CN102586866A - Method for restraining bulbs in process of growing slice-shaped sapphire in guiding mold mode - Google Patents
Method for restraining bulbs in process of growing slice-shaped sapphire in guiding mold mode Download PDFInfo
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- CN102586866A CN102586866A CN2012100281330A CN201210028133A CN102586866A CN 102586866 A CN102586866 A CN 102586866A CN 2012100281330 A CN2012100281330 A CN 2012100281330A CN 201210028133 A CN201210028133 A CN 201210028133A CN 102586866 A CN102586866 A CN 102586866A
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Abstract
The invention discloses a method for restraining bulbs in a process of growing slice-shaped sapphire in guiding mold mode. Sapphire fragments grown through a high-purity flame melt method are adopted as the raw materials, a molybdenum mold with top surface smoothness reaching mirror surface effect is adopted, the raw materials are smashed for growth in high-purity argon atmosphere and stand for 2-3 hours with temperature rising by 20 DEG C after the materials are smashed totally. Sapphire single crystal which grows in a pulling method and has end face normal direction to be m are adopted as seed crystal, two lateral directions of the seed crystal are a-direction and b-direction, the a-face serves as a main growing face and is pulled by 2-3cm in equal-diameter mode in seeding, the seed crystal grows in shoulder-expanding mode after being necked down effectively, the pulling speed is 15mm/hour, and power and pulling speed can be changed in real time according to the growth condition of the crystal so as to obtain the slice-shaped sapphire crystal. The prepared slice-shaped sapphire crystal is regular in appearance, flat in surface, free of bulbs and stress stripe and high in quality.
Description
Technical field
The present invention relates to the synthetic sapphire technical field, be specifically related to utilize the control method of bubble in the guided mode method growth flaky sapphire process.
Background technology
Sapphire is a kind of α-Al
2O
3Monocrystalline, claim corundum again.Sapphire crystal has excellent heat conductive insulating property, chemerosiveness resistent; Its surface elevation is level and smooth; High permeability is arranged; Can under near 2000 ℃ of pyritous conditions, work, thereby be widely used in window material and fine optical material of satellite spatial technology, military infrared equipment, high intensity laser beam device or the like.In recent years, along with the fast development of semiconductor technology, sapphire is with its unique crystalline network, excellent mechanical property, the semi-conductor GaN/Al that good thermal property becomes practical application
2O
3Photodiode (LED), large-scale integrated circuit SOI and ideal substrate materials such as SOS and superconducting nano structural membrane.
The guided mode method claims that again (edge-defined film-fed crystal growth method is abbreviated as edge limited-membrane process
EFG), be mainly used in the growth specified shape crystal.The characteristics of guided mode method are the crystal that sheet, band shape, tubulose, specified shape such as fibrous and size can accurately control of can growing, and utilize this method crystalline fast growth, and following process is simple.Therefore, the sapphire sheet crystal that adopts the growth of guided mode method to have large size, the high optical quality of specific direction becomes one of technology that the industry pays special attention to.USP 3591348 discloses a kind of method of guided mode method growing sapphire, and Chinese patent 90105983.8 and 200810153130.3 also discloses the method for growth flaky sapphire.But, when adopting the aforesaid method growing crystal, can not effectively suppress the generation of bubble, the use value of product is had a greatly reduced quality.
Summary of the invention
The objective of the invention is to address the above problem, provide a kind of and in adopting guided mode method growth flaky sapphire process, can effectively suppress the method that bubble produces, make the crystal of growth not have bubble and stressed cord, on quality and result of use, obvious improvement is arranged.
