and reaches steady state; Seed crystal is slowly declined, Touch liquid level; Rapid lifting growth neck; Slow pulling growth shoulder; The isometrical portion of micro-pulling growth, completes to long crystalline substance; Lower the temperature, take out crystal; Crystal pro cessing is in blocks, use KOH corrosion, adopt X-ray
tOPO GRAPHY,microscope, scanning electron microscope and the spectrophotometer test dislocation desity of crystal, light transmission and monocrystalline; It is characterized in that: described tungsten lagging material shape is square, and well heater is square, and crucible is square.
2. the square growth method of sapphire single crystal of large size according to claim 1, is characterized in that: the interior length of side of described square tungsten lagging material is 850mm ~ 950mm.
3. the square growth method of sapphire single crystal of large size according to claim 1, is characterized in that: the interior length of side of described square heater is 650mm ~ 750mm.
4. the square growth method of sapphire single crystal of large size according to claim 1, is characterized in that: the outer length of side of described square crucible is 200mm ~ 500mm.
5. the square growth method of sapphire single crystal of large size according to claim 4, is characterized in that: the outer length of side of described square crucible is 300mm ~ 400mm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410481654.0A CN104264224A (en) | 2014-09-19 | 2014-09-19 | Growth method of large-size square sapphire crystal |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410481654.0A CN104264224A (en) | 2014-09-19 | 2014-09-19 | Growth method of large-size square sapphire crystal |
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| CN104264224A true CN104264224A (en) | 2015-01-07 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117418313A (en) * | 2023-12-19 | 2024-01-19 | 天通控股股份有限公司 | Large-size sapphire crystal growth method based on automatic filling |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103451729A (en) * | 2013-09-17 | 2013-12-18 | 无锡鼎晶光电科技有限公司 | Growth method of square sapphire |
| CN103556223A (en) * | 2013-11-18 | 2014-02-05 | 河北工业大学 | Method for growing large-size square sapphire single crystal |
| CN103806101A (en) * | 2012-11-15 | 2014-05-21 | 上海中电振华晶体技术有限公司 | Growth method and equipment of square sapphire crystal |
-
2014
- 2014-09-19 CN CN201410481654.0A patent/CN104264224A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103806101A (en) * | 2012-11-15 | 2014-05-21 | 上海中电振华晶体技术有限公司 | Growth method and equipment of square sapphire crystal |
| CN103451729A (en) * | 2013-09-17 | 2013-12-18 | 无锡鼎晶光电科技有限公司 | Growth method of square sapphire |
| CN103556223A (en) * | 2013-11-18 | 2014-02-05 | 河北工业大学 | Method for growing large-size square sapphire single crystal |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117418313A (en) * | 2023-12-19 | 2024-01-19 | 天通控股股份有限公司 | Large-size sapphire crystal growth method based on automatic filling |
| CN117418313B (en) * | 2023-12-19 | 2024-02-27 | 天通控股股份有限公司 | Large-size sapphire crystal growth method based on automatic filling |
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Application publication date: 20150107 |
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