CN107974712A - A kind of preparation method of Semi-insulating silicon carbide mono-crystal - Google Patents
A kind of preparation method of Semi-insulating silicon carbide mono-crystal Download PDFInfo
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- CN107974712A CN107974712A CN201711122061.5A CN201711122061A CN107974712A CN 107974712 A CN107974712 A CN 107974712A CN 201711122061 A CN201711122061 A CN 201711122061A CN 107974712 A CN107974712 A CN 107974712A
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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
- C30B29/36—Carbides
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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
Abstract
The invention belongs to technical field of crystal growth, and in particular to a kind of preparation method of Semi-insulating silicon carbide mono-crystal.The present invention by adulterating shallow energy level recipient element Group IIIA element in the feed, it is brilliant using doping SiC raw material length in crystal growing process, shallow energy level recipient element is introduced into SiC crystal, shallow energy level donor impurity is adequately compensated for so as to reach, realizes the semi-insulating characteristic of SiC crystal.Using introducing of the growing semi-insulated SiC crystal of the present invention without realizing high concentration spot defect by fast cooling, so as to reduce crystal stress, crystal quality is improved；The point defect of low concentration reduces the unstability of electric property；In addition, by controlling doping concentration, it is possible to achieve to the controllable adjustment of crystal resistivity.
Description
Technical field
The invention belongs to technical field of crystal growth, and in particular to a kind of preparation method of Semi-insulating silicon carbide mono-crystal.
Background technology
Carborundum (SiC) monocrystalline has broad stopband, high heat conductance, high critical breakdown strength and high saturated electrons drift speed
The advantages that, thus one of core material as third generation semiconductor.Wherein, semi-insulation SiC single crystalline substrate in high frequency can
Effectively reduce the dielectric loss of device and reduce ghost effect, therefore be the preferred material of high frequency, microwave device.
During common physical vapor transport (PVT) method growth single-crystal silicon carbide, due to raw material, thermal insulation material and growth
Electrically active impurity (such as nitrogen, boron, aluminium) in equipment containing high level.These impurity are not easy completely in crystal growing process
Remove and as crystal growth enters lattice position.Major impurity into lattice position is nitrogen impurity, its shallow energy introduced
Level position (E at 0.09eV under conduction bandC- 0.09eV), it is in n-type low-resistance characteristic to make crystal.
The SiC crystal for unintentionally carrying out Control of Impurities typically exhibits N-shaped conductive characteristic.This is because enter lattice position
Major impurity be nitrogen impurity, its shallow energy level position introduced (E at 0.09eV under conduction bandC- 0.09eV), make it in crystal
As shallow energy level donor impurity, unnecessary electronics is provided for SiC crystal.In addition, the N concentration entered in SiC crystal is much high
In entering the shallow energy level acceptor impurity in crystal, therefore the net carrier in crystal is mainly electronics, so that it is low to show N-shaped
Hinder characteristic.
Carried to realize the semi-insulating characteristic of carborundum crystals, it is necessary to reduce the nitrogen as shallow energy level alms giver with reducing
Flow sub- concentration.The research of CREE shows, the semi-insulating characteristic for realizing SiC crystal by introducing intrinsic point defects in crystal.This
It is due to that these intrinsic point defects can introduce the electronics that deep energy level capture shallow energy level alms giver discharges in forbidden band, so as to reduce
Net carrier concentration in SiC crystal, realizes its semi-insulating characteristic.But in the prior art, introducing is quickly cooled down by high temperature
Point defect, easily introduces larger thermal stress in crystal, causes crystal cleavage or substrate quality to be deteriorated；Point defect is easy at high temperature
Bury in oblivion in diffusion with compound.The point defect of high concentration may cause crystal electric property in subsequent epitaxial and device fabrication process
It is unstable.
The content of the invention
In view of the above-mentioned problems, the present invention proposes a kind of preparation method of Semi-insulating silicon carbide mono-crystal, the present invention by
Shallow energy level recipient element is adulterated in raw material, it is brilliant using doping SiC raw material length in crystal growing process, by shallow energy level recipient element
It is introduced into SiC crystal, shallow energy level donor impurity is adequately compensated for so as to reach, realizes the semi-insulating characteristic of SiC crystal.Cause
This, using introducing of the growing semi-insulated SiC crystal of the present invention without realizing high concentration spot defect by fast cooling, so as to reduce
Crystal stress, improves crystal quality；The point defect of low concentration reduces the unstability of electric property；In addition, pass through
Control doping concentration, it is possible to achieve to the controllable adjustment of crystal resistivity.
