CN108166056A - A kind of growing method that can effectively reduce silicon carbide epitaxy surface defect - Google Patents
A kind of growing method that can effectively reduce silicon carbide epitaxy surface defect Download PDFInfo
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- CN108166056A CN108166056A CN201810041295.5A CN201810041295A CN108166056A CN 108166056 A CN108166056 A CN 108166056A CN 201810041295 A CN201810041295 A CN 201810041295A CN 108166056 A CN108166056 A CN 108166056A
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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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/20—Epitaxial-layer growth characterised by the substrate the substrate being of the same materials as the epitaxial layer
-
- 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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/183—Epitaxial-layer growth characterised by the substrate being provided with a buffer layer, e.g. a lattice matching layer
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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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Abstract
The present invention solves the technical problem of propose a kind of growing method that can effectively reduce silicon carbide epitaxy surface defect.Buffer growth is carried out using the online etched substrate technique in situ of low and high temperature combination and under conditions of higher than epitaxial growth temperature, based on currently used chemical vapor deposition and epitaxial stove, on silicon carbide substrates by improving online etching technics in situ and buffer layer (buffer layer) growth technique, reduce the extension of defect and crystallization growth on substrate, epi-layer surface defect is effectively reduced, obtains the silicon carbide homoepitaxy chip of high quality.The process compatible is epitaxial furnace suitable for existing commercialized monolithic and multi-disc, has higher promotional value in conventional silicon carbide epitaxy technique.
Description
Technical field
The present invention relates to a kind of growing method that can effectively reduce silicon carbide epitaxy surface defect, suitable for monolithic extension
Stove and planetary multi-disc epitaxial furnace.By using the etched substrate technique in situ of low and high temperature combination and higher than epitaxial temperature
Grown buffer layer high temperature low speed epitaxy technique, silicon carbide epitaxy defect density is effectively reduced, particularly to device
Performance has the defects of detrimental effects, such as triangle, carrot dislocation, the control for falling object and big triangle, such as Fig. 1 and Fig. 3
Shown, epitaxial surface defect concentration can be by 2/cm2It is reduced to 0.5/cm2Below.And this method technological process is simple, is easy to grasp
Make, repeatability and consistency are preferable, are suitable for bulk production and application.
Background technology
Silicon carbide (SiC) as third generation semi-conducting material, have big energy gap, excellent stability, high heat conductance,
The good characteristics such as high critical breakdown strength, high saturated electron drift velocity are that make high temperature, high frequency, high-power and intense radiation electric
The ideal semiconductor material of power electronic device.Compared with traditional silicon device, the breakdown electric field of carbofrax material is one higher than silicon
Magnitude, pressure resistance are 10 times of silicon materials, and thermal conductivity is 3 times of silicon materials, and junction temperature reaches as high as 200 DEG C, and performance is far superior to silicon
Base device.It is typically that the silicon carbide epitaxy of growth on silicon carbide substrates is brilliant for making the carbofrax material of silicon carbide device
Piece.Silicon carbide epitaxial growth has been realized in being commercialized at present, and the method for generally use CVD (chemical vapor deposition) grows carbon
SiClx epitaxial wafer.
However, due to the features such as SiC material crystal form is more, growth conditions is harsher, the substrate material currently used for SiC extensions
Material is substantially edge<11-20>The inclined 4 ° of silicon faces homo-substrate in direction.The introducing of drift angle substrate can cause epitaxial layer along step surface
Growth, and then realize that lattice structure replicates, greatly improve the crystalline quality of epitaxial layer.But many defect meetings of substrate material
As epitaxial growth is gradually spread or developed to epitaxial layer, lead to that SiC epitaxial wafer surface defect is more, and late device is fabricated to
Product rate is not high, hinders promotion and application of the SiC material in power electronic devices field.
Therefore, by improving epitaxy technique, epitaxial layer defects are controlled, reduce the generation of epitaxy defect, Neng Gouyou
Effect improves the output yield of SiC epitaxial wafers, plays the role of to the cost of manufacture for reducing SiC device positive.
In conclusion carbonization can be greatly lowered by optimizing etching and buffer growth technique in situ in the epitaxy method
The surface defect of silicon epitaxy.Process compatible has higher promotional value in conventional SiC epitaxy techniques.
Invention content
Goal of the invention：In view of the above problems, the present invention, which proposes one kind, can effectively reduce silicon carbide epitaxy surface defect
Growing method.
