CN106012002A - Method for growth of SiC crystal for off-axis substrate and method for preparing N type SiC substrate with high electric uniformity - Google Patents
Method for growth of SiC crystal for off-axis substrate and method for preparing N type SiC substrate with high electric uniformity Download PDFInfo
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- CN106012002A CN106012002A CN201610389489.5A CN201610389489A CN106012002A CN 106012002 A CN106012002 A CN 106012002A CN 201610389489 A CN201610389489 A CN 201610389489A CN 106012002 A CN106012002 A CN 106012002A
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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 invention relates to a method for growth of a SiC crystal for an off-axis substrate and a method for preparing an N type SiC substrate with high electric uniformity. A deviating SiC seed crystal is adopted, a mechanism of controlling facet growth by a seed crystal asymmetric bonding way is used, and a SiC single-crystal material having the diameter increased by 20 mm than a standard diameter is obtained through an atmosphere guide plate. The asymmetrical rounding work is performed, and the SiC single-crystal material without facets is obtained. The N type SiC single-crystal substrate material with low defect density and electrical deviation of 3.5% or less can be obtained by the method.
Description
Technical field
The present invention relates to growth and fabricating low-defect-density, N-type SiC of high electricity uniformity of a kind of off-axis substrate SiC crystal
Single crystalline substrate preparation method, belongs to technical field of crystal growth.
Background technology
Carborundum is that third generation wide bandgap semiconductor represents, and has the excellent electricity such as energy gap is big, mobility is high, thermal conductivity is high
Learn thermal characteristic, become making high frequency, high-power, the high temperature resistant and ideal material of radioprotective device.In terms of device development,
The commercialization of carborundum blue-ray LED；The research and development of silicon carbide power device have become Novel power semiconductor research and development
Main flow；See CN104246979A " high voltage semiconductor device on SiC ".In terms of High temperature semiconductor device, utilize
Carborundum JFET and silicon carbide device that carbofrax material makes can be without under 600 DEG C of high temperature under any neck but cooling system
Normal work.Along with the further development of manufacturing silicon carbide semiconductor technology, carbofrax material is more and more wide with the application of device,
The fields such as white-light illuminating, automotive circuit diagram, radar communication, oil drilling, Aero-Space, nuclear reactor system and military equipment
Play vital effect.
There is a need to towards inclined 4 ° of<11-20>direction in the development of power device, resistivity is less than 0.03Ohm-cm SiC substrate material,
The preparation of the inclined 4 ° of SiC substrate in described court<11-20>direction has two approach: one is to use forward seeded growth, round as a ball and cutting
Time correct be 4 ° of backing materials.The defect of the method is, round as a ball with when cutting, can cause the loss of crystal thickness, cutting
Difficulty is higher；Two is the seed crystal using deflection, and direct growth is towards the inclined 4 ° of SiC crystal in<11-20>direction；The crystal of the program
Growth has facet growth and the boundary of Step Growth pattern, is easily caused the increase of micro-pipe and dislocation density, and deflection growth can be produced
Give birth to and promote slippage defect.Meanwhile, the preparation method of the existing 4 ° of SiC substrate of above two, all can on the surface of SiC crystal
Little (facet) occurs.The crystal of forward growth, little (facet) occurs in center；And inclined 4 ° growth crystal little
Face (facet) occurs in the little Bian position, edge of crystal.Due to the difference of mechanism of doping effect, the resistance of little (facet) position
Rate is on the low side.The resistivity deviation of the least position and other positions is more than 10%, and the resistivity deviation of the biggest degree is difficult to full
The needs of foot high performance power device.
Summary of the invention
For above problems of the prior art, the present invention proposes the growing method of a kind of off-axis substrate SiC crystal, with
And fabricating low-defect-density, the preparation method of high electricity uniformity N-type SiC substrate, its defect concentration can be reduced, and electricity is inclined
Difference controls below 3.5%.
Term is explained:
The big limit of seed crystal: { in 10-10} face and be parallel to<11-20>direction.
