CN102832101A - Method for cleaning crystalline silicon - Google Patents
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- CN102832101A CN102832101A CN2011101578231A CN201110157823A CN102832101A CN 102832101 A CN102832101 A CN 102832101A CN 2011101578231 A CN2011101578231 A CN 2011101578231A CN 201110157823 A CN201110157823 A CN 201110157823A CN 102832101 A CN102832101 A CN 102832101A
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Abstract
The embodiment of the invention discloses a method for cleaning crystalline silicon, which comprises the following steps: placing crystalline silicon in pure water to carry out ultrasonic or mega-sound heating pre-cleaning; placing the crystalline silicon in a mixed acid solution to carry out corrosion; cleaning the crystalline silicon by the pure water; and drying the crystalline silicon. The crystalline silicon cleaning method adopts a combination manner of physic cleaning and chemical cleaning to clean the crystalline silicon, can effectively remove the impurities and particles on the surface of crystalline silicon (especially reclaimed materials) and can reduce the amount of the chemical solution, the damage of the chemical solution to the human body, equipment and environment, the corrosion loss of the chemical solution to the crystalline silicon and the follow-up treatment of the waste solution, thereby reducing the cleaning cost.
Description
Technical field
The present invention relates to the solar cell making process technical field, more particularly, relate to a kind of crystalline silicon cleaning method.
Background technology
In recent years; Because the fast development of solar photovoltaic technology; Caused the demand of crystalline silicon constantly surging; This just makes leftover pieces that many solar silicon wafers manufacturer all uses defective item, scrap and excision in the Si semiconductor components and parts production process as reclaimed materials, is used for the production of solar level crystalline silicon after said reclaimed materials is handled.In solar level crystalline silicon production process; Because the silicon material needs by fusing once more; And the silicon material under the high temperature easily and crucible, foreign gas etc. react; And then cause having in the silicon chip manufacture process part silicon material and excised, in order to reduce production costs, the silicon material that often will be excised is handled so that it can be utilized once more.
The silicon material that above-mentioned quilt is recycled again; After through technologies such as cutting, surface oxidation, mechanical grinding, polishings; Its surface or near surface zone will have been stain from impurity or particle in cutting fluid, air, the polishing dust with multiple modes such as physical absorption, mechanical parcel, chemisorbed, chemical bond, thereby form the impurity layer of one deck amorphous substance.Therefore, must carry out surface clean to it before using these silicon material, impurity and pollutant that it is surperficial remove.
Quality after silicon material (or crystalline silicon) cleaned directly has influence on the rate of finished products of the crystal forming rate and the polycrystal silicon ingot of silicon single crystal rod; The silicon material cleans unclean; Impurity component in the crystalline silicon increases, have a strong impact on crystal minority carrier life time, increase all kinds of defectives of crystal, finally cause the generation of the bad electric properties such as electricity conversion reduction, optical attenuation increase, electric leakage, local pyrexia of solar cell; Therefore, must strictly hold the quality that the silicon material cleans.
When in the traditional handicraft crystalline silicon being cleaned, generally be it to be thrown in the middle of mixed acid solution corrode a period of time, use the pure water ultrasonic cleaning afterwards, final drying; In particular cases can make crystalline silicon through pickling and alkali cleaning twice technology.But the conventional clean method has certain effect to primary silicon, and concerning reclaimed materials, impurity and dirt that not only can not it is surperficial be removed fully, but also can produce the phenomenons such as secondary pollution, selective oxidation of partial impurities on silicon material surface.And the chemicals kind of using in the conventional clean method is many, concentration is high, and this not only produces bigger harm to people, equipment, environment; And make that the loss of silicon material is bigger; Increased the intractability of waste liquid simultaneously, therefore, improved the cleaning cost and cleaned difficulty.
Summary of the invention
In view of this; The present invention provides a kind of crystalline silicon cleaning method, and this method all has cleaning performance preferably to primary silicon and reclaimed materials, and the chemicals that uses in the cleaning process is less; Can reduce harm, can reduce production costs and the production difficulty simultaneously people, equipment, environment.
For realizing above-mentioned purpose, the present invention provides following technical scheme:
A kind of crystalline silicon cleaning method, this method comprises:
Place pure water to carry out ultrasonic or million acoustic heating prerinse crystalline silicon;
Place mixed acid solution to corrode crystalline silicon;
Adopt pure water that said crystalline silicon is washed;
With said crystalline silicon oven dry.