A kind of preparation method of Semi-insulating silicon carbide mono-crystal of the present invention, it is concretely comprised the following steps：
(1) Si powder is uniformly mixed with C powder, it is spare；
(2) Group IIIA element is placed in crystal vessel, it is spare；
(3) crystal vessel for containing Group IIIA element is placed on to the position of graphite crucible bottom centre, then will be mixed equal
Even Si powder and C powder is filled in graphite crucible, crystal vessel is embedded in Si powder and C powder；
(4) after graphite crucible is positioned in SiC Material synthesis stoves, burner hearth is sealed；
(5) pressure in burner hearth is evacuated to 10-3Pa and after keeping 2-5h, is progressively passed through protective atmosphere into furnace chamber；
(6) furnace pressure is promoted to by 600-800mbar with the speed of 30-50mbar/h, while with the speed of 10-20 DEG C/h
Temperature in burner hearth is promoted to 1900-2100 DEG C by rate, keeps 20-50h at this temperature, completes Material synthesis process；
(7) after Material synthesis process, stop heating furnace, after fire box temperature is reduced to room temperature naturally, open stove
Thorax takes out graphite crucible, you can obtains the SiC synthesis materials containing Group IIIA element；
(8) SiC single crystal growth is carried out using the SiC synthesis materials containing Group IIIA element.
In step (1), in order to make Si powder and C powder react the molar ratio 1 of generation SiC powders, Si powder and C powder completely：1 to
1.05:1.Excessive or height molar ratio can make Si powder react incomplete with C powder, cause in the SiC powders of synthesis containing remnants
Si powder or C powder, so as to influence the quality of SiC crystal grown using this raw material.
In step (2), in order to ensure Group IIIA Elements Atom in the SiC crystal grain of synthesis accounting 1016-1018cm-3It
Between, Group IIIA element and the molar ratio of C powder are controlled 10-6:1 to 10-4:Between 1；Too high or too low molar ratio will cause to close
Into SiC powders in the doping Group IIIA concentration of element that contains it is excessive or insufficient, cause the electroactive shallow energy level that doping introduces by
Main impurity can not be fully compensated with the shallow energy level donor impurity in carborundum, and the carborundum crystals of growth can not realize semi-insulating spy
Property.
It is well known that Group IIIA element is B, Al, Ga, In, Tl, it is larger to be limited to the atomic size of Ga, In, Tl, is not easy
Doping enters in crystal；B and Al be with the immediate recipient element of C, Si atomic size, be easiest to doping and into crystal occupy crystalline substance
Case is put and contributes hole, so that the electric property of SiC crystal is influenced, therefore Group IIIA element of the present invention is B or Al.
In step (3), the crystal vessel of Group IIIA element is placed on to the position of graphite crucible bottom centre, so that graphite
The Group IIIA element held in container can fully be discharged and is uniformly doped into the SiC powders of synthesis along temperature gradient.
The crystal vessel of the present invention i.e. container made of graphite material, is container commonly used in the art.
In step (5), vacuum keeps 10 in furnace chamber-3Pa and when keeping 2-5 small, to remove the residual air in furnace chamber and have
Evil impurity.Too low vacuum or too short time can cause remaining control and objectionable impurities to remove not exclusively；Excessive vacuum
Degree or long time can cause cost increase, efficiency to reduce
In step (6), the pressure 600-800mabr of holding furnace intracavitary, 1900-2100 DEG C of temperature, the reaction time, 20-50 was small
When, so that Si powder and C powder fully react.Too low pressure, excessive temperature, long time can cause overreact, produce
SiC powders decompose the problems such as carbonization again；Excessive pressure, too low temperature, that the too short time can produce reaction is incomplete
Problem.
SiC single crystal growth is carried out using the SiC synthesis materials containing Group IIIA element, physical carbon burdening can be used
(PVT) known conditions or parameter of conventionally fabricated scheme carry out crystal growth, shape, crystal growth temperature from graphite crucible
The influence of degree and pressure, protective atmosphere and crystal growth rate etc., specifically may be referred to United States Patent (USP) No.RE34861 and patent
CN197364A。
In crystal growing process of the present invention, introduced in SiC raw materials and have electroactive Group IIIA, Group IIIA element with
The distillation of SiC material and discharge, and participate in SiC single crystal growth course, occupy the lattice position of Si and C atoms.Due to doping
The electroactive acceptor impurity of Group IIIA being introduced into directly by being mutually compensated for shallow energy level alms giver N remaining in carborundum crystals, from
And carrier concentration concentration is reduced, improve the resistivity of crystal.
