CN107460541A - The aluminum nitride crystal growth device controllable for raw material distillation and application method - Google Patents
The aluminum nitride crystal growth device controllable for raw material distillation and application method Download PDFInfo
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- CN107460541A CN107460541A CN201710816537.9A CN201710816537A CN107460541A CN 107460541 A CN107460541 A CN 107460541A CN 201710816537 A CN201710816537 A CN 201710816537A CN 107460541 A CN107460541 A CN 107460541A
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- crucible
- heater
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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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
- C30B23/06—Heating of the deposition chamber, the substrate or the materials to be evaporated
- C30B23/066—Heating of the material to be evaporated
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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
- C30B29/38—Nitrides
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- Crystallography & Structural Chemistry (AREA)
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention relates to a kind of aluminum nitride crystal growth device controllable for raw material distillation and application method, in aluminum nitride crystal seed crystal long-time growth course, by below crucible, moveable bottom heater is set inside side heater 2, realize the controllable adjustment of crucible top temperature, crucible bottom temperature and crucible interior temperature distribution, reach the first crucible bottom temperature for the maximum temperature in crucible, material transport direction is fully upward, in constant charge level spacing, raw material height gradually reduces as crystal thickness increases；The temperature of second plane of crystal is constant, and degree of supersaturation does not change with crystal growth, and crystal growth is stable；3rd in the case where crucible bottom temperature highest and plane of crystal temperature are certain, realize that the stabilization of raw material transports by the cooperation of two heaters, have the technical effect that to form the distillation of the stable degree of supersaturation of seed crystal face and raw material stabilization and transport process, crystal growth stability is improved, reaches the purpose of growth high-crystal quality aluminium nitride.
Description
Technical field
The present invention relates to a kind of aluminum nitride crystal growth device, is related to a kind of controllable aluminum nitride crystal that distilled for raw material
Grower and application method.
Background technology
Aluminium nitride has excellent physical property, such as energy gap (6.2eV), the high disruptive field intensity of ultra-wide（11.7×
106V•cm-1）, high thermal conductivity（Measured value 2.85W cm-1•K-1）, excellent heat endurance and corrosion resistance, good light
Learn property and mechanical property.Aluminium nitride material will have particularly significant with its excellent performance in photoelectron and microelectronic
Application, as aluminium nitride material has weak thermal excitation, direct band gap, ABSORPTION EDGE（200nm）The deep ultraviolet band the characteristics of.This
Outside, when as the substrate of AlGaN bases and GaN base epitaxial material, also with the incomparable advantage of other substrates, aluminium nitride with
AlGaN belongs to material of the same clan, and lattice mismatch is small, and lattice mismatch between the two is up to 2.4%, and aluminium nitride and AlGaN's is hot swollen
Swollen coefficient is closest, in growth and cooling procedure prepared by device, can avoid the cracking of epitaxial structure.Aluminium nitride can be with
GaN forms continuous solid solution AlxGa1-xN, energy gap is 3.39 ~ 6.2, and continuously adjustabe, can launch 365 ~ 200nm wavelength
Ultraviolet light.Based on These characteristics, aluminium nitride have in following Aero-Space, life medical treatment, environmental monitoring etc. it is huge
Application prospect.
At present, physical vapor transmission (PVT) method is acknowledged as one of growing aluminum nitride crystal most efficient method, seed crystal
Growth is the final goal of aluminum nitride crystal growth.The requirement of seeded growth aluminium nitride seed crystal is in longer growth cycle（15 days with
On）The degree of supersaturation of middle seed crystal face keeps constant, degree of supersaturation（S）It is represented by such as formula（1）It is shown：
（1）
In formula, PAlFor Al partial vapour pressures, PN2For N2Qi leel pressure,K(T)For seed crystal face temperature.Therefore in crystal growing process
In, the degree of supersaturation S for nitrogenizing aluminum vapor is mainly together decided on by Temperature Distribution in crucible and vapour pressure.This is required in crucible
The distillation transmission of portion's thermal field and raw material has good matching, that is, require Temperature Distribution and raw material distillation transmit it is controllable.But
Aluminum nitride crystal growth device can not meet requirement of the seed crystal aluminum nitride crystal growth to degree of supersaturation at present, be mainly manifested in
Lower aspect：
（1）Thermal field distribution is uncontrollable：As crystal growth and raw material shrink, thermal field gradually changes inside crucible, especially crystal table
Cause plane of crystal temperature to raise towards high-temperature region movement, cause the reduction of plane of crystal degree of supersaturation, reduce crystal growth rate,
Even result in crystal distillation.
