CN106012002B - A kind of preparation method of the N-type SiC substrate of the growth of off-axis substrate SiC crystal and high electricity uniformity - Google Patents
A kind of preparation method of the N-type SiC substrate of the growth of off-axis substrate SiC crystal and high electricity uniformity Download PDFInfo
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- CN106012002B CN106012002B CN201610389489.5A CN201610389489A CN106012002B CN 106012002 B CN106012002 B CN 106012002B CN 201610389489 A CN201610389489 A CN 201610389489A CN 106012002 B CN106012002 B CN 106012002B
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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
- C30B23/025—Epitaxial-layer growth characterised by the substrate
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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
-
- 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 relates to a kind of preparation methods of the N-type SiC substrate of the growth and high electricity uniformity of off-axis substrate SiC crystal.Using SiC seed crystals are biased to, the mechanism of its facet growth is controlled using the mode of asymmetric cohesive seed crystal, 20mmSiC monocrystal materials can be increased than normal diameter by being obtained by atmosphere deflector.The round as a ball work of asymmetry is carried out, obtains the SiC single crystal material of no facet.The N-type SiC single crystal substrate material of low-defect-density, electricity deviation below 3.5% can be obtained by the method for present aspect.
Description
Technical field
The N-type of growth and low-defect-density, high electricity uniformity the present invention relates to a kind of off-axis substrate SiC crystal
SiC single crystal substrate fabrication method, belongs to technical field of crystal growth.
Background technology
Silicon carbide is that third generation wide bandgap semiconductor represents, and it is excellent to have that energy gap is big, mobility is high, thermal conductivity is high etc.
Electricity thermal characteristic, become the ideal material for making high frequency, high-power, high temperature resistant and radioresistance device.In device development side
Face, silicon carbide blue-ray LED have been commercialized；The research and development of silicon carbide power device have become novel power semiconductor research and have opened
The mainstream of hair；Referring to CN104246979A " high voltage semiconductor device on SiC ".In terms of High temperature semiconductor device, utilize
The silicon carbide JFET and silicon carbide device that carbofrax material makes can be under without 600 DEG C of high temperature under any neck but cooling system
Normal work.With the further development of manufacturing silicon carbide semiconductor technology, the application of carbofrax material and device is more and more wide,
It rises in the fields such as white-light illuminating, automotive circuit diagram, radar communication, oil drilling, aerospace, nuclear reactor system and military equipment
To vital effect.
The court in need in the development of power device<11-20>Direction is 4 ° inclined, resistivity is served as a contrast less than 0.03Ohm-cm SiC
Bottom material, the court<11-20>There are two approach for the preparation of the inclined 4 ° of SiC substrates in direction：When using positive seeded growth, it is round as a ball
It is 4 ° of substrate materials with correction during cutting.The defects of this method is, in round as a ball and cutting, can cause crystal thickness loss,
It is higher to cut difficulty；Second is that using the seed crystal being biased to, it is directly grown to court<11-20>The inclined 4 ° of SiC crystals in direction；The crystalline substance of the program
Body grows the boundary for having facet growth and Step Growth pattern, is easy to cause the increase of micro-pipe and dislocation density, and be biased to growth
It can generate and promote slippage defect.Meanwhile the preparation method of the existing 4 ° of SiC substrates of above two, on the surface of SiC crystal all
It will appear facet (facet).The crystal of forward direction growth, facet (facet) appear in center；And the crystal of inclined 4 ° of growths is small
Face (facet) appears in edge-small side position of crystal.Due to the difference of mechanism of doping effect, the resistance of facet (facet) position
Rate is relatively low.The resistivity deviation of general facet position and other positions is more than 10%, and the resistivity deviation of so big degree is difficult
Meet the needs of high performance power device.
Invention content
For more than problems of the prior art, the present invention proposes a kind of growth side of off-axis substrate SiC crystal
Method and low-defect-density, the preparation method of high electricity uniformity N-type SiC substrate, can reduce its defect concentration, and will be electric
Deviation control is learned below 3.5%.
Term is explained：
The big side of seed crystal：In { 10-10 } face and it is parallel to<11-20>Direction.
