CN102534779A - Preparation method of single component oxide crystal - Google Patents
Preparation method of single component oxide crystal Download PDFInfo
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- CN102534779A CN102534779A CN2010106035203A CN201010603520A CN102534779A CN 102534779 A CN102534779 A CN 102534779A CN 2010106035203 A CN2010106035203 A CN 2010106035203A CN 201010603520 A CN201010603520 A CN 201010603520A CN 102534779 A CN102534779 A CN 102534779A
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Abstract
The invention provides a preparation method of a single component oxide crystal. The preparation method comprises a preparing step, a crystal guiding step, a heat conveying step and a power regulation step, wherein in the crystal guiding step, a seed crystal extending out of a hot fluid director is transferred downwards, the hot fluid director is in a sleeve shape and clamps the seed crystal from the top of the seed crystal; in the heat conveying step, cooling water entering a seed crystal rod from a cooling water system is controlled to be evenly cooled from a first temperature value to a second temperature value so as to control raw material melt to start to crystallize on the periphery of the seed crystal, the seed crystal rod evenly conveys heat of the cooling water entering the seed crystal rod to the seed crystal through the hot fluid director; and in the power regulation step, after the heat conveying step is finished, the power of a heating element is kept unchanged during a third preset time, the cooling water in the seed crystal rod is kept unchanged at the second temperature value simultaneously during the third preset time, and power of the heating element is adjusted until crystal growth is finished. The method controls growth speed of the crystal at an initial stage by means of hot directed fluid at the top of the seed crystal.
Description
Technical field
The present invention relates to a kind of crystal preparation method, relate in particular to a kind of preparation method of one-component oxide crystal.
Background technology
Sapphire aluminum oxide (the Al that consists of
2O
3); Because of its in advantageous characteristic that the aspect had such as chemistry, electricity, machinery, optics, surface property, thermodynamics and weather resistance, be widely used in the first-selected window of infrared military device, guided missile, submarine, aerospace, satellite spatial technology, detection and superpower light laser etc.Sapphire Substrate is that the existing market commercialization is maximum, the most sophisticated product of technology, is the GaN base LED of substrate with the sapphire, is mainly used in solid-state illumination, backlight etc., and market outlook are wide.Sapphire crystal growth method mainly contains crystal pulling method, kyropoulos, heat-exchanging method etc. at present.
In the aforesaid method, crystal pulling method adopts Iridium Crucible usually, and cost is higher, and owing to the restriction of process characteristic and sapphire self character, its resulting crystalline size is difficult to above 4 inches on the other hand;
Kyropoulos can obtain high quality more than 8 inches, large-sized sapphire crystal, but because hot system is a metal screen, its stability, poor repeatability, the too much experience that depends on the technician in the production process;
Heat-exchanging method can obtain high-quality crystal, owing to the motivating force, the crucible that need in complex equipments, the crystal growing process to adopt helium to do heat exchange generation crystal growth only can use several times, causes production cost very high, and taking a long view does not have the market competitiveness.
Summary of the invention
To the problem that exists in the correlation technique, the object of the present invention is to provide a kind of preparation method of one-component oxide crystal, thereby can control the speed of growth of crystal initial period through seed crystal top thermally induced flow.
For realizing above-mentioned purpose; The present invention provides a kind of preparation method of one-component oxide crystal; Comprise the steps: preparation step; With the one-component oxide raw material in the crucible that is contained in crystal growing furnace fusing, make in the crystal growing furnace power of heating element remain unchanged then and continued for first scheduled time, in first scheduled time, make the temperature of cooling water of cooling water system remain first temperature value simultaneously; The seeding step is transferred the seed crystal that from the thermally induced flow device, stretches out, after seed crystal is accomplished roasting crystalline substance; Continuing to transfer seed crystal kept for second scheduled time to immerse in the raw material liquation and to continue; Wherein, the thermally induced flow device is a sleeve-like and from the top clamping seed crystal of seed crystal, also is connected with seed rod on the thermally induced flow device; The heat transportation step; Control gets into water coolant in the seed rod from first temperature value uniform decrease in temperature to the second temperature value by cooling water system; Wherein, the heat of water coolant evenly is transferred to seed crystal through the thermally induced flow device in the seed rod, so that the raw material liquation begins crystallization around seed crystal; The power regulation step; After accomplishing the heat transportation step; Make the power of heating element keep for the 3rd scheduled time constant, keep simultaneously in the 3rd scheduled time that water coolant keeps second temperature value constant in the seed rod, the power of regulating heating element then is until accomplishing crystal growth.
