CN209456611U - The trans- injection of one kind synthesizes continuous VGF crystal growing crucible and device - Google Patents
The trans- injection of one kind synthesizes continuous VGF crystal growing crucible and device Download PDFInfo
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- CN209456611U CN209456611U CN201822102284.1U CN201822102284U CN209456611U CN 209456611 U CN209456611 U CN 209456611U CN 201822102284 U CN201822102284 U CN 201822102284U CN 209456611 U CN209456611 U CN 209456611U
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Abstract
The trans- injection of one kind synthesizes continuous VGF crystal growing crucible and device, is related to the device of semiconductor crystal preparation and crystal growth, and in particular to a kind of continuous VGF method of trans- injection synthesis carries out crystal growing apparatus.Device includes furnace body, is mounted on the intracorporal crucible of furnace, heat-insulation system, heating system, temperature control system and pressure regulation system, the crucible top is combining unit, lower part is crystal growth portion and seed crystal portion, is connected between combining unit and crystal growth portion by pore.It using pore, is controlled by temperature and pressure, in the materials synthesis stage, phosphorus bubble rises to indium melt, and two kinds of substances can be made sufficiently to merge, and after the completion of phosphorus gasification, indium phosphorus melt instills growing part, completes the growth in situ of crystal.
Description
Technical field
The utility model relates to the devices of semiconductor crystal preparation and crystal growth, and in particular to a kind of trans- injection synthesis
Continuous VGF method carries out crystal growing apparatus, is particularly suitable for what the needs such as indium phosphide, gallium phosphide were synthesized with volatile element
The VGF crystal growth of semiconductor crystalline material.
Background technique
Compound semiconductor, such as indium phosphide, gallium phosphide, GaAs, gallium nitride and silicon carbide etc., are widely used in military affairs
And photoelectron and microelectronic field involved in civil field, wherein indium phosphide, gallium phosphide, the compounds such as GaAs need melt
Method is grown, these semiconductor materials or first to be carried out synthesizing and is then carried out crystal growth again, or directly synthesis company
Continuous crystal growth.Material due to directly synthesizing continuous growing method has the characteristics of characteristic of purity is high, save the cost,
Therefore it is increasingly subject to the attention of people.
Vertical temperature gradient technology (VGF) is one of the preferred method for preparing low defect crystal.Therefore directly synthesis is continuous
The exploitation of VGF crystal technique is extremely important.This lays a good foundation to prepare high-purity low defect single crystalline substrate.
Current technology, such as Chinese patent " the VGF pressure furnace that a kind of compound in situ synthesizes continuous crystal growth " (application
Number 201610135278.9), (application number that " carrying gas utilized to carry out phosphide injection synthetic method in situ "
201711298581.1) it is all utilized in the gasification that the upper surface of raw material (such as indium) position carries out phosphorus, then infuses the phosphorus after gasification
Enter into melt；When crystal growth, need that indium phosphide polycrystal material is added to protect seed crystal in advance, prevent it by indium melt attack or
Person's fusing.
Summary of the invention
The purpose of the utility model is to provide one kind to efficiently synthesize the semiconductor materials such as indium phosphide, gallium phosphide, and in situ
Carry out the device of crystal growth.
In order to achieve the above purposes, the technical solution adopted by the utility model is:
A kind of continuous VGF crystal growing crucible of trans- injection synthesis, the seed crystal including combining unit, crystal growth portion and bottom end
Portion, the top in crystal growth portion is arranged in the combining unit, and is connected to by intermediate pore with crystal growth portion；The seed crystal
Portion is below crystal growth portion, and the two is connected to.
Further, the quantity of the pore is more than one, and the radius of pore is 0.1mm-0.15mm.
A kind of continuous VGF crystal growing apparatus of trans- injection synthesis, including furnace body, it is mounted on the intracorporal crucible of furnace, heat preservation
System, heating system, temperature control system and pressure regulation system, key are: the crucible is that trans- injection synthesis is continuous
VGF crystal growing crucible.
In the present invention, growing part is there are two function, and 1, the materials synthesis stage places volatile material such as red phosphorus and heats makes
Gasification, 2, carry out crystal growth after materials synthesis.Pore there are two function, 1, the substance of gasification enter synthesis from growing part
Portion, 2, melt from growing part enter combining unit.
By taking indium phosphide as an example, after red phosphorus gasification, combining unit is entered from bottom by pore, is filled in combining unit and liquid indium
Divide fusion.After the completion of fusion, indium phosphorus melt drop instills crystal growth portion from combining unit by pore, in the process, leads to
Seed crystal is protected in excess temperature control and boron oxide fluid-tight, and it is raw then to carry out crystal by the gradient distribution of temperature in control growing part
It is long.
