CN103806101A - Growth method and equipment of square sapphire crystal - Google Patents
Growth method and equipment of square sapphire crystal Download PDFInfo
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- CN103806101A CN103806101A CN201210461724.7A CN201210461724A CN103806101A CN 103806101 A CN103806101 A CN 103806101A CN 201210461724 A CN201210461724 A CN 201210461724A CN 103806101 A CN103806101 A CN 103806101A
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Abstract
The invention discloses a growth method and equipment of a square sapphire crystal. The method disclosed by the invention comprises the following steps of: S1, putting a high-purity aluminium oxide blocky material or powder material in pre-set weight into a crucible, and then, putting the crucible in a crystal growth furnace; S2, vaccumizing the crystal growth furnace; S3, increasing the temperature of the crystal growth furnace through a heater so that the aluminium oxide raw material is molten into melt; S4, selecting an oriented seed crystal, fixing the oriented seed crystal in the centre of the crucible, and seeding when the temperature is proper; S5, after seeding, upwardly lifting the seed crystal, and beginning to grow the crystal; S6, after growing the crystal, slowly decreasing the temperature; S7, after decreasing the temperature in the furnace to the pre-set temperature, taking out the crystal, and cutting and processing into a wafer of required size. According to the growth method and equipment of the square sapphire crystal provided by the invention, sapphire crystals shaped as square, roundness and the like can be prepared; the utilization rate of the sapphire crystal is effectively increased while the high-quality crystal is prepared.
Description
Technical field
The invention belongs to crystal technique field, relate to a kind of growing method, relate in particular to a kind of growth method of square sapphire crystal; Meanwhile, the invention still further relates to a kind of growth apparatus of square sapphire crystal.
Background technology
Sapphire aluminum oxide (the Al that consists of
2o
3), be to be combined into covalent linkage pattern by three Sauerstoffatoms and two aluminium atoms, its crystalline structure is hexagonal lattice structure.Because sapphire has the features such as the high velocity of sound, high temperature resistant, anticorrosive, high rigidity, high light transmittance, fusing point high (2045 ℃), be therefore often used as the material of sealed cell.At present super brightness white/quality of blue-ray LED depends on the material quality of gan (GaN) epitaxial film, epitaxial layer of gallium nitride quality is closely bound up with used Sapphire Substrate surface working quality.Due to sapphire (monocrystalline Al
2o
3) lattice constant mismatch rate between c face and III-V and II-VI family deposit film is little, simultaneously can be high temperature resistant, make 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 (is Kyropolos method, be called for short Ky method), guided mode method (is edge defined film-fed growth techniques method, be called for short EFG method, belong to the one of TPS method), heat-exchanging method (is heat exchange method method, be called for short HEM method), Bridgman method (be Bridgman method, or falling crucible method), crystal pulling method (be Czochralski, be called for short Cz method) etc.But different growing methods designs for sapphire different purposes.At present, for the growth method of the above-mentioned sapphire crystal of sapphire growing method in LED field conventional have two kinds:
1, the long brilliant method of Kai Shi (Kyropoulos method), is called for short KY method, also claims kyropoulos.(Czochralski method) is similar for its principle and Chai Shi crystal pulling method, first heating raw materials is melted to formation melt to fusing point, touch bath surface with the seed crystal of monocrystalline again, in the solid-liquid interface of seed crystal and melt, start the monocrystalline of growth and seed crystal same crystal structure, seed crystal with the utmost point slowly speed up draw high, but seed crystal up crystal pulling for some time to form brilliant neck, after the solidification rate at melt and seed crystal interface is stablized, seed crystal just no longer draws high, also do not rotate, only to control rate of cooling mode, monocrystalline is down solidified gradually from top, final set becomes a whole monocrystalline crystal ingot.Then draw rod processing, draw along vertical axial the crystal bar that standard LED processed uses.Its effective rate of utilization is lower, generally in 30% left and right, causes the cost of LED relatively high.