（2）Material transport is uncontrollable：, can be by raw material sublimation process according to the difference of thermaltransmission mode between raw material and crucible
It is divided into three phases, i.e., 1）Heat transfer stage when crucible internal walls are in close contact with raw material, 2）Crucible internal walls connect with feedstock portions
Tactile heat transfer is to the heat radiation transformation stage, and 3）Crucible internal walls and raw material discontiguous heat radiation stage.The stable distillation of raw material with
Stable transmission is the necessary factor of seed crystal aluminum nitride crystal growth, generally brilliant in the three phases growing aluminum nitride of raw material distillation
Body.But in the three phases of whole raw material distillation, raw material is also gradually changing with crucible internal walls distance, result in raw material distillation
Amount and the change of transmission, in addition raw material distillation are only carried out around raw material, raw material bottom distillation amount very little, cause raw material whole
It is highly constant in crystal growing process, as crystal thickness increase plane of crystal and ingredient upper surface distance are gradually reduced, greatly
Ground influences the stability of degree of supersaturation.
In view of above-mentioned 2 points, for the growth strategy of seeded growth aluminium nitride, require first at aluminum nitride crystal growth face
Temperature is constant, secondly also requires that nitridation aluminum vapor distillation amount is constant in crucible, and require crucible bottom temperature and plane of crystal
Temperature difference is constant.
The content of the invention
In order to obtain the plane of crystal degree of supersaturation stability that the growth of seed crystal aluminium nitride requires, the temperature of the invention based on equipment
Field design, there is provided a kind of aluminum nitride crystal growth device controllable for raw material distillation and application method, concrete technical scheme
It is a kind of controllable aluminum nitride crystal growth device that distilled for raw material, including side heater and crucible, it is characterised in that：Also
Including bottom heater, crucible tray and crucible tray support bar, described side heater is 80 ~ 200mm of diameter, height 100 ~
300mm cylindrical body, bottom heater are the ring body of any attachment structure of the external diameter less than side 10 ~ 30mm of heater internal diameter, and
When crucible tray support bar passes through ring body, the outer span bottom heater ring body internal diameter of crucible tray support bar is 2-8 mm, crucible tray
A diameter of 5 ~ the 8mm of support bar, crucible tray diameter are less than bottom heater external diameter, and crucible tray (3) bottom face center is fluted and earthenware
Crucible support support bar coordinates, and crucible diameter is less than crucible tray diameter, and it is connected as bottom heater and is located at side heater body, crucible
Support support bar passes through from bottom heater center, and crucible tray is fixed on crucible tray post upper, and crucible (1) is placed on crucible tray
Upper surface is placed in side heater body.
2nd, a kind of controllable aluminum nitride crystal growth device that distilled for raw material as claimed in claim 1, its feature exist
In：Side heater, bottom heater, crucible tray, crucible tray support bar and crucible material are the tungsten that purity is not less than 99.9%
Metal.
3rd, a kind of controllable aluminum nitride crystal growth device that distilled for raw material as claimed in claim 1, its feature exist
In：Side heater structure is tungsten watt, tungsten bar or tungsten silk screen, and bottom heater structure is tungsten watt, and tungsten tilt sickness is 1 ~ 3mm.
