CN110093660A - It is a kind of can be with the grower and technique of high-speed rapid growth bubble-free crystalline material - Google Patents
It is a kind of can be with the grower and technique of high-speed rapid growth bubble-free crystalline material Download PDFInfo
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- CN110093660A CN110093660A CN201910415638.4A CN201910415638A CN110093660A CN 110093660 A CN110093660 A CN 110093660A CN 201910415638 A CN201910415638 A CN 201910415638A CN 110093660 A CN110093660 A CN 110093660A
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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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/003—Heating or cooling of the melt or the crystallised material
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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
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/06—Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
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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
- 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
- C30B29/12—Halides
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- Crystallography & Structural Chemistry (AREA)
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Abstract
The invention discloses one kind can be with the grower and technique of high-speed rapid growth bubble-free crystalline material, it is related to the technical field of producing of vacuum coating crystalline material, it is slow to solve rate of crystalline growth, and crystalizing interface is small, unstable, rate of crystalline growth once too fast the defects of will generating a large amount of bubbles comprising bracket and the furnace body on bracket are provided with the annular crucible for containing raw material in furnace body, it is provided with lid on annular crucible, and is provided with heater and insulating layer in furnace body；Through-hole is formd at the center of annular crucible, and is provided with heat-exchange tube in through-hole, and is provided with temperature measuring equipment on furnace body, and heat-exchange tube side is provided with the supporting plate abutted with annular crucible bottom.The novelty of the invention patent is that crucible is annular, centre be it is empty, can accommodate heat-exchange tube, by increasing cooling medium offer crystallization driving force in heat-exchange tube when growing crystal, can high-speed rapid growth be substantially free of the crystalline material of bubble.
Description
Technical field
The present invention relates to the technical field of producing of vacuum coating crystalline material, more specifically, it relates to which one kind can
With the grower and technique of high-speed rapid growth bubble-free crystalline material.
Background technique
Vacuum coating crystalline material especially electron level vacuum coating crystalline material requires purity is high, and air entrapment is few, with
Guarantee that vacuum is stablized during vacuum coating, permeation does not collapse a little, guarantees good coating effects and plating membrane efficiency.
Vacuum coating crystalline material is quickly cooled down after mainly using high-temperature vacuum to melt at present, and crucible is in crystal growth
When position it is constant, growth can only be controlled by power/temperature, temperature gradient very little on heterogeneity phantom, temperature is excessively high
It does not crystallize, rapid crystallization is unable to control when temperature is slightly lower, and internal single crystal grain is smaller, and crystallization direction is on the whole from export-oriented
It is interior, cause material internal to be easy to be mingled with a large amount of bubble and various crucible pollutants etc., purity is by larger impact, in coating process
In be easy to produce deflation, collapse a little, dodge phenomena such as quick-fried, largely effect on coating quality, the especially plated film in high requests such as electron levels
Upper using effect is bad.
Bulk single crystal material is highly suitable as high-end plated film due to directional solidification and impurities removal effect, bubble-free with high purity
Material, but since growth cycle is long, price is very expensive, production capacity is small, and market can not receive.
Summary of the invention
It is slow for rate of crystalline growth in the prior art, and crystalizing interface is small, unstable, rate of crystalline growth is once too fast
The defects of a large amount of bubbles will be generated, the purpose of the present invention one are that providing one kind can be given birth to high-speed rapid growth bubble-free crystalline material
Growth device, by dramatically increasing heat exchange contact area, to solve above-mentioned skill by the way that heat exchange is arranged at annular crucible center
Art problem, which give very big interface gradients and interface stability, can high-speed rapid growth bubble-free polycrystalline material.
