CN107904657A - A kind of growing method of PVT methods growing large-size Semi-insulating silicon carbide mono-crystal - Google Patents
A kind of growing method of PVT methods growing large-size Semi-insulating silicon carbide mono-crystal Download PDFInfo
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- CN107904657A CN107904657A CN201711189841.1A CN201711189841A CN107904657A CN 107904657 A CN107904657 A CN 107904657A CN 201711189841 A CN201711189841 A CN 201711189841A CN 107904657 A CN107904657 A CN 107904657A
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- 239000013078 crystal Substances 0.000 title claims abstract description 80
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 76
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 41
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000007789 gas Substances 0.000 claims abstract description 36
- 239000000843 powder Substances 0.000 claims abstract description 32
- 229910052786 argon Inorganic materials 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 238000000137 annealing Methods 0.000 claims abstract description 12
- 239000012535 impurity Substances 0.000 claims abstract description 9
- 230000006837 decompression Effects 0.000 claims abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 14
- 229910002804 graphite Inorganic materials 0.000 claims description 14
- 239000010439 graphite Substances 0.000 claims description 14
- 239000011856 silicon-based particle Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 4
- 238000000354 decomposition reaction Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 230000006641 stabilisation Effects 0.000 claims description 3
- 238000011105 stabilization Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 230000001186 cumulative effect Effects 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 6
- 229910021421 monocrystalline silicon Inorganic materials 0.000 abstract description 2
- 230000008569 process Effects 0.000 description 6
- 229910021431 alpha silicon carbide Inorganic materials 0.000 description 5
- 238000009413 insulation Methods 0.000 description 4
- 239000000758 substrate Substances 0.000 description 3
- 229910052720 vanadium Inorganic materials 0.000 description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000004377 microelectronic Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
Classifications
-
- 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
- C30B23/002—Controlling or regulating
-
- 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
- C30B29/36—Carbides
Abstract
The present invention provides a kind of growing method of PVT methods growing large-size Semi-insulating silicon carbide mono-crystal, it mainly includes the following control stage:Prepared by SiC powder, shove charge vacuumizes, despumation gas, the pressurization that is rapidly heated, decompression constant temperature, crystal growth, finishing phase and annealing.Single-crystal silicon carbide is grown using PVT methods, raw material is pre-processed first, improve the purity and density of raw material, reduce the defects of being likely to occur in crystal, by SiC powder shove charge, by controlling temperature a period of time in the range of 1300 ~ 1400 DEG C with despumation gas, to be rapidly heated after being filled with high-purity argon gas to 2100 ~ 2400 DEG C after vacuumizing.After constant temperature is in a certain value, air pressure is gradually reduced in the case where keeping temperature plateau, powder source starts to sublime up into and starts to grow at seed crystal at this time, and crystal growth carries out finishing phase to a certain extent, it is filled with argon gas and stops the growth that heating terminates SiC crystal, finally completes crystal growth by annealing.The present invention can reduce the defects of crystal and impurity concentration obtains the semi-insulating 4H SiC single crystals of large scale.
Description
Technical field
The invention belongs to silicon carbide monocrystal growth field, and in particular to a kind of PVT methods growing large-size semi-insulating silicon carbide
The growing method of monocrystalline.
Background technology
As the representative of third generation semiconductor material with wide forbidden band, SiC single crystal has broad-band gap, high heat conductance, high critical hits
The advantages that wearing electric field and high electronics saturation migration rate, is particularly suitable for making the microelectronic component of high power density and is operated in
Power electronic device under the extreme conditions such as high temperature, high frequency, high pressure, high-power and intense radiation.As silicon carbide-based electronic device is ground
That studies carefully reaches its maturity, and large scale, the semi-insulation SiC demand of high quality are increasingly urgent, becomes one of the focus area of SiC researchs.
