CN105401213A - Method for preparing large flake-like sapphire single crystals by utilizing crucible rising pulling method - Google Patents
Method for preparing large flake-like sapphire single crystals by utilizing crucible rising pulling method Download PDFInfo
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- CN105401213A CN105401213A CN201510876763.7A CN201510876763A CN105401213A CN 105401213 A CN105401213 A CN 105401213A CN 201510876763 A CN201510876763 A CN 201510876763A CN 105401213 A CN105401213 A CN 105401213A
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- crucible
- crystal
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- heating element
- growth
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Classifications
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/20—Controlling or regulating
- C30B15/206—Controlling or regulating the thermal history of growing the ingot
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/10—Crucibles or containers for supporting the melt
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/20—Aluminium oxides
Abstract
The invention relates to a method for preparing large flake-like sapphire single crystals by utilizing a crucible rising pulling method. According to the method, a flat structure crucible with the open upper end is adopted, and a plurality of resistance type heating elements are symmetrically horizontally arranged on the two sides of the crucible. The heating elements surround the crucible to form two temperature regions, namely a crystalline region and a melting region located below the crystalline region. The two temperature regions are heated independently, undergo temperature control independently, and display temperatures on panels independently. By controlling the temperature of the crystalline region, the interface temperature for crystal growth conforms to the optimal temperature range for sapphire crystal growth. The crystal growth interface temperature is controlled accurately by moving the crucible from bottom to top, the large-size flake-like sapphire single crystals can be prepared, and the sapphire single crystals are short in growth cycle, high in rate of finished products and crystal utilization rate and low in production cost. The prepared large flake-like sapphire single crystals can meet the requirements of some large-size special optical windows.
Description
Technical field
The present invention relates to large sheet sapphire single-crystal preparing technical field, specifically a kind of method utilizing crucible rising crystal pulling method to prepare large sheet sapphire monocrystal.
Background technology
Sapphire (α-Al
2o
3single crystal) there is excellent optics, mechanics, calorifics, dielectric, the performance such as corrosion-resistant, at visible and infrared band, there is higher transmittance and wider through band, compared with other optical window materials numerous, there are more stable chemical property and thermomechanical property, as antiacid caustic corrosion, high temperature resistant, high rigidity, high tensile, high heat conductance and significant thermal-shock resistance.Above-mentioned character makes sapphire material be widely used in the aspect such as substrate, femto-second laser substrate material, military infrared window, aerospace medium wave infra-red transmitting window gate material of semiconductor material with wide forbidden band as gan, relates to the numerous areas such as science and technology, national defence and civilian industry.The growth of large-size sapphire single-crystal is the technical bottleneck of the application of sapphire growth always, and the anisotropy sapphire that size is greater than 250 × 300mm can meet the requirement of some large size special optical windows especially.
At present, the method for growing large-size sapphire single-crystal body mainly contains kyropoulos, EFG technique, heat-exchanging method etc., and often kind of growth method all has its relative merits.Kyropoulos is first by raw materials melt, then in being immersed by seed crystal and being contained in suitable crucible melt, when seed crystal micro-molten after, then reduce furnace temperature or the way by cooling seed rod, make melt undercooling near seed crystal, crystal growth began.For making crystal constantly grow up, just need the temperature reducing melt gradually, simultaneously with inapparent crystal lift, to expand radiating surface, this causes the crystal growth in low-temperature gradient crucible.Crystal does not contact with sidewall of crucible in process of growth or at the end of growth, this greatly reduces the stress of crystal, but, when crystal and remaining melt depart from, usually can produce larger thermal shocking.Kyropoulos is that existing market applies maximum sapphire growth methods, main advantage is the advantage of lower cost of crystal growth, weak point is crystal preparation yield rate not high (the highest be about 70-80%), the crystal of growth needs to carry out drawing to cut and could apply, following process difficulty is large, and crystal utilization ratio lower (the highest be about 80%).EFG technique and Edge-Defined Film feed pulling growth technology, first raw material is put into crucible heat fused, then will the mould of slit be had to put into melt, melt rises to die tip under capillary action along mould, die top liquid level connects seed crystal lifting melt, make seed crystal on the interface of melt, constantly carry out rearranging of atom or molecule, solidify gradually with cooling and grow the single crystal identical with die edge shape, the section shape and size of crystal is then by the shape and size at die top edge are determined.Therefore, EFG technique can grow various, rod, pipe, silk and other special shape crystal, there is the ability directly controlling growth amorphous from melt, thus eliminate the cutting of sapphire crystal and the manufacturing procedure such as shaping, decrease material loss, save process period, thus reduce sapphire application cost.Weak point is EFG technique equipment complex structure, and the defect concentration of the large-size sapphire single-crystal body of preparation is higher.Heat-exchanging method utilizes heat exchanger to take away heat, make the longitudinal temperature gradient forming a cold lower part and hot upper part in growth furnace, control warm field by the size controlling gas flow and heating power in heat exchanger, thus realize the growth of crystal, its essence is melt directly solidifying in crucible.Advantage to obtain high-quality large size sapphire crystal, and the defect of crystal and unrelieved stress lower, weak point is a large amount of helium of crystal preparation process need consumption, and cost is higher.