Preferably, in preparation step, the one-component oxide raw material that is contained in the crucible is that density is 3.0g/cm
3, purity is the alumina raw material more than 99.996%, behind the furnace chamber of sealing crystal growing furnace; Under inert atmosphere, rise to 48kw, with the fusing alumina raw material, wherein through 12 hours power with heating element; The time that heating element keeps permanent power to continue is said first scheduled time; First scheduled time, wherein, first temperature value was selected from arbitrary value in 30 ± 1 ℃ in order to be selected from arbitrary value in 4-6 hour; In the seeding step; Under inert atmosphere conditions; Speed with 20-50mm/h is transferred seed crystal; Transferring to accomplishing apart from the position of the liquid level 5-10mm of raw material liquation roasting brilliantly, the seed crystal behind the wherein roasting crystalline substance remains on that the time is said second scheduled time in the raw material liquation, and second scheduled time was arbitrary value in 30-60 minute; In the heat transportation step, the water coolant that in 10-20 hour time, will enter into seed rod is from first temperature value uniform decrease in temperature to the second temperature value, and wherein, when first temperature value was 30 ℃, second temperature value was 20 ℃; In the power regulation step; Second temperature value of water coolant continued for the 4th scheduled time in the power of heating element, the seed rod; The 4th scheduled time was the arbitrary value in 6-10 hour; Wherein, after the 4th scheduled time, power regulation to the mode of 45kw of heating element is accomplished described crystal growth through speed with average 0.03kw/h.
Preferably, in the seeding step, second scheduled time that the seed crystal behind the roasting crystalline substance remains in the raw material liquation is 20 minutes; In the heat transportation step, the time length of crystal growth is 10-20 hour.
Preferably, preparation method of the present invention also comprises: after the power regulation step, the pyrotoxin in the crystal growing furnace is lowered the temperature, annealed; And after accomplishing cooling, annealing steps, the dismounting crystal growing furnace is to take out the crystal after growth is accomplished.
Preferably; Cooling, annealing steps is: with the speed of 0.4kw/h the power of heating element is dropped to 5kw from 45kw; After 5 hours, the power of heating element is reduced to 0 then, further, the other system in the crystal growing furnace except heating element was closed after working on 30-50 hour.
Preferably, the furnace chamber of crystal growing furnace is made up of furnace bottom, body of heater and bell, between furnace bottom and the body of heater; And be connected with removably between bell and the body of heater, wherein, the crucible that is contained in the furnace chamber is the miramint crucible; The heating element that is contained in the furnace chamber has heat generating part, the tungsten silk screen of heat generating part for being provided with around crucible, and miramint is made up of the molybdenum of the tungsten and 70% (weight percent) of 30% (weight percent); Wherein, Also be provided with heat protection screen between body of heater and the tungsten silk screen, heat protection screen centers on said tungsten silk screen setting, and is configured to by tungsten sheet and/or the molybdenum sheet stratiform overlaying structure alternate with pyroceramic.
Preferably, in the power regulation step, the crystal diameter after growth is accomplished is 150-200mm, highly is 320mm.
Preferably, in the power regulation step, crystal height and diameter ratio after growth is accomplished reach 2: 1.
Preferably, in the power regulation step, the crystal diameter after growth is accomplished is 4/5 of a crucible inside diameter.
Preferably, it is characterized in that in the seeding step, in the heat transportation step, in the power regulation step, the crystalline growth is in the inert atmosphere all the time; The one-component oxide crystal is a sapphire crystal.
