CN104810248B - Suitable for the in-situ treatment method of 4 ° and 8 ° off-axis silicon face silicon carbide substrates - Google Patents
Suitable for the in-situ treatment method of 4 ° and 8 ° off-axis silicon face silicon carbide substrates Download PDFInfo
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- CN104810248B CN104810248B CN201510161527.7A CN201510161527A CN104810248B CN 104810248 B CN104810248 B CN 104810248B CN 201510161527 A CN201510161527 A CN 201510161527A CN 104810248 B CN104810248 B CN 104810248B
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- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02367—Substrates
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- H01L21/02373—Group 14 semiconducting materials
- H01L21/02378—Silicon carbide
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
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Abstract
The present invention is a kind of while suitable for edge<11‑20>The in-situ treatment method of the 4 ° and 8 ° off-axis silicon face silicon carbide substrates in direction.Based on chemical vapor deposition growing technology, using same technique, on edge<11‑20>The SiC epitaxial films of specific preferably surface quality are prepared in the silicon face silicon carbide substrates of 4 ° of direction off-axis and 8 ° of off-axis.Wherein substrate pre-treatment processing step：After reative cell heating reaches 1500 DEG C, it is passed through a small amount of hydrogen chloride additional substrate to reative cell and etches.Advantage：It is that the in-situ treatment method is applied to edge simultaneously<11‑20>4 ° and 8 ° of direction off-axis silicon face silicon carbide substrates.In multi-disc SiC epitaxial systems, it is possible to achieve 4 ° of off-axis and the same heat growth of 8 ° of off-axis SiC substrates, while can more accurately compare the difference of 4 ° of off-axis and 8 ° of off-axis extensive properties.
Description
Technical field
Proposed by the present invention is that one kind is applied to edge<11-20>At the original position of 4 ° and 8 ° of direction off-axis silicon face silicon carbide substrates
Reason method, using same in-situ treatment technique, on edge<11-20>The silicon face carborundum of 4 ° of direction off-axis and 8 ° of off-axis（SiC）Lining
The SiC epitaxial films of specific preferably surface quality can be prepared on bottom.Belong to technical field of semiconductor.
Background technology
SiC semiconductor material, is widely used in power electronic devices（Diode, FET, transducer；Motor drives
Device；Output rectifier）, microwave device（Broadband communications, Connectors for Active Phased Array Radar）, opto-electronic device（Semiconductor lighting）Deng neck
Domain, belongs to international high end advanced material.At present, SiC device has been used for hybrid vehicle and electric automobile equipment, SiC devices
In part power module, SiC convertible frequency air-conditioners, SiC inverters.Meanwhile, many companies use in its IGBT frequency conversion or inverter
This device replaces silicon fast recovery diode, improves working frequency, the positive effect of switching loss is greatly lowered, it is totally imitated
Benefit is considerably beyond SiC device and the price differential of silicon device.SiC power electronic devices will replace Si devices in the near future.
SiC power electronic devices, which is developed, needs the individual layer or multilayer silicon carbide epitaxy material of specific doping concentration and thickness
Material, current SiC epitaxial materials are mainly prepared using the method for chemical vapor deposition.In SiC homoepitaxies, in order to ensure extension
Material can effectively inherit the stacking sequences of substrate, it is ensured that crystal mass, use mostly along the inclined ＜ 11-20 ＞ sides in c-axis direction
To the substrate of cutting.The meaning of substrate drift angle cutting is the step that atomic level is introduced in substrate surface.In epitaxial process, inhale
Attached atom tends to the nucleating growth at step, it is ensured that epitaxial process presses step stream（step-flow）Pattern carry out.
Before epitaxial growth is started, typically can all in-situ high temperature hydrogen etching processing be carried out to substrate, to eliminate surface
The Micro scratching that chemical polishing is not eliminated, improves epitaxial wafer surface quality.Mainly there are 4 ° and 8 ° in the drift angle of conventional SiC substrate at present
Two kinds.But it is due to the step density difference on 4 ° of off-axis and 8 ° of off-axis SiC substrate surfaces, etch rate and platform of the hydrogen to substrate
Silicon vapor equilibrium partial pressure above face is different, it is therefore desirable to which the online etching technics of use is different.