To achieve the above object one, the present invention provides the following technical scheme that
One kind can be with high-speed rapid growth bubble-free crystal material growth device, and furnace body including bracket and on bracket is described
It is provided with the annular crucible for containing raw material in furnace body, lid is provided on annular crucible, and is provided with and is used in furnace body
To the heater that crucible is heated, and play the insulating layer of insulation effect；Through-hole is formd at the center of annular crucible, and is led to
It is provided with heat-exchange tube in hole, and is provided with temperature measuring equipment on furnace body, heat-exchange tube side is provided with to be supported with annular crucible bottom
The supporting plate connect.
By using above-mentioned technical proposal, heat-exchange tube is set at annular crucible center, is formed inside melt outer high
Interior temperature gradient low, upper relative superiority or inferiority is low allows melt to carry out controllable unidirectional solidification life with biggish interface fltting speed
It is long, can be with the polycrystalline material of high-speed rapid growth bubble-free, while air entrapment and various pollutants are arranged by the way that interface is unidirectionally mobile
Except crystalline material outer edge is arrived, crystalline material is with high purity, simultaneously because growth interface dramatically increases, so that the volume solidification of melt
Speed is also very big, and production efficiency increases considerably.Using device bulk single crystal material produced due to directional solidification and row
Miscellaneous effect, bubble-free with high purity are highly suitable as high-end Coating Materials, and the period is short, and production capacity is big, and market applicability is good, especially
Its demand for being applied to electron level high-end market.
Further preferably, the heat-exchange tube is in contact with the lateral wall that crucible is located at through hole, and contact area can
To be up to 50-500cm2。
By using above-mentioned technical proposal, in existing heat exchange Hem method, at the top of heat-exchange tube and cylindrical type crucible bottom
Portion is in contact, contact area (generally 10-15cm2) very little, causes the cooling capacity provided limited, rate of crystalline growth 1-
5mm/hr or so.And in the present invention, contact area can be up to 50-500cm2, it is capable of providing very strong cooling capacity, is formed non-
Often big temperature gradient, can make rate of crystalline growth be increased to 15-30mm/hr, can high-speed rapid growth be substantially free of the more of bubble
Crystalline material.
Further preferably, the heat-exchange tube includes inner tube and the outer tube for being set in inner tube side, the top envelope of outer tube
It closes, the top of inner tube is connected to the inside of outer tube.
By using above-mentioned technical proposal, cooling medium enters outer tube after rising to top from inner tube, and liquid can be from outer tube
Entering inner tube after rising to top, outer tube exchanges heat with crucible, thus increase the heat exchange area of cooling medium and crucible, and
Heat exchange uniformly, keeps crystalizing interface big and stablizes, and is conducive to improve crystal production efficiency.
The purpose of the present invention two is to provide one kind can be with high-speed rapid growth bubble-free crystal material growth technique, using the work
The crystalline material purity is high bubble-free of skill preparation, and high production efficiency.
To achieve the above object two, the present invention provides following technical solutions, the specific steps are as follows:
Raw material is packed into the cavity of crucible, covers lid by step 1, and heater starts to generate heat, and it is super to temperature to heat raw material
Fusing point is crossed, raw material all melts, high temperature clarification, firm power a few hours, and cooling medium consumption maintains initially in heat-exchange tube
Flow, the initial flow is substantially for 0.2-0.5L/min；
Step 2 starts to step up cooling medium consumption and is passed through speed, and the flow of cooling medium is within a certain period of time from initial
Flow gradually rises to flow needed for long crystalline substance, and the rate that cooling medium consumption rises is 0.5-23 (L/min)/h, a timing
Between depend on crucible size, generally at 10-30 hour or so, it is described it is long brilliant needed for flow depending on crystalline material type and charging
Amount, in 150-250L/min；
Step 3 keeps cooling medium consumption constant, finishes to crystal growth, it is synchronous reduce cooling medium consumption be passed through speed and
Power takes out crystal after cooling to 0.
