CN109560023A - A kind of nitration mixture and its cleaning method cleaning monocrystalline silicon piece - Google Patents
A kind of nitration mixture and its cleaning method cleaning monocrystalline silicon piece Download PDFInfo
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- CN109560023A CN109560023A CN201811257851.9A CN201811257851A CN109560023A CN 109560023 A CN109560023 A CN 109560023A CN 201811257851 A CN201811257851 A CN 201811257851A CN 109560023 A CN109560023 A CN 109560023A
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- nitration mixture
- monocrystalline silicon
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- silicon piece
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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
- H01L21/02041—Cleaning
- H01L21/02057—Cleaning during device manufacture
-
- 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
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/67005—Apparatus not specifically provided for elsewhere
- H01L21/67011—Apparatus for manufacture or treatment
- H01L21/67017—Apparatus for fluid treatment
- H01L21/67028—Apparatus for fluid treatment for cleaning followed by drying, rinsing, stripping, blasting or the like
- H01L21/6704—Apparatus for fluid treatment for cleaning followed by drying, rinsing, stripping, blasting or the like for wet cleaning or washing
- H01L21/67057—Apparatus for fluid treatment for cleaning followed by drying, rinsing, stripping, blasting or the like for wet cleaning or washing with the semiconductor substrates being dipped in baths or vessels
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- 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)
- Cleaning Or Drying Semiconductors (AREA)
Abstract
The invention discloses a kind of nitration mixture and its cleaning method for cleaning monocrystalline silicon piece, and nitration mixture includes 20-30 parts of nitric acid；5-10 parts of hydrofluoric acid；15-25 parts of acetic acid；Remaining is water.Cleaning method includes step 1: monocrystalline silicon piece being dipped into nitration mixture and is impregnated；Step 2: taking-up monocrystalline silicon piece, which is put into deionized water, after immersion first rinses, then impregnates in deionized water.Nitration mixture of the invention can effectively remove metal impurities and sull on monocrystalline silicon piece, control removal degree and speed, will not only generate damage to monocrystalline silicon sheet surface, but also can reach cleannes requirement of the manufacturing process to silicon wafer.
Description
Technical field
The present invention relates to semiconductor device cleaning technique fields, and in particular to a kind of nitration mixture for cleaning monocrystalline silicon piece and its clear
Washing method.
Background technique
Ordinary silicon chip resistivity is all 1-5 Ω-cm, and low-resistivity is more than the doping of conventional, electric-resistance rate, leads to material
Matter is different.In silicon process of producing product, almost every procedure has the problem of Wafer Cleaning, and the quality of Wafer Cleaning is to device
Part performance has serious influence, and dealing with improperly may be such that whole silicon wafers scrap, and Wafer Cleaning from silicon wafer either for processing
People still for be engaged in semiconductor devices production people for suffer from important meaning, so semiconductor devices produce
In, silicon product must be cleaned strictly, because micropollution also results in component failure.The purpose of cleaning is to remove surface dirt
Contaminate impurity, including organic matter and inorganic matter.These impurity some with state of atom or ionic condition, some in the form of a film or
Particle shape formula is present in silicon chip surface, and chemical cleaning is exactly in order to except sightless pollutions such as removal atom, ions.
The prior art is primarily directed to a kind of cleaning process of mortar cutting monocrystalline silicon piece, and to applied to semiconductor
When monocrystalline silicon piece in industry is cleaned, this kind of cleaning process etch period is too long, is easy to during impregnating etching
The functionality of monocrystalline silicon piece is damaged, while can also shorten the service life of itself.Due to the mixed acid solution cleaning in the technique
Requirement of the manufacturing process to cleaning of silicon wafer degree is not achieved, a simple processing can only be carried out to silicon chip surface, is more not achieved
Except the effect of damaged layer on surface of silicon slice.
Summary of the invention
The present invention in view of the above technical problems, provides a kind of nitration mixture and its cleaning method for cleaning monocrystalline silicon piece,.
In order to solve the above technical problems, the technical solution adopted by the present invention is that: a kind of nitration mixture cleaning monocrystalline silicon piece, nitration mixture
It in parts by weight include following components: 20-30 parts of nitric acid；5-10 parts of hydrofluoric acid；15-25 parts of acetic acid；Remaining is water.
Wherein, nitration mixture score by weight includes following components: 25 parts of nitric acid；8 parts of hydrofluoric acid；20 parts of acetic acid；Remaining is water.
The invention also discloses a kind of cleaning methods cleaned using above-mentioned nitration mixture to monocrystalline silicon piece:
The cleaning method the following steps are included:
Step 1: monocrystalline silicon piece is dipped into nitration mixture and is impregnated；
Step 2: taking-up monocrystalline silicon piece, which is put into deionized water, after immersion first rinses, then impregnates in deionized water.