2, guided mode method (also claiming edge limited film feed method), it is also the one of TPS method, is mainly used in growing thin material.It has utilized capillary principle, melt is imported to the top of mould, then with seed crystal, this part melt is lifted to generation single-chip.Then utilize and draw sheet processing, draw and make the workprint that LED uses.In long brilliant process, the two-sided of thin plate all has large-area bubble, so the thickness of sheet material is greater than the substrate thickness that standard LED uses, causes the removal amount in wafer process process large, directly increased wafer process cost.Owing to leading the long brilliant speed of embrane method, cause the even inner impurity of crystal edge more, crystal mass is not high simultaneously.
In view of this, can guarantee that in the urgent need to one crystal has better quality, can improve again the long crystal method of crystal service efficiency.
Summary of the invention
Technical problem to be solved by this invention is: a kind of growth method of square sapphire crystal is provided, can under the prerequisite that guarantees crystal mass, effectively improves the utilization ratio of sapphire crystal.
In addition, the present invention also provides a kind of growth apparatus of square sapphire crystal, can under the prerequisite that guarantees crystal mass, effectively improve the utilization ratio of sapphire crystal.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A growth method for square sapphire crystal, described method comprises the steps:
Step S1: the high purity aluminium oxide piece material of setting weight or powder are packed in square crucible, then square crucible is placed in crystal growing furnace;
Step S2: crystal growing furnace is vacuumized, make low vacuum in crystal growing furnace in 6 × 10
-3pa;
Step S3: be warming up to 2000-2100 ℃ by well heater control crystal growing furnace, treat that alumina raw material is molten into melt;
Step S4: select oriented seed, oriented seed is fixed on to the central position of crucible, guarantee that oriented seed c face is parallel to plane corresponding to the long limit of crucible, determines the suitable rear seeding of temperature;
Step S5: after seeding finishes, upwards lift seed crystal with the speed of 0.1 ~ 3mm/h, start crystal growth;
Step S6: after long crystalline substance finishes, with the speed slow cooling of 10 ~ 50 ℃/h;
Step S7: in stove, temperature is down to after room temperature, takes out square crystal, cuts and be processed into the wafer of desired size.
As a preferred embodiment of the present invention, the oriented seed of selecting in described step S4 be m to or a to.
As a preferred embodiment of the present invention, described square crucible is square crucible, in step S4, guarantees that oriented seed c face is parallel to crucible plane corresponding to one side arbitrarily.
As a preferred embodiment of the present invention, described method further comprises, regulates as required the shape of crucible, well heater, in order to regulate the shape of crystal cross section.
A growth method for square sapphire crystal, described method comprises the steps:
Step S1: the high purity aluminium oxide piece material of setting weight or powder are packed in square crucible, then square crucible is placed in crystal growing furnace;
Step S2: crystal growing furnace is evacuated to setting vacuum tightness;
Step S3: heat up by well heater control crystal growing furnace, make alumina raw material be molten into melt;
Step S4: select oriented seed, oriented seed is fixed on to the central position of crucible, the suitable rear seeding of temperature;
Step S5: after seeding finishes, upwards lift seed crystal, start crystal growth;
Step S6: after long crystalline substance finishes, slow cooling;
Step S7: in stove, temperature is down to after design temperature, takes out crystal, cuts and be processed into the wafer of desired size.
A growth apparatus for square sapphire crystal, described equipment includes crystal growing furnace, vacuum extractor, thermal field;
Described thermal field comprises well heater, crucible, crucible cover, heat shielding;
Described well heater is placed in crystal growing furnace, and crucible is placed in the central position of well heater, and crucible cover is placed in crucible top.
As a preferred embodiment of the present invention, described crucible is square crucible, and the cross section of crucible is rectangular; Or the cross section of described crucible is the rectangle with fillet, the radius of four fillets is at 1 ~ 20mm.
