CN103949429A - Silicon carbide monocrystal washing method - Google Patents
Silicon carbide monocrystal washing method Download PDFInfo
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- CN103949429A CN103949429A CN201410178793.6A CN201410178793A CN103949429A CN 103949429 A CN103949429 A CN 103949429A CN 201410178793 A CN201410178793 A CN 201410178793A CN 103949429 A CN103949429 A CN 103949429A
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- hydrogen peroxide
- sulfuric acid
- concentrated sulfuric
- mixed solution
- silicon carbide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/02—Cleaning by the force of jets or sprays
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
A silicon carbide monocrystal washing method relates to a monocrystal washing method. The invention aims to solve the technical problem that the steps of the conventional SiC washing method are complicated. The method comprises the following steps: soaking SiC monocrystal in a mixed solution A at a temperature of 75-85DEG C for 15-25min; then flushing the SiC monocrystal with deionized water, and blow-drying by nitrogen gas. The mixed solution A is a mixed solution of concentrated sulfuric acid and hydrogen peroxide, and the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is (2.8-3.2) : 1. The SiC monocrystal washing method has great repeatability, the washed SiC monocrystal has high cleanliness, only three elements of Si, O and C are available in the surface of the washed SiC monocrystal, and the carbon impurity content is 10% per tone. Equipment adopted for washing are simple, the operation is convenient and easy to grasp, and the process is safe and pollution-free. The invention belongs to the field of monocrystal washing.
Description
Technical field
The present invention relates to a kind of cleaning method of monocrystalline.
Background technology
Carborundum (SiC) is IV-IV compounds of group, have that thermal conductivity is high, critical breakdown electric field is high, flow the advantages such as sub-saturation drift velocity is high, energy gap is large, unique a kind of solid carbon compound in ShiⅣ family, has huge application potential at aspects such as high temperature, high frequency, high power, photoelectron and radioresistances.SiC is as semiconductor device material, very high to its surface cleanness requirement, because surface contaminant has great impact to SiC performance of semiconductor device, stability and circuit yield; SiC is as the base material of GaN film growth, because the contaminating impurity of its polished surface can directly have influence on the quality of epitaxial layer, badly influences the luminescent properties of GaN based light-emitting diode (LED); SiC is as a kind of spacing reflection mirror material of function admirable, and the cleannes of burnishing surface can have influence on the optical property of SiC speculum.To sum up, to the effectively clean of SiC, be very important.
The surface clean method of SiC monocrystalline has plasma cleaning, hydrogen to process cleaning, Chemical cleaning etc. at present.Plasma cleaning easily causes surface, and sub-surface damage even affects service life and the stability of device; Hydrogen is processed to clean needs special experimental facilities, and energy loss is large; At present wet-cleaned in SiC single-crystal surface purifies still in leading position.And though wet-cleaning method has a lot, substantially continue to use the method for clean monocrystalline silicon, for SiC, complex steps, cleaning performance is undesirable.
Summary of the invention
The object of the invention is, in order to solve the loaded down with trivial details technical problem of method step of existing cleaning SiC, provides a kind of cleaning method of single-crystal silicon carbide.
The cleaning method of single-crystal silicon carbide carries out according to following steps:
SiC monocrystalline in being the mixed solution A of 75～85 ℃, temperature is soaked to 15～25min, then use deionized water rinsing SiC monocrystalline, nitrogen dries up again, and described mixed solution A is the mixed liquor of the concentrated sulfuric acid and hydrogen peroxide, and wherein the volume ratio of the concentrated sulfuric acid and hydrogen peroxide is 2.8～3.2:1.
The cleaning method of single-crystal silicon carbide carries out according to following steps:
One, adopt surfactant to scrub SiC monocrystalline 3～5min, then use deionized water rinsing SiC monocrystalline;
Two, the SiC monocrystalline of processing through step 1 in being the mixed solution A of 75～85 ℃, temperature is soaked to 15～25min, then use deionized water rinsing SiC monocrystalline, nitrogen dries up again, described mixed solution A is the mixed liquor of the concentrated sulfuric acid and hydrogen peroxide, and wherein the volume ratio of the concentrated sulfuric acid and hydrogen peroxide is 2.8～3.2:1.
Surfactant in this experimental procedure one is produced by Liqui-Nox or deconex.
The cleaning method of SiC monocrystalline of the present invention is a kind of wet-chemical clean method of multi-step, can effectively solve the problem that SiC single-crystal surface is difficult to surface contaminant to clean up because of the stable not soluble existing cleaning method causing of surface nature.The cleaning method of SiC monocrystalline of the present invention is reproducible, clean SiC monocrystalline cleanliness factor high, the SiC single-crystal surface after cleaning only has Si, O, tri-kinds of elements of C, wherein carbon impurity content <10%.Clean the equipment adopting simple, easy to operate, be easy to grasp process safety, pollution-free.
