CN112490122A - Metal-assisted photochemical n-type silicon carbide etching method - Google Patents
Metal-assisted photochemical n-type silicon carbide etching method Download PDFInfo
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- CN112490122A CN112490122A CN202011502997.2A CN202011502997A CN112490122A CN 112490122 A CN112490122 A CN 112490122A CN 202011502997 A CN202011502997 A CN 202011502997A CN 112490122 A CN112490122 A CN 112490122A
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- silicon carbide
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- 238000005530 etching Methods 0.000 title claims abstract description 73
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 63
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 57
- 239000002184 metal Substances 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000013078 crystal Substances 0.000 claims abstract description 34
- 238000004544 sputter deposition Methods 0.000 claims abstract description 11
- 238000002791 soaking Methods 0.000 claims abstract description 7
- 238000001259 photo etching Methods 0.000 claims abstract description 6
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 7
- 229910052753 mercury Inorganic materials 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 4
- 230000010355 oscillation Effects 0.000 claims description 4
- 238000000137 annealing Methods 0.000 claims description 3
- 238000000059 patterning Methods 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 238000002844 melting Methods 0.000 abstract description 5
- 230000008018 melting Effects 0.000 abstract description 5
- 239000002923 metal particle Substances 0.000 abstract description 4
- 150000002739 metals Chemical class 0.000 abstract description 3
- 238000006552 photochemical reaction Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 238000001039 wet etching Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000001020 plasma etching Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000005289 physical deposition Methods 0.000 description 1
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
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- 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
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/30604—Chemical etching
-
- 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
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/308—Chemical or electrical treatment, e.g. electrolytic etching using masks
- H01L21/3081—Chemical or electrical treatment, e.g. electrolytic etching using masks characterised by their composition, e.g. multilayer masks, materials
Abstract
The invention relates to a metal-assisted photochemical n-type silicon carbide etching method, which divides an etching process into three stages, wherein the first stage comprises the following steps: sputtering a metal film on the surface of the n-type silicon carbide and carrying out graphical treatment; and a second stage: laser scanning is carried out before etching, and the light receiving position exceeds the photochemical etching melting threshold value, so that the depth-to-width ratio of etching can be effectively improved; and a third stage: soaking n-type silicon carbide single crystal chip in H2O2Etching reaction is carried out in HF solution, and photochemical reaction is carried out with the assistance of ultraviolet light. The invention adopts inert metals such as Pt, W, Ti and the like as metal masks and adopts H2O2And HF is used as an etching solution, no metal element exists in the etching solution, the etching solution and the metal mask can not react in the etching process, and metal particles of the metal mask can not be released into the etching solution, so that metal pollution is effectively avoided.
Description
Technical Field
The invention relates to the technical field of silicon carbide etching, in particular to a metal-assisted photochemical n-type silicon carbide etching method.
Background
SiC is a new-generation semiconductor material having excellent material characteristics such as three times the energy band width, 10 times the high insulating and electric field resistance, 2 times the saturated electron velocity, and 3 times the excellent thermal conductivity as compared with silicon materials; the power consumption is relatively low, the generated heat is less, and the efficiency is high.
SiC single crystals are very inert materials to chemical agents, and wet etching of SiC single crystals is very difficult. Neither acid nor base can corrode SiC single crystals at room temperature.
The current SiC etching methods mainly include dry plasma reactive ion etching and molten salt wet etching. Among them, dry plasma reactive ion etching of SiC single crystals is easy, but obtaining a mask material with a high selectivity ratio is challenging; the metal mask material can effectively improve the etching selection ratio, but in the etching process, metal particles sputtered from the metal mask can generate non-volatile metal byproducts, so that metal pollution in the whole device process is formed. Compared with wet process equipment, dry process equipment is relatively invested, element is mostly adopted as reaction gas, and the atmospheric environment is destroyed by reaction tail gas, so tail gas treatment is also a difficulty of the process. The molten salt wet etching method is to etch SiC single crystal at 450-600 deg.CoKOH, NaOH or Na meltable under C2O2And (6) corrosion. In these molten salts, SiC is first oxidized, and then the oxide is removed by the molten salt. The low aspect ratio of the molten salt wet etching method is not favorable for the preparation of the micro-electromechanical structure with the nanometer scale, and can easily cause serious K, Na contamination.
Therefore, the present invention was made in view of the above problems of the silicon carbide etching method, and the present invention was made.
