CN102832101B - Crystalline silicon cleaning method - Google Patents
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- CN102832101B CN102832101B CN201110157823.1A CN201110157823A CN102832101B CN 102832101 B CN102832101 B CN 102832101B CN 201110157823 A CN201110157823 A CN 201110157823A CN 102832101 B CN102832101 B CN 102832101B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The embodiment of the invention discloses a kind of crystalline silicon cleaning method, the method includes: is placed in pure water by crystalline silicon and carries out ultrasonic or million acoustic heating prerinse; Crystalline silicon is placed in mixed acid solution and corrodes; Adopt pure water that described crystalline silicon is rinsed; Described crystalline silicon is dried. Crystalline silicon cleaning method provided by the present invention, adopt the mode that physical cleaning and Chemical cleaning combine that crystalline silicon is carried out, can effectively remove impurity and the granule on crystalline silicon (especially reclaimed materials) surface, and the consumption of chemical liquid can be reduced, reduce the chemical liquid harm to people, equipment and environment, alleviate the chemical liquid corrosion losses to crystalline silicon, alleviate the follow-up process work to waste liquid, thus cleaning cost can be reduced.
Description
Technical field
The present invention relates to solar cell making process technical field, more particularly, it relates to a kind of crystalline silicon cleaning method.
Background technology
In recent years, fast development due to solar photovoltaic technology, result in the demand to crystalline silicon constantly surging, this allows for many solar silicon wafers manufacturers and all uses the leftover pieces of the defective work in silicon semiconductor components and parts production process, scrap and excision as reclaimed materials, is used for the production of solar level crystalline silicon after being processed by described reclaimed materials. In solar level crystalline silicon production process, owing to silicon material needs again to be melted, and the silicon material under high temperature easily reacts with crucible, foreign gas etc., and then it is cut to cause having part silicon material in silicon chip manufacture process, in order to reduce production cost, often cut silicon material is carried out process allow it to by again with.
The above-mentioned silicon material again recycled, after the techniques such as cutting, surface oxidation, mechanical grinding, polishing, its surface or near-surface region are by having stain from the impurity in cutting fluid, air, polishing dust or granule with various ways such as physical absorption, machinery parcel, chemisorbed, chemical bond, thus defining the impurity layer of one layer of amorphous substance. Therefore, it must be carried out surface clean before using these silicon material, the impurity on its surface and pollutant are removed.
Quality after silicon material (or crystalline silicon) is carried out directly influences the crystal forming rate of silicon single crystal rod and the yield rate of polycrystal silicon ingot, silicon material does not wash clean clearly, impurity component in crystalline silicon increases, have a strong impact on the minority carrier life time of crystal, increase all kinds of defects of crystal, ultimately result in the generation of the bad electric properties such as the electricity conversion reduction of solaode, optical attenuation increase, electric leakage, local pyrexia, therefore, it is necessary to strictly hold the quality that silicon material cleans.
When crystalline silicon is carried out by traditional handicraft, it is usually and is thrown corrosion a period of time in the middle of mixed acid solution, use pure water ultrasonic cleaning, final drying afterwards; Crystalline silicon in particular cases can be made through pickling and alkali cleaning twice technique. But, original silicon is had certain effect by Conventional cleaning methods, and for reclaimed materials, not only can not by fully erased to the impurity on its surface and dirt, but also can in phenomenons such as the secondary pollution of silicon material surface generating section impurity, selective oxidations. And, the chemical species used in Conventional cleaning methods is many, concentration is high, and people, equipment, environment are not only produced bigger harm by this, and make the loss of silicon material bigger, add the intractability of waste liquid simultaneously, this improves cleaning cost and clean difficulty.
Summary of the invention
In view of this, the present invention provides a kind of crystalline silicon cleaning method, and original silicon and reclaimed materials are respectively provided with good cleaning performance by the method, and the chemical drugs used in cleaning process is less, can reduce to people, equipment, environment harm, simultaneously can reduce production cost and production difficulty.
For achieving the above object, the present invention provides following technical scheme:
A kind of crystalline silicon cleaning method, the method includes:
Crystalline silicon is placed in pure water and carries out ultrasonic or million acoustic heating prerinse;
Crystalline silicon is placed in mixed acid solution and corrodes;
Adopt pure water that described crystalline silicon is rinsed;
Described crystalline silicon is dried.