By using above-mentioned technical proposal, cooling medium is passed through in heat-exchange tube, meanwhile, the control of cooling medium consumption size
System, forms the low temperature gradient of high outside and low outside, upper relative superiority or inferiority inside melt, allows melt with biggish interface fltting speed
Controllable unidirectional solidification growth is carried out, melt gradually from the upwardly-directed solidification outward of crucible center and bottom, can obtain big
Unidirectionally movement is rejected to material outer edges edge by interface for the monocrystal of grain, air entrapment and various pollutants, and material internal is without gas
Bubble, purity is high；Simultaneously because growth interface dramatically increases, so that the volume solidification speed of melt is also very big, production efficiency is improved
50% or more, there is good production application effect.
Further preferably, the raw material is crystal of fluoride material powder, and the raw material is calcirm-fluoride, magnesium fluoride, fluorination
Any one in barium, lithium fluoride, sodium fluoride etc..
By using above-mentioned technical proposal, magnesium fluoride, barium fluoride, lithium fluoride, sodium fluoride belong to halide single crystals, fluoride
Monocrystalline has higher transmitance, low-refraction and low luminous reflectivity, and chemistry in ultraviolet, visible and infrared band spectral regions
Stability is good.
Further preferably, the rate that raw material heats up in the step 1 is 50-100 DEG C/h.
Further preferably, the temperature that raw material is heated to its fusing point or more in the step 2 is 50-200 DEG C.
By using above-mentioned technical proposal, guarantee that raw material sufficiently melts, is conducive to the monocrystal that the later period forms purity is high.
Further preferably, the cooling medium is inert gas, mainly helium, argon gas or nitrogen.
By using above-mentioned technical proposal, using inert gas, when being heated at high temperature, cooling stick will not be caused to invade
Erosion, is improved the cooling service life of cooling tube, guarantees cooling effect.
In conclusion compared with prior art, the invention has the following advantages:
(1) heat-exchange tube is arranged by crucible center, forms very big, the low temperature ladder of high outside and low outside upper relative superiority or inferiority inside melt
Degree allows melt to carry out controllable unidirectional solidification growth with biggish interface fltting speed, can be with high-speed rapid growth bubble-free
Polycrystalline material, be conducive to improve production efficiency；
(2) simultaneously, in process of production, unidirectionally movement is rejected to by interface for the air entrapment of annular crucible and various pollutants
Material outer edges edge, the high bubble-free of material purity, the crystal made quality with higher.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of crystal material growth device in the present invention；
Appended drawing reference: 1, bracket；2, furnace body；3, movable span；4, crucible；5, heater；6, insulating layer；7, lid；8, heat exchange
Pipe；81, the air inlet inner tube；82, outlet outer tube；9, supporting plate；10, heat insulating block；11, through-hole；12, temperature measuring equipment.
Specific embodiment
With reference to the accompanying drawings and examples, the present invention will be described in detail.
Embodiment 1: as shown in Figure 1, one kind can be with high-speed rapid growth bubble-free crystal material growth device, the branch of rectangular frame-shaped
Frame 1 and the furnace body 2 on bracket 1, furnace body 2 are rectangular-shape, and 2 bottom of furnace body offers rectangular movable span 3, furnace body
Cylindrical annular crucible 4 is set in 2, is provided with the lid 7 to match on annular crucible 4.It is provided with and is used in furnace body 2
To the heater 5 that crucible 4 is heated, and the insulating layer 6 of insulation effect is played, heater 5 includes four Si-Mo rods, four silicon
Molybdenum bar runs through 2 side wall of furnace body and is located at the two sides of annular crucible 4, and the material selection asbestos in insulating layer 6.Meanwhile furnace
Temperature measuring equipment 12 is provided in body 2, temperature measuring equipment 12 can be selected as laser infrared temperature sensor.
