CN101775662A - Etch-cleaning method for high purity polycrystalline silicon briquette - Google Patents
Etch-cleaning method for high purity polycrystalline silicon briquette Download PDFInfo
- Publication number
- CN101775662A CN101775662A CN201010300736A CN201010300736A CN101775662A CN 101775662 A CN101775662 A CN 101775662A CN 201010300736 A CN201010300736 A CN 201010300736A CN 201010300736 A CN201010300736 A CN 201010300736A CN 101775662 A CN101775662 A CN 101775662A
- Authority
- CN
- China
- Prior art keywords
- polycrystalline silicon
- hydrofluoric acid
- briquette
- acid solution
- corrosion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Silicon Compounds (AREA)
Abstract
The invention discloses an etch-cleaning method for a high purity polycrystalline silicon briquette, which relates to a cleaning method for a high purity polycrystalline silicon briquette in the field of polycrystalline silicon production. In the method, hydrofluoric acid solution etching process is arranged after mixed acid etching and pure water (EW-I) rinsing processes; hydrofluoric acid solution is diluted from electronic grade hydrofluoric acid and pure water (EW-I) in a proportion of 1:2-5 (weight part), and the etching soaking time is determined according to the thickness of an oxygen layer on the surface of the silicon briquette and the concentration of the hydrofluoric acid solution; and after ultrasonic cleaning, the briquette is subjected to hot nitrogen water shearing and vacuum drying to obtain the high-purity disposable polycrystalline silicon briquette meeting the requirements of Czochralski single crystals. By adding the hydrofluoric acid solution etching process, the surface oxygen layer of the silicon briquette, which is generated when the polycrystalline silicon briquette is subjected to mixed acid etching and is contacted with air once again, can be removed so as to obtain the disposable high-purity polycrystalline silicon material with good metal glossiness of the surface and better surface quality.
Description
Technical field
The present invention relates to the method that the high purity polycrystalline silicon briquette in the field of polysilicon production cleans, the zone of oxidation that the surface produces when being used to remove the polycrystalline silicon briquette ingress of air.
Background technology
Polysilicon is the important raw and processed materials of semicon industry and sun power industry, and for finally obtaining the high purity polycrystalline silicon that quality meets the demands, the step that is absolutely necessary is cleaned in acid corrosion.The method afford that corrosion of polysilicon is not cleaned in the design of Russia rare metal research institute specifies, and still along with the fast development of global electronic information industry and photovoltaic industry, the inherent and external quality of polysilicon is had higher requirement.
Original process is a polycrystalline silicon briquette through a certain proportion of hydrofluoric acid (electronic-grade) and nitric acid (electronic-grade) nitration mixture burn into pure water (EW-I) rinsing, ultrasonic cleaning vacuum drying afterwards.But nitration mixture corrosion back silico briquette can produce zone of oxidation on the surface during ingress of air once more, has influenced the surface gloss and the surface quality of silico briquette.
Summary of the invention
Technical problem to be solved by this invention provides the method that a kind of high purity polycrystalline silicon briquette corrosion is cleaned, and can remove the silico briquette process nitration mixture corrosive polycrystalline silicon briquette zone of oxidation of ingress of air rear surface generation once more.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is: the method that a kind of high purity polycrystalline silicon briquette corrosion is cleaned may further comprise the steps:
Behind nitration mixture corrosion and pure water (EW-I) rinsing process, the hydrofluoric acid solution corrosion process is set;
To be electronic-stage hydrofluoric acid and pure water (EW-I) form by the proportioning dilution of 1: 2～5 (weight parts) hydrofluoric acid solution, and the corrosion soak time is according to the zone of oxidation thickness on silico briquette surface and the strength of solution decision of hydrofluoric acid;
Thereby reusable heat nitrogen is cut the high-purity disposable polycrystalline silicon briquette that water, vacuum drying are met the pulling of crystals requirement after the ultrasonic cleaning.
The corrosion soak time is 8～60s in the hydrofluoric acid solution corrosion process.
The method that a kind of high purity polycrystalline silicon briquette corrosion provided by the invention is cleaned, by increasing the hydrofluoric acid solution corrosion process, remove the silico briquette process nitration mixture corrosive polycrystalline silicon briquette zone of oxidation of ingress of air rear surface generation once more, thereby obtain the disposable high purity polycrystalline silicon material that the surface metal glossiness is good, surface quality is more excellent.
