CN102560631A - Growth method and equipment of sapphire crystal - Google Patents
Growth method and equipment of sapphire crystal Download PDFInfo
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- CN102560631A CN102560631A CN2012100179578A CN201210017957A CN102560631A CN 102560631 A CN102560631 A CN 102560631A CN 2012100179578 A CN2012100179578 A CN 2012100179578A CN 201210017957 A CN201210017957 A CN 201210017957A CN 102560631 A CN102560631 A CN 102560631A
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Abstract
The invention discloses a growth method and equipment of a sapphire crystal. The growth method comprises the following steps of: step S1, placing a high purity sapphire lump material or powder material of a set weight into a crucible, and then placing the crucible into a crystal growth furnace, wherein a guide die is arranged in the crucible; step S2, vacuumizing the crystal growth furnace; step S3, controlling the temperature rise of the crystal growth furnace to 2,000-2,100 DEG C through a main heater until sapphire is smelted into a fusant; step S4, discharging a seed crystal, and carrying out seeding; step S5, growing the crystal at the speed of 10-100 mm/h until the crystal growth ends; step S6, carrying out annealing treatment on a crystal bar, wherein the annealing temperature is 1,600-2,000 DEG C, and the annealing time is for 10-20 hr; step S7, slowly cooling at the speed of 10-60 DEG C per h; and step S8, cooling the temperature in the furnace to room temperature, and taking out the crystal bar. According to the growth method and equipment of the sapphire crystal provided by the invention, a bar-shaped sapphire crystal can be prepared, and the utilization rate of the sapphire crystal is effectively improved. The crystal which grows by using the method is subjected to forming and processing and can be used, as a substrate, for manufacturing LED (Light Emitting Diode) and LD (Laser Diode) devices.
Description
Technical field
The invention belongs to the crystal technique field, relate to a kind of growing method, relate in particular to a kind of growth method of sapphire crystal; Simultaneously, the invention still further relates to a kind of growth apparatus of sapphire crystal.
Background technology
Sapphire aluminum oxide (the Al that consists of
2O
3), be by three Sauerstoffatoms and two aluminium atoms with covalent linkage pattern be combined into, its crystalline structure is a hexagonal lattice structure.Because sapphire has the high velocity of sound, high temperature resistant, anticorrosive, high firmness, high light transmittance, the high characteristics such as (2045 ℃) of fusing point, therefore often be used as the material of sealed cell.At present super brightness white/quality of blue-ray LED depends on the material quality of epitaxial layer of gallium nitride (GaN), the epitaxial layer of gallium nitride quality is then closely bound up with employed Sapphire Substrate surface working quality.Because sapphire (monocrystalline Al
2O
3) lattice constant mismatch rate between c face and III-V and the II-VI family deposit film is little, meets resistant to elevated temperatures requirement in the GaN epitaxial manufacture process simultaneously, makes sapphire wafer become the critical material of making white/indigo plant/green light LED.
The at present existing a variety of methods of the growth method of sapphire crystal material; Mainly contain: kyropoulos (be the Kyropolos method, be called for short the Ky method), guided mode method (are edge defined film-fed growth techniques method, are called for short the EFG method; Belong to a kind of of TPS method), heat-exchanging method (is heat exchange method method; Be called for short the HEM method), Bridgman method (be the Bridgman method, or falling crucible method), crystal pulling method (be Czochralski, be called for short the Cz method) etc.But the crystals with different growth method designs to sapphire different purposes.At present, be used for the sapphire growing method in LED field, commonly used has two kinds:
1, the long brilliant method (Kyropoulos method) of Kai Shi is called for short the KY method, also claims kyropoulos.(Czochralski method) is similar for its principle and Chai Shi crystal pulling method, and fusing formed melt after elder generation was heated to fusing point with raw material, and the seed crystal (SeedCrystal) with monocrystalline touches bath surface again; Monocrystalline with the seed crystal same crystal structure begins to grow on the solid-liquid interface of seed crystal and melt; Seed crystal with the utmost point slowly speed up draw high, but seed crystal up crystal pulling for some time to form brilliant neck, treat that the solidification rate at melt and seed crystal interface is stable after; Seed crystal just no longer draws high; Also do not rotate, only with controlled chilling speed mode monocrystalline is down solidified gradually from the top, final set becomes the brilliant heavy stone used as an anchor of a whole monocrystalline.Then, utilize and draw rod processing, draw the crystal bar that system standard LED uses along vertical axial.Its effective rate of utilization generally about 30%, has limited the cost of LED substrate slice.