Therefore, prepare large-size sapphire single-crystal body in the urgent need to improving existing crystal growth technique or equipment, or Development of Novel sapphire growth method and apparatus, to reduce the cost preparing large-size sapphire single-crystal body.
Summary of the invention
For in above-mentioned prior art, sapphire crystal utilization ratio is low, energy consumption is high, crystal growth temperature cannot the problem such as the crystal growth that causes of accuracy controlling is slow, of poor quality, the invention provides a kind of method utilizing crucible rising crystal pulling method to prepare large sheet sapphire monocrystal.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A kind of method utilizing crucible rising crystal pulling method to prepare large sheet sapphire monocrystal, present method adopts the flats structure crucible of upper end open, the horizontally disposed multiple resistance-type heating element of zygomorphy of crucible, heating element surrounds crucible and forms two warm areas, i.e. crystallizing field and the melting zone be positioned at below crystallizing field, two warm area independent heatings, independent temperature control, independently displays temperature on panel, the interface temperature of crystal growth is made to meet the optimum temperature range of sapphire crystal growth by the temperature in crystallization control district, the large sheet sapphire monocrystal of vertical junction crystals growth under vacuum, in process of growth, heating element does not move, moved from bottom to top by crucible, remain that the warm field relative position that the interface of crystal growth and heating element are formed is constant,
Described crucible thickness is 10 ~ 200mm, and width is 10 ~ 1000mm, is highly 100 ~ 1000mm;
Described heating element is heating element of tungsten, molybdenum heating element, graphite heater or zirconium diboride composite ceramic heating unit;
The horizontally disposed both sides at crucible of described heating element, arrange that 5 ~ 50 arrange up and down;
Described sapphire single-crystal antibody preparation procedures is: feed-close the door-vacuumize-heat-regulate each warm area temperature-melting sources-inoculation-startup running gear-crystal growth-crystal growth terminate-lower the temperature-open fire door-taking-up crystal, whole crystallisation process, move the auto-control with crystal growth interface by crucible, realize the preparation of crystal.
Beneficial effect of the present invention:
The method utilizing crucible rising crystal pulling method to prepare large sheet sapphire monocrystal provided by the invention, adopt the flats structure crucible of upper shed, heating element is horizontally disposed in crucible both sides, adopt resistance-type heating element that the warm field of different warm area is set, form two warm fields, i.e. crystallizing field and melting zone, two warm field independent heatings, independent temperature control, independently displays temperature on panel, the interface temperature of crystal growth is made to meet the optimum temperature range of sapphire crystal growth by the temperature in crystallization control district, the large sheet sapphire monocrystal of vertical junction crystals growth under vacuum, in process of growth, heating element does not move, moved from bottom to top by crucible, remain that the warm field relative position that the interface of crystal growth and heating element are formed is constant, the present invention accurately controls crystal growth interface temperature by crucible is mobile from bottom to top, large-size flaky sapphire single crystal can be prepared, and the growth cycle of sapphire monocrystal is short, yield rate is high, crystal utilization ratio is high, production cost is low, the large sheet sapphire monocrystal of preparation can meet the requirement of some large size special optical windows.
Accompanying drawing explanation
Fig. 1 crucible schematic shapes of the present invention;
Fig. 2 heating element of the present invention arranges schematic diagram one;
Fig. 3 heating element of the present invention arranges schematic diagram two;
Reference numeral: 1, crucible, 2, heating element.
Embodiment
Below in conjunction with embodiment, the present invention is further elaborated.
As shown in the figure: a kind of method utilizing crucible rising crystal pulling method to prepare large sheet sapphire monocrystal, present method adopts the flats structure crucible of upper end open, the horizontally disposed multiple resistance-type heating element of zygomorphy of crucible, heating element surrounds crucible and forms two warm areas, i.e. crystallizing field and the melting zone be positioned at below crystallizing field, two warm area independent heatings, independent temperature control, independently displays temperature on panel, the interface temperature of crystal growth is made to meet the optimum temperature range of sapphire crystal growth by the temperature in crystallization control district, the large sheet sapphire monocrystal of vertical junction crystals growth under vacuum, in process of growth, heating element does not move, moved from bottom to top by crucible, remain that the warm field relative position that the interface of crystal growth and heating element are formed is constant, .