Through-hole 11 is formd at the center of annular crucible 4, and is provided with heat-exchange tube 8 in through-hole 11, and heat-exchange tube 8 includes
Inner tube 81 and the outer tube 82 for being set in 81 side of inner tube, the top closure of outer tube 82, the top of inner tube 81 and the inside of outer tube 82
Connection.Heat-exchange tube 8 is in contact with the lateral wall that crucible 4 is located at through-hole 11, according to the difference of production scale and instrument size,
Its contact area can be up to 50-500cm2。
8 side of heat-exchange tube is provided with the supporting plate 9 abutted with 4 bottom of annular crucible, supporting plate 9 far from annular crucible 4 one
Side is provided with the heat insulating block 10 being mutually clamped with air-tight movable hole 3, and heat insulating block 10 is fixed on the side wall of heat-exchange tube 8, and
Heat insulating block 10 and insulating layer 6 select thermal insulation material of the same race.
Heat-exchange tube 8 is set at 4 center of annular crucible, forms the low temperature of high outside and low outside, upper relative superiority or inferiority inside melt
Gradient allows melt to carry out controllable unidirectional solidification growth with biggish interface fltting speed, can be with high-speed rapid growth without gas
The polycrystalline material of bubble.Meanwhile using device bulk single crystal material produced due to directional solidification and impurities removal effect, purity
High bubble-free is highly suitable as high-end Coating Materials, and the period is short, and production capacity is big, and market applicability is good, is applied especially to electronics
The demand of grade high-end market.
In work, raw material is packed into the cavity of crucible 4, covers lid 7, heater 5 starts to generate heat, and heats raw material and arrive
Temperature be more than fusing point, raw material all melt, high temperature clarification, then in heat-exchange tube 8 cooling medium consumption from initial flow gradually
Increase, and gradually rise to flow needed for long crystalline substance, then keeps cooling medium consumption constant, finished to crystal growth, it is synchronous to reduce
Cooling medium consumption is passed through speed and power to 0, takes out crystal after cooling.
Embodiment 2: one kind can be specifically comprised the following steps: with high-speed rapid growth bubble-free crystal material growth technique
Magnesium fluoride powder is packed into the cavity of crucible, covers lid, heater starts to generate heat, and heats raw material and arrive by step 1
Temperature is more than fusing point, and raw material all melts, and the rate of raw material heating is 75 DEG C/h, and temperature is 50 DEG C, high temperature clarification, firm power
2h, helium gas flow maintains initial flow in heat-exchange tube, and the initial flow is substantially for 0.2L/min；
Step 2, beginning are stepped up helium gas flow and are passed through speed, the flow of helium within a certain period of time from initial flow gradually on
Flow needed for rising to long crystalline substance, the rate that helium gas flow rises is 0.5 (L/min)/h, generally at 10 hours, the long brilliant required stream
Amount is 150L/min；
Step 3 keeps helium gas flow constant, finishes to crystal growth, and the synchronous helium gas flow that reduces is passed through speed and power to 0,
Crystal is taken out after cooling.
Embodiment 3: one kind can be specifically comprised the following steps: with high-speed rapid growth bubble-free crystal material growth technique
Lithium fluoride powder is packed into the cavity of crucible, covers lid, heater starts to generate heat, and heats raw material and arrive by step 1
Temperature is more than fusing point, and raw material all melts, and the rate of raw material heating is 75 DEG C/h, and temperature is 200 DEG C, high temperature clarification, constant function
Rate 5h, helium gas flow maintains initial flow in heat-exchange tube, and the initial flow is substantially for 0.5L/min；
Step 2, beginning are stepped up helium gas flow and are passed through speed, the flow of helium within a certain period of time from initial flow gradually on
Flow needed for rising to long crystalline substance, the rate that helium gas flow rises is 23 (L/min)/h, generally at 30 hours, the long brilliant required stream
Amount is 250L/min；
Step 3 keeps helium gas flow constant, finishes to crystal growth, and the synchronous helium gas flow that reduces is passed through speed and power to 0,
Crystal is taken out after cooling.