2, guided mode method (also claiming edge limited film feed method), it also belongs to a kind of of TPS method, is mainly used in the thin panel material.It has utilized the capillary principle, and melt is imported the top of mould, with seed crystal this part melt is lifted the generation single-chip.Utilize then and draw sheet processing, draw and make the workprint that LED one by one uses.Because in the long brilliant process, the two-sided of thin plate all has large-area bubble, so the substrate thickness that the thickness overgauge LED of sheet material uses causes the removal amount in the wafer process process big, directly increased the wafer process cost.
Relating to the manufacturing technology of sapphire crystal like Chinese patent CN201010147683.5, specifically is a kind of growth method of large-size flaky sapphire crystals.Its crystal growing process carries out in monocrystal growing furnace, and crucible and guided mode are set in the stove, and crystal growing process comprises the heating of sapphire raw material, seeding, shouldering, isometrical lifting and cooling step successively; The pressure control system that the shielding gas that can feed and discharge shielding gas passes in and out gas system and may command furnace pressure is set in the said monocrystal growing furnace; In stove, feed shielding gas in the step the heating of sapphire raw material, seeding, shouldering, isometrical lifting; Make shielding gas formation flowing gas in the stove through shielding gas turnover gas system; Its charge flow rate is 0.1-50slpm, makes through pressure control system simultaneously that pressure pressure is 100pa-90kpa in the stove.
This shows, the sapphire crystal that above-mentioned each class methods make, working (machining) efficiency is lower, and the wafer manufacture cost is high.In view of this, press for a kind of method that can improve the sapphire crystal preparation efficiency.
Summary of the invention
Technical problem to be solved by this invention is: a kind of growth method of sapphire crystal is provided, can makes bar-shaped sapphire crystal, effectively improve the sapphire crystal preparation efficiency.
In addition, the present invention also provides a kind of growth apparatus of sapphire crystal, can make bar-shaped sapphire crystal, effectively improves the sapphire crystal preparation efficiency.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of growth method of sapphire crystal, said method comprises the steps:
Step S1: high-purity sapphire piece material of setting weight or powder are packed in the crucible, then crucible is placed in the crystal growing furnace;
Be provided with the guided mode mould in the said crucible; The cross section of said guided mode mould is square or rectangle, and its center has can make the sapphire melt form the aperture of capillarity; Perhaps, said guided mode mould is that the cross section is square or rectangular ring mould; The material of guided mode mould and sapphire melt have infiltrating high temperature material or its alloy material;
Step S2: with the crystal growth stove evacuation, vacuum tightness is～10
-3Pa;
Step S3: be warming up to 2000-2100 ℃ through primary heater control crystal growing furnace, treat that sapphire is fused into melt;
Step S4: select for use a to or m to oriented seed, following seed crystal carries out seeding;
The cross section of guided mode mould is square or rectangle, when the center has aperture, utilize the capillary principle that the sapphire melt is imported the top end face of guided mode mould, and the seed crystal with setting the crystal orientation lifts the sapphire melt, thereby carries out the growth of rhabdolith;
The guided mode mould is that the cross section is when being square or rectangular ring mould; Part sapphire melt is limited in the ring mould, utilizes this guided mode moulding stock and sapphire wellability, with the seed crystal of setting the crystal orientation; Confined melt is lifted, thereby carry out the growth of rhabdolith;
Step S5: the speed with 10～100mm/hr is carried out crystal growth, finishes to crystal growth;
Step S6: carry out the anneal of crystal bar, 1600～2000 ℃ of annealing temperatures, annealing time 10～20hr;
Step S7: the speed with 10～60 ℃/hr is slowly lowered the temperature;
Step S8: after temperature is reduced to room temperature in the stove, take out crystal bar.
A kind of growth method of sapphire crystal, said method comprises the steps:
Step S1: high-purity sapphire piece material of setting weight or powder are packed in the crucible, then crucible is placed in the crystal growing furnace; Be provided with the guided mode mould in the said crucible;
Step S2: with the crystal growth stove evacuation;
Step S3: be warming up to 2000-2100 ℃ through primary heater control crystal growing furnace, treat that sapphire is fused into melt, mold top forms melt films;
Step S4: following seed crystal, carry out seeding;
Step S5: the speed with 10～100mm/hr is carried out crystal growth, finishes to crystal growth;
Step S6: carry out the anneal of crystal bar, 1600～2000 ℃ of annealing temperatures, annealing time 10～20hr;
Step S7: the speed with 10～60 ℃/hr is slowly lowered the temperature;
Step S8: after temperature is reduced to room temperature in the stove, take out crystal bar.