4th, using a kind of user of aluminum nitride crystal growth device controllable for raw material distillation described in claim 1
Method, it is characterised in that：Application method comprises the following steps:
1）, be heated to using side heater (2) side crucible (1) head temperature after 1700 DEG C ~ 1900 DEG C, to open lower curtate heater
(4) crucible (1) bottom temp is higher than 20 ~ 150 DEG C of its head temperature, start crystal growth；
2）, by crucible supporting bar (5), raise crucible (1), lifting speed is 0.1mm/h ~ 2mm/h, during this, is increased
Lower curtate heater (4) power, keep crucible (1) bottom temp to be higher than 20 ~ 150 DEG C of its head temperature, complete crystal growth；
3）, lower curtate heater (4) power is gradually decrease to close, make crucible top temperature decrease rate be less than or equal to 5 DEG C/
Min, start to cool；
The present invention operation principle be：
In aluminum nitride crystal seed crystal long-time growth course, by below crucible, moveable bottom is set inside side heater 2
Portion's heater, the controllable adjustment of crucible top temperature, crucible bottom temperature and crucible interior temperature distribution is realized, can be achieved,
First crucible bottom temperature is the maximum temperature in crucible, and material transport direction fully upward, and ensures between constant charge level
Away from upper, raw material height gradually reduces as crystal thickness increases；The temperature of second plane of crystal is constant, degree of supersaturation not with
Crystal growth and change, crystal growth is stable；3rd in the case where crucible bottom temperature highest and plane of crystal temperature are certain, lead to
The cooperation for crossing two heaters realizes that the stabilization of raw material transports, what the degree of supersaturation and raw material that formation seed crystal face is stablized were stablized
Distillation and transport process, crystal growth stability is improved, reach the purpose of growth high-crystal quality aluminium nitride.
It is an advantage of the invention that by setting pyrotoxin to crucible bottom in aluminum nitride crystal growth device, and with crystal
Gradual mobile crucible and thermal source are grown, plane of crystal temperature is kept constant, also controllable raw material distillation amount.
Brief description of the drawings
Fig. 1 is principle schematic diagram of the present invention,
Fig. 2 is bottom heater loop configuration schematic diagram of the present invention；
Fig. 3 is bottom heater triangular structure schematic diagram of the present invention；
Fig. 4 is raw material filling situation schematic side view before crystal growth of the embodiment of the present invention；
Fig. 5 is that raw material shrinks situation schematic side view in crystal growing process of the embodiment of the present invention；
Fig. 6 is that raw material shrinks situation schematic side view in traditional heating structure crystal growth course.
Embodiment
As shown in figures 1 to 6,
Embodiment 1
Side heater 2 is tungsten tile structure, and its a diameter of 80mm, height 100mm, wall thickness 2mm, bottom heater 4 is that tungsten watt is in
Y-connection structure, external diameter 70mm, open pore size 10mm, wall thickness 2mm, 5 a diameter of 6mm of crucible tray support bar, crucible
3 a diameter of 60mm of support, 1 a diameter of 50mm of crucible, material are the tungsten metal that purity is not less than 99.9%.
Bottom heater 4 is located inside side heater 2, and crucible tray support bar 5 passes through from the center of bottom heater 4, crucible
Support 3 is fixed on the upper end of crucible tray support bar 5, and crucible 1 is placed on the upper surface of crucible tray 3 and is placed in inside side heater 2；
Load aln raw material 8 inside to crucible 1, aluminium nitride seed crystal 9 is pasted on substrate 6, aluminium nitride gas is in gas phase transmission
Region 7 is transmitted, and is carried out in accordance with the following steps in crystal growing process,
1）, be heated to using side heater 2 head temperature of side crucible 1 after 1800 DEG C, to open lower curtate heater 4, making the bottom of crucible 1
Portion's temperature is higher than 100 DEG C of its head temperature, starts crystal growth；
2）, by crucible supporting bar 5, raise crucible 1, lifting speed is 1mm/h, during this, the work(of increase lower curtate heater 4
Rate, keep the bottom temp of crucible 1 to be higher than 100 DEG C of its head temperature, complete crystal growth；
3）, the power of lower curtate heater 4 is gradually decrease to close, crucible top temperature decrease rate is less than or equal to 5 DEG C/min,
Start to cool；
Embodiment 2
The present embodiment no power of bottom heater 4 as different from Example 1, is not moved, only by the electrified regulation of side heater 2,
The distribution of this kind of thermal field is equivalent to traditional thermal field situation, and in the present embodiment after crystal growth, surplus stock shape is as shown in Figure 6.