For realizing above-mentioned purpose, the technical scheme that the present invention takes is:
In adopting guided mode method growth flaky sapphire process, suppress the method for bubble, it is characterized in that, may further comprise the steps:
(1) raw material choosing and handling
Raw material adopts the sapphire particle of high-purity flame melt method growth, through 500～800 ℃ high-temperature heating treatment after, with the deionized water pulverizing of quenching, again through 5～6 times with the deionized water clean after dry for standby;
(2) employing of mould and processing
Adopt V-type forging and pressing molybdenum molding jig, the die tip inner surface adopts the mechanical polishing processing and reaches mirror effect; The mould slit width is 0.5mm, and crucible is cleaned subsequent use with deionized water;
(3) raw material shove charge
The sapphire particle that step (1) was handled is put into the crucible of the molybdenum molding jig that step (2) handled, and crucible is placed the guided mode stove, accomplishes shove charge;
(4) adopt guided mode method growth flaky sapphire monocrystalline
1. with vacuumizing 1 * 10 in the guided mode stove
-4Pa adopts Frequency Induction Heating molybdenum electro-heat equipment, and when treating in the stove glow, slowly charging into high-purity argon gas to gauge pressure is 0.01, leaves standstill 20～30 minutes, every then at a distance from intensification in 15～20 minutes once, melt fully until raw material; After raw material melts fully, left standstill 15～20 minutes, and then heat up 20 ℃ (higher 20 ℃ than fusing point) and left standstill 2～3 hours, the gas that raw material is introduced during making material slowly overflows from melt;
2. to adopt the normal line of butt end direction be m to the sapphire single-crystal of Czochralski grown as seed crystal, two side surface direction of seed crystal be a to c to, with a face as main aufwuchsplate;
3. melt temperature is dropped to 2050 ℃, shake down seed rod, seed crystal is dropped to and the be separated by position of 0.5～1cm of melt; Observe: become slick and sly if turn white in the seed crystal bottom; Shaken seed rod, lowered the temperature 5～10 ℃, left standstill and turn down the seed rod observation after 15～20 minutes again; Under seed crystal bottom no change can continue, shake seed rod, seed crystal is contacted with melt also mention rapidly; If the band material raises temperature 1～3 ℃, leave standstill 5～20 minutes continued and sow, until not being with material can attempt lifting;
4. the process of lifting comprises seeding, necking down, expansion shoulder, isodiametric growth step, wherein, makes crystal diameter constant during seeding, and length lifts 2～3cm; Through 2～5 ℃ of processes that realize necking down that heat up, effectively expand the shoulder growth after the necking down more again; The pulling rate that expands the shoulder stage whenever increased by 2～4mm/ hour at a distance from 20 minutes, until isometrical stage pulling rate 15mm/ hour along with growing up of crystal shoulder is fast by reaching slowly; The isometrical stage when seeing the indent of growing crystal, reducing pulling rate is 1～3mm/ hour, reduces by 1～2 ℃ of temperature, every at a distance from 20 minutes observation growing crystals crystal formation and handle accordingly;
5. after crystal growth is accomplished, reduce to room temperature gradually, obtain almost not have the flaky sapphire crystals of bubble with 20～30 ℃ rate of temperature fall per hour.
Further, the 2. said m of step (4) is ± 5 ° to the direction error scope of seed crystal.
Positively effect of the present invention is:
(1) a kind of method that in adopting guided mode method growth flaky sapphire process, effectively suppresses bubble is provided;
(2) preparation the flaky sapphire crystals neat appearance, have an even surface, do not have bubble and stressed cord, be high-quality flaky sapphire crystals;
(3) be semi-conductor GaN/Al
2O
3Photodiode (LED), large-scale integrated circuit SOI and SOS and superconducting nano structural membrane etc. provide the ideal substrate material.
Description of drawings
Accompanying drawing 1 suppresses the FB(flow block) of the method for bubble in adopting guided mode method growth flaky sapphire process for the present invention.
Embodiment
Continue to explain that below in conjunction with accompanying drawing the present invention suppresses the practical implementation situation of the method for bubble in adopting guided mode method growth flaky sapphire process, 7 embodiment are provided.But enforcement of the present invention is not limited to following embodiment.
Embodiment 1
In adopting guided mode method growth flaky sapphire process, suppress the method for bubble, may further comprise the steps:
(1) adopting the sapphire particle of high-purity flame melt method growth is raw material, through 500 ℃ of high-temperature heating treatment after, with the deionized water pulverizing of quenching, again through 5 times with the deionized water clean after dry for standby.
(2) adopt V-type forging and pressing molybdenum molding jig, the die tip inner surface adopts the mechanical polishing processing and reaches mirror effect; The mould slit width is 0.5mm, and crucible is cleaned subsequent use with deionized water.
(3) the sapphire particle of step (1) being handled is put into the crucible of the molybdenum molding jig that step (2) handled, and crucible is placed the guided mode stove, accomplishes shove charge.
