CN206204470U - A kind of growth apparatus of achievable monocrystalline online annealing - Google Patents
A kind of growth apparatus of achievable monocrystalline online annealing Download PDFInfo
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- CN206204470U CN206204470U CN201621174480.4U CN201621174480U CN206204470U CN 206204470 U CN206204470 U CN 206204470U CN 201621174480 U CN201621174480 U CN 201621174480U CN 206204470 U CN206204470 U CN 206204470U
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Abstract
The utility model provides a kind of growth apparatus of achievable monocrystalline online annealing, and the growth apparatus include：Body of heater, inflation system, vacuum system, gas extraction system, the method for annealing is by seed crystal, polycrystalline material, boron oxide is put into crucible, and monocrystal rod is grown by vertical gradient temperature methods, and growth is passed through chlorine after terminating, the boron oxide of monocrystal rod surface attachment becomes gas with chlorine reaction, outside by vavuum pump drain tank, while carrying out annealing heating process to monocrystal rod, growth monocrystalline online annealing is realized.
Description
Technical field
The utility model is related to crystal growth preparation facilities, is more particularly to partly led for III-V race or II-IV compounds of group
The growth apparatus of the achievable monocrystalline online annealing of body material.
Background technology
The industrial development by over half a century of China's artificial crystal material, in the joint efforts of numerous scientific workers
Under, huge achievement is achieved, with technical merit and larger production capacity higher, and the crystal of adequate and systematic service for it
Growth apparatus-single crystal growing furnace has also obtained development at full speed therewith.
Conventional method for monocrystal growth has VGF, abbreviation VGF methods at present.AT＆T Labs of the U.S. and previous generation
Record and prepare III-V compounds of group using VGF methods first the eighties, the method be will be equipped with indium phosphide polycrystal raw material container it is vertical
The relevant temperature gradient position set in stove is placed in, after crystalline substance material long is entirely molten, is slowly crystallized from lower end thereof and is extended to
The growing method of portion one end.Domestic single crystal growing furnace is compared with import single crystal growing furnace and there are a certain distance, is mainly manifested in and is set
In standby automaticity and the reliable and stable degree of component.
Artificial crystal material constantly develops to major diameter, high-quality, industrialization direction, and this requires the people being adapted therewith
Work crystal growth equipment develops to maximization direction, possesses good stability, quality high, high degree of automation, easy for operation
The advantages of.
Monocrystalline is important backing material, and the monocrystal material for growing out needs to cut into standard-sized chip, then
By process such as chamfering, grinding, polishing, cleanings, as commodity chip for users to use.In whole process, protect
Hold chip mechanical strength, avoid it is broken for improve production yield rate, reduces cost it is critical that.Scarce annealing can subtract
Residual stress less and in elimination monocrystal material, obtains high-quality monocrystal material.
But the stove of current main-stream can only carry out crystal growth, it is necessary to other annealing furnace carries out monocrystalline annealing.
Utility model content
The purpose of this utility model is to provide a kind of growth apparatus of achievable monocrystalline online annealing, can be in growth course
Middle accurate control temperature, substantially reduces crystal defect to meet the requirement of production high quality single crystal material.
To achieve the above object, the single crystal growth apparatus of achievable online annealing provided by the utility model include：Stove
Body, inflation system, vacuum system, gas extraction system,
The body of heater, top is followed successively by housing, heat-insulation layer, heater, quartz equipped with tank door, body of heater externally to inside
Sealing flange is inlayed at pipe, crucible, the quartz ampoule two ends, and equipped with pipeline opening, top connection inflation system, bottom connection row
Gas system and evacuation system；
The inflation system, is made up of pressure sensor and two-way loading line, wherein special feed channel is connected to all the way, separately
Chlorine pipeline is connected to all the way；
The vacuum system is made up of vacuum line, and vacuum line is connected to inside quartz ampoule by bottom of furnace body, vacuum
The pipeline other end is connected to vavuum pump, and vacuum pump outlet is connected to tail gas recycle pipeline.
The gas extraction system, is made up of discharge duct, air bleeding valve, and discharge duct one end is connected to bottom of furnace body, the other end
It is connected to tail gas recycle pipeline.
Preferably, the heater point has 5 thermostats, and five warm areas in body of heater are controlled respectively.
Preferably, five warm areas, compared to existing three warm areas, with the addition of the Ith and the Vth warm area, wherein the Ith He
II warm area controls temperature close, IV and V warm area control temperature close, equivalent to extending II and IV warm area so that II, III, IV
Warm area two ends heat losses it is less, can preferably keep the stabilization of thermograde between II, III, IV warm area.
Preferably, the vacuum system also includes evacuation valve, vacuum meter, vacuum pump group into connecting successively on vacuum pipe
Connect.