Physical vapor transport (Physical Vapor Transport-PVT) is large scale SiC more mature at present
Crystal technique, i.e., be attached to graphite crucible by SiC chips and cover as seed crystal, equipped with being used as growth raw material in graphite crucible
SiC powder, growth temperature controlled between 2100 DEG C to 2400 DEG C, and growth raw material is resolved into after gaseous component in graphite crucible
Crystalline growth SiC crystal at seed crystal is transported under the driving of internal axial-temperature gradient.
Making of the semi-insulation SiC material to SiC device has very important meaning.The head of GaN/SiC microwave HEMT devices
Select substrate.Domestic high-power GaN/SiC HEMT devices are mostly to mix the semi-insulating 4H- of vanadium using semi-insulation SiC single crystalline substrate at present
SiC single crystal, causes device performance to decline or even fail, vanadium can be in microwave device using the back-gate effect for mixing vanadium semi-insulation SiC substrate
The defects of back-gate effect is produced in part causes current collapse, and the leakage current under different frequency is discrete and reduces output power.This hair
The bright intrinsic defect using SiC single crystal introduces deep energy level compensation shallow level impurity, grows undoped high-purity semi-insulating 4H-
SiC single crystal.
The content of the invention
It is an object of the invention to propose a kind of growthing process parameter of optimization SiC single crystal, and then grow high-purity half absolutely
Edge 4H-SiC monocrystalline, improves the efficiency, yield rate, the PVT method growing large-size semi-insulating silicon carbides of stability of SiC single crystal growth
The growing method of monocrystalline.
The object of the present invention is achieved like this:Single-crystal silicon carbide is grown using PVT methods, is included the following steps:SiC powder
Prepare, shove charge vacuumizes, despumation gas, the pressurization that is rapidly heated, decompression constant temperature, crystal growth, finishing phase and annealing.It is first
First raw material is pre-processed, the purity and density of raw material is improved, reduces the defects of being likely to occur in crystal, by SiC powder
After last shove charge, vacuumized through shove charge, despumation gas, be rapidly heated, be depressured constant temperature, crystal growth, finishing phase and annealing
Crystal growth is completed etc. technical process.The present invention obtains the semi insulating silicon carbide of high quality by optimizing the technological parameter of crystal growth
Silicon single crystal, its technical process are as follows:Raw material is pre-processed, shove charge vacuumize after by controlling temperature at 1300 ~ 1400 DEG C
In the range of a period of time with despumation gas, be rapidly heated after being filled with high-purity argon gas to 2100 ~ 2400 DEG C.When constant temperature exists
After a certain value, air pressure is gradually reduced in the case where keeping temperature plateau, powder source starts to sublime up into and starts to grow at seed crystal at this time,
Crystal growth carries out finishing phase to a certain extent, is filled with argon gas and stops the growth that heating terminates SiC crystal, finally by annealing
Complete crystal growth.
The present invention also has this to have some technical characteristics:
(1)The preparation of high-purity alpha-SiC powder:C powder is put into graphite crucible before SiC is synthesized, in 2200 DEG C ~ 2300 DEG C Gao Zhen
When the lower sintering 3 of sky is small, to reduce the gaseous impurity adsorbed in C powder and graphite crucible.By C powder and the uniform dispenser of Si particles in crucible
It is interior, air pressure is evacuated to 10-3Below Pa, is to slowly warm up to the gaseous impurity adsorbed in 1300 DEG C ~ 1400 DEG C discharge raw materials, is filled with height
Pure argon to 60000Pa ~ 80000Pa, be warming up to 2100 DEG C-~ 2150 DEG C.Stop heating after keeping the temperature 1h ~ 2h, obtain high-purity alpha-SiC