Preferably, in the said method, the temperature of used pure water is 60 ℃～70 ℃ when placing pure water to carry out ultrasonic or million acoustic heating prerinse crystalline silicon.
Preferably, in the said method, place pure water to carry out million acoustic heating prerinse crystalline silicon, and the frequency of mega sonic wave is greater than 800kHz, million scavenging periods are 10min～20min.
Preferably, in the said method, said mixed acid solution comprises nitric acid and hydrofluoric acid, and the volume ratio of said nitric acid and hydrofluoric acid is 7: 1～15: 1.
Preferably, in the said method, place pure water to carry out ultrasonic heating prerinse crystalline silicon, and frequency of ultrasonic is 20kHz～40kHz, the ultrasonic cleaning time is 20min～30min.
Preferably, in the said method, said mixed acid solution comprises nitric acid and hydrofluoric acid, and the volume ratio of said nitric acid and hydrofluoric acid is 10: 1～15: 1.
Preferably, in the said method, the time that said crystalline silicon corrodes in mixed acid solution is 20s～60s.
Preferably, in the said method, the concentration of said nitric acid is 65%～68%, and the concentration of said hydrofluoric acid is 38%～41%, and the purity level of said nitric acid and hydrofluoric acid is MOS level or UP level.
Preferably, in the said method, adopt pure water that said crystalline silicon is washed and comprise: directly wash and ultrasonic irrigation; Wherein, the time of ultrasonic irrigation is 20min～40min.
Preferably, in the said method, said pure water is the pure water of resistivity greater than 16M Ω cm.
Can find out that from technique scheme crystalline silicon cleaning method provided by the present invention comprises: place pure water to carry out ultrasonic or million acoustic heating prerinse crystalline silicon; Place mixed acid solution to corrode crystalline silicon; Adopt pure water that said crystalline silicon is washed; With said crystalline silicon oven dry.Crystalline silicon cleaning method provided by the present invention; At first adopt pure water to carry out ultrasonic to crystalline silicon or million acoustic heating prerinse; Said ultrasonic or million acoustic heating prerinse can be removed surface of crystalline silicon with impurity and particle that the physical absorption form exists, adopt mixed acid solution that crystalline silicon is corroded afterwards, and the result of corrosion can remove impurity and the particle that surface of crystalline silicon exists with the chemisorbed form; Therefore, it is preferable finally to remove the effect of surface of crystalline silicon impurity and particle.This method is particularly useful for surface impurity and the more reclaimed materials of particle.
In addition; Crystalline silicon cleaning method provided by the present invention; Owing to before the employing mixed acid solution corrodes crystalline silicon, at first adopt pure water to carry out ultrasonic to it or million acoustic heating prerinse, therefore; The concentration of the follow-up mixed acid solution that adopts is lower, volume is less, and this can reduce the harm of mixed acid solution to people, equipment and environment on the one hand; Also can reduce corrosion losses on the other hand to crystalline silicon; Its three, also can alleviate follow-up work of treatment 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, cleans the back liquid waste processing and is easier to.
Description of drawings
In order to be illustrated more clearly in the embodiment of the invention or technical scheme of the prior art; To do to introduce simply to the accompanying drawing of required use in embodiment or the description of the Prior Art below; Obviously, the accompanying drawing in describing below only is some embodiments of the present invention, for those of ordinary skills; Under the prerequisite of not paying creative work, can also obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is the schematic flow sheet of a kind of crystalline silicon cleaning method that the embodiment of the invention provided.
Embodiment
To combine the accompanying drawing in the embodiment of the invention below, the technical scheme in the embodiment of the invention is carried out clear, intactly description, obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, those of ordinary skills are not making the every other embodiment that is obtained under the creative work prerequisite, all belong to the scope of the present invention's protection.
Said as the background technology part, the conventional clean method has certain effect to primary silicon, but concerning reclaimed materials, cleaning performance is not good, and this is owing to existing way with state different cause of primary silicon with reclaimed materials surface both impurity.The conventional clean method adopts mixed acid solution that crystalline silicon is corroded, and it has mainly considered the chemical property of surface of crystalline silicon impurity, and therefore, the employed chemical agent kind of conventional clean method is many, concentration is high, thus the potential safety hazard of being easy to generate; Have, the silicon material is by the chemicals seriously corroded, and chemicals consumption is more, thereby has increased the cleaning cost again.