Preferably, the gas extraction system and the vacuum system common exhaust pipe road, are connected with bottom of furnace body.
Preferably, the housing and the flanged plate are stainless steel material.
The single crystal growth apparatus of achievable online annealing described in the utility model, using double-layer stainless steel housing, by cold
But water is lowered the temperature, and internal layer environmental protection refractory material insulation design, outer wall surface temperature is low, and thermal field control is accurate, can be direct
Being passed through chlorine carries out annealing process, and heating rate is fast, energy-efficient.The utility model is simple to operate, and temperature-controlled precision is high, Neng Gousheng
Grow various semi-conducting materials and realize annealing function, product quality is high.
Brief description of the drawings
Embodiment is described by with reference to accompanying drawings below, features described above of the present utility model and technological merit will
Become more fully apparent and be readily appreciated that.
Fig. 1 is the schematic diagram of the single crystal growth apparatus for being capable of achieving online annealing.
Fig. 2 is the detection temperature curve map using the single crystal growth apparatus of achievable online annealing of the present utility model.
Description of reference numerals：Stainless steel tank body 1, sealed bottom flange 2, support base 3, graphite pad 4, heater element 5 is protected
Warm layer 6, locks flange 7, lifting cylinder 8, top sealing flange 9, tank door 10, gas tube 11, pressure sensor 12, charge valve
13, charge valve 14, special feed channel 15, chlorine pipeline 16, quartz ampoule 17, crucible 18, boron oxide 19, crystalline substance material 20 long, seed crystal 21,
Thermocouple 22, thermocouple 23, thermocouple 24, thermocouple 25, gas exhaust piping 26, air bleeding valve 27, evacuation valve 28, vacuum meter 29, vavuum pump 30
Specific embodiment
The reality of the single crystal growth apparatus of achievable online annealing described in the utility model described below with reference to the accompanying drawings
Apply example.One of ordinary skill in the art will recognize, in the case of without departing from spirit and scope of the present utility model, can
Described embodiment is modified with a variety of modes or its combination.Therefore, accompanying drawing and description be inherently
It is illustrative, it is not intended to limit the scope of the claims.Additionally, in this manual, accompanying drawing draws not in scale,
And identical reference represents identical part.
The present embodiment is described in detail with reference to Fig. 1 and Fig. 2.The single crystal growth apparatus of the line annealing described in the present embodiment
Including：Referring to Fig. 1, the growth apparatus of achievable monocrystalline online annealing described in the utility model include body of heater, inflation system, true
Empty set system, gas extraction system.
The body of heater, is made up of double-layer stainless steel housing, and equipped with tank door, body of heater is followed successively by stainless externally to inside at top
Steel sheel, heat-insulation layer, heater, Ying Guan, stone crucible.Wherein described heater point has 5 thermostats.The quartz ampoule two ends edge
Embedding sealing top of stainless steel sealing flange 9 and sealed bottom flange 2, and equipped with pipeline opening, top sealing flange 9 and bottom are close
The equal center perforate connection inflation system of envelope flange 2, sealed bottom flange 2 and tank body are close to marginal position perforate connection row
Gas system and evacuation system.Crucible is placed on the sealed bottom flange 2 of quartz ampoule bottom, crucible internal storage crystal growth material
Material.
The body of heater includes stainless steel tank body 1, base 2, support base 3, graphite pad 4, heater element 5, heat-insulation layer 6, lock
Tight flange 7, lifting cylinder 8, sealing flange cap 9, tank door 10, quartz ampoule 17, crucible 18, thermocouple 22, thermocouple 23, thermocouple 24, heat
Even 25.
Stainless steel tank body 1 is in body of heater outermost, and divide has 5 warm areas, respectively I warm areas bottom-up, the IIth temperature
Area, the IIIth warm area, the IVth warm area, the Vth warm area are used to provide gradient temperature, are controlled respectively by 5 thermostats.
Base 2 in the inner lower of stainless steel tank body 1, for the support of crucible 18 and the grade of support base 3.
Support base 3 is fixed on base 2, its upper end placing graphite pad 4, and for support crucible 18, the outer wall of crucible 18 connects
Connect 4 thermocouples (being followed successively by 22,23,24,25 from top to bottom).
Quartz ampoule 17 is surrounded on outside crucible 18, and bottom is located on base 2, and top connects sealing flange cap 9, heater element
5 are surrounded on the side of quartz ampoule 17.
Heat-insulation layer 6 is used for the periphery of heater element 5, be incubated and heat-insulated.
Locking flange 7 is configured at the top of stainless steel tank body 1, for locking stainless steel tank body 1.
Tank door 10, positioned at the top of stainless steel tank body 1, for the folding of stainless steel tank body 1.
Lifting cylinder 8, release locking and lifting for controlling tank door 10 decline.