The present invention adulterates the concentration of the shallow energy level recipient element introduced by being controlled in SiC synthesis materials, can be very good
Control is incorporated into the concentration of the shallow energy level recipient element in crystal, and then can obtain the controllable semi-insulation SiC monocrystalline of resistivity.
The present invention need not introduce intrinsic point defects by fast cooling process, reduce in SiC single crystal because of temperature shock
Caused by internal stress, reduce the cracking risk of monocrystalline processing, improve the processing quality of substrate；Can be by adjusting in raw material
The shallow energy level recipient element concentration of doping realizes the semi-insulating characteristic to SiC crystal；It is incorporated into by control shallow in raw material
The concentration of energy level acceptor impurity, can obtain the controllable SiC single crystal of resistivity.
Embodiment
Embodiment 1
A kind of preparation method for hindering single-crystal silicon carbide, it is concretely comprised the following steps：
(1) Si powder is uniformly mixed with C powder, it is spare；
(2) Group IIIA element is placed in crystal vessel, it is spare；
(3) crystal vessel for holding Group IIIA element is placed on to the position of graphite crucible bottom centre, then will mixing
Uniform Si powder and C powder are filled in graphite crucible, crystal vessel is embedded in Si powder and C powder；
(4) after graphite crucible is positioned in SiC Material synthesis stoves, burner hearth is sealed；
(5) pressure in burner hearth is evacuated to 10-3Pa and after keeping 2h, is progressively passed through protective atmosphere into furnace chamber；
(6) furnace pressure is promoted to by 600mbar with the speed of 40mbar/h, while with the speed of 20 DEG C/h by burner hearth
Temperature be promoted to 2000 DEG C, keep 20h at this temperature, complete Material synthesis process；
(7) after Material synthesis process, stop heating furnace, after fire box temperature is reduced to room temperature naturally, open stove
Thorax takes out graphite crucible, you can obtains the SiC synthesis materials containing Group IIIA element；
(8) SiC single crystal growth is carried out using the SiC synthesis materials containing Group IIIA element.
The Si powder and the molar ratio of C powder are 1.01:1.
The Group IIIA element is Ge.
The molar ratio of the Group IIIA element and C powder is 10-5:1。
The SiC single crystal substrate finally obtained is showed as follows in the form of resistivity：
Overall resistivity is higher than 1E12 Ω cm, the resistivity average value 1.3E11 Ω cm that can be monitored, median
1.3E11 Ω cm, substrate have excellent half insulation energy.
Embodiment 2
A kind of preparation method of Semi-insulating silicon carbide mono-crystal, it is concretely comprised the following steps：
(1) Si powder is uniformly mixed with C powder, it is spare；
(2) Group IIIA element is placed in crystal vessel, it is spare；
(3) crystal vessel for holding Group IIIA element is placed on to the position of graphite crucible bottom centre, then will mixing
Uniform Si powder and C powder are filled in graphite crucible, crystal vessel is embedded in Si powder and C powder；
(4) after graphite crucible is positioned in SiC Material synthesis stoves, burner hearth is sealed；
(5) pressure in burner hearth is evacuated to 10-3Pa and after keeping 3h, is progressively passed through protective atmosphere into furnace chamber；
(6) furnace pressure is promoted to by 800mbar with the speed of 30mbar/h, while with the speed of 20 DEG C/h by burner hearth
Temperature be promoted to 2100 DEG C, keep 50h at this temperature, complete Material synthesis process；
(7) after Material synthesis process, stop heating furnace, after fire box temperature is reduced to room temperature naturally, open stove
Thorax takes out graphite crucible, you can obtains the SiC synthesis materials containing Group IIIA element；
(8) SiC single crystal growth is carried out using the SiC synthesis materials containing IVA races element.
The Si powder and the molar ratio of C powder are 1.02:1.
The Group IIIA element is Sn.
The molar ratio of the Group IIIA element and C powder is 10-6:1。
The SiC single crystal substrate finally obtained is showed as follows in the form of resistivity：
Overall resistivity is higher than 1E12 Ω cm, the resistivity average value 3.2E11 Ω cm that can be monitored, median
3.2E11 Ω cm, substrate have excellent half insulation energy.