Hydrogen is as follows to the etching process of SiC substrate under high temperature：
SiC(s)↔Si(l)+C(s) (3-1)
2C(s)+H2↔C2H2 (g) (3-2)
Si(l)↔Si(g) (3-3)
Step density on the substrate of 8 ° of drift angles is more than the substrate and positive crystal orientation substrate of 4 ° of drift angles, quarter of the hydrogen to substrate
Lose speed most fast, reaction（3-2）Speed be more than reaction（3-3）Speed, reaction（3-1）The silicon of generation can not be in time by anti-
Should（3-3）In distillation, therefore 8 ° of off-axis SiC substrate epitaxy techniques of routine, etch stages, need more than 1400 DEG C in the original location
Extra propane is added to suppress reaction（2）, prevent overetch occur silica drop cause surface roughness rise introduce lack
Fall into；On the substrate of 4 ° of drift angles, reaction（3-2）,（3-3）Quite, the silicon vapor equilibrium partial pressure above table top is less than 8 ° partially to speed
Silicon vapor equilibrium partial pressure on the substrate at angle is general that etching processing in situ is carried out to substrate using pure hydrogen.If to 4 ° of off-axis
SiC substrate, if using the in-situ treatment method for being applied to 8 ° of off-axis substrates, the auxiliary of extra propane is added more than 1500 DEG C
Hydrogen is helped to etch, the epitaxial wafer surface of 4 ° of off-axis substrates will produce substantial amounts of micro-crack and step pack pattern, cause table
The situation that face pattern is degenerated.Current SiC chemical gas-phase deposition systems are largely planetary multi-disc epitaxial furnace, due to 4 ° of off-axis
It is different with the etching technics in situ of 8 ° of off-axis SiC substrates, cause 4 ° of off-axis and 8 ° of off-axis substrates to realize same stove growth.In addition
Different due to etching technics in situ, the SiC substrate extension difference of 4 ° of off-axis and 8 ° of off-axis also can not accurately compare.
It is a kind of while suitable for 4 ° of off-axis and the SiC substrate in-situ treatment method of 8 ° of off-axis, it is necessary to suppress 8 ° partially
Avoid 4 ° of off-axis substrate original position etching insufficient situations occur while silica drop formation in axle substrate etching engineering.This patent
By introducing HCl gases in high temperature etch stages, react to form gas phase SiCl by Si components and HClx, effectively accelerate reaction
（3-3）Speed, it is to avoid in high temperature etching process, the formation of 8 ° of off-axis substrate surface silica drops, at the same time, in turn ensure that 4 ° partially
Effective etching at axle bush bottom.With reference to low speed, low-carbon silicon than buffering layer process, it is possible to prevente effectively from 4 ° of off-axis substrate surface steps gather
The generation of beam pattern.
The content of the invention
The present invention is a kind of suitable for edge<11-20>The silicon face carborundum of 4 ° of direction off-axis and 8 ° of off-axis（SiC）Substrate
In-situ treatment method.Based on chemical vapor deposition growing technology, using same technique, on edge<11-20>4 ° of direction off-axis
With the silicon face carborundum of 8 ° of off-axis（SiC）The SiC epitaxial films of specific preferably surface quality can be prepared on substrate.The party
Method is applied to the growth technique of any SiC epitaxial structures, it is possible to achieve 4 ° of off-axis and the same heat growth of 8 ° of off-axis SiC substrates,
It can more accurately compare the difference of 4 ° of off-axis and 8 ° of off-axis extension extensive properties simultaneously.
The technical solution of the present invention：One kind is applied to edge<11-20>4 ° and 8 ° of direction off-axis silicon face silicon carbide substrates
In-situ treatment method, it is characterized in that this method is comprised the technical steps that：
1）Choose deviation<11-20>The silicon face silicon carbide substrates in 4 ° or 8 ° of direction, SiC epitaxial systems are placed in by substrate
On the graphite base for having ramet coating in reative cell；
2）System is warming up to 1400 DEG C, and setting pressure is 100-200 mbar, in H2Flow 68-80L/min, remains anti-
Answer room temperature 15-25 minutes, pure hydrogen H is carried out to substrate2Etching；
3）Continue heating to reach after 1500 DEG C, being passed through a small amount of hydrogen chloride HCl additional substrates to reative cell etches, wherein
HCl/H2Flow-rate ratio Application Range 0.01%-0.15%；
4）Continue to heat up, reach after growth temperature, maintain growth temperature 10-15 minutes, H is aided in using HCl2Continuation pair
Substrate carries out etching in situ；
5）Low discharge silane SiH is passed through to reative cell4And propane C3H8, control SiH4/H2Flow-rate ratio is less than 0.025%, is aided with
Low inlet end C/Si ratios are less than 1, and adjust HCl gas flows, and Cl/Si is than 2 or so for control, is passed through doped source nitrogen N2, growth
1-5 μm of thickness, doping concentration 1 × 1018 cm-3Cushion；
6）Growth source is closed, a small amount of hydrogen chloride gas is passed through and etching in situ, HCl/H is carried out to cushion2Flow-rate ratio is selected
Scope 0.01%-0.15%, etch period 2-6 minutes；
7）Growth source, the epitaxial structure required for growth are passed through again；
8）After epitaxial structures growth needed for completing, growth source and doped source, cooling are closed.