The small side of seed crystal：In { 11-20 } face and it is parallel to<10-10>Direction, when SiC substrate Si is face-up, small side is big
On the left of side, and it is in 90 °.
Inclined 4 ° of SiC substrate：＜ 11-20 ＞ are biased in normal to a surface direction, with<0001>4 ° of angle.Also referred to as 4 degree of off-axis linings
Bottom.
PVT methods：Physical vapor transport is a kind of prior art of SiC crystal growth；This method includes carborundum powder
Distillation, the silicon carbide of distillation are transported to seed crystal, and crystallize in seeded growth face.
The angle theta of atmosphere deflector and thermal field central shaft：Refer to atmosphere deflector vertical section inner edge and thermal field center
The angle of axis.As shown in Figure 5.
Technical scheme is as follows：
A kind of growing method of off-axis substrate SiC crystal is as follows including step：
(1) seed crystal grown using the SiC substrate being biased to as SiC crystal, the SiC substrate of the deviation refers to and SiC
Crystal<11-20>Direction deflection angle is 2 °~8 °；
(2) seed crystal is sticked to using asymmetric bonding way on graphite crucible upper cover or seed crystal support；
(3) atmosphere deflector is provided in the small side side of seed crystal, blocking atmosphere is flowed to no seeded region, to assist seed crystal
The expanding growth of crystal of small side side；The angle of the atmosphere deflector and thermal field central shaft is 20~70 °；
(4) silicon carbide source powder is placed in crucible bottom, SiC crystal is grown using PVT methods, including：It is put after sealed crucible
Enter growth room, growth room's vacuum degree control is 1 × 10-6~1 × 10-8Mbar, to establish heat between silicon carbide source powder and seed crystal
The mode heating crucible of gradient is heated to 50-200 DEG C of the sublimation temperature more than of silicon carbide, with nitrogen as doped source, is made inclined
The N-type SiC single crystal at bushing bottom.
According to currently preferred, in above-mentioned steps (2), the asymmetric bonding way of seed crystal is：Make in the small side of seed crystal
Heart site is reduced to (0~0.8) r with thermal field central shaft distance, and wherein r is seed crystal small side center site when central symmetry is placed
With thermal field central shaft apart from distance.
According to currently preferred, in above-mentioned steps (3), the atmosphere deflector is graphite piece；It is further preferred that institute
It states atmosphere deflector and cuts shape in 100-180 °, up-narrow and down-wide horn mouth in 100-180 ° of arc panel or radian for radian
Plate.The atmosphere deflector can hinder atmosphere, so as to which polycrystalline be prevented to grow, to be conducive to seed crystal to the area transmissions of no seed crystal
The expanding growth of crystal of small side side.
According to currently preferred, in above-mentioned steps (3), the angle of the atmosphere deflector and thermal field central shaft is 40~
60°；Further preferred angle is 42~50 °, and most preferably angle is 45 °.
The fixed form of above-mentioned atmosphere deflector is according to circumstances selected, and can be fixed on by modes such as bonding, connectors
In crucible upper cover or seed crystal support.Currently preferred, the atmosphere deflector is manufactured into a single integrated structure with crucible upper cover.
Based on different technology paths, seed crystal is optionally fixed on graphite upper cover, graphite seed support or metal
On seed crystal support, seed crystal bonds scheme using technology generally in the art, repeats no more.
The technology of above step (4) PVT methods growth SiC crystal of the present invention does not add the equal with reference to state of the art of restriction
.Crucible used is graphite crucible.
The preparation method of a kind of low-defect-density, high electricity uniformity N-type SiC substrate includes the use of the above-mentioned side of the present invention
N-type SiC single crystal prepared by method, including step：
1st, it is asymmetrical to remove the expanding part in small side in round as a ball by the round as a ball SiC crystal for normal diameter of N-type SiC crystal
Crystal, so as to will remove along the small rim portion of seed crystal to the facet component of outgrowth；
2nd, the SiC crystal of normal diameter by cutting is adjusted, obtains the standard SiC substrate material of 4 ° of deviation.
Normal diameter described above is 2-8 inches (inch).