Embodiment 3
A kind of preparation method of Semi-insulating silicon carbide mono-crystal, it is concretely comprised the following steps：
(1) Si powder is uniformly mixed with C powder, it is spare；
(2) Group IIIA element is placed in crystal vessel, it is spare；
(3) crystal vessel for holding Group IIIA element is placed on to the position of graphite crucible bottom centre, then will mixing
Uniform Si powder and C powder are filled in graphite crucible, crystal vessel is embedded in Si powder and C powder；
(4) after graphite crucible is positioned in SiC Material synthesis stoves, burner hearth is sealed；
(5) pressure in burner hearth is evacuated to 10-3Pa and after keeping 4h, is progressively passed through protective atmosphere into furnace chamber；
(6) furnace pressure is promoted to by 700mbar with the speed of 50mbar/h, while with the speed of 15 DEG C/h by burner hearth
Temperature be promoted to 1900 DEG C, keep 30h at this temperature, complete Material synthesis process；
(7) after Material synthesis process, stop heating furnace, after fire box temperature is reduced to room temperature naturally, open stove
Thorax takes out graphite crucible, you can obtains the SiC synthesis materials containing IVA races element；
(8) SiC single crystal growth is carried out using the SiC synthesis materials containing Group IIIA element.
The Si powder and the molar ratio of C powder are 1.03:1.
The Group IIIA element is Sn.
The molar ratio of the Group IIIA element and C powder is 10-4:1。
The SiC single crystal substrate finally obtained is showed as follows in the form of resistivity：
Overall resistivity is higher than 1E12 Ω cm, the resistivity average value 3.1E11 Ω cm that can be monitored, median
3.0E11 Ω cm, substrate have excellent half insulation energy.
Embodiment 4
A kind of preparation method of Semi-insulating silicon carbide mono-crystal, it is concretely comprised the following steps：
(1) Si powder is uniformly mixed with C powder, it is spare；
(2) Group IIIA element is placed in crystal vessel, it is spare；
(3) crystal vessel for holding Group IIIA element is placed on to the position of graphite crucible bottom centre, then will mixing
Uniform Si powder and C powder are filled in graphite crucible, crystal vessel is embedded in Si powder and C powder；
(4) after graphite crucible is positioned in SiC Material synthesis stoves, burner hearth is sealed；
(5) pressure in burner hearth is evacuated to 10-3Pa and after keeping 5h, is progressively passed through protective atmosphere into furnace chamber；
(6) furnace pressure is promoted to by 650mbar with the speed of 45mbar/h, while with the speed of 10 DEG C/h by burner hearth
Temperature be promoted to 1950 DEG C, keep 40h at this temperature, complete Material synthesis process；
(7) after Material synthesis process, stop heating furnace, after fire box temperature is reduced to room temperature naturally, open stove
Thorax takes out graphite crucible, you can obtains the SiC synthesis materials containing Group IIIA element；
(8) SiC single crystal growth is carried out using the SiC synthesis materials containing Group IIIA element.
The Si powder and the molar ratio of C powder are 1.04:1.
The Group IIIA element is Ge.
The molar ratio of the Group IIIA element and C powder is 10-6:1。
The SiC single crystal substrate finally obtained is showed as follows in the form of resistivity：
Overall resistivity is higher than 1E12 Ω cm, the resistivity average value 3.0E11 Ω cm that can be monitored, median
3.1E11 Ω cm, substrate have excellent half insulation energy.
Embodiment 5
A kind of preparation method of Semi-insulating silicon carbide mono-crystal, it is concretely comprised the following steps：
(1) Si powder is uniformly mixed with C powder, it is spare；
(2) Group IIIA element is placed in crystal vessel, it is spare；
(3) crystal vessel for holding Group IIIA element is placed on to the position of graphite crucible bottom centre, then will mixing
Uniform Si powder and C powder are filled in graphite crucible, crystal vessel is embedded in Si powder and C powder；
(4) after graphite crucible is positioned in SiC Material synthesis stoves, burner hearth is sealed；
(5) pressure in burner hearth is evacuated to 10-3Pa and after keeping 3.5h, is progressively passed through protective atmosphere into furnace chamber；
(6) furnace pressure is promoted to by 750mbar with the speed of 35mbar/h, while with the speed of 20 DEG C/h by burner hearth
Temperature be promoted to 1900 DEG C, keep 35h at this temperature, complete Material synthesis process；
(7) after Material synthesis process, stop heating furnace, after fire box temperature is reduced to room temperature naturally, open stove
Thorax takes out graphite crucible, you can obtains the SiC synthesis materials containing Group IIIA element；
(8) SiC single crystal growth is carried out using the SiC synthesis materials containing Group IIIA element.