As a preferred embodiment of the present invention, described heat shielding mainly comprises heat shielding and outer heat shielding; Upper heat shielding is placed in crucible top, and its shape of cross section is identical with crucible; Outer heat shielding is placed in well heater outside, and it is shaped as circular or square; Being shaped as of described well heater, crucible cover is circular or square.
As a preferred embodiment of the present invention, described heater material is tungsten; Described crucible cover and heat-shield material are molybdenum or tungsten or iridium or tantalum, or are two or more elementary composition alloys in molybdenum, tungsten, iridium, tantalum.
Beneficial effect of the present invention is: growth method and the equipment of sapphire crystal that the present invention proposes, can make the sapphire crystal of the shape such as square, circular, and in making high quality crystal, effectively improve the utilization ratio of sapphire crystal.The thermal field of growth apparatus of the present invention can adopt the circular thermal field in traditional kyropoulos stove, and also replaceable is other specified shape thermal field, and thermal field component mainly comprises crucible and crucible cover, well heater, heat shielding etc.The shape of cross section of thermal field component can recently be selected according to the size of final crystal and length and width.Use this equipment can make square sapphire crystal, effectively improve the utilization ratio of sapphire crystal.
Accompanying drawing explanation
Fig. 1 is the structural representation of sapphire crystal growth equipment of the present invention.
Fig. 2 is the schema of the inventive method.
Fig. 3 is the schematic cross-section of square crystal rod.
Embodiment
Describe the preferred embodiments of the present invention in detail below in conjunction with accompanying drawing.
Embodiment mono-
Refer to Fig. 1, the present invention has disclosed a kind of growth apparatus of sapphire crystal, and described equipment includes crystal growing furnace, vacuum extractor, thermal field; Described thermal field comprises well heater 1, crucible 4, crucible cover, heat shielding.
Described well heater puts 1 in crystal growing furnace, and crucible 4 is placed in the central position of well heater 1, and crucible cover is placed in crucible 4 tops.Described heat shielding mainly comprises heat shielding and outer heat shielding; Upper heat shielding is placed in the top of crucible 4, and its shape of cross section is identical with crucible 4; Outer heat shielding is placed in well heater 1 outside, and its shape can be circular or square.
In the present embodiment, the material of described well heater 1 is tungsten; The material of described crucible cover and heat shielding is molybdenum or tungsten or iridium or tantalum, or is two or more elementary composition alloys in molybdenum, tungsten, iridium, tantalum.
The shape of cross section of described thermal field all parts (comprising well heater 1, crucible 4, crucible cover, heat shielding) can be circular square or oval, can certainly be that other are irregularly shaped; The shape of cross section that generates crystal can be controlled by the shape that changes thermal field.
In the present embodiment, described crucible 4 can be square crucible, and the cross section of crucible 4 is rectangular; The ratio on length limit is between 1 ~ 6, and minor face is not less than 120mm.Certainly, the cross section of described crucible also can be for having the rectangle (as shown in Figure 3) of fillet, and the radius of four fillets is at 1 ~ 20mm.Or described crucible 4 is circular crucible or oval crucible, the cross section of crucible is rounded or oval.
Under normal circumstances, if crucible is circular, the utilization ratio of crystal is lower, is usually less than 30%; And use square crucible, utilization ratio can reach 60%, and also can realize in actual production operation, be a more applicable technology.
More than introduced the structure of the growth apparatus of sapphire crystal of the present invention, the present invention, in disclosing aforesaid device, also discloses a kind of growth method of sapphire crystal; Refer to Fig. 2, described method comprises the steps:
[step S1] packs the high purity aluminium oxide piece material of setting weight or powder in square crucible 4 into, then crucible 4 is placed in crystal growing furnace.
[step S2] vacuumizes crystal growing furnace, make vacuum tightness in crystal growing furnace be better than (lower than) 6 × 10
-3pa.
[step S3] is warming up to 2000-2100 ℃ by well heater control crystal growing furnace, treats that alumina raw material is molten into melt 3.