(4) adopt guided mode method growth flaky sapphire monocrystalline
1. with vacuumizing 1 * 10 in the guided mode stove
-4Pa adopts Frequency Induction Heating molybdenum electro-heat equipment, and when treating in the stove glow, slowly charging into high-purity argon gas to gauge pressure is 0.01, leaves standstill 20 minutes, every then at a distance from intensification in 15 minutes once, melt fully until raw material; After raw material melts fully, left standstill 15 minutes, and heated up then 20 ℃ (higher 20 ℃ than fusing point) and left standstill 2 hours, the gas that raw material is introduced during making material slowly overflows from melt.
2. to adopt the normal line of butt end direction be m to the sapphire single-crystal of Czochralski grown as seed crystal, two side surface direction of seed crystal be a to c to, as main aufwuchsplate, the limit of error that requires the seed crystal direction is in ± 5 ° with a face.
3. melt temperature is dropped to 2050 ℃; Under shake seed rod, seed crystal is dropped to the be separated by position of 0.5cm of melt observes several minutes: become slick and sly if turn white in the seed crystal bottom, shaken seed rod; Lower the temperature 5 ℃; Leave standstill and turn down the seed rod observation after 15 minutes again, under seed crystal bottom no change can continue, shake seed rod, seed crystal is contacted with melt also mention rapidly; If the band material raises temperature 1 ℃, leave standstill 5 minutes continued and sow, until not being with material can attempt lifting.
4. the process of lifting comprises seeding, necking down, expansion shoulder, isodiametric growth step, wherein, makes crystal diameter constant during seeding, and length lifts 2cm; Through the 2 ℃ of processes that realize necking down that heat up, effectively expand the shoulder growth after the necking down more again; The pulling rate that expands the shoulder stage whenever increased 2mm/ hour at a distance from 20 minutes, until isometrical stage pulling rate 15mm/ hour along with growing up of crystal shoulder is fast by reaching slowly; The isometrical stage when seeing the indent of growing crystal, reducing pulling rate is 1mm/ hour, reduces by 1 ℃ of temperature, every at a distance from 20 minutes observation growing crystals crystal formation and handle accordingly.
5. after crystal growth is accomplished, reduce to room temperature gradually, obtain flaky sapphire crystals with 20 ℃ rate of temperature fall per hour.
The flaky sapphire crystals of said acquisition is the flaky sapphire monocrystalline, has regular profile, has an even surface, and under 100 W incandescent light, observes no bubble; After cutting out the optical polishing of 20 * 20 * 5mm lamina of light, under stressometer, observe unstressed.
Embodiment 2
In adopting guided mode method growth flaky sapphire process, suppress the method for bubble, may further comprise the steps:
(1) adopting the sapphire particle of high-purity flame melt method growth is raw material, through 800 ℃ of high-temperature heating treatment after, with the deionized water pulverizing of quenching, again through 6 times with the deionized water clean after dry for standby.
Step (2), (3) are with embodiment 1.
(4) adopt guided mode method growth flaky sapphire monocrystalline
1. with vacuumizing 1 * 10 in the guided mode stove
-4Pa adopts Frequency Induction Heating molybdenum electro-heat equipment, and when treating in the stove glow, slowly charging into high-purity argon gas to gauge pressure is 0.01, leaves standstill 30 minutes, every then at a distance from intensification in 20 minutes once, melt fully until raw material; After raw material melts fully, left standstill 20 minutes, and heated up then 20 ℃ (higher 20 ℃ than fusing point) and left standstill 3 hours, the gas that raw material is introduced during making material slowly overflows from melt.
2. with embodiment 1.
3. melt temperature is dropped to 2050 ℃, shake down seed rod, seed crystal is dropped to and the be separated by position of 1cm of melt; Observe several minutes: become slick and sly if turn white in the seed crystal bottom; Shaken seed rod, lowered the temperature 10 ℃, left standstill and turn down the seed rod observation after 20 minutes again; Under seed crystal bottom no change can continue, shake seed rod, seed crystal is contacted with melt also mention rapidly; If the band material raises temperature 3 ℃, leave standstill 20 minutes continued and sow, until not being with material can attempt lifting.
4. the process of lifting comprises seeding, necking down, expansion shoulder, isodiametric growth step, wherein, makes crystal diameter constant during seeding, and length lifts 3cm; Through the 5 ℃ of processes that realize necking down that heat up, effectively expand the shoulder growth after the necking down more again; The pulling rate that expands the shoulder stage whenever increased 4mm/ hour at a distance from 20 minutes, until isometrical stage pulling rate 15mm/ hour along with growing up of crystal shoulder is fast by reaching slowly; The isometrical stage when seeing the indent of growing crystal, reducing pulling rate is 3mm/ hour, reduces by 2 ℃ of temperature, every at a distance from 20 minutes observation growing crystals crystal formation and handle accordingly.