The little limit of seed crystal: { in 11-20} face and be parallel to<10-10>direction, when SiC substrate Si faces up, little limit is left on big limit
Side, and in 90 °.
The SiC substrate of inclined 4 °: normal to a surface direction deflection ＜ 11-20 ＞, with<0001>angle 4 °.Also referred to as 4 degree off-axis linings
The end.
PVT method: physical vapor transport, is the prior art of a kind of SiC crystal growth；The method includes the liter of carborundum powder
China, the carborundum of distillation be transported to seed crystal, and crystallize in seeded growth face.
Atmosphere deflector and the angle theta of temperature field central shaft: refer to the folder of atmosphere deflector vertical section inner edge and temperature field central shaft
Angle.As shown in Figure 5.
Technical scheme is as follows:
The growing method of a kind of off-axis substrate SiC crystal, comprises the following steps that
(1) using the seed crystal that the SiC substrate of deflection grows as SiC crystal, the SiC substrate of described deflection refers to brilliant with SiC
Body<11-20>direction deflection angle is 2 °～8 °；
(2) the asymmetric bonding way of described seed crystal employing is bonded on graphite crucible upper cover or seed crystal support；
(3) it is provided with atmosphere deflector in side, seed crystal little limit, stops that atmosphere flows to without seeded region, to assist the little limit of seed crystal
The expanding growth of crystal of side；Described atmosphere deflector is 20～70 ° with the angle of temperature field central shaft；
(4) silicon carbide source powder is placed in crucible bottom, uses PVT method growth SiC crystal, including: put into after sealed crucible
Growth room, growth room's vacuum degree control is 1 × 10-6～1 × 10-8Mbar, to set up thermal gradient between silicon carbide source powder and seed crystal
Mode heating crucible, be heated to above 50-200 DEG C of the sublimation temperature of carborundum, with nitrogen as doped source, prepare off-axis lining
The N-type SiC single crystal at the end.
According to currently preferred, in above-mentioned steps (2), the asymmetric bonding way of described seed crystal is: make seed crystal little limit centre bit
Point is reduced to (0～0.8) r with temperature field central shaft distance, and wherein r is the site, seed crystal little Bian center during centrosymmetry placement and temperature
Field central shaft distance distance.
According to currently preferred, in above-mentioned steps (3), described atmosphere deflector is graphite piece；It is further preferred that it is described
Atmosphere deflector is radian at the arc of 100-180 °, or radian 100-180 °, up-narrow and down-wide horn mouth cut shape plate.
This atmosphere deflector can hinder atmosphere to not having the area transmissions of seed crystal, thus prevents the little limit of the growth of polycrystalline, beneficially seed crystal
The expanding growth of crystal of side.
According to currently preferred, in above-mentioned steps (3), described atmosphere deflector is 40～60 ° with the angle of temperature field central shaft；
Further preferably 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 crucible by modes such as bonding, connectors
On lid or seed crystal support.Currently preferred, described atmosphere deflector and crucible upper cover are made into integrative-structure.
Based on different technology paths, optionally seed crystal is fixed on graphite upper cover, graphite seed torr or the seed crystal support of metal
On, seed crystal bonding scheme uses technology generally in the art, repeats no more.
Above step of the present invention (4) PVT method growth SiC crystal technology do not add restriction all with reference to state of the art.
Crucible used is graphite crucible.
A kind of fabricating low-defect-density, the preparation method of high electricity uniformity N-type SiC substrate, including using said method system of the present invention
Standby N-type SiC single crystal, including step:
1, by round as a ball for the N-type SiC crystal SiC crystal for normal diameter, round as a ball in, the asymmetrical expanding part in little limit of removing
Crystal, thus will remove along the little rim portion of seed crystal to the facet component of outgrowth；
2, the SiC crystal of normal diameter is adjusted by cutting, it is thus achieved that be partial to the standard SiC substrate material of 4 °.
The above normal diameter is 2-8 inch (inch).