In material synthesis processes, there is the power of several interactions:σ, the interfacial tension of melt,P1, crystal growth portion
Pressure (saturated vapor pressure of phosphorus),P2, the pressure of combining unit,P3, the pressure that indium melt height generates,ΔP, interfacial tension generation
Additonal pressure.
What crystal growth portion generated upwards pressureP 1 , i.e. the saturated vapor pressure (atm) of red phosphorus:
At 590 DEG C, the saturated vapor pressure of red phosphorus is 4.3MPa, and at 650 DEG C, the saturated vapor pressure of red phosphorus is 12.4MPa.
The downward pressure that bubble generates, the i.e. interfacial tension of indium meltσ:σ=559.7 - 0.089(T - 429)
When T=1335K,σ=479.066mN/m2, the density of indium meltρ=6409.7Kg/m3。
When being synthesized, the downward additonal pressure Δ of interfacial tension generationPAre as follows:
Wherein,rFor capillary radius,r=0.1mm。
It can be obtained based on above-mentioned data, Δ when 1335KP=980Pa=0.0092MPa。
The pressure that 100mm melt itself generates isP 3 =ρgh=6281.5Pa=0.0062815MPa.The height of indium melt is
Indium melt is convenience of calculation, the height of combining unit can be taken to replace in the height of combining unit.
The pressure of combining unitP2It is mainly generated by the air pressure of inert gas, the lower limit value of the pressure is greater than the saturated vapor of phosphorus
Pressure, hereP2=4.0MPa。
Downward pressure=ΔP+P 3 +P 2 =0.0098+0.0062815+4.0=4.0154815MPa。
Downward pressure < < red phosphorus saturated vapor pressure, red phosphorus bubble can rise to composite part, and indium liquid will not flow
Arrive growing part down.
In crucible, the height of general indium melt is in 40-50mm.
The present invention can achieve it is following the utility model has the advantages that
1, it using pore, is controlled by temperature and pressure, different objects can be effectively isolated in equipment preliminary work
Matter, in the materials synthesis stage, phosphorus bubble rises to indium melt, and after the completion of phosphorus gasification, indium phosphorus melt instills growing part, completes crystal
Growth in situ.2, phosphorus gas rises to always top from the bottom of indium melt, and two kinds of substances can be made sufficiently to merge.3, indium phosphorus
Melt instills growing part, by realizing that the boron oxide placed reduces temperature, protects seed crystal.
Detailed description of the invention
Fig. 1 is the crucible schematic diagram of the utility model；
Fig. 2 is that trans- injection synthesizes continuous VGF crystal growing apparatus furnace body installation diagram.
In figure, 8: melt synthesizes thermocouple；9: crystal growth portion thermocouple；10: crucible；10-1: combining unit；10-2: pore；
10-3: crystal growth portion；10-4: seed crystal portion；11: charge and discharge feed channel；12: insulating layer: 13: solid synthesizes covering boron oxide；
14: high purity indium；15: thermal insulation layer；16: boron oxide is used in solid seed crystal protection；17: high-purity red phosphorus；18: seed crystal；19: observation window；28
Heater strip.
Specific embodiment
The present invention will be further described with reference to the accompanying drawing.
In the present embodiment, the crystal of growth is indium phosphide.
The continuous VGF crystal growing crucible of a kind of trans- injection synthesis, as shown in Figure 1, combining unit is respectively set from up to down
10-1, pore 10-2, crystal growth portion 10-3 and the seed crystal portion of bottom end 10-4, combining unit 10-1 are with crystal growth portion 10-3's
It is connected to by pore 10-2；Seed crystal portion 10-4 is connected to crystal growth portion 10-3.
Pore is at least arranged one, be theoretically arranged it is The more the better, in the present embodiment, be arranged 10.
After high purity indium fusing, under hot conditions, the height value of indium melthWith the radius of porerRelationship:。
ρFor the density of melt, in the present embodiment,ρFor the density of indium melt；gFor acceleration of gravity,σFor the interface of melt
Tension, in the present embodiment,σFor the interfacial tension of indium melt,hFor the height of indium melt, including indium melt combining unit height
With the height flowed into pore.Due to the high speed of the super only combining unit 10-1 of the height of melt, in the present embodiment,hFor synthesis
The height of portion 10-1.
In the present embodiment, the radius of pore 10-2 is 0.1mm-0.15mm.
A kind of trans- injection synthesizes continuous VGF crystal growing apparatus, as shown in Fig. 2, including furnace body, to be mounted on furnace intracorporal
Crucible 10, heat-insulation system, heating system, temperature control system and pressure regulation system, the crucible are that trans- injection synthesis connects
Continuous VGF crystal growing crucible.
Thermal insulation layer 15 is set between crucible combining unit 10-1 and crystal growth portion 10-3.
Observation window 19 is equipped at the top of furnace body.
Insulating layer 12 constitutes heat-insulation system.