Powder;Raw materials used selection is that Si particles and particle diameter that particle diameter is 8N for 1 ~ 2mm or so purity are that 70 ~ 90um or so purity is
The C powder of 9N;The purity range of high-purity argon gas is 99.9990%-99.9996%;
(2)Shove charge, vacuumize:After shove charge, after furnace chamber air pressure is evacuated to 10 ~ 15Pa using mechanical pump, using molecular pump by air pressure
It is evacuated to 10-3~10-4Pa;
(3)Despumation gas:1300 DEG C ~ 1400 DEG C are to slowly warm up to, vacuum maintains 10 in holding chamber-3~10-4Pa,
The main purpose of this step is the foreign gas for excluding to adsorb in graphite crucible and SiC powder;
(4)Be rapidly heated pressurization:After despumation gas, as temperature raises, the equilibrium partial pressure of Si steam gradually increases, and is
Suppress the decomposition of SiC seed crystals, high-purity argon gas be filled with before heating, by air pressure in furnace body maintain 60000Pa ~ 80000Pa it
Between, it is rapidly heated to 2200 DEG C ~ 2400 DEG C;When the time range being rapidly heated that slowly heats up relatively is 2.5-3.5 small
(5)It is depressured constant temperature:Heating power supply power is adjusted, makes temperature stabilization at 2200 DEG C ~ 2400 DEG C, butterfly valve is opened, to avoid out
Existing excessive temperature fluctuation so that constant temperature and pressure reduction are carried out at the same time;The pressure of constant temperature decompression is dropped to by 60000-80000Pa
1000-10000Pa, dip time scope is when 8-12 is small;
(6)Crystal growth:The growing environment of SiC crystal is constant temperature and pressure, and stable gas pressure is at 1000Pa ~ 10000Pa, crucible bottom
The temperature in portion is in the range of 2200 DEG C ~ 2400 DEG C, and appropriate to adjust the distance between raw material seed crystal, raw material, which is sublimed up at seed crystal, to be started
Growth, grows high quality SiC single crystal;
(7)Finishing phase:High-purity argon gas is filled with into furnace body, stops heating, terminates the growth of SiC single crystal;
(8)Annealing:After completing crystal growth, temperature is persistently filled with argon gas in the range of 2000 DEG C ~ 2100 DEG C, controls in furnace chamber
For pressure between 10000Pa ~ 20000Pa, soaking time is 10 ~ 15h, is then slowly dropped to room temperature with 10 ~ 20 DEG C/min
After take out carborundum crystals, 2200 DEG C of annealing region arrives room temperature.
The beneficial effects of the present invention are:
This patent grows high-purity semi-insulating 4H-SiC monocrystalline by optimizing the growthing process parameter of SiC single crystal.
(1)Using high-purity alpha-SiC powder, 1300 DEG C ~ 1400 DEG C are to slowly warm up to, vacuum maintains 10 in holding chamber-3~
10-4Pa, effectively excludes the gaseous impurity adsorbed in raw material and graphite crucible, is conducive to grow high-purity semi-insulating SiC single crystal;
(2)In crystal growing process, by adjusting heating power, vacuum and argon pressure, close thermal field distribution in furnace chamber
Reason, beneficial to the SiC single crystal for obtaining large scale, high quality and low defect;
(3)The SiC crystal grown using this technique, is reduced the micropipe density in crystal, the resistivity of crystal greatly improved,
It is adapted to make the microelectronic component of high power density and is operated in the extreme bars such as high temperature, high frequency, high pressure, high-power and intense radiation
Power electronic device under part.
Brief description of the drawings
Fig. 1 is growing method flow chart of the present invention;
Fig. 2 prepares schematic diagram for SiC powder;
Fig. 3 grows schematic diagram for SiC crystal.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments to the present invention
It is further elaborated.It should be appreciated that specific embodiment described herein is not used to limit only to explain the present invention
The fixed present invention.