The technical characterstic and excellent results of the present invention：
During PVT grows SiC, the growth pattern of use is the center that graphite crucible is placed on thermal field.Due to temperature
Field is axial symmetry, and the central shaft of crucible is exactly thermal field central shaft.Lower Fig. 1 show the distribution map of thermal field after heating, black in figure
Color solid line is thermoisopleth, and white line with the arrow is thermal field central shaft.For axisymmetric thermal field, SiC crystal growth finishes
Afterwards, the interface of crystal is axisymmetric Raised key axis, shape such as thermoisopleth, and be centrally formed facet regions (facet) in crystal.
The growth pattern of facet regions can cause N impurity to be more easy to enter crystal, so that resistivity is unevenly distributed.For being biased to 4 °
Standard SiC seed crystals, there are two kinds of growth patterns, one is step stream growth pattern along growth step, and one kind is small
It looks unfamiliar long pattern.There are a large amount of dislocation and micro-pipes for facet growth pattern and step stream growth pattern juncture area.Due to thermal field
Central shaft and the normal angle of facet be always maintained at 4 °.As growth carries out, thermoisopleth becomes convex.Facet needs to move to center
So as to ensure the angle with thermal field central shaft.This can cause the interface area of two kinds of growth districts to become larger, i.e., high density dislocation and
Micro-pipe region becomes larger.Due to the difference of the mechanism of doping effect of the facet growth pattern and other region step stream growth patterns of crystal,
The resistivity deviation of general facet position and other positions is more than 10%.
In the present invention, using asymmetric cohesive seed crystal, atmosphere water conservancy diversion graphite piece and asymmetric round as a ball technical combinations come
Overcome the above problem.In single crystal growth process, the central shaft of thermal field is still at geometric center.Seed crystal bonds deviation center axle position
It puts.In growth course, crystal facet needs are displaced outwardly ensureing that its normal and the angle of thermal field central shaft are maintained at 4 °.
Atmosphere is hindered to the area transmissions of no seed crystal using atmosphere water conservancy diversion graphite piece, so as to which polycrystalline be prevented to grow, is conducive to
The expanding growth of monocrystalline.Compared with prior art, the advantage of the invention is that：
1st, the present invention is applied in combination using asymmetric seed crystal and atmosphere deflector graphite piece, effectively makes to produce in growth course
Raw crystal facet moves outside seeded region.After growth can very convenient ground roll fall facet regions, facet and step
Junctional area is flowed, so as to obtain the complete SiC substrate material of diameter.The normal diameter of N-type SiC crystal prepared than conventional method can
Increase 20mm.
2nd, the present invention eliminates facet area, facet and step stream outside seeded region when making inclined 4 ° of N-type SiC substrates
Junctional area, the defects of reducing entire crystal density, improve the resistivity evenness that substrate is made.Resistance on entire substrate
Rate deviation is no more than 3.5%.
Description of the drawings
Fig. 1 be PVT methods growth SiC heating after thermal field distribution map in crucible.Solid black lines in figure are thermoisopleth, white
Arrow is thermal field central shaft.
Fig. 2 is the crystal growth schematic diagram that the asymmetric seed crystal of the present invention bonds.Wherein, 1, SiC powders, 2, graphite crucible,
3rd, thermal field central axis, 4, the SiC crystal of growth, 5, facet push out shift-in journey (dash area), 6, atmosphere deflector, 7, seed
It is brilliant.
Fig. 3 is traditional symmetrical bonding seed crystal schematic diagram.In figure, 8, crucible upper cover；9th, the geometric center of crucible upper cover is (same
When be also thermal field central shaft), 10, the geometric center of seed crystal；11st, the big side of seed crystal；12nd, the small side of seed crystal；The centre bit on the small side of seed crystal
Put the geometric center distance L=r=50mm with crucible upper cover.
Fig. 4 is the asymmetric cohesive seed crystal schematic diagram of the present invention.
Fig. 5 is the schematic front view of atmosphere deflector graphite piece, and Fig. 6 is the stereoscopic schematic diagram of atmosphere deflector.