The invention has the beneficial effects as follows:
(1), for the surface characteristic of SiC monocrystalline, two kinds of wet chemical cleans methods for the monocrystal SiC of different pollution levels have been probed into.The single-crystal surface obtaining is enough clean, in the future single-crystal surface performance study and commercial Application being laid a good foundation.
(2) overcome the shortcoming of the wet chemical cleans method of cleaning for SiC material at present, for example, RCA method, step is various, and cleaning performance is not good enough.Cleaning method in the present invention is simple, and energy consumption is few, and cost is low, and cleaning performance is good.
Accompanying drawing explanation
Fig. 1 is the AFM photo of undressed SiC monocrystalline in experiment one;
Fig. 2 is through testing the AFM photo of the SiC monocrystalline of a processing;
Fig. 3 is the AFM photo of undressed SiC monocrystalline in experiment two;
Fig. 4 is through testing the AFM photo of the SiC monocrystalline of two processing.
The specific embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises any combination between each specific embodiment.
The specific embodiment one: the cleaning method of present embodiment single-crystal silicon carbide carries out according to following steps:
One, adopt surfactant to scrub SiC monocrystalline 3～5min, then use deionized water rinsing SiC monocrystalline;
Two, the SiC monocrystalline of processing through step 1 in being the mixed solution A of 75～85 ℃, temperature is soaked to 15～25min, then use deionized water rinsing SiC monocrystalline, nitrogen dries up again, described mixed solution A is the mixed liquor of the concentrated sulfuric acid and hydrogen peroxide, and wherein the volume ratio of the concentrated sulfuric acid and hydrogen peroxide is 2.8～3.2:1.
The mass concentration of the concentrated sulfuric acid described in present embodiment is 98%, and hydrogen peroxide is that mass concentration is 30% commercially available hydrogen peroxide.
The concentrated sulfuric acid described in present embodiment, hydrogen peroxide are commercially available prod.
The specific embodiment two: what present embodiment was different from the specific embodiment one is that surfactant described in step 1 is anion surfactant.Other is identical with the specific embodiment one.
The specific embodiment three: present embodiment is different from one of the specific embodiment one or two is that the time of scrubbing SiC monocrystalline described in step 1 is 4min.Other is identical with one of the specific embodiment one or two.
The specific embodiment four: present embodiment is different from one of specific embodiment one to three is to soak in temperature is the mixed solution A of 80 ℃ in step 2.Other is identical with one of specific embodiment one to three.
The specific embodiment five: what present embodiment was different from one of specific embodiment one to four is that in step 2, mixed solution A is the mixed liquor of the concentrated sulfuric acid and hydrogen peroxide, and wherein the volume ratio of the concentrated sulfuric acid and hydrogen peroxide is 3:1.Other is identical with one of specific embodiment one to four.
The specific embodiment six: what present embodiment was different from one of specific embodiment one to five is that in step 2, mixed solution A is the mixed liquor of the concentrated sulfuric acid and hydrogen peroxide, and wherein the volume ratio of the concentrated sulfuric acid and hydrogen peroxide is 3.1:1.Other is identical with one of specific embodiment one to five.
The specific embodiment seven: the cleaning method of present embodiment single-crystal silicon carbide carries out according to following steps:
SiC monocrystalline in being the mixed solution A of 75～85 ℃, temperature is soaked to 15～25min, then use deionized water rinsing SiC monocrystalline, nitrogen dries up again, and described mixed solution A is the mixed liquor of the concentrated sulfuric acid and hydrogen peroxide, and wherein the volume ratio of the concentrated sulfuric acid and hydrogen peroxide is 2.8～3.2:1.
The specific embodiment eight: present embodiment is different from the specific embodiment seven is that SiC monocrystalline is soaked in temperature is the mixed solution A of 78 ℃.Other is identical with the specific embodiment seven.
The specific embodiment nine: what present embodiment was different from the specific embodiment seven or eight is that described mixed solution A is the mixed liquor of the concentrated sulfuric acid and hydrogen peroxide, and wherein the volume ratio of the concentrated sulfuric acid and hydrogen peroxide is 2.9:1.Other is identical with the specific embodiment seven or eight.
The specific embodiment ten: what present embodiment was different from one of specific embodiment seven to nine is that described mixed solution A is the mixed liquor of the concentrated sulfuric acid and hydrogen peroxide, and wherein the volume ratio of the concentrated sulfuric acid and hydrogen peroxide is 3.1:1.Other is identical with one of specific embodiment seven to nine.