Preferably, in said method, being placed in pure water by crystalline silicon when carrying out ultrasonic or million acoustic heating prerinse the temperature of pure water used is 60 DEG C��70 DEG C.
Preferably, in said method, being placed in pure water by crystalline silicon and carry out million acoustic heating prerinse, and the frequency of mega sonic wave is more than 800kHz, million sound scavenging periods are 10min��20min.
Preferably, in said method, described mixed acid solution includes nitric acid and Fluohydric acid., and the volume ratio of described nitric acid and Fluohydric acid. is 7: 1��15: 1.
Preferably, in said method, being placed in pure water by crystalline silicon and carry out Ultrasonic Heating prerinse, and hyperacoustic frequency is 20kHz��40kHz, the ultrasonic cleaning time is 20min��30min.
Preferably, in said method, described mixed acid solution includes nitric acid and Fluohydric acid., and the volume ratio of described nitric acid and Fluohydric acid. is 10: 1��15: 1.
Preferably, in said method, the time that described crystalline silicon carries out corroding in mixed acid solution is 20s��60s.
Preferably, in said method, the concentration of described nitric acid is 65%��68%, and the concentration of described Fluohydric acid. is 38%��41%, and the purity level of described nitric acid and Fluohydric acid. is MOS level or UP level.
Preferably, in said method, pure water is adopted to be rinsed including to described crystalline silicon: directly to rinse and ultrasonic irrigation; Wherein, the time of ultrasonic irrigation is 20min��40min.
Preferably, in said method, described pure water is the resistivity pure water more than 16M �� cm.
From technique scheme it can be seen that crystalline silicon cleaning method provided by the present invention includes: crystalline silicon is placed in pure water and carries out ultrasonic or million acoustic heating prerinse; Crystalline silicon is placed in mixed acid solution and corrodes; Adopt pure water that described crystalline silicon is rinsed; Described crystalline silicon is dried. Crystalline silicon cleaning method provided by the present invention, initially with pure water, crystalline silicon carried out ultrasonic or million acoustic heating prerinse, described ultrasonic or million acoustic heating prerinse can remove impurity and the granule that surface of crystalline silicon exists with physical absorption form, adopt mixed acid solution that crystalline silicon is corroded afterwards, the result of corrosion can remove impurity and the granule that surface of crystalline silicon exists with chemisorbed form, therefore, the effect of final removal surface of crystalline silicon impurity and granule is preferably. The method is particularly suited for surface impurity and the more reclaimed materials of granule.
In addition, crystalline silicon cleaning method provided by the present invention, due to before adopting mixed acid solution that crystalline silicon is corroded, initially with pure water, it is carried out ultrasonic or million acoustic heating prerinse, therefore, the concentration of follow-up adopted mixed acid solution is relatively low, small volume, and this can reduce the mixed acid solution harm to people, equipment and environment on the one hand; Also can reduce the corrosion losses to crystalline silicon on the other hand; Its three, also can alleviate the follow-up process work to waste liquid.
Therefore, crystalline silicon cleaning method provided by the present invention, not only cleaning performance is good, and it is low to clean cost, and cleaning process is less to the harm of people, equipment and environment, and after cleaning, liquid waste processing is easier to.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, the accompanying drawing used required in embodiment or description of the prior art will be briefly described below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the premise not paying creative work, it is also possible to obtain other accompanying drawing according to these accompanying drawings.
The schematic flow sheet of a kind of crystalline silicon cleaning method that Fig. 1 provides for the embodiment of the present invention.
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments. Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under not making creative work premise, broadly fall into the scope of protection of the invention.
Just as described in the background section, original silicon is had certain effect by Conventional cleaning methods, but for reclaimed materials, cleaning performance is not good, and this is to cause owing to original silicon is different from the existing way of reclaimed materials surface both impurity and state. Conventional cleaning methods adopts mixed acid solution that crystalline silicon is corroded, and it mainly considers the chemical property of surface of crystalline silicon impurity, and therefore, the chemical agent kind that Conventional cleaning methods uses is many, concentration is high, thus easily producing potential safety hazard; Further, silicon material is by chemical drugs seriously corroded, and chemical drugs consumes more, thus adding cleaning cost.