Than prior art; Beneficial effect of the present invention is: in the heat transportation step; Regulate the temperature of the water coolant of supplying with seed rod through temperature regulator; Because the heat of water coolant evenly is transferred to seed crystal through seed rod, thermally induced flow device, seed crystal top in the seed rod, thereby can control the speed of growth of crystal initial period;
The crystalline diameter that can grow is 4/5 of a crucible inside diameter, and crystal height and diameter ratio can reach 2: 1 simultaneously, have improved the crystalline availability fully;
Seeding technology is simple, does not need repeatedly necking down, has reduced the experienced requirement to the Technology personnel; And,
In crystal growing process, only there is the natural convection that causes by gravity in the melt, melt spontaneous nucleation under the effect of the guiding of seed crystal and thermally induced flow device forms, and has guaranteed high-quality crystal.
Description of drawings
Fig. 1 is the structural representation of the crystal growing furnace that adopts of the present invention;
Fig. 2 shows the thermally induced flow device structural representation that uses in the heat transportation step;
Fig. 3 show with Fig. 2 in the T type seed crystal that is connected of thermally induced flow device.
Embodiment
Specific embodiment of the present invention is below described.
The preparation method of one-component oxide crystal of the present invention (growing method) mainly is applicable to the large size sapphire crystal growth, equally also is applicable to the growth of other one-component high-temp oxide crystals.
Method of the present invention is top seed crystal thermally induced flow crystal preparation method; It comprises: preparation step, seeding step, heat transportation step, power regulation step, cooling and annealing steps, tear the stove step open; In the heat transportation step; Regulate the inflow temperature (being fed to the temperature of cooling water in the seed rod) of seed rod by cooling water system through temperature regulator; The heat of water coolant evenly transmits to the top of seed crystal through the thermally induced flow device in the seed rod, thereby can control the speed of growth of crystal initial period.In addition, the crystal that takes out among the present invention after growth is accomplished is accomplished in tearing the stove step open.Be the method for embodiment of the present invention, seed rod can adopt the water-cooled seed rod, and promptly seed rod has the cavity that holds frozen water (water coolant a kind of), and seed rod is installed in an end of thermally induced flow device, seed chuck is contained in the other end of thermally induced flow device.
Below in conjunction with the first embodiment of the present invention, preparing method's step of the present invention is further described as follows:
(1) preparation step; One-component oxide raw material in the crucible that is contained in crystal growing furnace is melted; Make in the said crystal growing furnace power of heating element remain unchanged then and continued for first scheduled time; In said first scheduled time, make the temperature of cooling water of cooling water system remain first temperature value simultaneously.More particularly, in the first embodiment of the present invention, in preparation step, the one-component oxide raw material that is contained in the crucible is that density is 3.0g/cm
3, purity is the alumina raw material more than 99.996%, behind the furnace chamber of sealing crystal growing furnace; Under inert atmosphere, rise to 48kw through 12 hours power with heating element; With the fusing alumina raw material, wherein, first scheduled time that heating element keeps permanent power to continue is selected from arbitrary value in 4-6 hour; Wherein, first temperature value of cooling water system is selected from arbitrary value in 30 ± 1 ℃.
(2) seeding step is transferred the seed crystal that from the thermally induced flow device, stretches out, and after seed crystal being accomplished roasting crystalline substance, continues to transfer seed crystal and keeps for second scheduled time to immerse in the raw material liquation and to continue, and wherein, the thermally induced flow device is a sleeve-like and from the top clamping seed crystal of seed crystal.In more detail; In above-mentioned first embodiment of the present invention; In the seeding step, under inert atmosphere conditions, transfer seed crystal with the speed of 20-50mm/h; Transferring to accomplishing apart from the position of the liquid level 5-10mm of raw material liquation roasting brilliantly, said second scheduled time that the seed crystal behind the wherein roasting crystalline substance remains in the raw material liquation is arbitrary value in 30-60 minute (being preferably 20 minutes).By this, seeding technology of the present invention is simple, does not need repeatedly necking down, has reduced the experienced requirement to the Technology personnel.
(3) heat transportation step; Temperature to be fed to the water coolant the seed rod from cooling water system is controlled; Make the temperature of water coolant in the seed rod from first temperature value uniform decrease in temperature to the second temperature value, wherein, the heat of water coolant evenly is transferred to seed crystal through the thermally induced flow device in the seed rod; Thereby, can control the raw material liquation and around seed crystal, begin crystallization through the temperature of water coolant in the control seed rod.In more detail, in above-mentioned first embodiment of the present invention, in the heat transportation step; The water coolant that in 10-20 hour time, will enter into seed rod is from first temperature value uniform decrease in temperature to the second temperature value, wherein, and when first temperature value is 30 ℃; Second temperature value is 20 ℃; Further, in the heat transportation step of this first embodiment, the time length of crystal growth is 10-20 hour.
