CN104505338B - Pre-cleaning method before a kind of silicon carbide wafer extension - Google Patents
Pre-cleaning method before a kind of silicon carbide wafer extension Download PDFInfo
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- CN104505338B CN104505338B CN201410814598.8A CN201410814598A CN104505338B CN 104505338 B CN104505338 B CN 104505338B CN 201410814598 A CN201410814598 A CN 201410814598A CN 104505338 B CN104505338 B CN 104505338B
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 60
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 44
- 238000004140 cleaning Methods 0.000 title claims abstract description 27
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 112
- 239000000758 substrate Substances 0.000 claims abstract description 47
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000002844 melting Methods 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 22
- 239000011259 mixed solution Substances 0.000 claims description 12
- 230000003746 surface roughness Effects 0.000 claims description 9
- 238000009835 boiling Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims 1
- 230000008018 melting Effects 0.000 abstract description 6
- 238000000407 epitaxy Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 14
- 238000005498 polishing Methods 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 239000012670 alkaline solution Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- -1 are selected Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 4
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000003466 anti-cipated effect Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 229910001868 water Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- 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
- H01L21/02041—Cleaning
- H01L21/02043—Cleaning before device manufacture, i.e. Begin-Of-Line process
- H01L21/02052—Wet cleaning only
-
- H—ELECTRICITY
- 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
- H01L21/02041—Cleaning
- H01L21/02096—Cleaning only mechanical cleaning
Landscapes
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Cleaning Or Drying Semiconductors (AREA)
Abstract
The present invention relates to silicon carbide wafer cleaning technique field, pre-cleaning method before particularly a kind of silicon carbide wafer extension.The silicon carbide epitaxy prerinse that the present invention is provided includes：The H that the silicon carbide substrates of selection are immersed in2SO4And H2O2Deionized water rinsing is used after being boiled in the solution being made into；The NaOH and Na immersed the substrate in again2O2Boil, dried after deionized water rinsing in melting mixing solution, it is standby.Based on the silicon carbide substrates of the invention provided by delaying basal plane dislocation density is reduced to 100/cm outside2Hereinafter, and method is simple, good process repeatability, it is adapted to industrialized production.
Description
【Technical field】
The present invention relates to a kind of purification method of material, and in particular to pre-cleaning techniques before a kind of silicon carbide wafer extension.
【Background technology】
Carborundum (SiC) is after after first generation Semiconducting Silicon Materials, germanium and the second carrying semiconductor material GaAs, indium phosphide
The third generation semi-conducting material grown up, the broad stopband of carbofrax material is 2-3 times of silicon and GaAs so that semiconductor device
Part can at relatively high temperatures (more than 500 DEG C) work and with transmitting blue light ability；High breakdown electric field is than silicon and arsenic
Gallium is intended to be higher by an order of magnitude, and this, which just determines SiC as semiconductor devices, has high pressure, powerful characteristic and high saturation
Electron drift velocity and low-k, with the high frequency as semiconductor devices, the service behaviour of high speed；SiC thermal conductivitys are
3.3 times of silicon, 10 times of GaAs, this means that its good heat conductivity, can greatly improve the integrated level of circuit, reduces cold
But cooling system, so as to greatly reduce the volume of complete machine.It can thus be anticipated that in the near future, with carbofrax material and device
The constantly improve of part technique, it is within sight to substitute that part Si application fields are carbonized silicon.Because carborundum has broad-band gap, height
The features such as critical breakdown strength, high thermal conductivity, high electronics saturation elegant speed, it is particularly suitable for high-power, high-voltage power
Electronic device, the study hotspot as current power electronic applications.Research finds that carborundum isoepitaxial growth is restriction carbonization
The key technology of silicon device, especially to powder injection molding.The defect present in silicon carbide epitaxy material, which is directly affected, to be carbonized
The performance of silicon device, wherein high density of defects are main by screw dislocation (TSD), edge dislocation (TED), basal plane dislocation (BPD), stacking
Caused by fault (SF) and low-angle boundary etc..Basal plane dislocation is maximum to the performance impact of device in this several defect, basal plane position
Mistake can not only reduce the forward voltage drop of silicon carbide bipolar device, can also provide nucleating point for the generation of stacking fault, so that
The forward voltage drop of device is drifted about, and has a strong impact on the reliability of device.Therefore how to reduce the density of basal plane dislocation is always
The problem of technical staff pays close attention to.
The major significance of epitaxy pre-clean is to remove the machineries such as surface damage layer and grinding, the polishing of silicon carbide substrates
Scuffing that processing is brought etc., it is possible to provide condition in substrate surface formation etch pit for basal plane dislocation conversion.