The Si powder and the molar ratio of C powder are 1.05:1.
The Group IIIA element is Sn.
The molar ratio of the Group IIIA element and C powder is 10-4:1。
The SiC single crystal substrate finally obtained is showed as follows in the form of resistivity：
Overall resistivity is higher than 1E12 Ω cm, and substrate has excellent half insulation energy.
Claims (4)
- A kind of 1. preparation method of Semi-insulating silicon carbide mono-crystal, it is characterised in that：It is concretely comprised the following steps：(1) Si powder is uniformly mixed with C powder, it is spare；(2) Group IIIA element is placed in crystal vessel, it is spare；(3) crystal vessel for containing Group IIIA element is placed on the position of graphite crucible bottom centre, then will be uniformly mixed Si powder and C powder are filled in graphite crucible, crystal vessel is embedded in Si powder and C powder；(4) after graphite crucible is positioned in SiC Material synthesis stoves, burner hearth is sealed；(5) pressure in burner hearth is evacuated to 10-3Pa and after keeping 2-5h, is progressively passed through protective atmosphere into furnace chamber；(6) furnace pressure is promoted to by 600-800mbar with the speed of 30-50mbar/h, while will with the speed of 10-20 DEG C/h Temperature in burner hearth is promoted to 1900-2100 DEG C, keeps 20-50h at this temperature, completes Material synthesis process；(7) after Material synthesis process, stop heating furnace, after fire box temperature is reduced to room temperature naturally, open burner hearth and take Go out graphite crucible, you can obtain the SiC synthesis materials containing Group IIIA element；(8) SiC single crystal growth is carried out using the SiC synthesis materials containing Group IIIA element.
- A kind of 2. preparation method of Semi-insulating silicon carbide mono-crystal according to claim 1, it is characterised in that：The Si powder Molar ratio with C powder is 1-1.05:1.
- A kind of 3. preparation method of Semi-insulating silicon carbide mono-crystal according to claim 1, it is characterised in that：The IIIA Race's element is B or Al.
- A kind of 4. preparation method of Semi-insulating silicon carbide mono-crystal according to claim 1, it is characterised in that：The IIIA The molar ratio of race's element and C powder is 10-6:1 to 10-4:Between 1.
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| PCT/CN2018/084387 WO2019095632A1 (en) | 2017-11-14 | 2018-04-25 | Method for preparing semi-insulating silicon carbide single crystal |
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| CN109722712A (en) * | 2019-03-12 | 2019-05-07 | 广州南砂晶圆半导体技术有限公司 | A kind of method of the Uniform Doped of SiC single crystal metal impurities |
| CN111270305A (en) * | 2020-03-30 | 2020-06-12 | 山东天岳先进材料科技有限公司 | High-quality n-type silicon carbide and preparation method thereof |
| US11046582B2 (en) | 2019-11-11 | 2021-06-29 | Industrial Technology Research Institute | Method of purifying silicon carbide powder |
| CN114790573A (en) * | 2022-03-09 | 2022-07-26 | 山东大学 | Growth method of p-type SiC with high doping uniformity |
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| CN109722712A (en) * | 2019-03-12 | 2019-05-07 | 广州南砂晶圆半导体技术有限公司 | A kind of method of the Uniform Doped of SiC single crystal metal impurities |
| CN109722712B (en) * | 2019-03-12 | 2020-06-12 | 广州南砂晶圆半导体技术有限公司 | Method for uniformly doping SiC single crystal metal impurities |
| US11046582B2 (en) | 2019-11-11 | 2021-06-29 | Industrial Technology Research Institute | Method of purifying silicon carbide powder |
| CN111270305A (en) * | 2020-03-30 | 2020-06-12 | 山东天岳先进材料科技有限公司 | High-quality n-type silicon carbide and preparation method thereof |
| CN114790573A (en) * | 2022-03-09 | 2022-07-26 | 山东大学 | Growth method of p-type SiC with high doping uniformity |
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| WO2019095632A1 (en) | 2019-05-23 |
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