(4) power regulation step; After accomplishing the heat transportation step; Make the power of heating element keep for the 3rd scheduled time constant, in the 3rd scheduled time, keep the water coolant in the seed rod to keep second temperature value constant simultaneously, the power of regulating heating element then is until accomplishing crystal growth.In more detail; In above-mentioned first embodiment of the present invention, in the power regulation step, the time length of second temperature value of water coolant was the 4th scheduled time in the power of heating element, the seed rod; The 4th scheduled time was the arbitrary value in 6-10 hour; After the 4th scheduled time, with the speed of average 0.03kw/h with the power regulation of heating element to 45kw, accomplish crystal growth.By this; Crystal diameter after growth is accomplished is equivalent to 4/5 of crucible internal diameter, and preferably, the crystal diameter after growth is accomplished is 150-200mm; Highly be 320mm; Further preferably, crystal height and diameter ratio after growth is accomplished reach 2: 1, thereby have improved the crystalline availability fully.
(5) cooling, annealing steps after the power regulation step, are lowered the temperature, are annealed all pyrotoxins in the crystal growing furnace.In more detail; In above-mentioned first embodiment of the present invention; Cooling, annealing steps is: with the speed of 0.4kw/h the power of heating element is dropped to 5kw from 45kw; After 5 hours, the power of heating element is reduced to 0 then, further, the other system in the crystal growing furnace except heating element was closed after working on 30-50 hour.
(6) tear the stove step open, after accomplishing cooling, annealing steps, the dismounting crystal growing furnace is to take out the crystal after growth is accomplished.After tearing the completion of stove step open, preparation method of the present invention finishes.
Point out that further in above-mentioned preparation step, in the seeding step, in the heat transportation step, in the power regulation step, the crystalline growth is in the inert atmosphere all the time.Obviously adopting alumina raw material among above-mentioned first embodiment is in order to prepare sapphire crystal, but the present invention is not limited to this, and preparation method of the present invention can be used for the preparation of one-component oxide crystal.
To sum up; Preparation in accordance with the present invention can growth diameter approaches the crystal of crucible internal diameter, (be preferably growth back crystalline diameter be crucible inside diameter 4/5); Obtained diameter 150-200mm; Height is the sapphire crystal of 320mm, and crystal height and diameter ratio can reach 2: 1 simultaneously, have improved the crystalline availability fully; Seeding technology is simple, does not need repeatedly necking down, has reduced the experienced requirement to the Technology personnel; And, in crystal growing process, only there is the natural convection that causes by gravity in the melt, melt spontaneous nucleation under the effect of the guiding of seed crystal and thermally induced flow device forms, and has guaranteed high-quality crystal.
For can further understanding method of the present invention, below crystal growing furnace, thermally induced flow device, the seed crystal that relates in the inventive method is described in detail.