Compared with Example 1, raw material bottom temp can not be adjusted in the embodiment of the present invention, and raw material height is not with crystal growth
And decline, the transmission of raw material atmosphere persistently changes in whole crystal growing process, and thermal field is unstable.
Claims (4)
1. a kind of controllable aluminum nitride crystal growth device that distilled for raw material, including side heater (2) and crucible (1), it is special
Sign is：Also include bottom heater (4), crucible tray (3) and crucible tray support bar (5), described side heater (2) is diameter
80 ~ 200mm, 100 ~ 300mm of height cylindrical body, bottom heater (4) are that external diameter is less than side heater (2) 10 ~ 30mm of internal diameter
Any attachment structure ring body, and when crucible tray support bar (5) passes through ring body, the outer span bottom of crucible tray support bar (5)
Heater (4) ring body internal diameter is 2-8 mm, crucible tray support bar (5) a diameter of 5 ~ 8mm, and crucible tray (3) diameter adds less than bottom
Hot device (4) external diameter, crucible tray (3) bottom face center is fluted to be coordinated with crucible tray support bar (5), and crucible (1) diameter is less than earthenware
Crucible support (3) diameter, it is connected as bottom heater (4) and is located at side heater (2) inside, and crucible tray support bar (5) adds from bottom
Hot device (4) center passes through, and crucible tray (3) is fixed on crucible tray support bar (5) upper end, and crucible (1) is placed on crucible tray (3) upper end
It is internal that face is placed in side heater (2).
A kind of 2. controllable aluminum nitride crystal growth device that distilled for raw material as claimed in claim 1, it is characterised in that：Side
Heater (2), bottom heater (4), crucible tray (3), crucible tray support bar (5) and crucible (1) material are that purity is not less than
99.9% tungsten metal.
A kind of 3. controllable aluminum nitride crystal growth device that distilled for raw material as claimed in claim 1, it is characterised in that：Side
Heater (2) structure is tungsten watt, tungsten bar or tungsten silk screen, and bottom heater (4) structure is tungsten watt, and tungsten tilt sickness is 1 ~ 3mm.
4. a kind of application method of controllable aluminum nitride crystal growth device that distilled for raw material described in claim 1 is used,
It is characterized in that：Application method comprises the following steps:
1）, be heated to using side heater (2) side crucible (1) head temperature after 1700 DEG C ~ 1900 DEG C, to open lower curtate heater
(4) crucible (1) bottom temp is higher than 20 ~ 150 DEG C of its head temperature, start crystal growth；
2）, by crucible supporting bar (5), raise crucible (1), lifting speed is 0.1mm/h ~ 2mm/h, during this, is increased
Lower curtate heater (4) power, keep crucible (1) bottom temp to be higher than 20 ~ 150 DEG C of its head temperature, complete crystal growth；
3）, lower curtate heater (4) power is gradually decrease to close, make crucible top temperature decrease rate be less than or equal to 5 DEG C/
Min, start to cool.