5. after crystal growth is accomplished, reduce to room temperature gradually, obtain flaky sapphire crystals with 30 ℃ rate of temperature fall per hour.
The flaky sapphire crystals of said acquisition is the flaky sapphire monocrystalline, has regular profile, has an even surface, and under 100 W incandescent light, observes no bubble; After cutting out the optical polishing of 20 * 20 * 5mm lamina of light, under stressometer, observe unstressed.
Embodiment 3
Implement purpose, see the influence of raw material crystal mass
Different with embodiment 1 is the polycrystal raw material of choice of powder raw material rather than flame melt method.
The purity of choosing certain mass is 99.999% aluminum oxide (Al
2O
3) powder, with synthetic glass mould splendid attire, on hydropress, press knot, whole growth process thereafter is with the process of embodiment 1.
The plane of crystal that obtains is smooth, and complete nothing cracking is observed under the 100W incandescent light, and there is the uneven bubble of size of stochastic distribution inside; After cutting out the optical polishing of 20 * 20 * 5mm lamina of light, under stressometer, observing has stress.
Embodiment 4
Implement purpose, see the influence of mould crystal mass
Different with embodiment 1 is, adopts common V-type forging and pressing molybdenum molding jig, and the die tip inner surface does not carry out polished finish.All the other process of growth are with the process of embodiment 1.
The crystal perfection that obtains, surface undulation is bigger, and tangible longitudinal stripe is arranged; Under the 100W incandescent light, observe, there is vertical wire distribution bubble inside; After cutting out the optical polishing of 20 * 20 * 5mm lamina of light, under stressometer, observing has stress.
Embodiment 5
Implement purpose, see of the influence of seed crystal direction crystal mass
Different with embodiment 1 is, selects the seed crystal pulling growth of different directions for use, and seed crystal direction and crystal mass are as shown in table 1, and all the other process of growth are with the process of embodiment 1.
Table 1. seed crystal direction is to the influence of crystal mass
Embodiment 6
Implement purpose, see that feed liquid leaves standstill the influence to crystal mass
Different with embodiment 1 is, does not leave standstill the pulling growth of directly sowing 2～3 hours after changing material.All the other process of growth are with the process of embodiment 1.
The crystal perfection that obtains is observed under 100 W incandescent light, and there is the uneven bubble of stochastic distribution size inside; After cutting out the optical polishing of 20 * 20 * 5mm lamina of light, under stressometer, observing has stress.
Embodiment 7
Implement purpose, see seeding and necking down influence crystal mass
Different with embodiment 1 is, after feed liquid leaves standstill, does not carry out the process of seeding and necking down, directly expands the shoulder growth.All the other process of growth are with the process of embodiment 1.
The crystal that obtains is for there being the rimose crystal, and surface undulation is bigger, under the 100W incandescent light, observes, and plane of crystal has bubble to distribute; After cutting out the optical polishing of 20 * 20 * 5mm lamina of light, under stressometer, observing has stress.
The result of different embodiment proves; The method technology of the present invention's inhibition bubble in adopting guided mode method growth flaky sapphire process is reasonable; The flaky sapphire crystals of preparation has regular profile, has an even surface, and under 100 W incandescent light, observes no bubble; Under stressometer, observe unstressedly, reached the object of the invention fully.
The above is merely preferred implementation of the present invention; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the inventive method; Can also make some improvement and retouching, these improvement and retouching also should be regarded as in protection scope of the present invention.