Fig. 7 be embodiment 2 prepare SiC substrate, number chip 06；Fig. 8 is SiC substrate prepared by embodiment 2, and number is brilliant
Piece 20.
Specific embodiment
The invention will be further described with reference to the accompanying drawings and examples.
The grower that embodiment 1 uses is monocrystal growing furnace, including growth room, graphite crucible, thermal insulation material and sensing
Heating system, growth room's side wall have water cooling plant, and water cooling plant is the sealing bimetallic tube that quartz glass is formed, in bimetallic tube
Cycle operation medium is water, and water temperature is kept constant in growth course；Seed crystal is fixed on graphite upper cover；Crucible and thermal insulation material are put
It puts in growth room, growth room can reach 1 × 10-6The vacuum degree of more than mbar.Related grower is referring to CN1554808A's
Embodiment 1 is herein included itself and the reconcilable partial content of the present invention in the present invention by reference.
As a comparison case, traditional symmetrical seed crystal that bonds is illustrated as shown in figure 3,4 inches of (r=50mm) SiC seed crystals 7 are right
The graphite crucible upper cover 8 for being bonded in diameter 150mm claimed.The center on the small side 11 of seed crystal and the geometric center 9 of crucible upper cover
Distance L=r=50mm.
Embodiment 1：4 inches of (expanding crystal is 120mm) inclined 4 ° of N-type SiC growths
By the asymmetrical graphite crucible upper cover 8 for being bonded in diameter 150mm of 4 inches of (r=50mm) SiC seed crystals 7, seed crystal is small
The center on side 11 and the geometric center 9 of crucible upper cover are apart from for L=30mm.As shown in Figure 4.
Atmosphere deflector 6 is graphite piece with crucible upper cover one, the atmosphere deflector be horizontal profile radian be 180 °,
Up-narrow and down-wide horn mouth cuts shape plate, as shown in Figure 5, Figure 6, atmosphere deflector plate face and thermal field central shaft angle theta=45 °.Gas
Atmosphere deflector graphite piece is located at the side on the small side of seed crystal.
High-purity silicon carbide powder 1500g of the purity not less than 5N is contained in as source material in graphite crucible.After sealing
Growth room is put into, deoxygenation, water harmful substance are gone using vacuum condition before growing；Growth room's vacuum degree control is 1 × 10-6~1 ×
10-8Mbar, thermal field condition are that the temperature in crucible at seed crystal is minimum, and the thermal field for having larger gradient in the direction of growth is distributed；Crystal
The isothermal distribution less parallel of radial direction of growing surface, center is minimum, edge highest.Silicon carbide source powder is heated to 2200 DEG C
Distillation is passed through nitrogen as doped source, and growth N-type SiC single crystal is (since crucible has certain porosity, by transmitting diffused sheet
Formula nitrogen enters growth chamber).Growth time 60h.After cooling, the crystal that growth finishes is taken out.
Crystal growth schematic diagram such as Fig. 2, SiC crystal 4 is constantly expanding outward along atmosphere deflector 6, until obtaining crystal
A diameter of 120mm.Since the central shaft of thermal field and the normal angle of facet are always maintained at 4 °.As growth carries out, facet is in life
It is moved outside seeded region in growth process, as shown in 5 dash areas in Fig. 2.
Embodiment 2：The preparation of 4 inches of inclined 4 ° of N-type SiC substrates
1st, the SiC crystal for the diameter 120mm for obtaining embodiment 1 carries out round as a ball processing, removes along the small rim portion of seed crystal
To the facet and juncture area of outgrowth, make a diameter of 100mm of SiC single crystal stick,
2nd, the SiC single crystal stick of a diameter of 100mm cut, ground and polishing, obtain inclined 4 ° of N-type SiC substrates.
Fig. 7, Fig. 8 are manufactured inclined 4 ° of N-types SiC substrate material photo, and number is respectively chip 06 and chip 20.