The inflation system, by pressure sensor, two-way loading line composition.Special feed channel is wherein connected to all the way, separately
Chlorine pipeline is connected to all the way.It is made up of a charge valve and metal hose per road loading line.The inflation system includes filling
Tracheae 11, pressure sensor 12, charge valve 13, charge valve 14, special feed channel 15, chlorine pipeline 16.
The one end of gas tube 11 is connected to the top through hole of stainless steel tank body 1, and insertion tank door 10, sealing flange cap 9, the other end
Connection pressure sensor 12, connection charge valve 13 arrives special feed channel 15 respectively afterwards, and connection charge valve 14 arrives chlorine pipeline
16, for providing the gas with various atmosphere in crystal growing process, and annealing atmosphere.
The vacuum system by vacuum line, vacuum meter, evacuation valve, vacuum pump group into, control furnace interior vacuum.
Vacuum line is connected to inside quartz ampoule by bottom of furnace body, and vacuum meter and evacuation valve are arranged on vacuum pipe, vacuum pipe
The other end is connected to vavuum pump, and vacuum pump outlet is connected to tail gas recycle pipeline.The vacuum system includes gas exhaust piping 26, takes out
Empty valve 28, vacuum meter 29, vavuum pump 30.
The one end of gas exhaust piping 26 connects the other end of 1 bottom through-hole insertion sealed bottom flange of stainless steel tank body 2 and is sequentially connected
Evacuation valve 28, vacuum meter 29 and vavuum pump 30, evacuation valve 28 and vavuum pump 30 are controlled by vacuum meter 29, are made in tank at vacuum
Among manufacturing technique requirent, the exhaust emissions of extraction to tail gas recycle pipeline.
The gas extraction system, is made up of discharge duct, air bleeding valve.The gas extraction system includes gas exhaust piping 26 and air bleeding valve
27.Gas extraction system and vacuum system common exhaust pipe road 26, one end of discharge duct 26 are connected to bottom of furnace body, and the other end is connected to
Tail gas recycle pipeline.Gas in tank is discharged into by tail gas recycle pipeline by the opening and closing of air bleeding valve 27.
Monocrystal growing furnace with online annealing described in the utility model, III-V race or II of can be used to growing and anneal-
IV group iii v compound semiconductor material, production process is as follows：Seed crystal 21, polycrystalline material 20, boron oxide 19 are put into crucible, by hanging down
Vertical ladder degree temperature methods grow monocrystal rod, and growth is passed through chlorine, the boron oxide and chlorine reaction of monocrystal rod surface attachment after terminating
Become gas, by vavuum pump drain tank outside, while carry out annealing heating process to monocrystal rod, realize that growth monocrystalline is moved back online
Fire.
It is specific as follows：Take out crucible 18 and indium phosphide seed crystal 21 is put in crucible bottom, be then filled with indium phosphide polycrystal material
20, boron oxide 19 is reinstalled, crucible 15 is put within quartz ampoule 17, sealing flange cap 9 is tamping, close tank door 10.I, the II
At 1030 DEG C, the III, the IV warm area is controlled at 1070 DEG C or so, and is filled with 20~30kg/cm2 high pure nitrogens for warm area control, with flat
The pressure that weighing apparatus indium phosphide growth course is produced due to decomposition.
After crystal entered the growth cycle of 5 days or so, annealed.By pressure inside the tank pressure release, nitrogen is discharged, and taken out
It is empty.When vacuum in tank is below 100Pa, closes and evacuate, be passed through chlorine, wherein annealing is heated by following speed, room temperature-
500 DEG C, 100 DEG C/h；500-800 DEG C, 60 DEG C/h；800-950 DEG C, 30 DEG C/h；950, constant temperature 5 hours；Then press
Following speed cooling：950-800 DEG C, 30 DEG C/h；800-500 DEG C, 60 DEG C/h；500- room temperatures, 100 DEG C/h；Complete
Annealing, takes out detection.
Fig. 2 is the detection temperature curve map of the single crystal growth apparatus using achievable online annealing of the present utility model,
Annealing temperature control curve shown in Fig. 2, vertical coordinate axle represents temperature, degrees Celsius (DEG C), horizontal axis table
Show time, unit hour (h), curve represents that heating progress is：- 500 DEG C of room temperature, 100 DEG C/h；500-800 DEG C, 60 DEG C/small
When；800-950 DEG C, 30 DEG C/h；950, constant temperature 5 hours；Then lower the temperature by following speed：950-800 DEG C, 30 DEG C/h；
800-500 DEG C, 60 DEG C/h；500- room temperatures, 100 DEG C/h, vertical coordinate axle minimum point is room temperature.
The average dislocation density of monocrystalline that the method for monocrystal growth that the utility model is provided is obtained is low, and crystal forming rate is high.Together
When possess online annealing function, simple to operate, efficient energy-saving.