Disclosure of Invention
The invention aims to provide a metal-assisted photochemical n-type silicon carbide etching method which can effectively avoid metal pollution.
In order to achieve the purpose, the invention adopts the technical scheme that:
a metal-assisted photochemical n-type silicon carbide etching method comprising the steps of:
step 1, cleaning a silicon carbide single crystal chip;
step 2, sputtering a metal film on the surface of the n-type silicon carbide single crystal chip and carrying out graphical treatment, wherein the metal film is a Pt, W or Ti film; after patterning, heating to 1200 ℃ at 800 ℃ for 20-30 minutes under argon, maintaining the temperature for 10-15 minutes, and then annealing;
step 3, performing laser scanning on the n-type silicon carbide single crystal chip;
specifically, an n-type silicon carbide single crystal chip is placed on a moving platform, and femtosecond laser is used for full-area scanning;
step 4, carrying out photochemical etching treatment on the n-type silicon carbide single crystal chip after laser scanning;
specifically, mixing H2O2Mixing with HF to form etching solution, placing the etching solution in an ultrasonic cleaning tank, soaking the laser-scanned n-type silicon carbide single crystal chip in the etching solution for 30-90 min, and applying ultrasonic oscillation and ultraviolet mercury lamp irradiation while soaking.
In the step 2, before sputtering the metal film, the surface of the silicon carbide single crystal chip is sputtered by argon plasma, and cleaning is performed.
In the step 2, the thickness of the metal film is 150-300 nm.
In the step 3, the laser wavelength is 351--2(ii) a The laser spot diameter D was 10 ± 1 μm, the scanning speed was v, the laser pulse frequency f, and the number of accumulated pulses n = (D × f)/v.
In said step 4, H2O2The mixing ratio with HF is 1: 1.
in said step 4, H2O2In a concentration of 0.06mol L-1The concentration of HF was 1.31molL-1。
In the step 4, the light intensity of the ultraviolet mercury lamp is 15-30W, the peak wavelength is 254nm, and the light source is placed at a position 0.5-1mm away from the liquid level of the etching solution.
After the scheme is adopted, the etching process is divided into three stages, wherein the first stage comprises the following steps: sputtering a metal film on the surface of the n-type silicon carbide and carrying out graphical treatment; and a second stage: laser scanning is carried out before etching, and the light receiving position exceeds the photochemical etching melting threshold value, so that the depth-to-width ratio of etching can be effectively improved; and a third stage: soaking n-type silicon carbide single crystal chip in H2O2Etching reaction is carried out in HF solution, and photochemical reaction is carried out with the assistance of ultraviolet light. The invention adopts inert metals such as Pt, W, Ti and the like as metal masks and adopts H2O2And HF is used as an etching solution, no metal element exists in the etching solution, the etching solution and the metal mask can not react in the etching process, and metal particles of the metal mask can not be released into the etching solution, so that metal pollution is effectively avoided.
Drawings
FIG. 1 is a flow chart of a sputtering process of the present invention;
FIG. 2 is a schematic view of a laser scanning process of the present invention;
fig. 3 is a schematic diagram of an etching reaction of n-type silicon carbide.
Detailed Description
The invention discloses a metal-assisted photochemical n-type silicon carbide etching method, which specifically comprises the following steps:
step 1, cleaning the silicon carbide single crystal chip. The cleaning here is performed by a conventional liquid cleaning method, for example, RCA cleaning or the like.
Step 2, sputtering is carried out on the surface of the n-type silicon carbide single crystal chip, as shown in fig. 1, specifically as follows:
2.1, sputtering the surface of the silicon carbide single crystal chip by using argon plasma, and cleaning;
step 2.2, sputtering a metal film on the surface of the n-type silicon carbide single crystal chip by PECVD (physical deposition), wherein the metal film is a Pt, W or Ti film, and the film thickness is 150-300 nm. The metal film is used as a mask, which can be used as a catalyst in a subsequent etching reaction process to improve the etching efficiency.
And 2.3, after the metal film is sputtered, carrying out patterning treatment on the metal film, wherein the patterned part can expose the surface of the silicon carbide single crystal chip.
And 2.4, raising the temperature to 1200 ℃ at 800 ℃ for 20-30 minutes under argon, maintaining the temperature for 10-15 minutes, and then annealing. The conductivity of the metal film and the n-type silicon carbide single crystal chip can be effectively improved through the treatment, and the higher the conductivity is, the higher the subsequent etching rate is.