The embodiment of the crystal growing furnace that the inventive method adopts is described referring to Fig. 1; The furnace chamber of crystal growing furnace is made up of furnace bottom 14, body of heater 15 and bell 9; Between furnace bottom 14 and the body of heater 15, and be connected with removably between bell 9 and the body of heater 15, wherein; The crucible 7 that is contained in the furnace chamber is the miramint crucible, and the heating element that is contained in the furnace chamber is made up of with heat generating part 6 two portions tungsten silk screen heating electrode 17.The tungsten silk screen of heat generating part for being provided with around crucible; Miramint is made up of the molybdenum of the tungsten and 70% (weight percent) of 30% (weight percent); Also be provided with heat protection screen between body of heater 15 and the tungsten silk screen, heat protection screen centers on the tungsten silk screen setting and is configured to by tungsten sheet and/or the molybdenum sheet stratiform overlaying structure alternate with pyroceramic.Continuation is referring to Fig. 1; Between furnace bottom 14 and body of heater 15; And the connecting portion between bell 9 and the body of heater 15 with red copper sealing-ring 1 as sealed structure, compare with viton seal ring of the prior art, not only guaranteed good sealing effectiveness; Also solve the problem of sealing-ring material ageing, effectively improved the vacuum tightness of furnace chamber.The bottom of crucible 7 has the crucible supporting structure, and the top of crucible 7 has crucible cover 13.Wherein, the crucible supporting structure comprise the tungsten bar 4 that is supported in the crucible bottom central position and with the molybdenum pipe 5 of tungsten bar 4 co-axial hollows.The material that supporting structure is selected for use is consistent with the material component of crucible 7, and this consistence can prevent the difficulty of the Temperature Field Control aspect that the bad thermal conduction of generation causes in the heat-processed, has improved the stability of hot system.Tungsten bar 4 is sheathed in the molybdenum pipe 5, and the preferred diameter of tungsten bar 4 is 30mm, the preferred external diameter (outer dia) of molybdenum pipe 5 be crucible 7 external diameter 2/3～3/4.So, the tungsten bar 4 that is in center position can bear bigger anchorage force, and the molybdenum pipe 5 that diameter is bigger has then enlarged Area of bearing largely.The integrated structure of support component has guaranteed that effectively crucible 7 is in horizontality all the time and has increased its steadiness.Heat protection screen is coaxial with body of heater 15, and is arranged between body of heater 15 and the wire netting as the heat generating part of heating element.The heat protection screen stratiform overlaying structure alternate with pyroceramic 2 that be tinsel 12, tinsel 12, pyroceramic 2 set gradually along body of heater 15 radial direction from inside to outside.According to the requirement in concrete temperature field, the laminate structure that tungsten sheet and/or molybdenum sheet and pyroceramic 2 are formed can have one or more layers.Tungsten sheet and/or molybdenum sheet can deform under the long term high temperature condition, and with after pyroceramic 2 combines with layered structure, have increased the bulk strength of heat protection screen effectively, have reduced the probability of the high temperature deformation of tungsten sheet and/or molybdenum sheet, have improved the symmetry in temperature field.And then, using molten higher tungsten, the Mo of boiling point, can under long term high temperature, keep thermal-radiating reflecting effect, make the most of heat that is radiated on it to reflect back, thereby have good heat insulation effect.In addition, also have thermoscreen in the furnace chamber, comprise the following thermoscreen 3 that is positioned at crucible 7 belows and be positioned at the last thermoscreen 11 of crucible cover 13 tops.Thermoscreen and heat protection screen link together through web member, form crucible 7 is contained in heating chamber 16 wherein, fixedly mount heating element in the heating chamber 16.Heating element is release of heat in heating chamber 16, and the effect through heat protection screen and thermoscreen is trapped in heat in the heating chamber 16, to realize the heating to the raw material in the crucible 7.Heating element in the crystal growing furnace is made up of with heat generating part 6 two portions tungsten silk screen heating electrode 17.In addition, Fig. 1 also illustrates crystal growing furnace and also comprises copper electrode 8.One end of copper electrode 8 stretches out bell 9 outsides and is used to connect power supply, and the other end is arranged in furnace chamber and is connected with an end of tungsten silk screen heating electrode 17, and both mode of connection are preferably and are threaded.The other end of tungsten silk screen heating electrode 17 is connected with the heat generating part 6 of heating element, and the heat generating part 6 of heating element is positioned at heating chamber 16.Through the fixed action of web member, an end that is connected with heat generating part 6 of tungsten silk screen heating electrode 17 is stretched in the heating chamber 16, the other end that is connected with copper electrode 8 is positioned at outside the heating chamber 16.For heat insulation effect and the prevention electrode that does not influence heating chamber 16 conducts electricity to miscellaneous part, the web member of fixed tungsten silk screen heating electrode 17 adopts pyroceramic 2 and insulating ceramic 10.Crystal growing furnace referring to accompanying drawing 1 is described can be in order to growing sapphire crystal, other one-component high-temp oxide crystals etc.