Wherein, it in step 1, after monocrystalline silicon piece is dipped into nitration mixture, is first had children outside the state plan using ultrasonic wave, makes monocrystalline silicon sheet surface
Infiltration.
Wherein, in step 1, soaking time is 100-300 seconds.
Wherein, in step 1, nitration mixture is that temperature is 10-40 DEG C.
Wherein, in step 1, nitration mixture is that temperature is 15-25 DEG C.
Wherein, the excusing from death time is 5 minutes, and the soaking time is 200 seconds.
Wherein, in step 2, washing time is 3 minutes, and soaking time is 5 minutes.
Wherein, the deionization water temperature rinsed and impregnated in step 2 is 45-55 DEG C.
The beneficial effects of the present invention are:
Nitration mixture of the invention can effectively remove metal impurities and sull on monocrystalline silicon piece, control removal journey
Degree and speed, will not only generate damage to monocrystalline silicon sheet surface, but also can reach cleannes requirement of the manufacturing process to silicon wafer.
Specific embodiment
Exemplary embodiment is not intended to exhaustive all embodiments according to the present invention.It is appreciated that without departing from this hair
It under the premise of bright range, can use other embodiments, the modification of structure or logic can also be carried out.Therefore, with
Under specific descriptions and unrestricted, and the scope of the present invention is defined by the claims appended hereto.
The silicon wafer cleaned will be needed to be immersed in existing single groove ultrasonic slot first, opens ultrasonic wave soaking and washing 5 and divide
Clock is sufficiently humidified so as to silicon chip surface, then by the silicon wafer of low-resistivity (0.005-0.015) using novel kind nitration mixture into
Row etch cleaner 100-300 seconds, and this novel nitration mixture is by the nitric acid of 20%-30%, the hydrofluoric acid of 5%-10%, 15%-
25% acetic acid mixes, referred to as 413 nitration mixture, while low-resistance silicon wafer is performing etching cleaning work using nitration mixture 413
When industry, it need to guarantee that the temperature of nitration mixture is normal temperature state, it is optimal between 20 ± 2 DEG C.During performing etching operation, it is both needed to protect
Card silicon wafer is submerged by mixed acid solution completely, and after nitration mixture etch period, it is necessary at the first time by silicon wafer be put into from
It rinses 3 minutes, then impregnates again 5 minutes in sub- water, while guaranteeing water temperature between 50 ± 5 DEG C.Due to existing monocrystalline silicon piece
For heavily doped monocrystalline silicon, that is, the impurity level being doped with is relatively more, so the different situation of resistivity will occur, and one of which is just
Be low-resistance monocrystalline silicon piece, therefore also have different response feature for the acid etching of monocrystalline silicon piece, and according to oneself this
The many experiments that side is done show that low-resistance silicon wafer is suitable for being etched cleaning with nitration mixture 413, in this way can not only maximum limit
Degree ground removal silicon chip surface can also be effectively removed the impurity being entrained in monocrystalline silicon piece, together because of the damaging layer caused by processing
When reduce the silicon wafer risk that particulate matter is fallen during use, and can guarantee the in-built stability of silicon wafer with
And its it is functional.And it is directed to the residual of silicon chip surface acid pickling, use existing cleaning technique.
Embodiment 1:
The hydrofluoric acid 12.5g for the nitric acid 40g, 40% that mass percent is 50%, 50% acetic acid 30g, water are taken respectively
17.5g is added in a container and mixes, and stirs evenly, wherein in nitration mixture nitric acid 20 part spare as nitration mixture；5 parts of hydrofluoric acid；Acetic acid
15 parts；Remaining is water.
Nitration mixture is added in single groove ultrasonic slot, monocrystalline silicon piece is completely immersed in nitration mixture and is impregnated, in order to guarantee to soak
It is more preferable to steep effect, first being had children outside the state plan 5 minutes with ultrasonic wave makes silicon chip surface complete wetting, then stops excusing from death again and impregnates 300 seconds, passes through
Temperature regulating device controls the temperature of nitration mixture at 40 DEG C.
Silicon chip extracting is rinsed its surface with deionized water by silicon wafer at once after immersion, again by silicon after flushing
Piece, which is put into the container equipped with deionized water, to be impregnated, and the deionized water rinsed and impregnated is 45 DEG C or so.After immersion
It takes out silicon wafer and dries i.e. completion cleaning process.
Nitric acid and acetic acid by said ratio can effective erosion removal silicon chip surface metal impurities, and corruption will not occur
Erosion excessively generates new damage to silicon wafer, and hydrofluoric acid can remove the sull of silicon chip surface.Silicon chip surface is because processing institute
Caused by the impurity of damaging layer and doping again in silicon wafer can effectively be removed, and can guarantee silicon wafer internal structure
Stability and its functionality.