Embodiment 4: one kind can be specifically comprised the following steps: with high-speed rapid growth bubble-free crystal material growth technique
Sodium fluoride powder is packed into the cavity of crucible, covers lid, heater starts to generate heat, and heats raw material and arrive by step 1
Temperature is more than fusing point, and raw material all melts, and the rate of raw material heating is 75 DEG C/h, and temperature is 125 DEG C, high temperature clarification, constant function
Rate 3.5h, helium gas flow maintains initial flow in heat-exchange tube, and the initial flow is substantially for 0.35L/min；
Step 2, beginning are stepped up helium gas flow and are passed through speed, the flow of helium within a certain period of time from initial flow gradually on
Flow needed for rising to long crystalline substance, the rate that helium gas flow rises is 11.75 (L/min)/h, generally at 20 hours, needed for the length is brilliant
Flow is 200L/min；
Step 3 keeps helium gas flow constant, finishes to crystal growth, and the synchronous helium gas flow that reduces is passed through speed and power to 0,
Crystal is taken out after cooling.
Embodiment 5: one kind can be specifically comprised the following steps: with high-speed rapid growth bubble-free crystal material growth technique
Barium fluoride powder is packed into the cavity of crucible, covers lid, heater starts to generate heat, and heats raw material and arrive by step 1
Temperature is more than fusing point, and raw material all melts, and the rate of raw material heating is 75 DEG C/h, and temperature is 120 DEG C, high temperature clarification, constant function
Rate 3h, helium gas flow maintains initial flow in heat-exchange tube, and the initial flow is substantially for 0.2L/min；
Step 2, beginning are stepped up helium gas flow and are passed through speed, the flow of helium within a certain period of time from initial flow gradually on
Flow needed for rising to long crystalline substance, the rate that helium gas flow rises is 10 (L/min)/h, generally at 15 hours, the long brilliant required stream
Amount is 190L/min；
Step 3 keeps helium gas flow constant, finishes to crystal growth, and the synchronous helium gas flow that reduces is passed through speed and power to 0,
Crystal is taken out after cooling.
Embodiment 6: one kind can be existed with high-speed rapid growth bubble-free crystal material growth technique with the difference of embodiment 1
In specifically comprising the following steps:
Magnesium fluoride powder is packed into the cavity of crucible, covers lid, heater starts to generate heat, and heats raw material and arrive by step 1
Temperature is more than fusing point, and raw material all melts, and the rate of raw material heating is 75 DEG C/h, and temperature is 160 DEG C, high temperature clarification, constant function
Rate 3.5h, argon flow maintains initial flow in heat-exchange tube, and the initial flow is substantially for 0.4L/min；
Step 2, beginning are stepped up argon flow and are passed through speed, the flow of argon gas within a certain period of time from initial flow gradually on
Flow needed for rising to long crystalline substance, the rate that argon flow rises is 10 (L/min)/h, generally at 22 hours, the long brilliant required stream
Amount is 210L/min；
Step 3 keeps argon flow constant, finishes to crystal growth, and the synchronous argon flow that reduces is passed through speed and power to 0,
Crystal is taken out after cooling.
Embodiment 7: one kind can be existed with high-speed rapid growth bubble-free crystal material growth technique with the difference of embodiment 1
In specifically comprising the following steps:
Magnesium fluoride powder is packed into the cavity of crucible, covers lid, heater starts to generate heat, and heats raw material and arrive by step 1
Temperature is more than fusing point, and raw material all melts, and the rate of raw material heating is 75 DEG C/h, and temperature is 180 DEG C, high temperature clarification, constant function
Rate 4h, nitrogen flow maintains initial flow in heat-exchange tube, and the initial flow is substantially for 0.4L/min；
Step 2, beginning are stepped up nitrogen flow and are passed through speed, the flow of nitrogen within a certain period of time from initial flow gradually on
Flow needed for rising to long crystalline substance, rate 19 (L/min)/h that nitrogen flow rises, generally at 24 hours, flow needed for the long crystalline substance
For 210L/min；
Step 3 keeps nitrogen flow constant, finishes to crystal growth, and the synchronous nitrogen flow that reduces is passed through speed and power to 0,
Crystal is taken out after cooling.