Heat-insulation system and heating system include the heater strip 28 that 10 periphery of crucible is arranged in.
Temperature control system includes thermocouple 8 and 9.
Pressure regulation system includes the charge and discharge feed channel 11 probeed into crucible 10.
Based on the above equipment, the synthesis of material and the growth of crystal are completed.
Feed intake first: into furnace body, the seed crystal portion 10-4 of crucible 10 is packed into solid seed crystal 18, crystal growth portion 10-3
Red phosphorus 17 and boron oxide 16 are put into, combining unit 10-1 puts into indium 14 and boron oxide 13.Boron oxide 16 in crystal growth portion 10-3
It shields after liquefaction, the boron oxide 13 in combining unit 10-1 plays covering after liquefying.
Then it carries out materials synthesis: by the temperature and pressure in control furnace, so that red phosphorus 17 is distilled, pass through pore, 10-
2 enter growing part 10-1, sufficiently react and are absorbed with indium melt, until red phosphorus all volatilizees.
Carry out crystal growth after the completion of materials synthesis: indium phosphorus melt drop by pore 10-2, from combining unit 10-1 into
Enter crystal growth portion 10-3, the boron oxide after liquefaction protects seed crystal not melted by indium phosphorus melt drips, in crystal growth
Temperature gradient from top to down is set up in portion 10-3, is then controlled Temperature Distribution and is carried out VGF crystal growth.
Claims (8)
1. a kind of continuous VGF crystal growing crucible of trans- injection synthesis, including combining unit (10-1), crystal growth portion (10-3) and
The seed crystal portion (10-4) of bottom end, which is characterized in that the combining unit (10-1) is arranged in the top of crystal growth portion (10-3), and
It is connected to by intermediate pore (10-2) with crystal growth portion (10-3)；The seed crystal portion (10-4) is at crystal growth portion (10-3)
Lower section, and the two is connected to.
2. crucible according to claim 1, it is characterised in that: the quantity of the pore (10-2) be equipped with one with
On.
3. crucible according to claim 1 or 2, it is characterised in that: the radius of the pore (10-2)rWith combining unit
The height of (10-1)hBetween relationship are as follows:
Wherein,ρFor the density of melt,gFor acceleration of gravity,σFor the interfacial tension of melt.
4. crucible according to claim 1 or 2, it is characterised in that: the radius of the pore (10-2) is 0.1mm-
0.15mm。
5. a kind of trans- injection synthesizes continuous VGF crystal growing apparatus, including furnace body, it is mounted on the intracorporal crucible of furnace (10), guarantor
Warm system, heating system, temperature control system and pressure regulation system, it is characterised in that: the crucible (10) is trans- injection
Synthesize continuous VGF crystal growing crucible.
6. device according to claim 5, it is characterised in that: described device is in crucible combining unit (10-1) and crystal growth
Thermal insulation layer (15) are set between portion (10-3).
7. device according to claim 5, it is characterised in that: be equipped with observation window (19) at the top of the furnace body.
8. device according to claim 5, it is characterised in that: the heating system includes setting in crucible (10) periphery
Heater strip (28), the temperature control system include thermocouple, and the pressure regulation system includes the charge and discharge probeed into crucible (10)
Feed channel (11).
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| CN201822102284.1U CN209456611U (en) | 2018-12-14 | 2018-12-14 | The trans- injection of one kind synthesizes continuous VGF crystal growing crucible and device |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110760931A (en) * | 2019-11-22 | 2020-02-07 | 中国电子科技集团公司第十三研究所 | System for preparing indium phosphide crystal by indium phosphide mixture |
| CN113308738A (en) * | 2021-06-01 | 2021-08-27 | 中国电子科技集团公司第十三研究所 | Method for preparing compound semiconductor crystal by combining continuous LEC and VGF after injection synthesis |
| CN115198347A (en) * | 2022-07-15 | 2022-10-18 | 中国电子科技集团公司第十三研究所 | Device and method for centrifugally synthesizing and growing compound crystal |
-
2018
- 2018-12-14 CN CN201822102284.1U patent/CN209456611U/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110760931A (en) * | 2019-11-22 | 2020-02-07 | 中国电子科技集团公司第十三研究所 | System for preparing indium phosphide crystal by indium phosphide mixture |
| CN110760931B (en) * | 2019-11-22 | 2024-03-19 | 中国电子科技集团公司第十三研究所 | System for preparing indium phosphide crystal by utilizing indium-phosphorus mixture |
| CN113308738A (en) * | 2021-06-01 | 2021-08-27 | 中国电子科技集团公司第十三研究所 | Method for preparing compound semiconductor crystal by combining continuous LEC and VGF after injection synthesis |
| CN115198347A (en) * | 2022-07-15 | 2022-10-18 | 中国电子科技集团公司第十三研究所 | Device and method for centrifugally synthesizing and growing compound crystal |
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