The present invention adopts the flats structure crucible of upper end open, and crucible thickness is 10 ~ 200mm, and width is 10 ~ 1000mm, is highly 100 ~ 1000mm, adopt resistance-type heating element that the warm field of different warm area is set, heating element can be heating element of tungsten, molybdenum heating element, graphite heater, one in the middle of zirconium diboride composite ceramic heating unit, heating element is horizontally disposed in crucible both sides, arrange that 5 ~ 50 arrange up and down, form two warm fields, i.e. crystallizing field and melting zone, two warm field independent heatings, independent temperature control, independently displays temperature on panel, the interface temperature of crystal growth is made to meet the optimum temperature range of sapphire crystal growth by the temperature in crystallization control district, the large sheet sapphire monocrystal of vertical junction crystals growth under vacuum, in process of growth, heating element does not move, moved from bottom to top by crucible, remain that the warm field relative position that the interface of crystal growth and heating element are formed is constant.Under the slow movement of crucible, crystal constantly grows.Concrete sapphire single-crystal antibody preparation procedures is: feed-close the door-vacuumize-heat-regulate each warm area temperature-melting sources-inoculation-startup running gear-crystal growth-crystal growth terminate-lower the temperature-open fire door-taking-up crystal, whole crystallisation process, move the auto-control with crystal growth interface by crucible, realize the high quality preparation of sapphire monocrystal.
The present invention adopts the flats structure crucible of upper shed, heating element is horizontally disposed in crucible both sides, adopt resistance-type heating element that the warm field of different warm area is set, form two warm fields, i.e. crystallizing field and melting zone, two warm field independent heatings, independent temperature control, independently displays temperature on panel, the interface temperature of crystal growth is made to meet the optimum temperature range of sapphire crystal growth by the temperature in crystallization control district, the large sheet sapphire monocrystal of vertical junction crystals growth under vacuum, in process of growth, heating element does not move, moved from bottom to top by crucible, remain that the warm field relative position that the interface of crystal growth and heating element are formed is constant, the present invention accurately controls crystal growth interface temperature by crucible is mobile from bottom to top, large-size flaky sapphire single crystal can be prepared, and the growth cycle of sapphire monocrystal is short, yield rate is high, crystal utilization ratio is high, production cost is low, the large sheet sapphire monocrystal of preparation can meet the requirement of some large size special optical windows.
Claims (5)
1. the method utilizing crucible rising crystal pulling method to prepare large sheet sapphire monocrystal, it is characterized in that: present method adopts the flats structure crucible of upper end open, the horizontally disposed multiple resistance-type heating element of zygomorphy of crucible, heating element surrounds crucible and forms two warm areas, i.e. crystallizing field and the melting zone be positioned at below crystallizing field, two warm area independent heatings, independent temperature control, independently displays temperature on panel, the interface temperature of crystal growth is made to meet the optimum temperature range of sapphire crystal growth by the temperature in crystallization control district, the large sheet sapphire monocrystal of vertical junction crystals growth under vacuum, in process of growth, heating element does not move, moved from bottom to top by crucible, remain that the warm field relative position that the interface of crystal growth and heating element are formed is constant.
2. utilize crucible rising crystal pulling method to prepare the method for large sheet sapphire monocrystal as claimed in claim 1, it is characterized in that: described crucible thickness is 10 ~ 200mm, width is 10 ~ 1000mm, is highly 100 ~ 1000mm.
3. utilize crucible rising crystal pulling method to prepare the method for large sheet sapphire monocrystal as claimed in claim 1, it is characterized in that: described heating element is heating element of tungsten, molybdenum heating element, graphite heater or zirconium diboride composite ceramic heating unit.
4. utilize crucible rising crystal pulling method to prepare the method for large sheet sapphire monocrystal as claimed in claim 1, it is characterized in that: the horizontally disposed both sides at crucible of described heating element, arrange that 5 ~ 50 arrange up and down.
5. utilize crucible rising crystal pulling method to prepare the method for large sheet sapphire monocrystal as claimed in claim 1, it is characterized in that: described sapphire single-crystal antibody preparation procedures is: feed-close the door-vacuumize-heat-regulate each warm area temperature-melting sources-inoculation-startup running gear-crystal growth-crystal growth terminate-lower the temperature-open fire door-taking-up crystal, whole crystallisation process, move the auto-control with crystal growth interface by crucible, realize the preparation of crystal.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2018023335A1 (en) * | 2016-08-01 | 2018-02-08 | 三和德盛(洛阳)蓝宝石晶体制造有限公司 | Method and apparatus for preparing sapphire crystal by moving temperature-field gradient |
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