Consider above-mentioned reason, the present invention is to crystalline silicon (especially reclaimed materials) when cleaning, when paying close attention to surface of crystalline silicon impurity chemical property; Also studied the existence of impurity at surface of crystalline silicon; Because impurity generally exists with the form of absorption at surface of crystalline silicon, and absorption is divided into physical absorption and chemisorbed, therefore; The present invention is directed to two kinds of different adsorption modes and adopt different means that crystalline silicon is cleaned, thereby reached cleaning performance preferably.Describe crystalline silicon cleaning method provided by the present invention below in detail.
With reference to figure 1, Fig. 1 is the schematic flow sheet of a kind of crystalline silicon cleaning method that the embodiment of the invention provided, and this method specifically comprises the steps:
Step S1: place pure water to carry out ultrasonic or million acoustic heating prerinse crystalline silicon.
This step is mainly implemented with impurity or particle that physical adsorption way exists to surface of crystalline silicon.Said crystalline silicon can be primary silicon, also can be reclaimed materials.According to the difference of crystalline silicon material or thickness, can in pure water, use ultrasonic respectively or million it is heated prerinse, detailed process is following:
When said crystalline silicon is primary silicon, flaw-piece material or end to end when material, top bed material, generally make it in pure water, carry out ultrasonic heating prerinse.Pure water described in the present embodiment is the pure water of resistivity greater than 16M Ω cm, and pure water involved in describing below is all identical therewith.Used frequency of ultrasonic was 20kHz～40kHz when crystalline silicon was carried out ultrasonic heating prerinse, and the time of ultrasonic cleaning is 20min～30min.
For cleaning the relatively broken silicon material or the broken silicon wafers of difficulty, the general selection carried out pure water million acoustic heating prerinse to it.And before it is carried out million acoustic heating prerinse, can also carry out artificial separation to it earlier, isolate the impurity or the foreign matter of sneaking into wherein; Can also carry out mechanical grinding to remove foreign matter for the more serious silicon material of surface contamination; When having organic pollutants, can use acetone or alcohol that it is cleaned earlier for the surface.The frequency of used mega sonic wave should be greater than 800kHz when crystalline silicon was carried out million acoustic heating prerinse, and the time of cleaning for million is 10min～20min.
Making said crystalline silicon in pure water, carry out the prewashed time of million acoustic heatings is generally less than crystalline silicon is carried out the prewashed time of ultrasonic heating; This be because: the frequency and the energy of used mega sonic wave are all bigger in the million acoustic heating prerinse processes; This just makes bigger to the cleaning dynamics of surface of crystalline silicon; Can suitably shorten scavenging period when therefore, adopting mega sonic wave to carry out prerinse.
No matter crystalline silicon carries out ultrasonic heating prerinse or million acoustic heating prerinse in pure water; The temperature of said pure water all should be heated to 60 ℃～70 ℃; Like this; Crystalline silicon is under the effect of mechanical force and heat, and its surface can promptly be disengaged absorption with impurity and the particle that the physical absorption form exists, and then breaks away from surface of crystalline silicon.This prerinse process strength disposal is big, safety, no chemical agent, do not corrode the silicon material, and operating process is simple, control easily.
No matter it still is million cleanings that crystalline silicon is carried out ultrasonic cleaning; All can determine whether making crystalline silicon to proceed to clean through the change color of observing pure water; When the color of said pure water did not have obviously change in three minutes, can stop crystalline silicon being cleaned.Certainly, also can test the turbidity of the pure water after the cleaning, when the turbidity of continuous three pure water of surveying does not have significant change, can stop crystalline silicon being cleaned through transmissometer.Afterwards, place mixed acid solution to corrode said crystalline silicon rapidly.
Step S2: place mixed acid solution to corrode crystalline silicon.
This step is mainly implemented with impurity or particle that the chemisorbed mode exists to surface of crystalline silicon.
The mixed acid solution that is adopted in this step comprises nitric acid and hydrofluoric acid, and for the situation of in step S1, crystalline silicon being carried out ultrasonic cleaning, the volume ratio that nitric acid and hydrofluoric acid can be set in this step is 10: 1～15: 1; For in step S1, crystalline silicon being carried out the situation of cleaning for million; The volume ratio that nitric acid and hydrofluoric acid can be set in this step is 7: 1～15: 1; This is because the crystalline silicon that the latter cleaned; General its surperficial amount of oxidation is more relatively, therefore, can suitably improve the ratio of hydrofluoric acid in the mixed acid solution.