Consider above-mentioned reason, the present invention is when being carried out crystalline silicon (especially reclaimed materials), while paying close attention to surface of crystalline silicon impurity chemical property, also studied the impurity existence at surface of crystalline silicon, owing to impurity generally exists with the form of absorption at surface of crystalline silicon, and adsorb and be divided into physical absorption and chemisorbed, therefore, the present invention is directed to suction type two kinds different adopts different means that crystalline silicon is carried out, thus having reached good cleaning performance. Crystalline silicon cleaning method provided by the present invention is described below in detail.
With reference to the schematic flow sheet of a kind of crystalline silicon cleaning method that Fig. 1, Fig. 1 provide for the embodiment of the present invention, the method specifically includes following steps:
Step S1: crystalline silicon is placed in pure water and carries out ultrasonic or million acoustic heating prerinse.
This step is primarily directed to impurity or granule that surface of crystalline silicon exists with physical adsorption way and implements. Described crystalline silicon can be original silicon, it is also possible to for reclaimed materials. Difference according to crystalline silicon material or thickness, can use ultrasonic or million sound that it is heated prerinse respectively in pure water, and detailed process is as follows:
When described crystalline silicon be original silicon, edge skin material or end to end material, top bed material time, generally make it carry out Ultrasonic Heating prerinse in pure water. Pure water described in the present embodiment is the resistivity pure water more than 16M �� cm, and pure water involved in the following describes is all identical with this. When crystalline silicon carries out Ultrasonic Heating prerinse, hyperacoustic frequency used is 20kHz��40kHz, and the time of ultrasonic cleaning is 20min��30min.
For cleaning relatively difficult broken silicon material or broken silicon wafers, it is typically chosen and it is carried out pure water million acoustic heating prerinse. And before it is carried out million acoustic heating prerinse, it is also possible to first it is carried out artificial separation, isolate and be mixed into impurity therein or foreign body; Mechanical grinding can also be carried out to remove foreign body than more serious silicon material for surface contamination; When Organic Pollution is existed for surface, it is possible to first use acetone or ethanol that it is cleaned. When crystalline silicon is carried out million acoustic heating prerinse, the frequency of mega sonic wave used should be greater than 800kHz, and the time that million sound clean is 10min��20min.
Make described crystalline silicon carry out for million acoustic heating prewashed times in pure water to be generally less than crystalline silicon is carried out the Ultrasonic Heating prewashed time, this be due to: in million acoustic heating pre-cleaning process, the frequency of mega sonic wave used and energy are all bigger, it is bigger that this allows for the cleaning dynamics to surface of crystalline silicon, therefore, mega sonic wave is adopted can suitably to shorten scavenging period when carrying out prerinse.
No matter crystalline silicon is by Ultrasonic Heating prerinse or million acoustic heating prerinse in pure water, the temperature of described pure water all should be heated to 60 DEG C��70 DEG C, so, crystalline silicon is under the effect of mechanical force and heat, the impurity that its surface exists with physical absorption form can promptly be released from absorption with granule, and then departs from surface of crystalline silicon. This pre-cleaning process strength disposal is relatively big, safety, without chemical agent, do not corrode silicon material, and operating process is simple, it is easy to control.
Regardless of crystalline silicon being carried out ultrasonic cleaning or the cleaning of million sound, all can decide whether to make crystalline silicon proceed to clean by the color change of observation pure water, when in three minutes, nothing substantially changes the color of described pure water, it is possible to stop crystalline silicon being carried out. It is of course also possible to tested the turbidity of the pure water after cleaning by transmissometer, when the turbidity of continuous three surveyed pure water is without significant change, can stop crystalline silicon being carried out. Afterwards, described crystalline silicon is placed in mixed acid solution corrodes rapidly.
Step S2: crystalline silicon is placed in mixed acid solution and corrodes.
This step is primarily directed to impurity or granule that surface of crystalline silicon exists in chemisorbed mode and implements.
The mixed acid solution adopted in this step includes nitric acid and Fluohydric acid., and during in step sl crystalline silicon being carried out ultrasonic cleaning, the volume ratio that can arrange nitric acid and Fluohydric acid. in this step is 10: 1��15: 1; When in step sl crystalline silicon being carried out million sound cleanings, the volume ratio that can arrange nitric acid and Fluohydric acid. in this step is 7: 1��15: 1, this is the crystalline silicon owing to the latter cleans, the amount of oxidation on its surface general is relatively many, therefore, the ratio of Fluohydric acid. in mixed acid solution can be properly increased.