Inclined 4 ° of N-type SiC substrates that number is taken to be chip 06 and chip 20, carry out the test of resistivity, as a result as follows：Chip
Still there are remaining facet regions, 0.01792 ohm * centimetres of resistivity maximum value in 06 rightmost side, and minimum value is 0.01735 ohm of *
Centimetre, deviation 3.1%.And 20 facet regions of chip have been removed completely, 0.01996 ohm * centimetres of resistivity maximum value, most
Small value 0.01996, deviation 1.4%.It is demonstrated experimentally that inclined 4 ° of N-types SiC substrate resistivity evenness that this method makes, full wafer
Resistivity deviation on substrate is no more than 3.5%.
Claims (9)
1. a kind of growing method of off-axis substrate SiC crystal, as follows including step：
（1）The seed crystal grown using the SiC substrate of deviation as SiC crystal, the SiC substrate of the deviation refers to and SiC crystal<
11-20>Direction deflection angle is 2 ° ~ 8 °；
（2）The seed crystal is sticked to using asymmetric bonding way on graphite crucible upper cover or seed crystal support；
（3）Atmosphere deflector is provided in the small side side of seed crystal, blocking atmosphere is flowed to no seeded region, to assist the small side of seed crystal
The expanding growth of crystal of side；The angle of the atmosphere deflector and thermal field central shaft is 20 ~ 70 °；
（4）Silicon carbide source powder is placed in crucible bottom, SiC crystal is grown using PVT methods, including：Life is put into after sealed crucible
Long room, growth room's vacuum degree control is 1 × 10-6~1×10-8Mbar, to establish thermal gradient between silicon carbide source powder and seed crystal
Mode heating crucible, be heated to 50-200 DEG C of the sublimation temperature more than of silicon carbide, with nitrogen as doped source, off-axis lining be made
The N-type SiC single crystal at bottom.
2. the growing method of off-axis substrate SiC crystal as described in claim 1, it is characterised in that step（2）In, the seed
Brilliant asymmetric bonding way is：Seed crystal small side center site is made to be reduced to thermal field central shaft distance（0~0.8）During r, wherein r are
Seed crystal small side center site and thermal field central shaft distance when the heart is symmetrically placed.
3. the growing method of off-axis substrate SiC crystal as described in claim 1, it is characterised in that step（3）In, the gas
Atmosphere deflector cuts shape plate in 100-180 ° of arc panel or radian for radian in 100-180 °, up-narrow and down-wide horn mouth.
4. the growing method of off-axis substrate SiC crystal as described in claim 1, it is characterised in that step（3）In, the gas
Atmosphere deflector is graphite piece.
5. the growing method of off-axis substrate SiC crystal as described in claim 1 or 4, it is characterised in that step（3）In, institute
State atmosphere deflector manufactured with crucible upper cover it is into a single integrated structure.
6. the growing method of off-axis substrate SiC crystal as described in claim 1, it is characterised in that step（3）In, the gas
Atmosphere deflector normal direction and the angle of thermal field central shaft are 40 ~ 60 °.
7. the growing method of off-axis substrate SiC crystal as described in claim 1, it is characterised in that step（3）In, the gas
Atmosphere deflector normal direction and the angle of thermal field central shaft are 45 °.
8. a kind of preparation method of N-type SiC substrate includes the N-type SiC single crystal of any one of claim 1-7 the methods preparation,
Including step：
By the round as a ball SiC crystal for normal diameter of N-type SiC crystal, in round as a ball, the asymmetrical crystalline substance for removing the expanding part in small side
Body, so as to remove along the small rim portion of seed crystal to the facet component of outgrowth；
The SiC crystal of normal diameter by cutting is adjusted, obtains the SiC substrate material of 4 ° of deviation.
9. the preparation method of N-type SiC substrate as claimed in claim 8, it is characterised in that the normal diameter is 2-8 English
It is very little.
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| US11441235B2 (en) | 2018-12-07 | 2022-09-13 | Showa Denko K.K. | Crystal growing apparatus and crucible having a main body portion and a low radiation portion |
| CN111270305B (en) * | 2020-03-30 | 2021-02-19 | 山东天岳先进科技股份有限公司 | High-quality n-type silicon carbide and preparation method thereof |
| JP7245586B1 (en) * | 2022-06-02 | 2023-03-24 | 株式会社レゾナック | n-type SiC single crystal substrate |
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