Preferred embodiment of the present utility model is the foregoing is only, the utility model is not limited to, for this area
Technical staff for, the utility model can have various modifications and variations.It is all it is of the present utility model spirit and principle within,
Any modification, equivalent substitution and improvements made etc., should be included within protection domain of the present utility model.
Claims (6)
1. a kind of single crystal growth apparatus of achievable online annealing, it is characterised in that including：Body of heater, inflation system, vacuum system
System, gas extraction system,
The body of heater, top is followed successively by housing, heat-insulation layer, heater, quartz ampoule, earthenware equipped with tank door, body of heater externally to inside
Sealing flange is inlayed at crucible, the quartz ampoule two ends, and equipped with pipeline opening, top connection inflation system, bottom connection exhaust system
System and evacuation system；
The inflation system, is made up of pressure sensor and two-way loading line, wherein being connected to special feed channel, Ling Yilu all the way
It is connected to chlorine pipeline；
The vacuum system is made up of vacuum line, and vacuum line is connected to inside quartz ampoule by bottom of furnace body, vacuum pipe
The other end is connected to vavuum pump, and vacuum pump outlet is connected to tail gas recycle pipeline；
The gas extraction system, is made up of discharge duct, air bleeding valve, and discharge duct one end is connected to bottom of furnace body, other end connection
To tail gas recycle pipeline.
2. single crystal growth apparatus according to claim 1, it is characterised in that
Wherein described heater point has 5 thermostats, and five warm areas in body of heater are controlled respectively.
3. single crystal growth apparatus according to claim 2, it is characterised in that
Five warm areas, compared to existing three warm areas, with the addition of the Ith and the Vth warm area, wherein the Ith and II warm area control temperature
Degree is close, IV and V warm area control temperature close, equivalent to extending II and IV warm area so that II, III, IV warm area two ends heat
What is be lost in is less, can preferably keep the stabilization of thermograde between II, III, IV warm area.
4. single crystal growth apparatus according to claim 1, it is characterised in that
The vacuum system also includes that evacuation valve, vacuum meter are constituted, and evacuation valve, vacuum meter, vavuum pump be successively on vacuum pipe
Connection.
5. single crystal growth apparatus according to claim 1, it is characterised in that
The gas extraction system and the vacuum system common exhaust pipe road, are connected with bottom of furnace body.
6. single crystal growth apparatus according to claim 1, it is characterised in that
The housing and the flanged plate are stainless steel material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201621174480.4U CN206204470U (en) | 2016-10-26 | 2016-10-26 | A kind of growth apparatus of achievable monocrystalline online annealing |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201621174480.4U CN206204470U (en) | 2016-10-26 | 2016-10-26 | A kind of growth apparatus of achievable monocrystalline online annealing |
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| CN206204470U true CN206204470U (en) | 2017-05-31 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106400102A (en) * | 2016-10-26 | 2017-02-15 | 北京鼎泰芯源科技发展有限公司 | Growth equipment and method thereof capable of achieving online annealing of single crystal |
| CN108265327A (en) * | 2018-04-06 | 2018-07-10 | 深圳市东晶体技术有限公司 | A kind of pressure furnace for being used to prepare indium phosphide single crystal |
-
2016
- 2016-10-26 CN CN201621174480.4U patent/CN206204470U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106400102A (en) * | 2016-10-26 | 2017-02-15 | 北京鼎泰芯源科技发展有限公司 | Growth equipment and method thereof capable of achieving online annealing of single crystal |
| CN106400102B (en) * | 2016-10-26 | 2019-06-28 | 珠海鼎泰芯源晶体有限公司 | A kind of growth apparatus and its method of achievable monocrystalline online annealing |
| CN108265327A (en) * | 2018-04-06 | 2018-07-10 | 深圳市东晶体技术有限公司 | A kind of pressure furnace for being used to prepare indium phosphide single crystal |
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| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20170803 Address after: 100080 Haidian District street, Haidian, building B, block 10, level 340, level 3, Patentee after: Beijing Ding Tai Xinyuan Technology Development Co. Ltd. Address before: 519085 Guangdong province Zhuhai city road two Jinding Industrial Area high-tech zone on the south side of A1 building, Rui Patentee before: Zhuhai Ding Tai Xinyuan crystal Ltd |
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| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20170821 Address after: 519085 Guangdong province Zhuhai city road two Jinding Industrial Area high-tech zone on the south side of A1 building, Rui Patentee after: Zhuhai Ding Tai Xinyuan crystal Ltd Address before: 100080 Haidian District street, Haidian, building B, block 10, level 340, level 3, Patentee before: Beijing Ding Tai Xinyuan Technology Development Co. Ltd. |