Embodiment 2:
Taking mass percent respectively is 50% nitric acid 50g, 40% hydrofluoric acid 20g, and 80% acetic acid 25g, water 5g add
Enter and mixed in a container, stirs evenly, wherein in nitration mixture nitric acid 25 part spare as nitration mixture；8 parts of hydrofluoric acid；20 parts of acetic acid；Its
Yu Weishui.
Nitration mixture is added in single groove ultrasonic slot, monocrystalline silicon piece is completely immersed in nitration mixture and is impregnated, in order to guarantee to soak
It is more preferable to steep effect, first being had children outside the state plan 5 minutes with ultrasonic wave makes silicon chip surface complete wetting, then stops excusing from death again and impregnates 200 seconds, passes through
Temperature regulating device controls the temperature of nitration mixture at 20 DEG C.
Silicon chip extracting is rinsed its surface with deionized water by silicon wafer at once after immersion, rinses 3 minutes, punching
Silicon wafer is put into the container equipped with deionized water again after washing and is impregnated, is impregnated 5 minutes, the deionization for rinsing and impregnating
Water is 50 DEG C or so.Silicon wafer is taken out after immersion dries i.e. completion cleaning process.
Nitric acid and acetic acid by said ratio can effective erosion removal silicon chip surface metal impurities, and corruption will not occur
Erosion excessively generates new damage to silicon wafer, and hydrofluoric acid can remove the sull of silicon chip surface.Silicon chip surface is because processing institute
Caused by the impurity of damaging layer and doping again in silicon wafer can effectively be removed, and can guarantee silicon wafer internal structure
Stability and its functionality.
Embodiment 3:
Taking mass percent respectively is 70% nitric acid 43g, 40% hydrofluoric acid 25g, and 80% acetic acid 31g, water 1g add
Enter and mixed in a container, stirs evenly, wherein in nitration mixture nitric acid 30 part spare as nitration mixture；10 parts of hydrofluoric acid；25 parts of acetic acid；Its
Yu Weishui.
Nitration mixture is added in single groove ultrasonic slot, monocrystalline silicon piece is completely immersed in nitration mixture and is impregnated, in order to guarantee to soak
It is more preferable to steep effect, first being had children outside the state plan 5 minutes with ultrasonic wave makes silicon chip surface complete wetting, then stops excusing from death again and impregnates 100 seconds, passes through
Temperature regulating device controls the temperature of nitration mixture at 40 DEG C.
Silicon chip extracting is rinsed its surface with deionized water by silicon wafer at once after immersion, rinses 3 minutes, punching
Silicon wafer is put into the container equipped with deionized water again after washing and is impregnated, is impregnated 5 minutes, the deionization for rinsing and impregnating
Water is 55 DEG C or so.Silicon wafer is taken out after immersion dries i.e. completion cleaning process.
Nitric acid and acetic acid by said ratio can effective erosion removal silicon chip surface metal impurities, and corruption will not occur
Erosion excessively generates new damage to silicon wafer, and hydrofluoric acid can remove the sull of silicon chip surface.Silicon chip surface is because processing institute
Caused by the impurity of damaging layer and doping again in silicon wafer can effectively be removed, and can guarantee silicon wafer internal structure
Stability and its functionality.
Embodiment 4:
Taking mass percent respectively is 50% nitric acid 50g, 40% hydrofluoric acid 20g, and 80% acetic acid 25g, water 5g add
Enter and mixed in a container, stirs evenly, wherein in nitration mixture nitric acid 25 part spare as nitration mixture；8 parts of hydrofluoric acid；20 parts of acetic acid；Its
Yu Weishui.
Nitration mixture is added in single groove ultrasonic slot, monocrystalline silicon piece is completely immersed in nitration mixture and is impregnated, in order to guarantee to soak
It is more preferable to steep effect, first being had children outside the state plan 5 minutes with ultrasonic wave makes silicon chip surface complete wetting, then stops excusing from death again and impregnates 200 seconds, passes through
Temperature regulating device controls the temperature of nitration mixture at 15 DEG C.
Silicon chip extracting is rinsed its surface with deionized water by silicon wafer at once after immersion, rinses 3 minutes, punching
Silicon wafer is put into the container equipped with deionized water again after washing and is impregnated, is impregnated 5 minutes, the deionization for rinsing and impregnating
Water is 50 DEG C or so.Silicon wafer is taken out after immersion dries i.e. completion cleaning process.