A kind of processing method that high purity polycrystalline silicon briquette provided by the invention corrosion is cleaned compared with prior art has the following advantages: the oxide removal on silico briquette surface more thorough, and the surface quality of the silico briquette that obtains is better, and the metal luster on surface is better.Can provide large batch of high-quality disposable high-purity polycrystalline silicon raw material for the client.
Embodiment
Polycrystalline silicon briquette after the fragmentation through a certain proportion of hydrofluoric acid (electronic-grade) and nitric acid (electronic-grade) nitration mixture burn into pure water (EW-I) rinsing, hydrofluoric acid burn into pure water (EW-I) thus clean, ultrasonic cleaning afterwards reusable heat nitrogen cut the high-purity disposable polycrystalline silicon briquette that water, vacuum drying are met the pulling of crystals requirement.
The operation steps flow process is as follows:
Nitration mixture corrosion → pure water rinsing → hydrofluoric acid corrosion → pure water rinsing → ultrasonic cleaning → vacuum drying.
Wherein committed step is to have increased the hydrofluoric acid solution corrosion process in the cleaning process, hydrofluoric acid solution is the solution after hydrofluoric acid (electronic-grade) is used pure water (EW-I) dilution according to a certain percentage, hydrofluoric acid and pure water (EW-I) carry out proportioning with 1: 2～5 (weight parts), the corrosion soak time of silico briquette in hydrofluoric acid solution decides according to the size of the concentration of the zone of oxidation thickness of its real surface and hydrofluoric acid, its time is generally 8～60s, and the concrete process time need be determined according to practical situation.Be better than directly corrosive effect of hydrofluoric acid (electronic-grade) through diluent hydrofluoric acid solution corrosive effect, cooperate hot nitrogen to cut the cleaning way of water, to corrode once more the surface oxide layer that produces behind the ingress of air be the macula lutea phenomenon through nitration mixture to have removed silico briquette, thereby obtain the disposable high purity polycrystalline silicon material that the surface metal glossiness is good, surface quality is more excellent.
Claims (2)
1. a high purity polycrystalline silicon briquette corrodes the method for cleaning, and it is characterized in that may further comprise the steps:
Behind nitration mixture corrosion and pure water (EW-I) rinsing process, the hydrofluoric acid solution corrosion process is set;
To be electronic-stage hydrofluoric acid and pure water (EW-I) form by the proportioning dilution of 1: 2～5 (weight parts) hydrofluoric acid solution, and the corrosion soak time is according to the zone of oxidation thickness on silico briquette surface and the strength of solution decision of hydrofluoric acid;
Thereby reusable heat nitrogen is cut the high-purity disposable polycrystalline silicon briquette that water, vacuum drying are met the pulling of crystals requirement after the ultrasonic cleaning.
2. the method that a kind of high purity polycrystalline silicon briquette corrosion according to claim 1 is cleaned, it is characterized in that: the corrosion soak time is 8～60s in the hydrofluoric acid solution corrosion process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010300736A CN101775662A (en) | 2010-01-26 | 2010-01-26 | Etch-cleaning method for high purity polycrystalline silicon briquette |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010300736A CN101775662A (en) | 2010-01-26 | 2010-01-26 | Etch-cleaning method for high purity polycrystalline silicon briquette |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101775662A true CN101775662A (en) | 2010-07-14 |
Family
ID=42512243
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010300736A Pending CN101775662A (en) | 2010-01-26 | 2010-01-26 | Etch-cleaning method for high purity polycrystalline silicon briquette |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101775662A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101974785A (en) * | 2010-11-03 | 2011-02-16 | 天津市环欧半导体材料技术有限公司 | Cleaning method of policrystalline silicon raw material |