As a kind of preferred version of the present invention, the cross section of said guided mode mould is square or rectangle, and its center has can make the sapphire melt form the aperture of capillarity; The material of guided mode mould and sapphire melt have infiltrating high temperature material or its alloy material; Among the said step S3, utilize the top end face of capillary principle with sapphire melt importing guided mode mould, the seed crystal with setting the crystal orientation lifts the sapphire melt, thereby carries out the growth of rhabdolith.
As a kind of preferred version of the present invention, said guided mode mould is that the cross section is square or rectangular ring mould, and the material of guided mode mould and sapphire melt have infiltrating high temperature material or its alloy material; Among the said step S3, part sapphire melt is limited in the ring mould, utilizes this guided mode moulding stock and sapphire wellability, the seed crystal with setting the crystal orientation lifts confined melt, thereby carries out the growth of rhabdolith.
As a kind of preferred version of the present invention, the material of said guided mode mould is molybdenum, tungsten, iridium or tantalum, or its alloy.
As a kind of preferred version of the present invention, the material of said crucible is molybdenum, tungsten, iridium or tantalum, or its alloy.
As a kind of preferred version of the present invention, said guided mode mould has at least length on one side to be not less than 50.8mm.
As a kind of preferred version of the present invention, the seed crystal crystal orientation of being selected for use is that m is to
or the seed crystal of a to
.
As a kind of preferred version of the present invention, among the step S6, the position of said crystal bar is provided with auxilliary well heater, carries out anneal, 1600～2000 ℃ of annealing temperatures.
The growth apparatus that a kind of above-mentioned sapphire crystal growth method uses, said equipment comprises: guided mode mould, crucible, crystal growing furnace, primary heater, vacuum extractor, auxilliary well heater; Said guided mode mould places crucible, and crucible places crystal growing furnace, and primary heater is in order to heat crystal growing furnace, and auxilliary well heater is arranged at the position that crystal bar takes out.
Beneficial effect of the present invention is: the growth method and the equipment of the sapphire crystal that the present invention proposes, can make bar-shaped sapphire crystal, and effectively improve the sapphire crystal preparation efficiency.Utilize the crystal of this method growth,, can be used as substrate and be used for LED, the manufacturing of LD device through typing processing.
Description of drawings
Fig. 1 is the structural representation of sapphire crystal growth apparatus in the embodiment of the invention one.
Fig. 2 is the structural representation of sapphire crystal growth apparatus in the embodiment of the invention two.
Fig. 3 is the schema of the inventive method.
Fig. 4 is the schematic cross-section of square crystal bar.
Fig. 5 is the schematic cross-section of rectangle crystal bar.
Embodiment
Specify the preferred embodiments of the present invention below in conjunction with accompanying drawing.
Embodiment one
The present invention is a kind of growth method of sapphire rhabdolith; Select high temperature resistant and as far as the sapphire melt have can infiltrating material as the guided mode mould; (top end face like mould has specified shape through this kind material is carried out structure design; Like square, rectangle etc., utilize the capillary principle that the sapphire melt is imported its top end face; Or utilize die edge restricted part melt), guarantee that it forms certain thickness melt film or limits certain thickness melt film through it.Select certain crystal orientation seed crystal for use, cross this melt film is carried out the drawing of bar-shaped sapphire crystal, the crystal bar that is drawn satisfies the request for utilization of LED, LD industry.Growth method of the present invention is referred to as the TaVi method, is based on a kind of the improving one's methods of TPS technology (Technique of Pulling from Shapers), and is a kind of novel bar-shaped sapphire crystal growth method that mould carries out that passes through.
See also Fig. 3, the present invention has disclosed a kind of growth method of sapphire crystal, and said method comprises the steps:
[step S1] is as shown in Figure 1, and high-purity sapphire piece material of setting weight or powder are packed in the crucible 1, then crucible 1 is placed in the crystal growing furnace.The material of said crucible can be molybdenum, tungsten, iridium or tantalum, or its alloy.
Be provided with guided mode mould 3 in the said crucible 1; In the present embodiment, the cross section of said guided mode mould 3 is square or rectangle, and its center has can make the sapphire melt form the aperture of capillarity.The material of guided mode mould 3 and sapphire melt have infiltrating high temperature material or its alloy material.As, the material of said guided mode mould can be molybdenum, tungsten, iridium or tantalum, or its alloy.In the present embodiment, said guided mode mould 3 has at least length on one side to be not less than 50.8mm.