Advantages of the present invention：The epitaxy method is simultaneously suitable for edge<11-20>The silicon face carbon of 4 ° of direction off-axis and 8 ° of off-axis
SiClx（SiC）Substrate.In multi-disc SiC epitaxial systems, it is possible to achieve 4 ° of off-axis and the same heat growth of 8 ° of off-axis SiC substrates,
It can more accurately compare the difference of 4 ° of off-axis and 8 ° of off-axis extension extensive properties simultaneously.
Brief description of the drawings
Accompanying drawing 1-a is 4 ° of off-axis silicon carbide substrate epitaxial wafer surface topography schematic diagrames to be grown using this method.
Accompanying drawing 1-b is the 8 ° of off-axis silicon carbide substrate epitaxial wafer surface topographies signal grown using this method in same heat
Figure, epitaxial wafer surface scan uses the CS10 surface defect testers of Candela companies, using the scanning result of reflected light channel
Contrasted.
Embodiment
Embodiment 1
What is provided is applied to edge simultaneously in planetary multi-disc base SiC epitaxial systems<11-20>4 ° of direction off-axis and 8 ° are partially
The in-situ treatment method of the silicon face SiC substrate of axle comprises the following steps：
1）Choose deviation<11-20>4 ° of direction silicon face silicon carbide substrates, substrate is placed in SiC epitaxial system reative cells
On the graphite base for having ramet coating；
2）System is warming up to 1400 DEG C, and setting pressure is 100 mbar, in H2Flow 68L/min, maintenance reaction room temperature
15 minutes, pure hydrogen H is carried out to substrate2Etching；
3）Continue heating to reach after 1500 DEG C, being passed through a small amount of hydrogen chloride HCl additional substrates to reative cell etches, wherein
HCl/H2Flow-rate ratio Application Range 0.01%；
4）Continue to heat up, reach after growth temperature, maintain growth temperature 10 minutes, H is aided in using HCl2Continue to substrate
Carry out etching in situ；
5）Low discharge silane SiH is passed through to reative cell4And propane C3H8, control SiH4/H2Flow-rate ratio is less than 0.025%, is aided with
Low inlet end C/Si ratios are less than 1, and adjust HCl gas flows, and Cl/Si is than 2 or so for control, is passed through doped source nitrogen N2, growth
1 μm of thickness, doping concentration 1 × 1018 cm-3Cushion；
6）Growth source is closed, a small amount of hydrogen chloride gas is passed through and etching in situ, HCl/H is carried out to cushion2Flow-rate ratio is selected
Scope 0.01%, etch period 2 minutes；
7）Growth source, the epitaxial structure required for growth are passed through again；
8）After epitaxial structures growth needed for completing, growth source and doped source, cooling are closed.
Embodiment 2
What is provided is applied to edge simultaneously in planetary multi-disc base SiC epitaxial systems<11-20>4 ° of direction off-axis and 8 ° are partially
The in-situ treatment method of the silicon face SiC substrate of axle comprises the following steps：
1）Choose deviation<11-20>The silicon face silicon carbide substrates in 8 ° of direction, SiC epitaxial system reative cells are placed in by substrate
On the graphite base for inside having ramet coating；
2）System is warming up to 1400 DEG C, and setting pressure is 200 mbar, in H2Flow 80L/min, maintenance reaction room temperature
25 minutes, pure hydrogen H is carried out to substrate2Etching；
3）Continue heating to reach after 1500 DEG C, being passed through a small amount of hydrogen chloride HCl additional substrates to reative cell etches, wherein
HCl/H2Flow-rate ratio Application Range 0.15%；
4）Continue to heat up, reach after growth temperature, maintain growth temperature 15 minutes, H is aided in using HCl2Continue to substrate
Carry out etching in situ；
5）Low discharge silane SiH is passed through to reative cell4And propane C3H8, control SiH4/H2Flow-rate ratio is less than 0.025%, is aided with
Low inlet end C/Si ratios are less than 1, and adjust HCl gas flows, and Cl/Si is than 2 or so for control, is passed through doped source nitrogen N2, growth
5 μm of thickness, doping concentration 1 × 1018 cm-3Cushion；
6）Growth source is closed, a small amount of hydrogen chloride gas is passed through and etching in situ, HCl/H is carried out to cushion2Flow-rate ratio is selected
Scope 0.15%, etch period 6 minutes；
7）Growth source, the epitaxial structure required for growth are passed through again；
8）After epitaxial structures growth needed for completing, growth source and doped source, cooling are closed.