Embodiment 8: one kind can be existed with high-speed rapid growth bubble-free crystal material growth technique with the difference of embodiment 1
In specifically comprising the following steps:
Magnesium fluoride powder is packed into the cavity of crucible, covers lid, heater starts to generate heat, and heats raw material and arrive by step 1
Temperature is more than fusing point, and raw material all melts, and the rate of raw material heating is 50 DEG C/h, and temperature is 90 DEG C, high temperature clarification, firm power
1.8h, helium gas flow maintains initial flow in heat-exchange tube, and the initial flow is substantially for 0.3L/min；
Step 2, beginning are stepped up helium gas flow and are passed through speed, the flow of helium within a certain period of time from initial flow gradually on
Flow needed for rising to long crystalline substance, the rate that helium gas flow rises is 3.6 (L/min)/h, generally at 20 hours, the long brilliant required stream
Amount is 160L/min；
Step 3 keeps helium gas flow constant, finishes to crystal growth, and the synchronous helium gas flow that reduces is passed through speed and power to 0,
Crystal is taken out after cooling.
Embodiment 9: one kind can be existed with high-speed rapid growth bubble-free crystal material growth technique with the difference of embodiment 1
In specifically comprising the following steps:
Magnesium fluoride powder is packed into the cavity of crucible, covers lid, heater starts to generate heat, and heats raw material and arrive by step 1
Temperature is more than fusing point, and raw material all melts, and the rate of raw material heating is 100 DEG C/h, and temperature is 120 DEG C, high temperature clarification, constant function
Rate 4h, helium gas flow maintains initial flow in heat-exchange tube, and the initial flow is substantially for 0.3L/min；
Step 2, beginning are stepped up helium gas flow and are passed through speed, the flow of helium within a certain period of time from initial flow gradually on
Flow needed for rising to long crystalline substance, the rate that helium gas flow rises is 20 (L/min)/h, generally at 25 hours, the long brilliant required stream
Amount is 180L/min；
Step 3 keeps helium gas flow constant, finishes to crystal growth, and the synchronous helium gas flow that reduces is passed through speed and power to 0,
Crystal is taken out after cooling.
Comparative example 1: heat exchange crystal disclosed in the Chinese invention patent that application publication number is CN105369349A is selected
Embodiment one in growing system, cooling gas flow control methods and device.
Comparative example 2: heat exchange crystal disclosed in the Chinese invention patent that application publication number is CN105369349A is selected
Embodiment two in growing system, cooling gas flow control methods and device.
Comparative example 3: heat exchange crystal disclosed in the Chinese invention patent that application publication number is CN105369349A is selected
Embodiment three in growing system, cooling gas flow control methods and device.
Comparative example 4: heat exchange crystal disclosed in the Chinese invention patent that application publication number is CN105369349A is selected
Example IV in growing system, cooling gas flow control methods and device.
Comparative example 5: heat exchange crystal disclosed in the Chinese invention patent that application publication number is CN105369349A is selected
Embodiment five in growing system, cooling gas flow control methods and device.
Experimental test
Test method: recording the time required for the crystalline material of embodiment 2-9 and comparative example 1-5 production phase homogenous quantities respectively,
And the crystalline material of embodiment 2-9 and comparative example 1-5 production is splitted, whether there are bubble or impurity with amplification sem observation section.
Test result: the experimental test result of embodiment 2-9 and comparative example 1-5 are as shown in table 1.As shown in Table 1, by table 1
It is found that the time required for the crystalline material of embodiment 2-9 production phase homogenous quantities is much smaller than comparative example 1-5, production efficiency is improved
50% or more, and the crystalline material leaving no air bubbles inside and impurity produced, improve the purity of crystalline material.