Traditional prerinse only can effectively remove surface residue and metallic pollution, such as patent (CN
101783284) manufacture method of a kind of silicon carbide substrates, outer ophthalmic len and silicon carbide substrates is disclosed in, this method uses
One alkaline solution cleaning SiC is cleaned behind main surface using the second alkaline solution, and this method can only remove the residual of silicon carbide
Thing, for surface damage layer, scratches effectively removal, can not provide advantage to basal plane dislocation.
【The content of the invention】
Pre-cleaning method comprises the following steps before the silicon carbide wafer extension that the present invention is provided：
By silicon carbide substrates in H2SO4And H2O2With after deionized water rinsing after being boiled in mixed solution, then at NaOH and
Na2O2Melt solution in boil, after deionized water rinsing dry, it is standby；Wherein H2SO4And H2O2H in mixed solution2SO4With
H2O2Volume ratio be 1-3：1.
In the pre-cleaning method that the present invention is provided, silicon carbide substrates are 4H types, 6H types or 3C types.
In the pre-cleaning method that the present invention is provided, the Si faces of silicon carbide substrates are by chemically mechanical polishing (CMP) processing.
In the pre-cleaning method that the present invention is provided, the Si surface roughness of silicon carbide substrates is 0.01-1nm；Silicon carbide substrates
C surface roughness be 1-5nm.
In the pre-cleaning method that the present invention is provided, substrate is in H2SO4And H2O2Boiling temps are 80-120 in mixed solution
℃；Substrate is in H2SO4And H2O2Boiling time in mixed solution is 5-1200s.
NaOH and Na in the pre-cleaning method that the present invention is provided2O2NaOH and Na in melt solution2O2Mass ratio be 1-9:
1-5。
In the pre-cleaning method that the present invention is provided, substrate is in NaOH and Na2O2Fused solution in boiling temps be 400-
550℃。
NaOH and Na in the pre-cleaning method that the present invention is provided2O2The hybrid mode of fused solution is by Na2O2Powder is added to
Reheated or by Na after in NaOH powder2O2Powder is added in NaOH fused solutions.
Substrate is in NaOH and Na in the pre-cleaning method that the present invention is provided2O2Melting mixing liquation in boiling time be
3-900s。
The present invention by silicon carbide substrates by being immersed in H2SO4And H2O2Boil, be immersed in after flushing in the solution being made into
NaOH and Na2O2Last drying series of steps is boiled in melt solution prerinse, the basal plane dislocation delayed outside are carried out to epitaxial wafer
Density is reduced to 100/cm2Hereinafter, and method is simple, good process repeatability, it is adapted to industrialized production.
The H used in the present invention2SO4Percentage by weight can be used for 98% concentrated sulfuric acid, H2O2Available mass concentration
For 30%, and its temperature is without concrete restriction, can select room temperature or high temperature.
Compared with immediate prior art, the technical scheme that the present invention is provided has following excellent effect：
1. the silicon carbide substrates that the present invention is provided have the etch pit of big basal plane dislocation so that the basal plane in epitaxy technique
Dislocation is easier to be converted into screw dislocation, reaches the purpose of reduction basal plane dislocation density；
2. the method that the present invention is provided, preparation method is simple, good process repeatability, it is adapted to industrialized production；
3. being passed through outside based on the silicon carbide substrates that the present invention is provided, delaying basal plane dislocation density is reduced to 100/cm2Below.
【Brief description of the drawings】
Fig. 1 is a kind of schematic flow sheet of silicon carbide epitaxy pre-cleaning method provided by the present invention.
【Embodiment】
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the accompanying drawing used required in technology description to be briefly described.
Embodiment 1
A kind of pre-cleaning method before silicon carbide wafer extension, it is as follows：
(1) silicon carbide substrates, are selected, crystal formation is 4H, and Si faces are chemically mechanical polishing, and Si surface roughness is 0.3nm, C faces
Roughness is 3nm；
(2) H, is heated2SO4And H2O2(3:1) solution being made into is to 100 DEG C, wherein H2SO4Percentage by weight be 98%,
H2O2Percentage by weight be 30%；
(3) silicon carbide substrates, are immersed into 100 DEG C of H2SO4And H2O2(3:1) mixed solution, keeps 600s；
(4) deionized water rinsing, is used；
(5), by Na2O2Powder, by NaOH:Na2O2=4:1 ratio is added in NaOH powder；
(5) NaOH and Na, is heated2O2(4:1) powder reaches molten state to 500 DEG C；
(6) silicon carbide substrates, are immersed into 500 DEG C of NaOH and Na2O2(4:1) melting mixing solution, is kept for 900 seconds；
(7) deionized water rinsing, is used；
(8), dry, prepare extension.
The method that comparative example is announced in using publication No. for CN101783284A, the main surface of silicon carbide substrates uses
Cleaned after the cleaning of one alkaline solution using the second alkaline solution, the first alkaline solution is the molten of ammoniacal liquor and hydrogen peroxide mixture
Liquid, water, ammonia and hydrogen peroxide are in proportion：5:1:5 ratio mixing, scavenging period 900s.Second alkaline solution and the first alkalescence
Solution is same, and processing time is identical.