Further, referring to Fig. 2 and Fig. 3.Wherein, The structure of thermally induced flow device is as shown in Figure 2; Be sleeve-like, sleeve is being provided with screw thread 34 along centering on perisporium on the end of its axis direction, and sleeve is provided with annular radial protrusion 32 at the other end along its axis direction; Radial protrusion 32 is located on the inner side-wall of telescopic perisporium, and forms first diameter through hole 30 around the telescopic axis; The shape of the seed crystal of this thermally induced flow device clamping shown in Fig. 3, this seed crystal are the hierarchic structure with first shaft part 100 and second shaft part 200, the axis coaxle of the axis of first shaft part 100 and second shaft part 200.Seed crystal passes first diameter through hole 30 and is suspended on the thermally induced flow device; Particularly, radial protrusion 32 is arranged to cooperate with the ring surface of first shaft part 100 of seed crystal, promptly; First shaft part 100 is supported on the annular perimembranous of radial protrusion 32 formation; First diameter through hole 30 is set to cooperate with second shaft part, 200 axis holes of seed crystal, that is, second shaft part 200 stretches out from the thermally induced flow device through first diameter through hole 30.Thereby; When the seed rod (not shown) is threaded through between screw thread 34 and the thermally induced flow device; And seed crystal is when being clipped in the thermally induced flow device through first diameter through hole 30; The heat that is fed to the water coolant in the seed rod evenly is transferred to seed crystal via the thermally induced flow device, thereby makes fused raw material around seed crystal, begin crystallization.
The above is merely the preferred embodiments of the present invention, is not limited to the present invention, and for a person skilled in the art, the present invention can have various changes and variation.All within spirit of the present invention and principle, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. the preparation method of an one-component oxide crystal is characterized in that, comprises the steps:
Preparation step; One-component oxide raw material in the crucible that is contained in crystal growing furnace is melted; Make in the said crystal growing furnace power of heating element remain unchanged then and continued for first scheduled time, in said first scheduled time, make the temperature of cooling water of cooling water system remain first temperature value simultaneously;
The seeding step; Transfer the seed crystal that from the thermally induced flow device, stretches out; After said seed crystal is accomplished roasting crystalline substance, continue to transfer said seed crystal and kept for second scheduled time, wherein to immerse in the raw material liquation and to continue; Said thermally induced flow device is a sleeve-like and from the said seed crystal of top clamping of said seed crystal, also is connected with seed rod on the said thermally induced flow device;
The heat transportation step; Control gets into water coolant in the said seed rod from said first temperature value uniform decrease in temperature to the second temperature value by said cooling water system; Wherein, The heat of water coolant evenly is transferred to said seed crystal through said thermally induced flow device in the said seed rod, so that said raw material liquation begins crystallization around seed crystal;
The power regulation step; After accomplishing said heat transportation step; Make the power of said heating element keep for the 3rd scheduled time constant; In said the 3rd scheduled time, keep the water coolant in the said seed rod to keep second temperature value constant simultaneously, the power of regulating said heating element then is until accomplishing crystal growth.
2. preparation method according to claim 1 is characterized in that:
In said preparation step, the one-component oxide raw material that is contained in the said crucible is that density is 3.0g/cm
3, purity is the alumina raw material more than 99.996%, behind the furnace chamber of the said crystal growing furnace of sealing; Under inert atmosphere, rise to 48kw, to melt said alumina raw material, wherein through 12 hours power with said heating element; The time that said heating element keeps permanent power to continue is said first scheduled time; Said first scheduled time, wherein, said first temperature value was selected from arbitrary value in 30 ± 1 ℃ in order to be selected from arbitrary value in 4-6 hour;
In said seeding step; Under inert atmosphere conditions; Transfer said seed crystal with the speed of 20-50mm/h; Said roasting crystalline substance is accomplished in the position of liquid level 5-10mm transferring to the said raw material liquation of distance, and said second scheduled time that the seed crystal behind the wherein roasting crystalline substance remains in the raw material liquation is arbitrary value in 30-60 minute;
In said heat transportation step, the water coolant that in 10-20 hour time, will enter into said seed rod is from said first temperature value uniform decrease in temperature to the second temperature value, and wherein, when said first temperature value was 30 ℃, said second temperature value was 20 ℃;
In said power regulation step; Second temperature value of water coolant continued for the 4th scheduled time in the power of said heating element, the said seed rod; Said the 4th scheduled time is the arbitrary value in 6-10 hour; Wherein, after said the 4th scheduled time, power regulation to the mode of 45kw of said heating element is accomplished described crystal growth through speed with average 0.03kw/h.