The time that said crystalline silicon corrodes in mixed acid solution is can be controlled between 20s～60s, and etching time is long more, and the cleanliness factor of corrosion back surface of crystalline silicon is high more, therefore, can suitably control etching time as required.
The concentration of nitric acid described in the present embodiment is 65%～68%, and the concentration of said hydrofluoric acid is 38%～41%, and the purity level of said nitric acid and hydrofluoric acid is MOS level or UP level.Because crystalline silicon is from the higher pure water of temperature, to put into mixed acid solution rapidly through ultrasonic cleaning or after cleaning for million; Therefore, the initial temperature of surface of crystalline silicon is higher, and corrosion process is an exothermic process; So; The temperature of surface of crystalline silicon can be more and more hotter, so operating personnel can suitably reduce the concentration of nitric acid or hydrofluoric acid as the case may be, and the reduction of nitric acid or hydrofluoric acid concentration helps controlling corrosion reaction speed.
The mixed acid solution that is adopted in this step is mainly nitric acid and hydrofluoric acid, and this is to fall existing most impurity of surface of crystalline silicon and particle because nitric acid and hydrofluoric acid are corrodible.Certainly, also can adopt other mixed acid solution among other embodiment.
Adopted pure water to carry out ultrasonic to crystalline silicon or million acoustic heating prerinse among the step S1; Removed the impurity and the particle that exist with physical adsorption way on the surface of crystalline silicon, adopted mixed acid solution that crystalline silicon is corroded in this step again, these two steps combine and have following advantage: first; Utilize mixed acid solution can directly act on the impurity and the particle position of chemisorbed in this step; The surface of crystalline silicon temperature is higher in addition, and therefore, corrosion reaction can take place rapidly; Second; The amount of used mixed acid solution is compared prior art and will obviously be reduced in this step; The crystalline silicon that cleans one kilogram in the prior art approximately needs 0.2～0.3 kilogram mixed acid solution, and only needs to use 0.1 kilogram mixed acid solution among the present invention, thereby can save the cleaning cost; The 3rd, owing to the amount of used mixed acid solution has been lacked, therefore; Crystalline silicon has also reduced because of the amount of corrosion loss, and relative to existing technologies, the amount that surface of crystalline silicon loses because of corrosion can reduce more than 50%; Therefore the loss that has also alleviated crystalline silicon provides cost savings; The 4th, because the amount of used mixed acid solution has been lacked, therefore, reduced the harm of chemical liquid to people, equipment and environment, strengthened fail safe; The 5th; Because the impurity that adopts pure water to carry out ultrasonic cleaning or million cleaning back surface of crystalline silicon has been in relatively low level; Therefore, in the corrosion process variation of mixed acid solution concentration less, the stability of technical process increases; Operation easier reduces, and the work of treatment of follow-up waste liquid also is easier to; The 6th, the mode that adopts both to combine is handled impurity and the particle that can remove surface of crystalline silicon effectively to crystalline silicon, and removal effect is preferable, and said crystalline silicon is not limited to primary silicon, is more suitable in reclaimed materials.
After adopting mixed acid solution that crystalline silicon is etched, can carry out step S3.Mixed acid solution after the corrosion discharges after should passing through corresponding processing again.
Step S3: adopt pure water that said crystalline silicon is washed.
Adopt pure water that crystalline silicon is washed and can comprise in this step: directly to wash and ultrasonic irrigation; That is: at first adopt pure water that crystalline silicon is directly washed, generally wash three times to five times after, adopt pure water that crystalline silicon is carried out ultrasonic irrigation again, the time of may command ultrasonic irrigation is 20min～40min.In the ultrasonic irrigation process, also can the conductivity of pure water determine whether stopping ultrasonic irrigation behind the ultrasonic irrigation through detecting, generally, can stop crystalline silicon being carried out ultrasonic irrigation when the conductivity of the pure water behind the ultrasonic irrigation during less than 1 mho.Pure water after the use should discharge after treatment again.
Step S4: with said crystalline silicon oven dry.
Crystalline silicon is taken out from pure water and dries, can pack the crystalline silicon after the oven dry at last.