[step S2] with the crystal growth stove evacuation, vacuum tightness is～10
-3Pa;
[step S3] is warming up to 2000-2100 ℃ through primary heater 6 control crystal growing furnaces, treats that sapphire is fused into melt 2.
[step S4] select for use a to or m to oriented seed, following seed crystal carries out seeding.
In the present embodiment, the seed crystal crystal orientation of being selected for use is that m is to
or the seed crystal of a to
.Utilize the top end face of capillary principle with sapphire melt importing guided mode mould, the seed crystal with setting the crystal orientation lifts the sapphire melt, thereby carries out the growth of rhabdolith.
[step S5] carries out crystal growth with the speed of 10～100mm/h, grows into crystal bar 5, finishes to crystal growth.
[step S6] carries out the anneal of crystal bar 5,1600～2000 ℃ of annealing temperatures, annealing time 10～20hr.
[step S7] slowly lowers the temperature with the speed of 10～60 ℃/h.
After temperature is reduced to room temperature in [step S8] stove, take out crystal bar 5; The position that crystal bar 5 takes out is provided with auxilliary well heater 7.Because the cross section of guided mode mould 3 is a square or rectangular, the cross section of the feasible crystal bar 5 that makes is square (as shown in Figure 4) or rectangle (as shown in Figure 5).
Embodiment two
See also Fig. 2, the difference of present embodiment and embodiment one is that in the present embodiment, said guided mode mould 3 is square or rectangular ring mould for the cross section; The material of guided mode mould and sapphire melt have infiltrating high temperature material or its alloy material;
The difference of described method is among the growth method of the sapphire crystal of present embodiment and the embodiment one; In the present embodiment step 3; Part sapphire melt is limited in the annular guided mode mould 3, utilizes this guided mode mould 3 materials and sapphire wellability, with the seed crystal of setting the crystal orientation; Confined melt is lifted, thereby carry out the growth of rhabdolith.
In sum, the growth method and the equipment of the sapphire crystal that the present invention proposes can make bar-shaped sapphire crystal, effectively improve the sapphire crystal preparation efficiency.Utilize the crystal of this method growth,, can be used as substrate and be used for LED, the manufacturing of LD device through typing processing.
Here description of the invention and application is illustrative, is not to want with scope restriction of the present invention in the above-described embodiments.Here the distortion of the embodiment that is disclosed and change are possible, and the replacement of embodiment is known with the various parts of equivalence for those those of ordinary skill in the art.Those skilled in the art are noted that under the situation that does not break away from spirit of the present invention or essential characteristic, and the present invention can be with other form, structure, layout, ratio, and realize with other assembly, material and parts.Under the situation that does not break away from the scope of the invention and spirit, can carry out other distortion and change here to the embodiment that is disclosed.
Claims (10)
1. the growth method of a sapphire crystal is characterized in that, said method comprises the steps:
Step S1: high-purity sapphire piece material of setting weight or powder are packed in the crucible, then crucible is placed in the crystal growing furnace;
Be provided with the guided mode mould in the said crucible; The cross section of said guided mode mould is square or rectangle, and its center has can make the sapphire melt form the aperture of capillarity; Perhaps, said guided mode mould is that the cross section is square or rectangular ring mould; The material of guided mode mould and sapphire melt have infiltrating high temperature material or its alloy material;
Step S2: with the crystal growth stove evacuation, vacuum tightness～10
-3Pa;
Step S3: be warming up to 2000-2100 ℃ through primary heater control crystal growing furnace, treat that sapphire is fused into melt, mold top forms melt films;
Step S4: select for use a to or m to oriented seed, following seed crystal carries out seeding;
The cross section of guided mode mould is square or rectangle, when the center has aperture, utilize the capillary principle that the sapphire melt is imported the top end face of guided mode mould, and the seed crystal with setting the crystal orientation lifts the sapphire melt, thereby carries out the growth of rhabdolith;
The guided mode mould is that the cross section is when being square or rectangular ring mould; Part sapphire melt is limited in the ring mould, utilizes this guided mode moulding stock and sapphire wellability, with the seed crystal of setting the crystal orientation; Confined melt is lifted, thereby carry out the growth of rhabdolith;
Step S5: the speed with 10～100mm/hr is carried out crystal growth, finishes to crystal growth;
Step S6: carry out the anneal of crystal bar, 1600～2000 ℃ of annealing temperatures, annealing time 10～20hr;
Step S7: the speed with 10～60 ℃/hr is slowly lowered the temperature;
Step S8: after temperature is reduced to room temperature in the stove, take out crystal bar.