The experimental test of table 1 embodiment 2-9 and comparative example 1-5
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-described embodiment,
All technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It should be pointed out that for the art
For those of ordinary skill, several improvements and modifications without departing from the principles of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (8)
1. one kind can be with high-speed rapid growth bubble-free crystal material growth device, including bracket (1) and the furnace being located on bracket (1)
Body (2), which is characterized in that the annular crucible (4) for containing raw material is provided in the furnace body (2), annular crucible is set on (4)
The heater (5) for being equipped with lid (7), and being provided in furnace body (2) and being used to be heated to crucible (4), and play heat preservation and make
Insulating layer (6)；Through-hole (11) are formd at the center of annular crucible (4), and are provided with heat-exchange tube in through-hole (11)
(8), it and on furnace body (2) is provided with temperature measuring equipment (12), heat-exchange tube (8) side is provided with to abut with annular crucible (4) bottom
Supporting plate (9).
2. according to claim 1 can be with high-speed rapid growth bubble-free crystal material growth device, which is characterized in that the heat
Exchange pipe (8) is in contact with the lateral wall that crucible (4) is located at through-hole (11), and contact area can be up to 50-500cm2.
3. according to claim 1 can be with high-speed rapid growth bubble-free crystal material growth device, which is characterized in that the heat
Exchange pipe (8) includes inner tube (81) and the outer tube (82) for being set in inner tube (81) side, the top closure of outer tube (82), inner tube
(81) top is connected to the inside of outer tube (82).
4. one kind can be with high-speed rapid growth bubble-free crystal material growth technique, which is characterized in that appoint using in claims 1 to 33
It can be with high-speed rapid growth bubble-free crystal material growth device described in meaning one, the specific steps are as follows:
Raw material is packed into the cavity of crucible, covers lid by step 1, and heater starts to generate heat, and it is super to temperature to heat raw material
Fusing point is crossed, raw material all melts, high temperature clarification, firm power a few hours, and cooling medium consumption maintains initially in heat-exchange tube
Flow, the initial flow is substantially for 0.2-0.5L/min；
Step 2 starts to step up cooling medium consumption and is passed through speed, and the flow of cooling medium is within a certain period of time from initial
Flow gradually rises to flow needed for long crystalline substance, and the rate that cooling medium consumption rises is 0.5-23(L/min)/h, it is described certain
Time depends on crucible size, and generally at 10-30 hours or so, flow needed for the long crystalline substance depends on crystalline material type and dress
Doses, in 150-250L/min；
Step 3 keeps cooling medium consumption constant, finishes to crystal growth, it is synchronous reduce cooling medium consumption be passed through speed and
Power takes out crystal after cooling to 0.
5. according to claim 4 can be with high-speed rapid growth bubble-free crystal material growth technique, which is characterized in that the original
Material is crystal of fluoride material powder, and the raw material is calcirm-fluoride, any one in magnesium fluoride, barium fluoride, lithium fluoride, sodium fluoride etc.
Kind.
6. according to claim 4 can be with high-speed rapid growth bubble-free crystal material growth technique, which is characterized in that the step
The rate that raw material heats up in rapid one is 50-200 DEG C/h.
7. according to claim 4 can be with high-speed rapid growth bubble-free crystal material growth technique, which is characterized in that the step
It is 50-200 DEG C that raw material, which is heated to the temperature of its fusing point or more, in rapid two.
8. according to claim 4 can be with high-speed rapid growth bubble-free crystal material growth technique, which is characterized in that described cold
But medium is inert gas, mainly helium, argon gas or nitrogen.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910415638.4A CN110093660B (en) | 2019-05-18 | 2019-05-18 | Growth device and process capable of growing bubble-free crystal material at high speed |
Applications Claiming Priority (1)
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| CN114086240A (en) * | 2021-11-09 | 2022-02-25 | 北京华卓精科科技股份有限公司 | Annular crucible, and crystal transverse directional growth device and method |
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