Adopt following experimental verification effect of the present invention:
Experiment one:
The cleaning method of the single-crystal silicon carbide that pollution level is lower carries out according to following steps:
SiC monocrystalline is soaked to 17min in temperature is the mixed solution A of 76 ℃, then use deionized water rinsing SiC monocrystalline, then nitrogen dries up, described mixed solution A is the mixed liquor of the concentrated sulfuric acid and hydrogen peroxide, and wherein the volume ratio of the concentrated sulfuric acid and hydrogen peroxide is 3:1.
The mass concentration of the concentrated sulfuric acid described in this experiment is 98%, and hydrogen peroxide is that mass concentration is 30% commercially available hydrogen peroxide.
In this experiment, adopt polytetrafluoroethylcontainer container.
The nitrogen adopting in this experiment is the High Purity Nitrogen of mass fraction 99.999%.
To the lower SiC monocrystalline of the pollution level of processing without experiment one with through testing the SiC monocrystalline of a processing, carry out x-ray photoelectron spectroscopy (XPS) test.The SiC single-crystal surface carbon impurity content 15～18% cleaning without the method for experiment one, the SiC single-crystal surface carbon impurity content 8～9% after testing a processing.
To the lower SiC monocrystalline (Fig. 1) of the pollution level of processing without experiment one with through testing the SiC monocrystalline (Fig. 2) of a processing, carry out AFM (AFM) sign.The visible single-crystal surface of AFM photo by Fig. 1 has particulate contaminants, and surface is unclean; From the AFM photo of Fig. 2, surface, without any pollutant, shows platform-ledge structure.
The surface contact angle <5o of the SiC monocrystalline after testing a processing, water approaches and sprawls at α-Al2O3 single-crystal surface.
Visible, the SiC monocrystalline cleanliness factor after testing a processing is high, and it is simple, easy to operate to clean the equipment adopting, and is easy to grasp process safety, pollution-free.
Experiment two:
The cleaning method of the single-crystal silicon carbide that pollution level is higher carries out according to following steps:
One, adopt surfactant to scrub SiC monocrystalline 5min, then use deionized water rinsing SiC monocrystalline;
Two, the SiC monocrystalline of processing through step 1 in being the mixed solution A of 80 ℃, temperature is soaked to 20min, then use deionized water rinsing SiC monocrystalline, nitrogen dries up again, and described mixed solution A is the mixed liquor of the concentrated sulfuric acid and hydrogen peroxide, and wherein the volume ratio of the concentrated sulfuric acid and hydrogen peroxide is 3:1.
The mass concentration of the concentrated sulfuric acid described in this experiment is 98%, and hydrogen peroxide is that mass concentration is 30% commercially available hydrogen peroxide.
In this experiment, adopt polytetrafluoroethylcontainer container.
The nitrogen adopting in this experiment is the High Purity Nitrogen of mass fraction 99.999%.
The purification cleaning agent that surfactant in this experimental procedure one is produced by Liqui-Nox (mainly the homogeneous mixture by linear alkylaryl sodium sulfonate, sodium xylene sulfonate, alkanolamide and ethoxy alcohol forms).
To the higher SiC monocrystalline of the pollution level of processing without experiment two with through testing the SiC monocrystalline of two processing, carry out x-ray photoelectron spectroscopy (XPS) test, the SiC single-crystal surface carbon impurity content 18～21% cleaning without the method for experiment two, the SiC single-crystal surface carbon impurity content 8～9% after testing two processing.
To the higher SiC monocrystalline (Fig. 3) of the pollution level of processing without experiment two with through testing the SiC monocrystalline (Fig. 4) of two processing, carry out AFM (AFM) sign.The visible single-crystal surface of AFM photo by Fig. 3 has particulate contaminants, and surface is unclean; From the AFM photo of Fig. 4, surface, without any pollutant, shows platform-ledge structure.
The surface contact angle <5o of the SiC monocrystalline after testing two processing, water approaches and sprawls at α-Al2O3 single-crystal surface.
Visible, the SiC monocrystalline cleanliness factor after testing two processing is high, and it is simple, easy to operate to clean the equipment adopting, and is easy to grasp process safety, pollution-free.
Claims (10)
1. the cleaning method of single-crystal silicon carbide, is characterized in that the cleaning method of single-crystal silicon carbide carries out according to following steps:
One, adopt surfactant to scrub SiC monocrystalline 3～5min, then use deionized water rinsing SiC monocrystalline;
Two, the SiC monocrystalline of processing through step 1 in being the mixed solution A of 75～85 ℃, temperature is soaked to 15～25min, then use deionized water rinsing SiC monocrystalline, nitrogen dries up again, described mixed solution A is the mixed liquor of the concentrated sulfuric acid and hydrogen peroxide, and wherein the volume ratio of the concentrated sulfuric acid and hydrogen peroxide is 2.8～3.2:1.