| CN106115715A (en) * | 2016-06-26 | 2016-11-16 | 河南盛达光伏科技有限公司 | Polycrystalline silicon ingot casting partly melts the circulation tailing cleaning treatment method that technique produces |
| CN108172499A (en) * | 2017-12-11 | 2018-06-15 | 上海申和热磁电子有限公司 | A kind of process of super back of the body Feng Pinzai corrosion |
| CN111659640A (en) * | 2020-05-14 | 2020-09-15 | 富乐德科技发展（大连）有限公司 | Ultra-clean cleaning process for aluminum substrate porous gas distribution device in cavity of semiconductor equipment |
| CN112160032A (en) * | 2020-09-03 | 2021-01-01 | 深圳第三代半导体研究院 | Crystal processing method |
-
2010
- 2010-01-26 CN CN201010300736A patent/CN101775662A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101974785A (en) * | 2010-11-03 | 2011-02-16 | 天津市环欧半导体材料技术有限公司 | Cleaning method of policrystalline silicon raw material |
| CN106115715A (en) * | 2016-06-26 | 2016-11-16 | 河南盛达光伏科技有限公司 | Polycrystalline silicon ingot casting partly melts the circulation tailing cleaning treatment method that technique produces |
| CN108172499A (en) * | 2017-12-11 | 2018-06-15 | 上海申和热磁电子有限公司 | A kind of process of super back of the body Feng Pinzai corrosion |
| CN108172499B (en) * | 2017-12-11 | 2021-07-06 | 上海中欣晶圆半导体科技有限公司 | Process method for re-corroding super back seal product |
| CN111659640A (en) * | 2020-05-14 | 2020-09-15 | 富乐德科技发展（大连）有限公司 | Ultra-clean cleaning process for aluminum substrate porous gas distribution device in cavity of semiconductor equipment |
| CN111659640B (en) * | 2020-05-14 | 2022-03-18 | 富乐德科技发展（大连）有限公司 | Ultra-clean cleaning process for aluminum substrate porous gas distribution device in cavity of semiconductor equipment |
| CN112160032A (en) * | 2020-09-03 | 2021-01-01 | 深圳第三代半导体研究院 | Crystal processing method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| TWI511196B (en) | Method of Polishing Silica Flocking Cleaning Process | |
| CN101775662A (en) | Etch-cleaning method for high purity polycrystalline silicon briquette | |
| CN107364870B (en) | A kind of efficient impurity removal crushing process of fritting bottom seed crystal | |
| CN102629644A (en) | Reworking technology of finished crystalline silicon solar cell | |
| CN103993360B (en) | Polycrystalline silicon texturing adjuvant and application thereof | |
| CN104532196B (en) | A kind of forging method of tantalum target | |
| CN103668466A (en) | Polycrystalline silicon chip texturing liquid and texturing method | |
| CN101695697A (en) | Method for cleaning metallurgical silicon material | |
| CN103087850A (en) | Monocrystalline silicon wafer precleaning liquid and cleaning method thereof | |
| CN100547116C (en) | Be used for isolating etching solution of polycrystal '' carbon head material " silicon carbon and preparation method thereof | |
| CN105887206B (en) | Monocrystalline silicon wire cutting fragment cleaning treatment method | |
| CN101698473A (en) | Recovery method of high-purity silicon nitride | |
| CN102254953B (en) | Manufacturing method of N-type solar energy silicon wafer with minority carrier lifetime of more than 1000 microseconds | |
| CN102070146B (en) | Treatment method of broken materials of solar silicon cell pieces | |
| CN108847401B (en) | Method for cleaning primary polycrystalline silicon material | |
| JP6433674B2 (en) | Cleaning method for polycrystalline silicon | |
| CN105441200A (en) | Semiconductor silicon wafer degumming cleaning fluid and preparation method | |
| CN102364697B (en) | Method for removing micro-damage layer from crystalline silicon surface after RIE (Reactive Ion Etching) flocking | |
| CN113718257A (en) | Etching method of germanium ingot | |
| CN106733876B (en) | A kind of cleaning method of the crystal silicon chip of Buddha's warrior attendant wire cutting | |
| CN101875494A (en) | Preparation method of low-titanium and high-purity polycrystalline silicon | |
| CN106336953A (en) | Acidic ultrasonic cleaning agent for cleaning of silicon wafers | |
| CN103042009B (en) | A kind of polycrystalline silicon material produces the cleaning method of reduction furnace electrode protective cover | |
| CN103382578A (en) | Method for treating monocrystalline silicon wafer surface | |
| CN102962224B (en) | Method for cleaning parent polycrystalline carbon head material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Open date: 20100714 |