[step S4] selects oriented seed 2, oriented seed 2 is fixed on to the central position of crucible, guarantees that oriented seed c face (0001) is parallel to plane corresponding to the long limit of crucible, determines the suitable rear seeding of temperature; Wherein, the oriented seed of selecting be m to or a to.Certainly,, if described square crucible is square crucible, guarantee that oriented seed c face is parallel to crucible plane corresponding to one side arbitrarily.
As required, can increase seeding supplementary unit 6 and assist seeding.
After [step S5] seeding finishes, upwards lift seed crystal with the speed of 0.1 ~ 3mm/h (as the speed with 0.1mm/h, also can with the speed of 2mm/h or 3mm/h), start crystal growth.
After [step S6] long crystalline substance finishes, with 10 ~ 50 ℃/h(as the speed slow cooling of 10 ℃/h, 20 ℃/h or 50 ℃/h).
In [step S7] stove, temperature is down to after room temperature, takes out square crystal, cuts and be processed into the wafer of desired size.
Embodiment bis-
The present invention discloses a kind of growth method of sapphire crystal, and described method comprises the steps:
[step S1] packs the high purity aluminium oxide piece material of setting weight or powder in crucible into, then crucible is placed in crystal growing furnace.Can adjust as required the shape of cross section of crucible, if crucible can be square (can be rectangle, can be also square), circle, oval; Or other are irregularly shaped.
[step S2] vacuumizes crystal growing furnace, make vacuum tightness in crystal growing furnace be better than (lower than) 6 × 10
-3pa.
[step S3] heats up (as being warming up to 2050 ℃) by well heater control crystal growing furnace, makes alumina raw material be molten into melt.
[step S4] selects oriented seed, oriented seed is fixed on to the central position of crucible, the suitable rear seeding of temperature.
After [step S5] seeding finishes, upwards lift seed crystal (as the speed with 1mm/h upwards lifts seed crystal), start crystal growth.
After [step S6] long crystalline substance finishes, slow cooling (as the speed slow cooling with 30 ℃/h).
In [step S7] stove, temperature is down to after design temperature (as room temperature), takes out crystal, cuts and be processed into the wafer of desired size.
In sum, growth method and the equipment of square sapphire crystal that the present invention proposes, can make the sapphire crystal of the shape such as square, circular, in making high quality crystal, effectively improves the utilization ratio of sapphire crystal.The thermal field of growth apparatus of the present invention can adopt the circular thermal field in traditional kyropoulos stove, and also replaceable is other specified shape thermal field, and thermal field component mainly comprises crucible and crucible cover, well heater, heat shielding etc.The shape of cross section of thermal field component can recently be selected according to the size of final crystal and length and width.Use this equipment can make square sapphire crystal, effectively improve the utilization ratio of sapphire crystal.
Here description of the invention and application is illustrative, not wants scope of the present invention to limit in the above-described embodiments.Here the distortion of disclosed embodiment and change is possible, and for those those of ordinary skill in the art, the various parts of the replacement of embodiment and equivalence are known.Those skilled in the art are noted that in the situation that not departing 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.In the situation that not departing from the scope of the invention and spirit, can carry out other distortion and change to disclosed embodiment here.
Claims (9)
1. a growth method for square sapphire crystal, is characterized in that, described method comprises the steps:
Step S1: the high purity aluminium oxide piece material of setting weight or powder are packed in square crucible, then square crucible is placed in crystal growing furnace;
Step S2: crystal growing furnace is vacuumized, make low vacuum in crystal growing furnace in 6 × 10
-3pa;
Step S3: be warming up to 2000-2100 ℃ by well heater control crystal growing furnace, treat that alumina raw material is molten into melt;
Step S4: select oriented seed, oriented seed is fixed on to the central position of crucible, guarantee that oriented seed c face is parallel to plane corresponding to the long limit of crucible, determines the suitable rear beginning seeding of temperature;
Step S5: after seeding finishes, upwards lift seed crystal with the speed of 0.1 ~ 3mm/h, start crystal growth;
Step S6: after long crystalline substance finishes, with the speed slow cooling of 10 ~ 50 ℃/h;
Step S7: in stove, temperature is down to after room temperature, takes out square crystal, cuts and be processed into the wafer of desired size.