Data below is the pretreated silicon carbide substrates of the embodiment of the present invention by delaying outside and conventional process
Dislocation density Comparative result of the substrate through delaying outside.
The correction data of table 1
| The present invention | Comparative example | |
| Basal plane dislocation density (BPD) | 93cm-2 | 2345m-2 |
| TSD (screw dislocation) | 4468cm-2 | 2265cm-2 |
| TED (sword displacement) | 1368cm-2 | 1543cm-2 |
Embodiment 2
A kind of pre-cleaning method before silicon carbide wafer extension, the growing method is as follows：
(1) silicon carbide substrates, are selected, crystal formation is 4H, and Si faces are chemically mechanical polishing, and Si surface roughness is 0.5nm, C faces
Roughness is 2nm；
(2) H, is heated2SO4And H2O2(2:1) solution being made into is to 120 DEG C, wherein H2SO4Percentage by weight be 98%,
H2O2Percentage by weight be 30%；
(3) silicon carbide substrates, are immersed into 100 DEG C of H2SO4And H2O2(2:1) mixed solution, keeps 400s；
(4) deionized water rinsing, is used；
(5), by Na2O2Powder, by NaOH:Na2O2=3:1 ratio is added in NaOH powder；
(5) NaOH and Na, is heated2O2(3:1) powder reaches molten state to 500 DEG C；
(6) silicon carbide substrates, are immersed into 500 DEG C of NaOH and Na2O2(3:1) melting mixing solution, is kept for 700 seconds；
(7) deionized water rinsing, is used；
(8), dry, prepare extension.
Embodiment 3
A kind of pre-cleaning method before silicon carbide wafer extension, the growing method is as follows：
(1) silicon carbide substrates, are selected, crystal formation is 4H, and Si faces are chemically mechanical polishing, and Si surface roughness is 1nm, and C faces are thick
Rugosity is 1nm；
(2) H, is heated2SO4And H2O2(1:1) solution being made into is to 100 DEG C, wherein H2SO4Percentage by weight be 98%,
H2O2Percentage by weight be 30%；
(3) silicon carbide substrates, are immersed into 80 DEG C of H2SO4And H2O2(1:1) mixed solution, keeps 1000s；
(4) deionized water rinsing, is used；
(5), by Na2O2Powder, by NaOH:Na2O2=9:5 ratio is added in NaOH powder；
(5) NaOH and Na, is heated2O2(4:1) powder reaches molten state to 400 DEG C；
(6) silicon carbide substrates, are immersed into 400 DEG C of NaOH and Na2O2(9:5) melting mixing solution, is kept for 500 seconds；
(7) deionized water rinsing, is used；
(8), dry, prepare extension.
Embodiment 4
A kind of pre-cleaning method before silicon carbide wafer extension, the growing method is as follows：
(1) silicon carbide substrates, are selected, crystal formation is 4H, and Si faces are chemically mechanical polishing, and Si surface roughness is 0.2nm, C faces
Roughness is 5nm；
(2) H, is heated2SO4And H2O2(2:1) solution being made into is to 100 DEG C, wherein H2SO4Percentage by weight be 98%,
H2O2Percentage by weight be 30%；
(3) silicon carbide substrates, are immersed into 100 DEG C of H2SO4And H2O2(2:1) mixed solution, keeps 600s；
(4) deionized water rinsing, is used；
(5), by Na2O2Powder, by NaOH:Na2O2=9:1 ratio is added in NaOH powder；
(5) NaOH and Na, is heated2O2(9:1) powder reaches molten state to 500 DEG C；
(6) silicon carbide substrates, are immersed into 500 DEG C of NaOH and Na2O2(9:1) melting mixing solution, is kept for 900 seconds；
(7) deionized water rinsing, is used；
(8), dry, prepare extension.
Embodiment 5
A kind of pre-cleaning method before silicon carbide wafer extension, the growing method is as follows：
(1) silicon carbide substrates, are selected, crystal formation is 4H, and Si faces are chemically mechanical polishing, and Si surface roughness is 0.3nm, C faces
Roughness is 3nm；
(2) H, is heated2SO4And H2O2(3:1) solution being made into is to 100 DEG C, wherein H2SO4Percentage by weight be 98%,
H2O2Percentage by weight be 30%；
(3) silicon carbide substrates, are immersed into 100 DEG C of H2SO4And H2O2(3:1) mixed solution, keeps 600s；
(4) deionized water rinsing, is used；
(5), by Na2O2Powder, by NaOH:Na2O2=1:5 ratio is added in NaOH powder；
(5) NaOH and Na, is heated2O2(1:5) powder reaches molten state to 500 DEG C；
(6) silicon carbide substrates, are immersed into 500 DEG C of NaOH and Na2O2(1:5) melting mixing solution, is kept for 900 seconds；
(7) deionized water rinsing, is used；
(8), dry, prepare extension.