Making the time that described crystalline silicon carries out corroding in mixed acid solution can be controlled between 20s��60s, etching time is more long, and after corrosion, the cleanliness factor of surface of crystalline silicon is more high, therefore, and can suitable control corrosion rate time as required.
The concentration of nitric acid described in the present embodiment is 65%��68%, and the concentration of described Fluohydric acid. is 38%��41%, and the purity level of described nitric acid and Fluohydric acid. is MOS level or UP level. Owing to crystalline silicon is to put into rapidly in mixed acid solution after ultrasonic cleaning or million sound are cleaned from the higher pure water of temperature, therefore, the initial temperature of surface of crystalline silicon is higher, and corrosion process is exothermic process, therefore, the temperature of surface of crystalline silicon can be more and more hotter, and therefore operator can suitably reduce the concentration of nitric acid or Fluohydric acid. as the case may be, and the reduction of nitric acid or hydrofluoric acid concentration is conducive to control corrosion rate response speed.
The mixed acid solution adopted in this step is mainly nitric acid and Fluohydric acid., this be due to nitric acid and Fluohydric acid. corrodible fall most impurity existing for surface of crystalline silicon and granule. Certainly, other embodiments can also adopt other mixed acid solution.
Step S1 adopt pure water crystalline silicon has carried out ultrasonic or million acoustic heating prerinse, the impurity and granule that exist on surface of crystalline silicon are eliminated with physical adsorption way, this step adopt again mixed acid solution crystalline silicon is corroded, the two step combines and has the advantage that first, this step utilize mixed acid solution can be done directly on impurity and the particles sites of chemisorbed, in addition surface of crystalline silicon temperature is higher, and therefore, corrosion reaction can occur rapidly; Second, in this step, the amount of mixed acid solution used to significantly reduce compared to existing technology, cleaning cost prior art cleaned the crystalline silicon of a kilogram and takes around the mixed acid solution of 0.2��0.3 kilogram, and the present invention only need to use the mixed acid solution of 0.1 kilogram, thus can be saved; 3rd, owing to the amount of mixed acid solution used is few, therefore, the amount of crystalline silicon loss because of corrosion decreases, and relative to existing technologies, the amount that surface of crystalline silicon loses because of corrosion can reduce by more than 50%, therefore also mitigate the loss of crystalline silicon, provide cost savings; 4th, owing to the amount of mixed acid solution used is few, therefore, decreases the chemical liquid harm to people, equipment and environment, enhance safety; 5th, owing to adopting pure water to carry out after ultrasonic cleaning or million sound clean the impurity of surface of crystalline silicon already at relatively low level, therefore, in corrosion process, the change of mixed acid solution concentration is less, the stability of technical process increases, operation easier reduces, and the process work of follow-up waste liquid is relatively easy to; 6th, adopt the mode that both combine to carry out crystalline silicon processing impurity and the granule that can effectively remove surface of crystalline silicon, preferably, described crystalline silicon is not limited to original silicon to removal effect, is more suitable for reclaimed materials.
After adopting mixed acid solution that crystalline silicon is etched, step S3 can be carried out. Mixed acid solution after corrosion should discharge after processing accordingly again.
Step S3: adopt pure water that described crystalline silicon is rinsed.
This step adopt pure water crystalline silicon is rinsed comprising the steps that directly flushing and ultrasonic irrigation; That is: initially with pure water, crystalline silicon directly being rinsed, generally flush three times after five times, then adopt pure water that crystalline silicon is carried out ultrasonic irrigation, the time that can control ultrasonic irrigation is 20min��40min. In ultrasonic irrigation process, it is also possible to decide whether to stop ultrasonic irrigation by pure electrical conductivity of water after detecting ultrasonic irrigation, generally when the pure electrical conductivity of water after ultrasonic irrigation is less than 1 mho, can stop crystalline silicon being carried out ultrasonic irrigation. Pure water after using should discharge after treatment again.
Step S4: described crystalline silicon is dried.