2. the growth method of square sapphire crystal according to claim 1, is characterized in that:
The oriented seed of selecting in described step S4 be m to or a to.
3. the growth method of square sapphire crystal according to claim 1, is characterized in that:
Described square crucible is square crucible, in step S4, guarantees that oriented seed c face is parallel to crucible plane corresponding to one side arbitrarily.
4. the growth method of square sapphire crystal according to claim 1, is characterized in that:
Described method further comprises, regulates as required the shape of crucible, well heater, in order to regulate the shape of crystal cross section.
5. a growth method for square sapphire crystal, is characterized in that, described method comprises the steps:
Step S1: the high purity aluminium oxide piece material of setting weight or powder are packed in square crucible, then square crucible is placed in crystal growing furnace;
Step S2: crystal growing furnace is evacuated to setting vacuum tightness;
Step S3: heat up by well heater control crystal growing furnace, make alumina raw material be molten into melt;
Step S4: select oriented seed, oriented seed is fixed on to the central position of crucible, the suitable rear seeding of temperature;
Step S5: after seeding finishes, upwards lift seed crystal, start crystal growth;
Step S6: after long crystalline substance finishes, slow cooling;
Step S7: in stove, temperature is down to after design temperature, takes out crystal, cuts and be processed into the wafer of desired size.
6. a growth apparatus for square sapphire crystal, is characterized in that: described equipment includes crystal growing furnace, vacuum extractor, thermal field;
Described thermal field comprises well heater, crucible, crucible cover, heat shielding;
Described well heater is placed in crystal growing furnace, and crucible is placed in the central position of well heater, and crucible cover is placed in crucible top.
7. the growth apparatus of square sapphire crystal according to claim 5, is characterized in that:
Described crucible is square crucible, and the cross section of crucible is rectangular;
Or the cross section of described crucible is the rectangle with fillet, the radius of four fillets is at 1 ~ 20mm.
8. the growth apparatus of square sapphire crystal according to claim 5, is characterized in that:
Described heat shielding mainly comprises heat shielding and outer heat shielding; Upper heat shielding is placed in crucible top, and its shape of cross section is identical with crucible; Outer heat shielding is placed in well heater outside, and it is shaped as circular or square;
Being shaped as of described well heater, crucible cover is circular or square.
9. the growth apparatus of square sapphire crystal according to claim 5, is characterized in that:
Described heater material is tungsten; Described crucible cover and heat-shield material are molybdenum or tungsten or iridium or tantalum, or are two or more elementary composition alloys in molybdenum, tungsten, iridium, tantalum.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104264224A (en) * | 2014-09-19 | 2015-01-07 | 天通控股股份有限公司 | Growth method of large-size square sapphire crystal |
| CN105171940A (en) * | 2015-06-18 | 2015-12-23 | 江苏苏创光学器材有限公司 | Manufacturing method for sapphire frame-free touch screen panel |
| CN105369344A (en) * | 2015-12-15 | 2016-03-02 | 洛阳西格马炉业股份有限公司 | Method and device used for preparing platy monocrystals via temperature field gradient vertical shifting method |