Embodiment 5:
Taking mass percent respectively is 50% nitric acid 50g, 40% hydrofluoric acid 20g, and 80% acetic acid 25g, water 5g add
Enter and mixed in a container, stirs evenly, wherein in nitration mixture nitric acid 25 part spare as nitration mixture；8 parts of hydrofluoric acid；20 parts of acetic acid；Its
Yu Weishui.
Nitration mixture is added in single groove ultrasonic slot, monocrystalline silicon piece is completely immersed in nitration mixture and is impregnated, in order to guarantee to soak
It is more preferable to steep effect, first being had children outside the state plan 5 minutes with ultrasonic wave makes silicon chip surface complete wetting, then stops excusing from death again and impregnates 200 seconds, passes through
Temperature regulating device controls the temperature of nitration mixture at 25 DEG C.
Silicon chip extracting is rinsed its surface with deionized water by silicon wafer at once after immersion, rinses 3 minutes, punching
Silicon wafer is put into the container equipped with deionized water again after washing and is impregnated, is impregnated 5 minutes, the deionization for rinsing and impregnating
Water is 50 DEG C or so.Silicon wafer is taken out after immersion dries i.e. completion cleaning process.
The present invention comprehensively considers may be to the factor that monocrystalline silicon piece corrasion has an impact, and is directed to these factors
Improvement is made that, such as after obtaining the influence that low-resistance material act on silicon chip erosion by experiment, to configure newly
The mixed acid solution of type carries out more effective etch cleaner to the silicon wafer of the resistance, and ensure that the functionality of single crystal silicon product.Control
The component and proportion of mixed acid solution processed, in addition the control to time and temperature, is allowed to greatest extent performing etching silicon wafer
While, it can also guarantee that the total quality of product will not be influenced because etching excessively, while also can more effectively remove and mix
The miscellaneous impurity in monocrystalline silicon.
Claims (10)
1. a kind of nitration mixture for cleaning monocrystalline silicon piece, which is characterized in that the nitration mixture includes following components in parts by weight: nitric acid
20-30 parts；5-10 parts of hydrofluoric acid；15-25 parts of acetic acid；Remaining is water.
2. a kind of nitration mixture for cleaning monocrystalline silicon piece according to claim 1, which is characterized in that nitration mixture score by weight
Including following components: 25 parts of nitric acid；8 parts of hydrofluoric acid；20 parts of acetic acid；Remaining is water.
3. the cleaning cleaning method of the nitration mixture using a kind of cleaning monocrystalline silicon piece described in claim 1, which is characterized in that including
Following steps:
Step 1: monocrystalline silicon piece is dipped into nitration mixture and is impregnated；
Step 2: taking-up monocrystalline silicon piece, which is put into deionized water, after immersion first rinses, then impregnates in deionized water.
4. cleaning method according to claim 3, which is characterized in that in the step 1, monocrystalline silicon piece is dipped into nitration mixture
In after, first had children outside the state plan using ultrasonic wave, infiltrate monocrystalline silicon sheet surface.
5. cleaning method according to claim 4, which is characterized in that in the step 1, soaking time 100-300
Second.
6. cleaning method according to claim 3, which is characterized in that in the step 1, nitration mixture is that temperature is 10-40
℃。
7. cleaning method according to claim 6, which is characterized in that in the step 1, nitration mixture is that temperature is 15-25
℃。
8. cleaning method according to claim 5, which is characterized in that the excusing from death time is 5 minutes, when the immersion
Between be 200 seconds.
9. cleaning method according to claim 3, which is characterized in that in the step 2, washing time is 3 minutes,
Soaking time is 5 minutes.
10. cleaning method according to claim 9, which is characterized in that in the step 2 rinse and impregnate go from
Sub- water temperature is 45-55 DEG C.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113845917A (en) * | 2021-09-24 | 2021-12-28 | 上海提牛机电设备有限公司 | Cleaning solution and cleaning method for bent wafer |
| CN114653658A (en) * | 2022-04-11 | 2022-06-24 | 江苏鑫华半导体科技股份有限公司 | Method for cleaning electronic grade polycrystalline silicon |
| CN115537272A (en) * | 2022-10-26 | 2022-12-30 | 新疆晶科能源有限公司 | Monocrystalline silicon sample wafer cleaning agent and cleaning method |
| CN115975745A (en) * | 2023-01-04 | 2023-04-18 | 四川晶科能源有限公司 | Formula and method for pickling seed crystal |
| CN116631860A (en) * | 2023-07-18 | 2023-08-22 | 新美光(苏州)半导体科技有限公司 | Wet etching method |
| CN117602967A (en) * | 2023-11-28 | 2024-02-27 | 湖南德智新材料有限公司 | Purification method of ceramic material |
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| CN117602967A (en) * | 2023-11-28 | 2024-02-27 | 湖南德智新材料有限公司 | Purification method of ceramic material |
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Application publication date: 20190402 |