And 3, performing laser scanning on the n-type silicon carbide single crystal chip.
Specifically, as shown in fig. 2, a silicon carbide single crystal chip was placed on a two-dimensionally controlled moving stage, moved to a fineness of 40 to 50nm, and scanned over the entire area with a femtosecond laser. The laser wavelength is 351-353nm, and the light intensity is 100-150wcm-2(ii) a The laser spot diameter D was 10 ± 1 μm, the scanning speed was v, the laser pulse frequency f, and the number of accumulated pulses n = (D × f)/v.
Generally, the number of pulses and the light intensity are proportional to the aspect ratio of etching and the etching rate, and the larger the number of pulses, the larger the light intensity, the larger the aspect ratio of etching on the silicon carbide single crystal chip, and the faster the etching rate.
In the laser scanning process, for the part without the metal film coverage, laser enters the silicon carbide single crystal chip and gathers energy on the etching surface, and the energy is greater than the melting threshold of the silicon carbide, so that the static state of the etching surface is changed; and at the position where the metal film is provided, the laser energy is weakened, and the energy entering the silicon carbide after passing through the metal film is less than the melting threshold of the silicon carbide, so that the crystalline state of the part is not changed.
And 4, carrying out photochemical etching treatment on the n-type silicon carbide single crystal chip subjected to laser scanning.
Specifically, as shown in FIG. 3, H is2O2Mixing with HF to form etching solution, placing the etching solution in an ultrasonic cleaning tank, and scanning the laser-scanned n-type silicon carbide single crystalSoaking the chip in the etching solution for 30-90 min, and simultaneously applying ultrasonic oscillation and ultraviolet mercury lamp irradiation.
In this embodiment, H2O2In a concentration of 0.06mol L-1The concentration of HF was 1.31molL-1The mixing ratio of the two is 1: 1. wherein H2O2As an oxidizing agent, it reacts silicon carbide to silicon dioxide, which further reacts with HF to H2SiF 6. Ultraviolet mercury lamp irradiation generates hole electron on n-type silicon carbide surface. The light intensity of the ultraviolet mercury lamp is 15-30W, the peak wavelength is 254nm, and the light source is placed at a distance of 0.5-1mm from the liquid surface of the etching solution. In general, the light intensity is proportional to the etching speed, and the stronger the light intensity, the more hole electrons are formed on the surface of the n-type silicon carbide, the more hole electrons are formed, and the faster the etching speed is.
The ultrasonic oscillation can make the etching solution more uniform, so that the etching speed and the etching effect of each part on the single crystal chip are relatively consistent.
In summary, the key point of the present invention is that the etching process is divided into three stages, the first stage: sputtering a metal film on the surface of the n-type silicon carbide and carrying out graphical treatment; and a second stage: laser scanning is carried out before etching, and the light receiving position exceeds the photochemical etching melting threshold value, so that the depth-to-width ratio of etching can be effectively improved; and a third stage: soaking n-type silicon carbide single crystal chip in H2O2Etching reaction is carried out in HF solution, and photochemical reaction is carried out with the assistance of ultraviolet light. The invention adopts inert metals such as Pt, W, Ti and the like as metal masks and adopts H2O2And HF is used as an etching solution, no metal element exists in the etching solution, the etching solution and the metal mask can not react in the etching process, and metal particles of the metal mask can not be released into the etching solution, so that metal pollution is effectively avoided.
The above description is only exemplary of the present invention and is not intended to limit the technical scope of the present invention, so that any minor modifications, equivalent changes and modifications made to the above exemplary embodiments according to the technical spirit of the present invention are within the technical scope of the present invention.
Claims (7)
1. A metal-assisted photochemical n-type silicon carbide etching method is characterized in that: the method comprises the following steps:
step 1, cleaning a silicon carbide single crystal chip;
step 2, sputtering a metal film on the surface of the n-type silicon carbide single crystal chip and carrying out graphical treatment, wherein the metal film is a Pt, W or Ti film; after patterning, heating to 1200 ℃ at 800 ℃ for 20-30 minutes under argon, maintaining the temperature for 10-15 minutes, and then annealing;
step 3, performing laser scanning on the n-type silicon carbide single crystal chip;
specifically, an n-type silicon carbide single crystal chip is placed on a moving platform, and femtosecond laser is used for full-area scanning;
step 4, carrying out photochemical etching treatment on the n-type silicon carbide single crystal chip after laser scanning;
specifically, mixing H2O2Mixing with HF to form etching solution, placing the etching solution in an ultrasonic cleaning tank, soaking the laser-scanned n-type silicon carbide single crystal chip in the etching solution for 30-90 min, and applying ultrasonic oscillation and ultraviolet mercury lamp irradiation while soaking.