| CN105401213A (en) * | 2015-12-03 | 2016-03-16 | 河南西格马晶体科技有限公司 | Method for preparing large flake-like sapphire single crystals by utilizing crucible rising pulling method |
| CN105420809A (en) * | 2015-12-15 | 2016-03-23 | 河南西格马晶体科技有限公司 | Method and device for preparing platy monocrystal with temperature field vertical gradient moving method |
| CN105463569A (en) * | 2015-12-03 | 2016-04-06 | 河南西格马晶体科技有限公司 | Growth interface temperature measurement and control method for flaky sapphire monocrystals |
| CN109280971A (en) * | 2018-11-08 | 2019-01-29 | 内蒙古恒嘉晶体材料有限公司 | A method of preparing large-size sapphire single-crystal |
| CN111304735A (en) * | 2020-04-14 | 2020-06-19 | 四川省久宝晶体科技有限公司 | Cubic zirconium sapphire growth crystal furnace and cubic zirconium sapphire synthesis method |
| US11155930B2 (en) | 2019-08-21 | 2021-10-26 | Meishan Boya Advanced Materials Co., Ltd. | Open Czochralski furnace for single crystal growth |
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| CN104264224A (en) * | 2014-09-19 | 2015-01-07 | 天通控股股份有限公司 | Growth method of large-size square sapphire crystal |
| CN105171940A (en) * | 2015-06-18 | 2015-12-23 | 江苏苏创光学器材有限公司 | Manufacturing method for sapphire frame-free touch screen panel |
| CN105401213A (en) * | 2015-12-03 | 2016-03-16 | 河南西格马晶体科技有限公司 | Method for preparing large flake-like sapphire single crystals by utilizing crucible rising pulling method |
| CN105463569A (en) * | 2015-12-03 | 2016-04-06 | 河南西格马晶体科技有限公司 | Growth interface temperature measurement and control method for flaky sapphire monocrystals |
| CN105369344A (en) * | 2015-12-15 | 2016-03-02 | 洛阳西格马炉业股份有限公司 | Method and device used for preparing platy monocrystals via temperature field gradient vertical shifting method |
| CN105420809A (en) * | 2015-12-15 | 2016-03-23 | 河南西格马晶体科技有限公司 | Method and device for preparing platy monocrystal with temperature field vertical gradient moving method |
| CN109280971B (en) * | 2018-11-08 | 2021-06-25 | 内蒙古恒嘉晶体材料有限公司 | Method for preparing large-size sapphire single crystal |
| CN109280971A (en) * | 2018-11-08 | 2019-01-29 | 内蒙古恒嘉晶体材料有限公司 | A method of preparing large-size sapphire single-crystal |
| US11155930B2 (en) | 2019-08-21 | 2021-10-26 | Meishan Boya Advanced Materials Co., Ltd. | Open Czochralski furnace for single crystal growth |
| US11198947B2 (en) | 2019-08-21 | 2021-12-14 | Meishan Boya Advanced Materials Co., Ltd. | Open Czochralski furnace for single crystal growth |
| US11566341B2 (en) | 2019-08-21 | 2023-01-31 | Meishan Boya Advanced Materials Co., Ltd. | Open czochralski furnace for single crystal growth |
| US11566342B2 (en) | 2019-08-21 | 2023-01-31 | Meishan Boya Advanced Materials Co., Ltd. | Open Czochralski furnace for single crystal growth |
| US11566343B2 (en) | 2019-08-21 | 2023-01-31 | Meishan Boya Advanced Materials Co., Ltd. | Open Czochralski furnace for single crystal growth |
| US11572634B2 (en) | 2019-08-21 | 2023-02-07 | Meishan Boya Advanced Materials Co., Ltd. | Open Czochralski furnace for single crystal growth |
| US11851783B2 (en) | 2019-08-21 | 2023-12-26 | Meishan Boya Advanced Materials Co., Ltd. | Open Czochralski furnace for single crystal growth |
| US11851782B2 (en) | 2019-08-21 | 2023-12-26 | Meishan Boya Advanced Materials Co., Ltd. | Open Czochralski furnace for single crystal growth |
| US11885037B2 (en) | 2019-08-21 | 2024-01-30 | Meishan Boya Advanced Materials Co., Ltd. | Open Czochralski furnace for single crystal growth |
| CN111304735A (en) * | 2020-04-14 | 2020-06-19 | 四川省久宝晶体科技有限公司 | Cubic zirconium sapphire growth crystal furnace and cubic zirconium sapphire synthesis method |
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Application publication date: 20140521 |