The technical characterstic of the present invention and excellent results:
During PVT growth SiC, the growth pattern of employing is the center that graphite crucible is placed on temperature field.Owing to temperature field is
Axial symmetry, the central shaft of crucible is exactly temperature field central shaft.Lower Fig. 1 is the scattergram of warm field after showing heating, and the black in figure is real
Line is isothermal line, and the white line of band arrow is temperature field central shaft.For axisymmetric temperature field, after SiC crystal growth,
The interface of crystal is axisymmetric Raised key axis, shape such as isothermal line, and is centrally formed facet regions (facet) at crystal.Little
The growth pattern in region, face can cause N impurity to be more easy to enter crystal, so that resistivity skewness.For deflection 4 °
Standard SiC seed crystal, there are two kinds of growth patteries in it, one is the step stream growth pattern along growth step, and one is little
Look unfamiliar long pattern.There is substantial amounts of dislocation and micro-pipe in facet growth pattern and step stream growth pattern juncture area.Due to temperature field
The central shaft normal angle with little is always maintained at 4 °.Along with growth is carried out, isothermal line becomes convex.Little needs move to center
Thus ensure and the angle of temperature field central shaft.This can make the interface area of two kinds of growth districts become big, i.e. high density dislocation and micro-
Territory, area under control becomes big.Facet growth pattern and the mechanism of doping effect of other region step stream growth patteries different, typically due to crystal
The resistivity deviation of little position and other positions is more than 10%.
In the present invention, use asymmetric bonding seed crystal, atmosphere water conservancy diversion graphite piece and asymmetric round as a ball technology groups is incompatible overcome on
State problem.In single crystal growth process, the central shaft of temperature field is still at geometric center.Seed crystal bonding off-center shaft position.?
In growth course, crystal facet needs to be displaced outwardly thus ensures that its normal is maintained at 4 ° with the angle of temperature field central shaft.Use
Atmosphere water conservancy diversion graphite piece hinders atmosphere to not having the area transmissions of seed crystal, thus prevents the growth of polycrystalline, and beneficially monocrystalline expands
Diameter growth.Compared with prior art, it is an advantage of the current invention that:
1, the present invention uses asymmetric seed crystal and atmosphere deflector graphite piece to be applied in combination, and effectively makes the crystalline substance produced in growth course
Body is little to be moved outside seeded region.Facet regions, little and step stream junctional area can be fallen by very convenient ground roll after growth,
Thus obtain the SiC substrate material that diameter is complete.The normal diameter of the N-type SiC crystal prepared than traditional method can increase 20mm.
2, the present invention is when making inclined 4 ° of N-type SiC substrate, eliminates Wai little Mian district, seeded region, little and step stream
Junctional area, reduces the defect concentration of whole crystal, improves the resistivity evenness making substrate.Resistance on entire substrate
Rate deviation is less than 3.5%.
Accompanying drawing explanation
Fig. 1 be PVT method growth SiC heating after temperature field pattern in crucible.Solid black lines in figure is isothermal line, white arrow
Head is temperature field central shaft.
Fig. 2 is the crystal growth schematic diagram of the present invention asymmetric seed crystal bonding.Wherein, 1, SiC powder, 2, graphite crucible, 3,
Temperature field central axis, 4, the SiC crystal of growth, 5, the little passage process (dash area) that faces out, 6, atmosphere deflector, 7,
Seed crystal.
Fig. 3 is traditional symmetrical bonding seed crystal schematic diagram.In figure, 8, crucible upper cover；9, the geometric center of crucible upper cover is (same
Time be also temperature field central shaft), 10, the geometric center of seed crystal；11, the big limit of seed crystal；12, the little limit of seed crystal；The center on the little limit of seed crystal
Position and geometric center distance L=r=50mm of crucible upper cover.
Fig. 4 is the asymmetric bonding 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 schematic perspective view of atmosphere deflector.
Fig. 7 is the SiC substrate of embodiment 2 preparation, numbering wafer 06；Fig. 8 is the SiC substrate of embodiment 2 preparation, numbering
Wafer 20.
Detailed description of the invention
The invention will be further described with embodiment below in conjunction with the accompanying drawings.