3. preparation method according to claim 2 is characterized in that,
In said seeding step, said second scheduled time that the seed crystal behind the roasting crystalline substance remains in the raw material liquation is 20 minutes;
In said heat transportation step, the time length of crystal growth is 10-20 hour.
4. according to each described preparation method among the claim 1-3, it is characterized in that, also comprise:
After said power regulation step, all pyrotoxins in the said crystal growing furnace are lowered the temperature, annealed; And
After accomplishing said cooling, annealing steps, dismantle said crystal growing furnace to take out the crystal after growth is accomplished.
5. preparation method according to claim 4; It is characterized in that; Said cooling, annealing steps are: with the speed of 0.4kw/h the power of said heating element is dropped to 5kw from 45kw; After 5 hours, the power of heating element is reduced to 0 then, further, the other system in the said crystal growing furnace except said heating element was closed after working on 30-50 hour.
6. according to each described preparation method among the claim 1-3,5, it is characterized in that the furnace chamber of said crystal growing furnace is made up of furnace bottom, body of heater and bell, between said furnace bottom and the body of heater, and be connected with removably between said bell and the body of heater,
Wherein, the said crucible that is contained in the said furnace chamber is the miramint crucible, and the heating element that is contained in the said furnace chamber has heat generating part, the tungsten silk screen of said heat generating part for being provided with around said crucible, and said miramint is made up of 30% tungsten and 70% molybdenum,
Wherein, also be provided with heat protection screen between said body of heater and the tungsten silk screen, said heat protection screen centers on said tungsten silk screen setting, and is configured to by tungsten sheet and/or the molybdenum sheet stratiform overlaying structure alternate with pyroceramic.
7. preparation method according to claim 6 is characterized in that, in said power regulation step, the crystal diameter after growth is accomplished is 150-200mm, highly is 320mm.
8. preparation method according to claim 7 is characterized in that, in said power regulation step, crystal height and diameter ratio after growth is accomplished reach 2: 1.
9. preparation method according to claim 8 is characterized in that, in said power regulation step, the crystal diameter after growth is accomplished is 4/5 of a said crucible inside diameter.
10. according to each described preparation method among the claim 1-3,5, it is characterized in that,
In said seeding step, in said heat transportation step, in said power regulation step, the crystalline growth is in the inert atmosphere all the time; Said one-component oxide crystal is a sapphire crystal.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102797033A (en) * | 2012-08-15 | 2012-11-28 | 四川欣蓝光电科技有限公司 | Seeding process controlling method for growing large-size sapphire crystal with soaked-growth method |
| CN103147121A (en) * | 2013-04-03 | 2013-06-12 | 中国科学院上海硅酸盐研究所 | Device for growing crystals by using lifting and Kyropoulos method |
| KR20150053121A (en) * | 2013-11-07 | 2015-05-15 | 주식회사 엘지실트론 | Apparatus and method for manufacturing silicone single crystal ingot |
| CN105019023A (en) * | 2015-08-26 | 2015-11-04 | 江苏中电振华晶体技术有限公司 | Seeding method for growth of sapphire crystal with KY (Kyropoulos) method |
| CN105603510A (en) * | 2016-02-03 | 2016-05-25 | 江苏浩瀚蓝宝石科技有限公司 | Single crystal growth furnace |
| CN108588832A (en) * | 2018-04-28 | 2018-09-28 | 内蒙古恒嘉晶体材料有限公司 | Prepare the improved kyropoulos and crystal growing furnace of sapphire crystal |
| CN115433999A (en) * | 2021-09-10 | 2022-12-06 | 四川大学 | Method for growing all-inorganic non-lead perovskite single crystal |
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| CN105603510A (en) * | 2016-02-03 | 2016-05-25 | 江苏浩瀚蓝宝石科技有限公司 | Single crystal growth furnace |
| CN108588832A (en) * | 2018-04-28 | 2018-09-28 | 内蒙古恒嘉晶体材料有限公司 | Prepare the improved kyropoulos and crystal growing furnace of sapphire crystal |
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