Technical solution：A kind of growing method that can effectively reduce silicon carbide epitaxy surface defect of the present invention, packet
Include following steps：
The first step：It chooses and is biased to<11-20>The silicon face silicon carbide substrates in 4 ° or 8 ° of direction will serve as a contrast after carrying out standard cleaning
Bottom is placed in graphite base；
Second step：Graphite base is put into reative cell, after argon gas displaced air, it is backward that reative cell is evacuated to vacuum
Reative cell is passed through hydrogen, keeps H2120~200L/min of flow, chamber pressure are 100~150mbar, use radio frequency heating
Mode, with fixed 25~30 DEG C/min of heating rate, by reative cell by room temperature to 1400 DEG C；Then it will heat up speed
Degree is reduced to 15 DEG C/min, is warming up to and 15~20 DEG C of temperature is higher by than outer layer growth temperature, and constant temperature etches 8-12 minutes；
Third walks：Small flow silicon source and carbon source are passed through to reative cell, wherein silicon source flow is 50sccm~120sccm, C/
Between Si is 0.8~1.2, it is passed through high pure nitrogen (N2), 0.5-20 μm of growth thickness, doping concentration~1E18cm-3N-shaped buffering
Layer；
4th step：Cut-out source gas is passed through, and chamber pressure and hydrogen flowing quantity remain unchanged, by reaction chamber temperature by the 2) and
The 3) temperature is reduced to outer layer growth temperature in step, by growth source and doped source by the way of linear gradual (ramping)
Flow change to growth epitaxial structure needed for setting value, according to process grow epitaxial structure；
5th step：After epitaxial structures growth is completed, growth source and doped source are closed, by reative cell in hydrogen atmosphere
Greenhouse cooling to room temperature, reaction chamber temperature reach after room temperature by hydrogen it is exclusive after, carried out by argon gas to reacting indoor gas
Repeatedly displacement, after chamber pressure finally is inflated to atmospheric pressure with argon gas, begins to speak to take piece.
Available silicon source is suitable for the invention to include：Silane, dichloro hydrogen silicon, trichlorosilane or tetrachloro hydrogen silicon etc.；Carbon can be used
Source includes：Methane, ethylene, acetylene or propane etc..
Advantageous effect：The present invention proposes a kind of growing method that can effectively reduce silicon carbide epitaxy surface defect, can
To realize the accurate adjusting for substrate being etched and being buffered in situ layer process.Pass through the etching in situ combined by using low and high temperature
The buffer growth technique of technique and high temperature low speed considerably reduces the surface defect of silicon carbide epitaxial layers.The present invention carries
The method gone out is compatible with conventional SiC epitaxy techniques, suitable for existing commercialized monolithic and multiple-piece epitaxial furnace, have compared with
High promotional value.
Description of the drawings
Fig. 1 is the surface defect distribution schematic diagram of the silicon carbide epitaxial film prepared using conventional method, and substrate is edge<
11-20>The inclined 4 ° of silicon faces in direction.
Fig. 2 is heating curve schematic diagram of the present invention.
Fig. 3 is the surface defect distribution schematic diagram of silicon carbide epitaxial film prepared by the present invention, and substrate is edge<11-20>
The inclined 4 ° of silicon faces in direction.
Specific embodiment
Technical solution of the present invention is described in detail below, but protection scope of the present invention is not limited to the implementation
Example.
Embodiment one：
The carborundum films growing method using silane+propane+hydrogen chloride of offer, includes the following steps：
The first step：It chooses and is biased to<11-20>Substrate is placed in by the silicon face silicon carbide substrates in 4 ° of direction after carrying out standard cleaning
In graphite base；
Second step：This graphite base is put into reative cell, after argon gas displaced air, after reative cell is evacuated to vacuum
Hydrogen is passed through to reative cell, keeps H2Flow 160L/min, chamber pressure 100mbar, using the mode of radio frequency heating, with
Fixed 25 DEG C/min of heating rate, by reative cell by room temperature to 1400 DEG C；Then will heat up speed be reduced to 15 DEG C/
Minute, 1580 DEG C are warming up to, constant temperature etches 10 minutes；
Third walks：Silane (SiH is passed through to reative cell4)+propane+(C3H8The mixed gas of)+hydrogen chloride (HCl) sets silicon
Alkane flow 50sccm, C/Si 0.9, hydrogen chloride flow are 200sccm, use high pure nitrogen (N2) as doped source, growth thickness
1 μm of degree, doping concentration~1E18cm-3N-type buffer layer；
4th step：It closes silane, propane and hydrogen chloride, chamber pressure and hydrogen flowing quantity to remain unchanged, room temperature will be reacted
Degree is reduced to 1560 DEG C, changes silane, propane flow by the way of linear gradual (ramping), controls final silane flow rate
160sccm, propane flow control is 48sccm, and hydrogen chloride flow is set as 720 sccm, after temperature stabilization, by silane, third
Alkane and hydrogen chloride are passed through reative cell and are passed through high pure nitrogen (N2), growth thickness~12 μm, doping concentration~6E15cm-3N-shaped
Channel layer.