The grower that embodiment 1 uses is monocrystal growing furnace, heats including growth room, graphite crucible, insulation material and sensing
System, growth room's sidewall has water cooling plant, water cooling plant to be the sealing bimetallic tubes that quartz glass is constituted, the circulation in bimetallic tube
Working media is water, and water temperature keeps constant in growth course；Seed crystal is fixed on graphite upper cover；Crucible and insulation material are placed on
In growth room, growth room can reach 1 × 10-6The vacuum of more than mbar.Relevant grower sees the reality of CN1554808A
Execute example 1, it is comprised in the present invention with the reconcilable partial content of the present invention by quoting at this.
As a comparison case, traditional symmetrical bonding seed crystal signal is as it is shown on figure 3, by right for 4 inches of (r=50mm) SiC seed crystals 7
The graphite crucible upper cover 8 being bonded in diameter 150mm claimed.The center on the little limit of seed crystal 11 and the geometric center 9 of crucible upper cover
Distance L=r=50mm.
Embodiment 1:4 inch (crystal is expanding for 120mm) inclined 4 ° of N-types SiC growth
By 4 inches of asymmetrical graphite crucible upper covers 8 being bonded in diameter 150mm of (r=50mm) SiC seed crystal 7, the little limit of seed crystal
The geometric center 9 of the center of 11 and crucible upper cover is apart from for L=30mm.As shown in Figure 4.
Atmosphere deflector 6 is and the graphite piece of crucible upper cover one, this atmosphere deflector be horizontal profile radian be 180 °, on
Narrow lower wide horn mouth cuts shape plate, as shown in Figure 5, Figure 6, atmosphere deflector plate face and temperature central shaft angle theta=45 °, field.Gas
Atmosphere deflector graphite piece is positioned at the side on the little limit of seed crystal.
The high-purity silicon carbide powder 1500g that purity is not less than 5N is contained in graphite crucible as source material.Life is put into after sealing
Long room, uses vacuum condition to remove deoxygenation, water harmful substance before growth；Growth room's vacuum degree control is 1 × 10-6～1 × 10-8Mbar,
Temperature field condition is that temperature at seed crystal is minimum in crucible, and the direction of growth has the warm field distribution of bigger gradient；Crystal growing surface
The most isothermal distribution less parallel, center is minimum, and edge is the highest.Silicon carbide source powder is heated to 2200 DEG C of distillations, is passed through
Nitrogen (owing to crucible has certain porosity, is entered by transmission diffusion way nitrogen as doped source, growth N-type SiC single crystal
Enter growth chamber).Growth time 60h.After cooling, take out the crystal that growth is complete.
Crystal growth schematic diagram such as Fig. 2, SiC crystal 4 is the most expanding along atmosphere deflector 6, until it is straight to obtain crystal
Footpath is 120mm.Owing to the temperature central shaft of field is always maintained at 4 ° with the normal angle of little.Along with growth is carried out, little in growth
During move outside seeded region, as shown in 5 dash areas in Fig. 2.
The preparation of the inclined 4 ° of N-type SiC substrate of embodiment 2:4 inch
1, the SiC crystal of diameter 120mm embodiment 1 obtained carries out round as a ball processing, remove along the little rim portion of seed crystal to
Little of outgrowth and juncture area, make the SiC single crystal a diameter of 100mm of rod,
2, carry out cutting, grinding and polishing by the SiC single crystal rod of a diameter of 100mm, it is thus achieved that inclined 4 ° of N-type SiC substrate.
Fig. 7, Fig. 8 are the inclined 4 ° of N-type SiC substrate material photos made, and numbering is respectively wafer 06 and wafer 20.
Taking inclined 4 ° of N-type SiC substrate of numbered wafer 06 and wafer 20, carry out the test of resistivity, result is as follows: brilliant
Still there is the facet regions of remnants sheet 06 rightmost side, and resistivity maximum 0.01792 ohm * centimetre, minima is 0.01735 Europe
Nurse * centimetre, deviation is 3.1%.And wafer 20 facet regions is removed the most completely, resistivity maximum 0.01996 ohm * li
Rice, minima 0.01996, deviation is 1.4%.It is demonstrated experimentally that inclined 4 ° of N-type SiC substrate resistivity that this method makes are equal
Even property, the resistivity deviation on entire substrate is less than 3.5%.