By on can know; Crystalline silicon cleaning method provided by the present invention; Difference from the suction type of surface of crystalline silicon impurity; Adopt the method that physics cleans and chemical cleaning combines that crystalline silicon is cleaned, can wash the impurity and the particle on crystalline silicon (especially reclaimed materials) surface effectively; And, owing at first crystalline silicon has been carried out the physics cleaning, therefore; The concentration of used chemical liquid and consumption all decrease in the subsequent chemistry cleaning process, and this can reduce on the one hand chemical liquid to people, harm that equipment and environment caused, also can alleviate follow-up work of treatment to waste liquid on the other hand; The 3rd; Reduced the consumption of chemical liquid, alleviated the corrosion losses of chemical liquid, thereby saved the cleaning cost crystalline silicon.Therefore, adopt method provided by the present invention that crystalline silicon is cleaned, can obviously improve the whole synthesis benefit.
To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be conspicuous concerning those skilled in the art, and defined General Principle can realize under the situation that does not break away from the spirit or scope of the present invention in other embodiments among this paper.Therefore, the present invention will can not be restricted to these embodiment shown in this paper, but will meet and principle disclosed herein and features of novelty the wideest corresponding to scope.
Claims (10)
1. a crystalline silicon cleaning method is characterized in that, comprising:
Place pure water to carry out ultrasonic or million acoustic heating prerinse crystalline silicon;
Place mixed acid solution to corrode crystalline silicon;
Adopt pure water that said crystalline silicon is washed;
With said crystalline silicon oven dry.
2. method according to claim 1 is characterized in that, the temperature of used pure water is 60 ℃～70 ℃ when placing pure water to carry out ultrasonic or million acoustic heating prerinse crystalline silicon.
3. method according to claim 2 is characterized in that, places pure water to carry out million acoustic heating prerinse crystalline silicon, and the frequency of mega sonic wave is greater than 800kHz, and million scavenging periods are 10min～20min.
4. method according to claim 3 is characterized in that said mixed acid solution comprises nitric acid and hydrofluoric acid, and the volume ratio of said nitric acid and hydrofluoric acid is 7: 1～15: 1.
5. method according to claim 2 is characterized in that, places pure water to carry out ultrasonic heating prerinse crystalline silicon, and frequency of ultrasonic is 20kHz～40kHz, and the ultrasonic cleaning time is 20min～30min.
6. method according to claim 5 is characterized in that said mixed acid solution comprises nitric acid and hydrofluoric acid, and the volume ratio of said nitric acid and hydrofluoric acid is 10: 1～15: 1.
7. according to each described method of claim 1～6, it is characterized in that the time that said crystalline silicon corrodes is 20s～60s in mixed acid solution.
8. according to claim 4 or 6 described methods, it is characterized in that the concentration of said nitric acid is 65%～68%, the concentration of said hydrofluoric acid is 38%～41%, and the purity level of said nitric acid and hydrofluoric acid is MOS level or UP level.
9. according to each described method of claim 1～6, it is characterized in that, adopt pure water that said crystalline silicon is washed and comprise: directly wash and ultrasonic irrigation; Wherein, the time of ultrasonic irrigation is 20min～40min.
10. according to each described method of claim 1～6, it is characterized in that said pure water is the pure water of resistivity greater than 16M Ω cm.
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| 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 |
| CN108526123A (en) * | 2018-05-18 | 2018-09-14 | 盐城工学院 | Single slot chip purification cleaning device and cleaning method |
| CN108941061A (en) * | 2018-05-18 | 2018-12-07 | 中国人民解放军国防科技大学 | Quantitative cleaning device and method for optical element |
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| 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 |
| CN109712866A (en) * | 2017-10-26 | 2019-05-03 | 东莞新科技术研究开发有限公司 | The cleaning method of wafer |
| CN108526123A (en) * | 2018-05-18 | 2018-09-14 | 盐城工学院 | Single slot chip purification cleaning device and cleaning method |
| CN108941061A (en) * | 2018-05-18 | 2018-12-07 | 中国人民解放军国防科技大学 | Quantitative cleaning device and method for optical element |
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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 |
| CN112111790A (en) * | 2020-09-21 | 2020-12-22 | 北京石晶光电科技股份有限公司 | Artificial wafer corrosion cleaning process |
| 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 |
| CN114695083A (en) * | 2022-03-29 | 2022-07-01 | 广东高景太阳能科技有限公司 | Silicon wafer cleaning method |
| 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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