5th step：Growth source and doped source are closed, reaction chamber temperature is cooled to room temperature in hydrogen atmosphere.Pass through argon gas
Indoor hydrogen is reacted in displacement, and reative cell vacuum is evacuated to 0mbar, is maintained 5 minutes, and argon gas is filled with to atmospheric pressure to reative cell,
Reative cell is opened, takes out epitaxial wafer.
Embodiment two：
The carborundum films growing method using silane+propane+hydrogen chloride of offer, includes the following steps：
The first step：It chooses and is biased to<11-20>Substrate is placed in by the silicon face silicon carbide substrates in 4 ° of direction after carrying out standard cleaning
In graphite base；
Second step：This graphite base is put into reative cell, after argon gas displaced air, after reative cell is evacuated to vacuum
Hydrogen is passed through to reative cell, keeps H2Flow 180L/min, chamber pressure 150mbar, using the mode of radio frequency heating, with
Fixed 30 DEG C/min of heating rate, by reative cell by room temperature to 1400 DEG C；Then will heat up speed be reduced to 15 DEG C/
Minute, 1570 DEG C are warming up to, constant temperature etches 11 minutes；
Third walks：Silane (SiH is passed through to reative cell4)+propane+(C3H8The mixed gas of)+hydrogen chloride (HCl) sets silicon
Alkane flow 50sccm, C/Si 1.1, hydrogen chloride flow are 200sccm, use high pure nitrogen (N2) as doped source, growth thickness
1 μm of degree, doping concentration~1E18cm-3N-type buffer layer；
4th step：It closes silane, propane and hydrogen chloride, chamber pressure and hydrogen flowing quantity to remain unchanged, room temperature will be reacted
Degree is reduced to 1550 DEG C, changes silane, propane flow by the way of linear gradual (ramping), controls final silane flow rate
180sccm, propane flow control is 60sccm, and hydrogen chloride flow is set as 800 sccm, after temperature stabilization, by silane, third
Alkane and hydrogen chloride are passed through reative cell and are passed through high pure nitrogen (N2), growth thickness~12 μm, doping concentration~6E15cm-3N-shaped
Channel layer.
5th step：Growth source and doped source are closed, reaction chamber temperature is cooled to room temperature in hydrogen atmosphere.Pass through argon gas
Indoor hydrogen is reacted in displacement, and reative cell vacuum is evacuated to 0mbar, is maintained 5 minutes, and argon gas is filled with to atmospheric pressure to reative cell,
Reative cell is opened, takes out epitaxial wafer.
Embodiment three：
The carborundum films growing method using silane+propane+hydrogen chloride of offer, includes the following steps：
The first step：It chooses and is biased to<11-20>Substrate is placed in by the silicon face silicon carbide substrates in 4 ° of direction after carrying out standard cleaning
In graphite base；
Second step：This graphite base is put into reative cell, after argon gas displaced air, after reative cell is evacuated to vacuum
Hydrogen is passed through to reative cell, keeps H2Flow 180L/min, chamber pressure 150mbar, using the mode of radio frequency heating, with
Fixed 30 DEG C/min of heating rate, by reative cell by room temperature to 1400 DEG C；Then will heat up speed be reduced to 15 DEG C/
Minute, 1560 DEG C are warming up to, constant temperature etches 12 minutes；
Third walks：Silane (SiH is passed through to reative cell4)+propane+(C3H8The mixed gas of)+hydrogen chloride (HCl) sets silicon
Alkane flow 100sccm, C/Si 1.2, hydrogen chloride flow are 400sccm, use high pure nitrogen (N2) as doped source, growth thickness
1 μm of degree, doping concentration~1E18cm-3N-type buffer layer；
4th step：It closes silane, propane and hydrogen chloride, chamber pressure and hydrogen flowing quantity to remain unchanged, room temperature will be reacted
Degree is reduced to 1540 DEG C, changes silane, propane flow by the way of linear gradual (ramping), controls final silane flow rate
180sccm, propane flow control is 60sccm, and hydrogen chloride flow is set as 800 sccm, after temperature stabilization, by silane, third
Alkane and hydrogen chloride are passed through reative cell and are passed through high pure nitrogen (N2), growth thickness~12 μm, doping concentration~6E15cm-3N-shaped
Channel layer.
5th step：Growth source and doped source are closed, reaction chamber temperature is cooled to room temperature in hydrogen atmosphere.Pass through argon gas
Indoor hydrogen is reacted in displacement, and reative cell vacuum is evacuated to 0mbar, is maintained 5 minutes, and argon gas is filled with to atmospheric pressure to reative cell,
Reative cell is opened, takes out epitaxial wafer.
In conclusion although the present invention has been represented and described with reference to specific preferred embodiment, must not explain
For to the limitation of itself of the invention.It, can be right under the premise of the spirit and scope of the present invention that appended claims define are not departed from
It makes a variety of changes in the form and details.