Claims (8)
1. a growing method for off-axis substrate SiC crystal, comprises the following steps that
(1) using the seed crystal that the SiC substrate of deflection grows as SiC crystal, the SiC substrate of described deflection refers to brilliant with SiC
Body<11-20>direction deflection angle is 2 °～8 °；
(2) the asymmetric bonding way of described seed crystal employing is bonded on graphite crucible upper cover or seed crystal support；
(3) it is provided with atmosphere deflector in side, seed crystal little limit, stops that atmosphere flows to without seeded region, to assist the little limit of seed crystal
The expanding growth of crystal of side；Described atmosphere deflector is 20～70 ° with the angle of temperature field central shaft；
(4) silicon carbide source powder is placed in crucible bottom, uses PVT method growth SiC crystal, including: put into after sealed crucible
Growth room, growth room's vacuum degree control is 1 × 10-6～1 × 10-8Mbar, to set up thermal gradient between silicon carbide source powder and seed crystal
Mode heating crucible, be heated to above 50-200 DEG C of the sublimation temperature of carborundum, with nitrogen as doped source, prepare off-axis lining
The N-type SiC single crystal at the end.
2. the growing method of off-axis substrate SiC crystal as claimed in claim 1, it is characterised in that in step (2), described
The asymmetric bonding way of seed crystal is: make site, seed crystal little Bian center be reduced to (0～0.8) r, wherein r with temperature field central shaft distance
It is the site, seed crystal little Bian center during centrosymmetry placement and temperature field central shaft distance distance.
3. the growing method of off-axis substrate SiC crystal as claimed in claim 1, it is characterised in that in step (3), described
Atmosphere deflector is radian at the arc of 100-180 °, or radian 100-180 °, up-narrow and down-wide horn mouth cut shape plate.
4. the growing method of off-axis substrate SiC crystal as claimed in claim 1, it is characterised in that in step (3), described
Atmosphere deflector is graphite piece.
5. the growing method of the off-axis substrate SiC crystal as described in claim 1 or 4, it is characterised in that in step (3),
Described atmosphere deflector and crucible upper cover are made into integrative-structure.
6. the growing method of off-axis substrate SiC crystal as claimed in claim 1, it is characterised in that in step (3), institute
The angle stating atmosphere deflector normal direction and temperature field central shaft is 40～60 °；Preferably angle is 45 °.
7. a preparation method for N-type SiC substrate, N-type SiC prepared including method described in any one of claim 1-6 is mono-
Crystalline substance, including step:
-by round as a ball for the N-type SiC crystal SiC crystal for normal diameter, round as a ball in, the asymmetrical crystalline substance removing the expanding part in little limit
Body, thus will remove along the little rim portion of seed crystal to the facet component of outgrowth；
-SiC crystal of normal diameter is adjusted by cutting, it is thus achieved that it is partial to the SiC substrate material of 4 °.
8. the preparation method of N-type SiC substrate as claimed in claim 7, it is characterised in that described normal diameter is 2-8 English
Very little.
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| CN201610389489.5A CN106012002B (en) | 2016-06-04 | 2016-06-04 | A kind of preparation method of the N-type SiC substrate of the growth of off-axis substrate SiC crystal and high electricity uniformity |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN111286780A (en) * | 2018-12-07 | 2020-06-16 | 昭和电工株式会社 | Crystal growth device and crucible |
| CN117166056A (en) * | 2022-06-02 | 2023-12-05 | 株式会社力森诺科 | n-type SiC single crystal substrate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111286780A (en) * | 2018-12-07 | 2020-06-16 | 昭和电工株式会社 | Crystal growth device and crucible |
| 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 |
| 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 |
| CN117166056A (en) * | 2022-06-02 | 2023-12-05 | 株式会社力森诺科 | n-type SiC single crystal substrate |
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