Crystalline silicon taken out from pure water and dries, finally the crystalline silicon after drying can being packed.
As from the foregoing, crystalline silicon cleaning method provided by the present invention, difference from the suction type of surface of crystalline silicon impurity, adopt the method that physical cleaning and Chemical cleaning combine that crystalline silicon is carried out, it is possible to effectively to wash impurity and the granule on crystalline silicon (especially reclaimed materials) surface; And, owing to first crystalline silicon having been carried out physical cleaning, therefore, concentration and the consumption of chemical liquid used by subsequent chemistry cleaning process all decrease, and this can reduce the harm that people, equipment and environment are caused by chemical liquid on the one hand, also can alleviate the follow-up process work to waste liquid on the other hand, 3rd, decrease the consumption of chemical liquid, alleviate the chemical liquid corrosion losses to crystalline silicon, thus saving cleaning cost. Therefore, adopt method provided by the present invention that crystalline silicon is carried out, whole synthesis benefit can be significantly improved.
Described above to the disclosed embodiments, makes professional and technical personnel in the field be capable of or uses the present invention. The multiple amendment of these embodiments be will be apparent from for those skilled in the art, and generic principles defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments. Therefore, the present invention is not intended to be limited to the embodiments shown herein, and is to fit to the widest scope consistent with principles disclosed herein and features of novelty.
Claims (3)
1. a crystalline silicon cleaning method, it is characterised in that including:
Being placed in pure water by crystalline silicon to carry out ultrasonic or million acoustic heating prerinse, described to be placed in pure water by crystalline silicon when carrying out ultrasonic or million acoustic heating prerinse the temperature of pure water used be 60 DEG C��70 DEG C;
Crystalline silicon is placed in mixed acid solution and corrodes; The time that described crystalline silicon carries out corroding in mixed acid solution is 20s��60s; Wherein, when carrying out ultrasonic cleaning, the volume ratio arranging nitric acid and Fluohydric acid. is 10:1��15:1; When carrying out million sound cleanings, the volume ratio arranging nitric acid and Fluohydric acid. is 7:1��15:1;
Pure water is adopted to be rinsed including to described crystalline silicon: directly to rinse and ultrasonic irrigation; Wherein, the time of ultrasonic irrigation is 20min��40min;
Described crystalline silicon is dried;
Wherein, described being placed in pure water by crystalline silicon and carry out million acoustic heating prerinse, and the frequency of mega sonic wave is more than 800kHz, million sound scavenging periods are 10min��20min;
Or, crystalline silicon being placed in pure water and carries out Ultrasonic Heating prerinse, and hyperacoustic frequency is 20kHz��40kHz, the ultrasonic cleaning time is 20min��30min.
2. method according to claim 1, it is characterised in that the concentration of described nitric acid is 65%��68%, the concentration of described Fluohydric acid. is 38%��41%, and the purity level of described nitric acid and Fluohydric acid. is MOS level or UP level.
3. method according to claim 1, it is characterised in that described pure water is the resistivity pure water more than 16M �� cm.
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| CN104766793B (en) * | 2014-01-03 | 2017-10-31 | 北大方正集团有限公司 | A kind of acid tank back side silicon caustic solution |
| CN105177716A (en) * | 2015-10-28 | 2015-12-23 | 包头市山晟新能源有限责任公司 | N-type mono-crystal reclaimed material cleaning technology |
| CN107611016A (en) * | 2017-09-21 | 2018-01-19 | 晶科能源有限公司 | A kind of cleaning method of solar power silicon sheet stock |
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| CN111744870A (en) * | 2020-06-24 | 2020-10-09 | 中国科学院苏州纳米技术与纳米仿生研究所广东(佛山)研究院 | Cleaning method for semiconductor device after gold-tin soldering |
| CN112111790B (en) * | 2020-09-21 | 2022-03-29 | 北京石晶光电科技股份有限公司 | Artificial wafer corrosion cleaning process |
| CN114695083B (en) * | 2022-03-29 | 2023-01-06 | 高景太阳能股份有限公司 | Silicon wafer cleaning method |
| CN114951133A (en) * | 2022-05-10 | 2022-08-30 | 无锡领缔生物科技有限公司 | Plant surface corrosion cleaning system and cleaning method thereof |
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