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| CN201710816537.9A CN107460541A (en) | 2017-09-12 | 2017-09-12 | The aluminum nitride crystal growth device controllable for raw material distillation and application method |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108396384A (en) * | 2018-05-25 | 2018-08-14 | 深圳大学 | A kind of device and method preparing aluminum nitride crystal |
| CN111334863A (en) * | 2020-04-13 | 2020-06-26 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Non-bonding seed crystal aluminum nitride crystal growth device and aluminum nitride crystal preparation method |
| CN111676514A (en) * | 2020-07-23 | 2020-09-18 | 奥趋光电技术(杭州)有限公司 | Large-temperature-difference crystal growth furnace and method for preparing high-quality aluminum nitride single crystal |
| CN113652740A (en) * | 2021-08-27 | 2021-11-16 | 宁波合盛新材料有限公司 | Preparation method of silicon carbide single crystal, single crystal growing furnace and heating device of single crystal growing furnace |
| CN114134573A (en) * | 2021-11-30 | 2022-03-04 | 武汉大学 | Device for reducing aluminum nitride crystal growth stress |
| CN115928201A (en) * | 2023-03-10 | 2023-04-07 | 中国电子科技集团公司第四十六研究所 | Method for realizing temperature distribution required by growth of aluminum nitride single crystal |
| CN116427035A (en) * | 2023-03-10 | 2023-07-14 | 中国电子科技集团公司第四十六研究所 | Raw material loading and unloading method suitable for large-size aluminum nitride crystal growth |
| CN117535787A (en) * | 2023-11-14 | 2024-02-09 | 江苏超芯星半导体有限公司 | Thermal field structure, silicon carbide growth device and silicon carbide growth method |
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| CN103103611A (en) * | 2011-11-11 | 2013-05-15 | 深圳大学 | Device and process for preparing aluminum nitride crystals by adopting spontaneous crystal seed method |
| CN106149057A (en) * | 2015-03-10 | 2016-11-23 | 深圳大学 | The controlled aluminum nitride crystal growth device in temperature field and technique |
| CN106435736A (en) * | 2016-09-14 | 2017-02-22 | 苏州奥趋光电技术有限公司 | Aluminum nitride crystal growing furnace |
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| CN103103611A (en) * | 2011-11-11 | 2013-05-15 | 深圳大学 | Device and process for preparing aluminum nitride crystals by adopting spontaneous crystal seed method |
| CN106149057A (en) * | 2015-03-10 | 2016-11-23 | 深圳大学 | The controlled aluminum nitride crystal growth device in temperature field and technique |
| CN106435736A (en) * | 2016-09-14 | 2017-02-22 | 苏州奥趋光电技术有限公司 | Aluminum nitride crystal growing furnace |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108396384A (en) * | 2018-05-25 | 2018-08-14 | 深圳大学 | A kind of device and method preparing aluminum nitride crystal |
| CN111334863A (en) * | 2020-04-13 | 2020-06-26 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Non-bonding seed crystal aluminum nitride crystal growth device and aluminum nitride crystal preparation method |
| CN111676514A (en) * | 2020-07-23 | 2020-09-18 | 奥趋光电技术(杭州)有限公司 | Large-temperature-difference crystal growth furnace and method for preparing high-quality aluminum nitride single crystal |
| CN113652740A (en) * | 2021-08-27 | 2021-11-16 | 宁波合盛新材料有限公司 | Preparation method of silicon carbide single crystal, single crystal growing furnace and heating device of single crystal growing furnace |
| CN114134573A (en) * | 2021-11-30 | 2022-03-04 | 武汉大学 | Device for reducing aluminum nitride crystal growth stress |
| CN114134573B (en) * | 2021-11-30 | 2024-04-19 | 武汉大学 | Device for reducing growth stress of aluminum nitride crystal |
| CN115928201A (en) * | 2023-03-10 | 2023-04-07 | 中国电子科技集团公司第四十六研究所 | Method for realizing temperature distribution required by growth of aluminum nitride single crystal |
| CN116427035A (en) * | 2023-03-10 | 2023-07-14 | 中国电子科技集团公司第四十六研究所 | Raw material loading and unloading method suitable for large-size aluminum nitride crystal growth |
| CN115928201B (en) * | 2023-03-10 | 2023-07-18 | 中国电子科技集团公司第四十六研究所 | Method for realizing temperature distribution required by growth of aluminum nitride single crystal |
| CN116427035B (en) * | 2023-03-10 | 2024-05-17 | 中国电子科技集团公司第四十六研究所 | Raw material loading and unloading method suitable for large-size aluminum nitride crystal growth |
| CN117535787A (en) * | 2023-11-14 | 2024-02-09 | 江苏超芯星半导体有限公司 | Thermal field structure, silicon carbide growth device and silicon carbide growth method |
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Application publication date: 20171212 |