Above example of making is that actual adoptable production program is very in general embodiment of the invention, preparation method
Many, equivalent change and decoration that all claims under this invention are made belong to the covering scope of the present invention.
Claims (1)
1. one kind is applied to edge<11-20>The in-situ treatment method of the 4 ° and 8 ° off-axis silicon face silicon carbide substrates in direction, it is characterized in that
This method is comprised the technical steps that：
1）Choose deviation<11-20>The silicon face silicon carbide substrates in 4 ° or 8 ° of direction, the reaction of SiC epitaxial systems is placed in by substrate
Interior has on the graphite base of ramet coating；
2）System is warming up to 1400 DEG C, and setting pressure is 100-200 mbar, in H2Flow 68-80L/min, maintenance reaction room temperature
Degree 15-25 minutes, pure hydrogen H is carried out to substrate2Etching；
3）Continue heating to reach after 1500 DEG C, being passed through a small amount of hydrogen chloride HCl additional substrates to reative cell etches, wherein HCl/H2Stream
Amount is than Application Range 0.01%-0.15%；
4）Continue to heat up, reach after growth temperature, maintain growth temperature 10-15 minutes, H is aided in using HCl2Continuation is entered to substrate
Row etching in situ；
5）Low discharge silane SiH is passed through to reative cell4And propane C3H8, control SiH4/H2Flow-rate ratio is less than 0.025%, inlet end C/
Si ratios are less than 1, and adjust HCl gas flows, and it is 2 to control Cl/Si ratios, is passed through doped source nitrogen N2, 1-5 μm of growth thickness, mix
Miscellaneous concentration 1 × 1018 cm-3Cushion；
6）Growth source is closed, a small amount of hydrogen chloride gas is passed through and etching in situ, HCl/H is carried out to cushion2Flow-rate ratio Application Range
0.01%-0.15%, etch period 2-6 minutes；
7）It is passed through growth source, the epitaxial structure required for growth；
8）After epitaxial structures growth needed for completing, growth source and doped source, cooling are closed.
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| CN201510161527.7A CN104810248B (en) | 2015-04-08 | 2015-04-08 | Suitable for the in-situ treatment method of 4 ° and 8 ° off-axis silicon face silicon carbide substrates |
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| CN104810248B true CN104810248B (en) | 2017-08-08 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108166056A (en) * | 2018-01-16 | 2018-06-15 | 李哲洋 | A kind of growing method that can effectively reduce silicon carbide epitaxy surface defect |
| CN110117814A (en) * | 2018-02-05 | 2019-08-13 | 西安电子科技大学 | The preparation method of silicon carbide epitaxy with low-density C vacancy defect |
| CN109285909B (en) * | 2018-09-29 | 2021-09-24 | 扬州乾照光电有限公司 | Multi-junction solar cell and manufacturing method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4860687A (en) * | 1986-03-21 | 1989-08-29 | U.S. Philips Corporation | Device comprising a flat susceptor rotating parallel to a reference surface about a shift perpendicular to this surface |
| CN102301043A (en) * | 2009-01-30 | 2011-12-28 | 新日本制铁株式会社 | Epitaxial silicon carbide single crystal substrate and mehtod for producing same |
| CN102576666A (en) * | 2009-08-28 | 2012-07-11 | 昭和电工株式会社 | Silicon carbide epitaxial wafer and manufacturing method therefor |
| CN103614779A (en) * | 2013-11-28 | 2014-03-05 | 中国电子科技集团公司第五十五研究所 | Method for increasing uniformity of on-chip n-type doping concentration of silicon carbide epitaxial wafer |
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2015
- 2015-04-08 CN CN201510161527.7A patent/CN104810248B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4860687A (en) * | 1986-03-21 | 1989-08-29 | U.S. Philips Corporation | Device comprising a flat susceptor rotating parallel to a reference surface about a shift perpendicular to this surface |
| CN102301043A (en) * | 2009-01-30 | 2011-12-28 | 新日本制铁株式会社 | Epitaxial silicon carbide single crystal substrate and mehtod for producing same |
| CN102576666A (en) * | 2009-08-28 | 2012-07-11 | 昭和电工株式会社 | Silicon carbide epitaxial wafer and manufacturing method therefor |
| CN103614779A (en) * | 2013-11-28 | 2014-03-05 | 中国电子科技集团公司第五十五研究所 | Method for increasing uniformity of on-chip n-type doping concentration of silicon carbide epitaxial wafer |
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