The pretreated silicon carbide substrates of embodiment 1-5 embodiments are by delaying basal plane dislocation density is reduced to 100/ outside
cm2Below.
Claims (5)
1. a kind of pre-cleaning method before silicon carbide wafer extension, methods described includes：By silicon carbide substrates in H2SO4And H2O2It is mixed
Close after being boiled in solution with after deionized water rinsing, then at NaOH and Na2O2Melt solution in boil, after deionized water rinsing
Drying, it is standby；
The H2SO4And H2O2H in mixed solution2SO4And H2O2Volume ratio be 1-3:1；
The silicon carbide substrates are 6H types or 3C types；
The substrate is in H2SO4And H2O2Boiling temps are 80-120 DEG C in mixed solution；
The NaOH and Na2O2NaOH and Na in melt solution2O2Mass ratio be 1-9:1-5；
The substrate is in NaOH and Na2O2Fused solution in boiling temps be 400-550 DEG C；
The NaOH and Na2O2The hybrid mode of fused solution is by Na2O2Powder reheats after being added in NaOH powder or will
Na2O2Powder is added in NaOH fused solutions.
2. pre-cleaning method as claimed in claim 1, it is characterised in that：Chemical machinery is passed through in the Si faces of the silicon carbide substrates
Polish (CMP) processing；The Si surface roughness of the silicon carbide substrates is 0.01-1nm.
3. the pre-cleaning method as described in claim 1 or 2 is any, it is characterised in that：The C surface roughness of the silicon carbide substrates
For 1-5nm.
4. pre-cleaning method as claimed in claim 1, it is characterised in that：The substrate is in H2SO4And H2O2In mixed solution
Boiling time is 5-1200s.
5. pre-cleaning method as claimed in claim 1, it is characterised in that：The substrate is in NaOH and Na2O2Melting mixing melt
Boiling time in liquid is 3-900s.
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| CN104505338B true CN104505338B (en) | 2017-11-07 |
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| CN112259451B (en) * | 2020-09-22 | 2022-11-29 | 山东天岳先进科技股份有限公司 | Dislocation identification method of silicon carbide wafer, silicon carbide wafer and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3421956A (en) * | 1964-03-06 | 1969-01-14 | Ibm | Method of etching sic |
| CN102502637A (en) * | 2011-10-08 | 2012-06-20 | 江苏佳宇资源利用股份有限公司 | Method for removing silicon dioxide (SiO2) component in silicon carbide micropowder |
| CN103088426A (en) * | 2013-01-23 | 2013-05-08 | 保定科瑞晶体有限公司 | Method for reducing seed crystal growth face defects of silicon carbide crystals |
| CN103489760A (en) * | 2013-09-06 | 2014-01-01 | 西安电子科技大学 | SiC substrate homoepitaxy carbon silicon double-atomic-layer film method |
| CN103949429A (en) * | 2014-04-25 | 2014-07-30 | 哈尔滨工业大学 | Silicon carbide monocrystal washing method |
| CN104112652A (en) * | 2013-04-22 | 2014-10-22 | 住友电气工业株式会社 | Method for manufacturing silicon carbide substrate |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5519305B2 (en) * | 2010-01-25 | 2014-06-11 | トヨタ自動車株式会社 | Method for detecting defects in silicon carbide single crystal |
| US8900979B2 (en) * | 2011-11-23 | 2014-12-02 | University Of South Carolina | Pretreatment method for reduction and/or elimination of basal plane dislocations close to epilayer/substrate interface in growth of SiC epitaxial films |
-
2014
- 2014-12-24 CN CN201410814598.8A patent/CN104505338B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3421956A (en) * | 1964-03-06 | 1969-01-14 | Ibm | Method of etching sic |
| CN102502637A (en) * | 2011-10-08 | 2012-06-20 | 江苏佳宇资源利用股份有限公司 | Method for removing silicon dioxide (SiO2) component in silicon carbide micropowder |
| CN103088426A (en) * | 2013-01-23 | 2013-05-08 | 保定科瑞晶体有限公司 | Method for reducing seed crystal growth face defects of silicon carbide crystals |
| CN104112652A (en) * | 2013-04-22 | 2014-10-22 | 住友电气工业株式会社 | Method for manufacturing silicon carbide substrate |
| CN103489760A (en) * | 2013-09-06 | 2014-01-01 | 西安电子科技大学 | SiC substrate homoepitaxy carbon silicon double-atomic-layer film method |
| CN103949429A (en) * | 2014-04-25 | 2014-07-30 | 哈尔滨工业大学 | Silicon carbide monocrystal washing method |
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