Claims (6)
1. a kind of growing method that can effectively reduce silicon carbide epitaxy surface defect, it is characterized in that this method includes following step
Suddenly：
The first step：It chooses and is biased to<11-20>The silicon face silicon carbide substrates in 4 ° or 8 ° of direction put substrate after carrying out standard cleaning
In in graphite base；
Second step：Graphite base is put into reative cell, after argon gas displaced air, reative cell is evacuated to after vacuum to reaction
Room is passed through hydrogen, keeps H2120~200L/min of flow, chamber pressure are 100~150mbar, use the side of radio frequency heating
Formula, with fixed 25~30 DEG C/min of heating rate, by reative cell by room temperature to 1400 DEG C；Then it will heat up speed drop
It down to 15 DEG C/min, is warming up to and 15~20 DEG C of temperature is higher by than outer layer growth temperature, constant temperature etches 8-12 minutes；
Third walks：Small flow silicon source and carbon source are passed through to reative cell, wherein silicon source flow is 50sccm~120sccm, and C/Si is
Between 0.8~1.2, it is passed through high pure nitrogen (N2), 0.5-20 μm of growth thickness, doping concentration~1E18cm-3N-type buffer layer；
4th step：Cut-out source gas is passed through, and chamber pressure and hydrogen flowing quantity remain unchanged, by reaction chamber temperature by the 2) and the 3)
Temperature is reduced to outer layer growth temperature in step, by growth source and the stream of doped source by the way of linear gradual (ramping)
Amount changes to the setting value needed for growth epitaxial structure, grows epitaxial structure according to process；
5th step：After epitaxial structures growth is completed, growth source and doped source are closed, by reaction chamber temperature in hydrogen atmosphere
Be cooled to room temperature, reaction chamber temperature reach after room temperature by hydrogen it is exclusive after, by argon gas to react indoor gas carry out it is multiple
Displacement, after chamber pressure finally is inflated to atmospheric pressure with argon gas, begins to speak to take piece.
2. a kind of growing method that can effectively reduce silicon carbide epitaxy surface defect as described in claim 1, feature exist
In：The epitaxial growth, substrate use<11-20>4 ° of direction N-type or semi-insulating substrate, crystal form are 4H or 6H-SiC.
3. a kind of growing method that can effectively reduce silicon carbide epitaxy surface defect as described in claim 1, feature exist
In：Described etching in situ include cold stage etching (1400 DEG C start) and high temperature etch stages (epitaxial growth temperature+15~
20 DEG C) two parts composition.Cryo-etching is carried out by slow heating mode, and high temperature etch stages keep 8~12 points of temperature constant state
Clock.
4. a kind of growing method that can effectively reduce silicon carbide epitaxy surface defect as described in claim 1, feature exist
In：It needs to carry out low speed epitaxial growth buffer in the case where being higher by the temperature condition of 15~20 DEG C of epitaxial growth temperature.
5. a kind of growing method that can effectively reduce silicon carbide epitaxy surface defect as described in claim 1, feature exist
In：It can be included with silicon source：Silane, dichloro hydrogen silicon, trichlorosilane or tetrachloro hydrogen silicon etc.；It can be included with carbon source：Methane, ethylene, second
Alkynes or propane etc..
6. a kind of growing method that can effectively reduce silicon carbide epitaxy surface defect as described in claim 1, feature exist
In：The technique is suitable for existing one chip epitaxial furnace or planetary multi-disc epitaxial furnace.
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| CN111029245A (en) * | 2019-12-09 | 2020-04-17 | 中国电子科技集团公司第五十五研究所 | SiC epitaxial rate switching method |
| CN111029246A (en) * | 2019-12-09 | 2020-04-17 | 中国电子科技集团公司第五十五研究所 | Method for reducing triangular defects in SiC epitaxial layer |
| CN112366130A (en) * | 2020-10-09 | 2021-02-12 | 中国电子科技集团公司第五十五研究所 | Method for reducing defect density of silicon carbide epitaxial material |
| CN112490117A (en) * | 2020-12-08 | 2021-03-12 | 瀚天天成电子科技（厦门）有限公司 | Method for improving growth quality of silicon carbide epitaxial film |
| CN112701031A (en) * | 2020-12-29 | 2021-04-23 | 中国电子科技集团公司第五十五研究所 | Buffer layer growth method of silicon carbide epitaxial material |
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| CN113089089A (en) * | 2021-04-02 | 2021-07-09 | 眉山博雅新材料有限公司 | Silicon carbide crystal preparation device and growth method thereof |
| CN113488528A (en) * | 2021-07-01 | 2021-10-08 | 山东天岳先进科技股份有限公司 | Silicon carbide substrate with high surface cleanliness and cleaning method thereof |
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