With reference to Fig. 1, the present embodiment detailed process is as follows:
S1, the preparation of high-purity alpha-SiC powder:C powder 2 is put into graphite crucible 4 before SiC is synthesized, in 2200 DEG C ~ 2300 DEG C Gao Zhen
When the lower sintering 3 of sky is small, to reduce the gaseous impurity adsorbed in C powder and graphite crucible.It is alternately uniform by the way of multilayer powdering
Dispenser C powder and Si particles 1,10 are evacuated to by air pressure-3~10-4Pa, is to slowly warm up to what is adsorbed in 1300 DEG C ~ 1400 DEG C discharge raw materials
Gaseous impurity, is filled with high-purity argon gas to 60000Pa ~ 80000Pa, be warming up to 2100 DEG C-~ 2150 DEG C.Stop adding after keeping the temperature 1h ~ 2h
Heat, obtains high-purity alpha-SiC powder;Graphite crucible 4 is provided outside heating coil 3;
S2, shove charge, vacuumize:After shove charge, after furnace chamber air pressure is evacuated to 10 ~ 15Pa using mechanical pump, using molecular pump by air pressure
It is evacuated to 10-3~10-4Pa。
S3, despumation gas:1200 DEG C ~ 1400 DEG C are to slowly warm up to, vacuum maintains 10 in holding chamber-3~10- 4Pa, the main purpose of this step are the foreign gas for excluding to adsorb in graphite crucible and SiC powder;
S4, be rapidly heated pressurization:After being to slowly warm up to 1200 DEG C ~ 1400 DEG C holding a period of times, as temperature raises, Si steam
Equilibrium partial pressure gradually increase, in order to suppress the decomposition of SiC seed crystals 5, high-purity argon gas is filled with before heating, air pressure in furnace body is tieed up
Hold between 60000Pa ~ 80000Pa, be rapidly heated to 2200 DEG C ~ 2400 DEG C;
S5, is depressured constant temperature:Heating power supply power is adjusted, makes temperature stabilization at 2200 DEG C ~ 2400 DEG C, opens butterfly valve so that reduction of speed
Constant temperature and pressure reduction are carried out at the same time;
S6, crystal growth:The growing environment of SiC crystal is constant temperature and pressure, and stable gas pressure is in 1000Pa ~ 10000Pa, crucible bottom
Temperature in the range of 2200 DEG C ~ 2400 DEG C, it is appropriate to adjust the distance between raw material seed crystal, grow high quality SiC single crystal;
S7, finishing phase:High-purity argon gas is filled with into furnace body, stops heating, terminates the growth of SiC single crystal;
S8, annealing:After completing crystal growth, temperature is persistently filled with argon gas in the range of 2000 DEG C ~ 2100 DEG C, controls in furnace chamber
Pressure is between 10000Pa ~ 20000Pa, and soaking time is 10 ~ 15h, after being then slowly dropped to room temperature with 10 ~ 20 DEG C/min
Take out carborundum crystals 6.
Above content is to combine the further description that specific preferred embodiment is the present invention, it is impossible to is assert
The specific implementation of the present invention is only limited to these explanations., can be with for the personnel with fields rudimentary knowledge of the present invention
It is easy to make a change of the present invention and modification, these change and modification should all be considered as belonging to the right that the present invention is submitted will
Seek the scope of patent protection that book determines.
Claims (10)
1. a kind of growing method of PVT methods growing large-size Semi-insulating silicon carbide mono-crystal, it is characterised in that it includes the following steps:
SiC powder prepare, shove charge vacuumize, despumation gas, the pressurization that is rapidly heated, decompression constant temperature, crystal growth, finishing phase and
Annealing, raw material is pre-processed first, shove charge vacuumize after by control temperature in the range of 1300 ~ 1400 DEG C a period of time
With despumation gas, it is rapidly heated after being filled with high-purity argon gas to 2100 ~ 2400 DEG C;Temperature plateau is being kept after constant temperature
In the case of gradually reduce air pressure, at this time powder source start to sublime up into and start to grow at seed crystal, crystal growth carries out to a certain extent
Finishing phase, is filled with argon gas and stops the growth that heating terminates SiC crystal, finally complete crystal growth by annealing.
2. a kind of growing method of PVT methods growing large-size Semi-insulating silicon carbide mono-crystal according to claim 1, its feature
Being the preparation process of the SiC powder includes:C powder is put into graphite crucible before SiC is synthesized, 2200 DEG C ~ 2300
When sintering 3 is small under DEG C high vacuum, to reduce the gaseous impurity adsorbed in C powder and graphite crucible;By C powder and the uniform dispenser of Si particles
In crucible, air pressure is evacuated to 10-3Below Pa, is to slowly warm up to the gaseous impurity adsorbed in 1300 DEG C ~ 1400 DEG C discharge raw materials,
High-purity argon gas is filled with to 60000Pa ~ 80000Pa, be warming up to 2100 DEG C-~ 2150 DEG C;Stop heating after keeping the temperature 1h ~ 2h, obtain high
Pure SiC powder.