2. the cleaning method of single-crystal silicon carbide according to claim 1, is characterized in that surfactant described in step 1 is anion surfactant.
3. according to the cleaning method of single-crystal silicon carbide described in claim 1 or 2, the time that it is characterized in that scrubbing described in step 1 SiC monocrystalline is 4min.
4. according to the cleaning method of single-crystal silicon carbide described in claim 1 or 2, it is characterized in that in step 2 soaking in temperature is the mixed solution A of 80 ℃.
5. according to the cleaning method of single-crystal silicon carbide described in claim 1 or 2, it is characterized in that in step 2, mixed solution A is the mixed liquor of the concentrated sulfuric acid and hydrogen peroxide, wherein the volume ratio of the concentrated sulfuric acid and hydrogen peroxide is 3:1.
6. according to the cleaning method of single-crystal silicon carbide described in claim 1 or 2, it is characterized in that in step 2, mixed solution A is the mixed liquor of the concentrated sulfuric acid and hydrogen peroxide, wherein the volume ratio of the concentrated sulfuric acid and hydrogen peroxide is 3.1:1.
7. the cleaning method of single-crystal silicon carbide, is characterized in that the cleaning method of single-crystal silicon carbide carries out according to following steps:
SiC monocrystalline in being the mixed solution A of 75～85 ℃, temperature is soaked to 15～25min, then use deionized water rinsing SiC monocrystalline, nitrogen dries up again, and described mixed solution A is the mixed liquor of the concentrated sulfuric acid and hydrogen peroxide, and wherein the volume ratio of the concentrated sulfuric acid and hydrogen peroxide is 2.8～3.2:1.
8. the cleaning method of single-crystal silicon carbide according to claim 7, is characterized in that SiC monocrystalline to soak in temperature is the mixed solution A of 78 ℃.
9. the cleaning method of single-crystal silicon carbide according to claim 7, is characterized in that described mixed solution A is the mixed liquor of the concentrated sulfuric acid and hydrogen peroxide, and wherein the volume ratio of the concentrated sulfuric acid and hydrogen peroxide is 2.9:1.
10. the cleaning method of single-crystal silicon carbide according to claim 7, is characterized in that described mixed solution A is the mixed liquor of the concentrated sulfuric acid and hydrogen peroxide, and wherein the volume ratio of the concentrated sulfuric acid and hydrogen peroxide is 3.1:1.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104505338A (en) * | 2014-12-24 | 2015-04-08 | 国家电网公司 | Pre-cleaning method before epitaxy of silicon carbide wafer |
| CN104810255A (en) * | 2015-02-28 | 2015-07-29 | 株洲南车时代电气股份有限公司 | Method of removing carbon protection film on surface of silicon carbide device |
| CN105837259A (en) * | 2016-04-14 | 2016-08-10 | 中国科学院上海硅酸盐研究所 | Method for corroding silicon carbide ceramics |
| CN109037035A (en) * | 2018-07-31 | 2018-12-18 | 成都海威华芯科技有限公司 | A kind of method and system for improving SiC base GaN wafer and carrying on the back golden adhesiveness |
| CN112980599A (en) * | 2021-02-23 | 2021-06-18 | 哈尔滨工业大学 | Silicon carbide single crystal cleaning agent and application thereof |
| CN113862792A (en) * | 2021-09-27 | 2021-12-31 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Method for cleaning silicon carbide seed crystal |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104505338A (en) * | 2014-12-24 | 2015-04-08 | 国家电网公司 | Pre-cleaning method before epitaxy of silicon carbide wafer |
| CN104505338B (en) * | 2014-12-24 | 2017-11-07 | 国家电网公司 | Pre-cleaning method before a kind of silicon carbide wafer extension |
| CN104810255A (en) * | 2015-02-28 | 2015-07-29 | 株洲南车时代电气股份有限公司 | Method of removing carbon protection film on surface of silicon carbide device |
| CN105837259A (en) * | 2016-04-14 | 2016-08-10 | 中国科学院上海硅酸盐研究所 | Method for corroding silicon carbide ceramics |
| CN109037035A (en) * | 2018-07-31 | 2018-12-18 | 成都海威华芯科技有限公司 | A kind of method and system for improving SiC base GaN wafer and carrying on the back golden adhesiveness |
| CN112980599A (en) * | 2021-02-23 | 2021-06-18 | 哈尔滨工业大学 | Silicon carbide single crystal cleaning agent and application thereof |
| CN113862792A (en) * | 2021-09-27 | 2021-12-31 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Method for cleaning silicon carbide seed crystal |
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Application publication date: 20140730 |