2. A metal-assisted photochemical n-type silicon carbide etching process according to claim 1, wherein: in the step 2, before sputtering the metal film, the surface of the silicon carbide single crystal chip is sputtered by argon plasma, and cleaning is performed.
3. A metal-assisted photochemical n-type silicon carbide etching process according to claim 1, wherein: in the step 2, the thickness of the metal film is 150-300 nm.
4. A metal-assisted photochemical n-type silicon carbide etching process according to claim 1, wherein: in the step 3, theThe laser wavelength is 351-353nm, and the light intensity is 100-150wcm-2(ii) a The laser spot diameter D was 10 ± 1 μm, the scanning speed was v, the laser pulse frequency f, and the number of accumulated pulses n = (D × f)/v.
5. A metal-assisted photochemical n-type silicon carbide etching process according to claim 1, wherein: in said step 4, H2O2The mixing ratio with HF is 1: 1.
6. a metal-assisted photochemical n-type silicon carbide etching method according to claim 1 or 5, characterized in that: in said step 4, H2O2In a concentration of 0.06mol L-1The concentration of HF was 1.31molL-1。
7. A metal-assisted photochemical n-type silicon carbide etching process according to claim 1, wherein: in the step 4, the light intensity of the ultraviolet mercury lamp is 15-30W, the peak wavelength is 254nm, and the light source is placed at a position 0.5-1mm away from the liquid level of the etching solution.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011502997.2A CN112490122A (en) | 2020-12-18 | 2020-12-18 | Metal-assisted photochemical n-type silicon carbide etching method |
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| CN202011502997.2A CN112490122A (en) | 2020-12-18 | 2020-12-18 | Metal-assisted photochemical n-type silicon carbide etching method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114150382A (en) * | 2021-12-08 | 2022-03-08 | 浙江大学杭州国际科创中心 | Method and device for stripping n-type silicon carbide single crystal wafer based on photoetching |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08213358A (en) * | 1995-02-02 | 1996-08-20 | Hitachi Ltd | Opticallt pumped etching method |
| DE10256428A1 (en) * | 2002-12-02 | 2004-06-17 | Technische Universität Carolo-Wilhelmina Zu Braunschweig | Structuring surface of electrically conducting semiconductor material comprises applying metal mask on surface of semiconductor material, anodically oxidizing regions not protected, and further processing |
| TW200731018A (en) * | 2006-02-07 | 2007-08-16 | Univ Tsing Hua | Method and apparatus for photoelectrochemical etching |
| CN105845552A (en) * | 2016-03-14 | 2016-08-10 | 山东大学 | Photoelectrochemical etching method for removing SiC substrate epitaxial graphene buffer layer |
| CN111071986A (en) * | 2019-12-30 | 2020-04-28 | 北京航空航天大学 | Method for preparing silicon carbide multilevel microstructure with assistance of laser modification and acceleration sensor |
-
2020
- 2020-12-18 CN CN202011502997.2A patent/CN112490122A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08213358A (en) * | 1995-02-02 | 1996-08-20 | Hitachi Ltd | Opticallt pumped etching method |
| DE10256428A1 (en) * | 2002-12-02 | 2004-06-17 | Technische Universität Carolo-Wilhelmina Zu Braunschweig | Structuring surface of electrically conducting semiconductor material comprises applying metal mask on surface of semiconductor material, anodically oxidizing regions not protected, and further processing |
| TW200731018A (en) * | 2006-02-07 | 2007-08-16 | Univ Tsing Hua | Method and apparatus for photoelectrochemical etching |
| CN105845552A (en) * | 2016-03-14 | 2016-08-10 | 山东大学 | Photoelectrochemical etching method for removing SiC substrate epitaxial graphene buffer layer |
| CN111071986A (en) * | 2019-12-30 | 2020-04-28 | 北京航空航天大学 | Method for preparing silicon carbide multilevel microstructure with assistance of laser modification and acceleration sensor |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114150382A (en) * | 2021-12-08 | 2022-03-08 | 浙江大学杭州国际科创中心 | Method and device for stripping n-type silicon carbide single crystal wafer based on photoetching |
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Application publication date: 20210312 |