Claims (2)
1. a method that in adopting guided mode method growth flaky sapphire process, suppresses bubble is characterized in that, may further comprise the steps:
(1) raw material choosing and handling
Raw material adopts the sapphire particle of high-purity flame melt method growth, through 500～800 ℃ high-temperature heating treatment after, with the deionized water pulverizing of quenching, again through 5～6 times with the deionized water clean after dry for standby;
(2) employing of mould and processing
Adopt V-type forging and pressing molybdenum molding jig, the die tip inner surface adopts the mechanical polishing processing and reaches mirror effect; The mould slit width is 0.5mm, and crucible is cleaned subsequent use with deionized water;
(3) raw material shove charge
The sapphire particle that step (1) was handled is put into the crucible of the molybdenum molding jig that step (2) handled, and crucible is placed the guided mode stove, accomplishes shove charge;
(4) adopt guided mode method growth flaky sapphire monocrystalline
1. with vacuumizing 1 * 10 in the guided mode stove
-4Pa adopts Frequency Induction Heating molybdenum electro-heat equipment, and when treating in the stove glow, slowly charging into high-purity argon gas to gauge pressure is 0.01, leaves standstill 20～30 minutes, every then at a distance from intensification in 15～20 minutes once, melt fully until raw material; After raw material melts fully, left standstill 15～20 minutes, and heated up 20 ℃ and left standstill 2～3 hours then, the gas that raw material is introduced during making material slowly overflows from melt;
2. to adopt the normal line of butt end direction be m to the sapphire single-crystal of Czochralski grown as seed crystal, two side surface direction of seed crystal be a to c to, with a face as main aufwuchsplate;
3. melt temperature is dropped to 2050 ℃, shake down seed rod, seed crystal is dropped to and the be separated by position of 0.5～1cm of melt; Observe: become slick and sly if turn white in the seed crystal bottom; Shaken seed rod, lowered the temperature 5～10 ℃, left standstill and turn down the seed rod observation after 15～20 minutes again; Under seed crystal bottom no change can continue, shake seed rod, seed crystal is contacted with melt also mention rapidly; If the band material raises temperature 1～3 ℃, leave standstill 5～20 minutes continued and sow, until not being with material can attempt lifting;
4. the process of lifting comprises seeding, necking down, expansion shoulder, isodiametric growth step, wherein, makes crystal diameter constant during seeding, and length lifts 2～3cm; Through 2～5 ℃ of processes that realize necking down that heat up, effectively expand the shoulder growth after the necking down more again; The pulling rate that expands the shoulder stage whenever increased by 2～4mm/ hour at a distance from 20 minutes, until isometrical stage pulling rate 15mm/ hour along with growing up of crystal shoulder is fast by reaching slowly; The isometrical stage when seeing the indent of growing crystal, reducing pulling rate is 1～3mm/ hour, reduces by 1～2 ℃ of temperature, every at a distance from 20 minutes observation growing crystals crystal formation and handle accordingly;
5. after crystal growth is accomplished, reduce to room temperature gradually, obtain not have the flaky sapphire crystals of bubble with 20～30 ℃ rate of temperature fall per hour.
2. the method that in adopting guided mode method growth flaky sapphire process, suppresses bubble according to claim 1 is characterized in that the 2. said m of step (4) is ± 5 ° to the direction error scope of seed crystal.
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Cited By (14)
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| CN102943303A (en) * | 2012-11-14 | 2013-02-27 | 上海施科特光电材料有限公司 | Method to restrain bubbles in process of growing sapphire by using kyropoulos method |
| CN103014856A (en) * | 2013-01-10 | 2013-04-03 | 苏州巍迩光电科技有限公司 | Ferric-titanium-doped sapphire wafer and preparation method thereof |
| CN103060901A (en) * | 2013-02-05 | 2013-04-24 | 元亮科技有限公司 | Preparation process for growing plurality of crystals through edge-defined film-fed crystal growth method |