3. a kind of growing method of PVT methods growing large-size Semi-insulating silicon carbide mono-crystal according to claim 2, its feature
What C powder and Si particles described in being were selected is that the Si particles and particle diameter that particle diameter is 8N for 1 ~ 2mm or so purity are 70 ~ 90um left sides
Right purity is the C powder of 9N;The purity range of high-purity argon gas is 99.9990%-99.9996%.
4. a kind of growing method of PVT methods growing large-size Semi-insulating silicon carbide mono-crystal according to claim 3, its feature
It is that the shove charge vacuum step includes:After shove charge, after furnace chamber air pressure is evacuated to 10 ~ 15Pa using mechanical pump, using point
Air pressure is evacuated to 10 by son pump-3~10-4Pa。
5. a kind of growing method of PVT methods growing large-size Semi-insulating silicon carbide mono-crystal according to claim 4, its feature
It is that the despumation gas step includes:1300 DEG C ~ 1400 DEG C are to slowly warm up to, vacuum maintains in holding chamber
10-3~10-4Pa, the main purpose of this step are the foreign gas for excluding to adsorb in graphite crucible and SiC powder.
6. a kind of growing method of PVT methods growing large-size Semi-insulating silicon carbide mono-crystal according to claim 5, its feature
It is that the pressurization steps that are rapidly heated include:After despumation gas, as temperature raises, the equilibrium partial pressure of Si steam by
It is cumulative big, in order to suppress the decomposition of SiC seed crystals, high-purity argon gas is filled with before heating, by air pressure in furnace body maintain 60000Pa ~
Between 80000Pa, it is rapidly heated to 2200 DEG C ~ 2400 DEG C;The time range being rapidly heated that slowly heats up relatively is small for 2.5-3.5
When.
7. a kind of growing method of PVT methods growing large-size Semi-insulating silicon carbide mono-crystal according to claim 6, its feature
It is that the decompression constant temperature step includes:Heating power supply power is adjusted, makes temperature stabilization at 2200 DEG C ~ 2400 DEG C, opens butterfly
Valve, to avoid the occurrence of excessive temperature fluctuation so that constant temperature and pressure reduction are carried out at the same time;The pressure of constant temperature decompression is by 60000-
80000Pa drops to 1000-10000Pa, and dip time scope is when 8-12 is small.
8. a kind of growing method of PVT methods growing large-size Semi-insulating silicon carbide mono-crystal according to claim 7, its feature
It is that the crystal growth step includes:The growing environment of SiC crystal is constant temperature and pressure, stable gas pressure 1000Pa ~
10000Pa, the temperature of crucible bottom are appropriate to adjust the distance between raw material seed crystal, raw material liter in the range of 2200 DEG C ~ 2400 DEG C
Start to grow at China to seed crystal, grow high quality SiC single crystal.
9. a kind of growing method of PVT methods growing large-size Semi-insulating silicon carbide mono-crystal according to claim 8, its feature
It is that the finishing phase step includes:High-purity argon gas is filled with into furnace body, stops heating, terminates the growth of SiC single crystal.
10. a kind of growing method of PVT methods growing large-size Semi-insulating silicon carbide mono-crystal according to claim 9, it is special
Sign is that the annealing steps include:After completing crystal growth, temperature is persistently filled with argon in the range of 2000 DEG C ~ 2100 DEG C
Gas, control stove cavity pressure is between 10000Pa ~ 20000Pa, and soaking time is 10 ~ 15h, then with 10 ~ 20 DEG C/min
Carborundum crystals are taken out after being slowly dropped to room temperature, 2200 DEG C of annealing region arrives room temperature.
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