2. the growth method of a sapphire crystal is characterized in that, said method comprises the steps:
Step S1: high-purity sapphire piece material of setting weight or powder are packed in the crucible, then crucible is placed in the crystal growing furnace; Be provided with the guided mode mould in the said crucible;
Step S2: with the crystal growth stove evacuation;
Step S3: be warming up to 2000-2100 ℃ through primary heater control crystal growing furnace, treat that sapphire is fused into melt, mold top forms melt films;
Step S4: following seed crystal, carry out seeding;
Step S5: the speed with 10～100mm/hr is carried out crystal growth, finishes to crystal growth;
Step S6: carry out the anneal of crystal bar, 1600～2000 ℃ of annealing temperatures, annealing time 10～20hr;
Step S7: the speed with 10～60 ℃/hr is slowly lowered the temperature;
Step S8: after temperature is reduced to room temperature in the stove, take out crystal bar.
3. the growth method of sapphire crystal according to claim 2 is characterized in that:
The cross section of said guided mode mould is square or rectangle, and its center has can make the sapphire melt form the aperture of capillarity; The material of guided mode mould and sapphire melt have infiltrating high temperature material or its alloy material;
Among the said step S3, utilize the top end face of capillary principle with sapphire melt importing guided mode mould, the seed crystal with setting the crystal orientation lifts the sapphire melt, thereby carries out the growth of rhabdolith.
4. the growth method of sapphire crystal according to claim 2 is characterized in that:
Said guided mode mould is that the cross section is square or rectangular ring mould, and the material of guided mode mould and sapphire melt have infiltrating high temperature material or its alloy material;
Among the said step S3, part sapphire melt is limited in the ring mould, utilizes this guided mode mould
Material and sapphire wellability, the seed crystal with setting the crystal orientation lifts confined melt, thereby carries out the growth of rhabdolith.
5. according to the growth method of claim 3 or 4 described sapphire crystals, it is characterized in that:
The material of said guided mode mould is molybdenum, tungsten, iridium or tantalum, or its alloy.
6. the growth method of sapphire crystal according to claim 2 is characterized in that:
The material of said crucible is molybdenum, tungsten, iridium or tantalum, or its alloy.
7. the growth method of sapphire crystal according to claim 2 is characterized in that:
Said guided mode mould has at least length on one side to be not less than 50.8mm.
8. the growth method of sapphire crystal according to claim 2 is characterized in that:
Jingjing to the chosen seed of m to
or a to
a seed.
9. the growth method of sapphire crystal according to claim 2 is characterized in that:
Among the step S6, the position of said crystal bar is provided with auxilliary well heater, carries out anneal, 1600～2000 ℃ of annealing temperatures.
10. the growth apparatus that the said sapphire crystal growth method of claim 2 uses is characterized in that,
Said equipment comprises: guided mode mould, crucible, crystal growing furnace, primary heater, vacuum extractor, auxilliary well heater;
Said guided mode mould places crucible, and crucible places crystal growing furnace, and primary heater is in order to heat crystal growing furnace, and auxilliary well heater is used for crystal bar annealing.
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| CN104088014A (en) * | 2014-07-11 | 2014-10-08 | 江苏中电振华晶体技术有限公司 | Rod-like sapphire crystal growing equipment and rod-like sapphire crystal growing 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 |
| WO2016000617A1 (en) * | 2014-07-02 | 2016-01-07 | 攀时（上海）高性能材料有限公司 | Crucible for crystal cultivation |
| WO2018076902A1 (en) * | 2016-10-31 | 2018-05-03 | 福建晶安光电有限公司 | Crystal bar production method |
| CN109338467A (en) * | 2018-10-31 | 2019-02-15 | 江苏师范大学 | A kind of preparation method of coloring uniform color jewel |
| CN110318095A (en) * | 2019-06-27 | 2019-10-11 | 南京同溧晶体材料研究院有限公司 | A kind of novel crystal grower and its growing method |
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| CN109338467A (en) * | 2018-10-31 | 2019-02-15 | 江苏师范大学 | A kind of preparation method of coloring uniform color jewel |
| CN110318095A (en) * | 2019-06-27 | 2019-10-11 | 南京同溧晶体材料研究院有限公司 | A kind of novel crystal grower and its growing method |
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Application publication date: 20120711 |