| CN104047049A (en) * | 2014-06-30 | 2014-09-17 | 南京航空航天大学 | Preparation method for growing crack-free sapphire crystals by edge-defined film-fed growth process |
| CN104088011A (en) * | 2014-07-15 | 2014-10-08 | 天津市恒瑜晶体材料制造有限公司 | Preparation method of sapphire micro-capillary and die used in preparation method |
| CN104120487A (en) * | 2013-08-23 | 2014-10-29 | 江苏中电振华晶体技术有限公司 | Growth method and growth equipment of platelike sapphire crystals |
| CN104131354A (en) * | 2013-05-02 | 2014-11-05 | 周黎 | Recycling method of residual crystal scrap after processing of sapphire crystal |
| CN104499042A (en) * | 2014-12-15 | 2015-04-08 | 江苏苏博瑞光电设备科技有限公司 | Growth method of microporous sapphire crystal |
| CN104962994A (en) * | 2015-07-30 | 2015-10-07 | 山东大学 | Method for growing specific-size rare-earth-doped gallium-containing garnetite series crystal by edge-defined process |
| CN106676624A (en) * | 2017-03-31 | 2017-05-17 | 宁夏佳晶科技有限公司 | Guide mode processing method for flaky sapphire |
| CN104532342B (en) * | 2014-12-15 | 2017-06-27 | 江苏苏博瑞光电设备科技有限公司 | A kind of EFG technique grows the growing method of micropore sapphire crystal |
| CN107059115A (en) * | 2017-04-20 | 2017-08-18 | 山西中聚晶科半导体有限公司 | A kind of kyropoulos prepare the growing method of sapphire crystal |
| CN108411367A (en) * | 2018-03-06 | 2018-08-17 | 同济大学 | Flow atmosphere EFG technique multi-disc sapphire crystallization device and method |
| CN111455454A (en) * | 2020-04-28 | 2020-07-28 | 天通银厦新材料有限公司 | Kyropoulos growth process for 600kg sapphire crystal |
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| CN102943303A (en) * | 2012-11-14 | 2013-02-27 | 上海施科特光电材料有限公司 | Method to restrain bubbles in process of growing sapphire by using kyropoulos method |
| CN103014856A (en) * | 2013-01-10 | 2013-04-03 | 苏州巍迩光电科技有限公司 | Ferric-titanium-doped sapphire wafer and preparation method thereof |
| CN103014856B (en) * | 2013-01-10 | 2015-11-04 | 苏州巍迩光电科技有限公司 | Mix ferrotitanium sapphire wafer and preparation method thereof |
| CN103060901B (en) * | 2013-02-05 | 2015-04-22 | 元亮科技有限公司 | Preparation process for growing plurality of crystals through edge-defined film-fed crystal growth method |
| CN103060901A (en) * | 2013-02-05 | 2013-04-24 | 元亮科技有限公司 | Preparation process for growing plurality of crystals through edge-defined film-fed crystal growth method |
| CN104131354A (en) * | 2013-05-02 | 2014-11-05 | 周黎 | Recycling method of residual crystal scrap after processing of sapphire crystal |
| CN104120487A (en) * | 2013-08-23 | 2014-10-29 | 江苏中电振华晶体技术有限公司 | Growth method and growth equipment of platelike sapphire crystals |
| CN104047049A (en) * | 2014-06-30 | 2014-09-17 | 南京航空航天大学 | Preparation method for growing crack-free sapphire crystals by edge-defined film-fed growth process |
| CN104088011A (en) * | 2014-07-15 | 2014-10-08 | 天津市恒瑜晶体材料制造有限公司 | Preparation method of sapphire micro-capillary and die used in preparation method |
| CN104088011B (en) * | 2014-07-15 | 2017-01-18 | 牛玥 | Preparation method of sapphire micro-capillary and die used in preparation method |
| CN104499042A (en) * | 2014-12-15 | 2015-04-08 | 江苏苏博瑞光电设备科技有限公司 | Growth method of microporous sapphire crystal |
| CN104532342B (en) * | 2014-12-15 | 2017-06-27 | 江苏苏博瑞光电设备科技有限公司 | A kind of EFG technique grows the growing method of micropore sapphire crystal |
| CN104962994A (en) * | 2015-07-30 | 2015-10-07 | 山东大学 | Method for growing specific-size rare-earth-doped gallium-containing garnetite series crystal by edge-defined process |
| CN104962994B (en) * | 2015-07-30 | 2017-09-26 | 山东大学 | The method that EFG technique grows the rear-earth-doped serial crystal containing Ga garnet of specific dimensions |
| CN106676624A (en) * | 2017-03-31 | 2017-05-17 | 宁夏佳晶科技有限公司 | Guide mode processing method for flaky sapphire |
| CN106676624B (en) * | 2017-03-31 | 2019-01-29 | 宁夏佳晶科技有限公司 | A kind of guided mode processing method of flaky sapphire |
| CN107059115A (en) * | 2017-04-20 | 2017-08-18 | 山西中聚晶科半导体有限公司 | A kind of kyropoulos prepare the growing method of sapphire crystal |
| CN108411367A (en) * | 2018-03-06 | 2018-08-17 | 同济大学 | Flow atmosphere EFG technique multi-disc sapphire crystallization device and method |
| CN111455454A (en) * | 2020-04-28 | 2020-07-28 | 天通银厦新材料有限公司 | Kyropoulos growth process for 600kg sapphire crystal |
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