CN103480598A - Silicon wafer cleaning method for preparing high-efficiency solar cell and cleaning equipment - Google Patents
Silicon wafer cleaning method for preparing high-efficiency solar cell and cleaning equipment Download PDFInfo
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Abstract
The invention provides a silicon wafer cleaning method for preparing a high-efficiency solar cell and cleaning equipment. The surface hydrophobicity of a textured silicon wafer is poorer due to the fact that the proportion by weight of sulfuric acid to hydrogen peroxide is lower in the existing silicon wafer cleaning technology. The silicon wafer cleaning method for preparing the high-efficiency solar cell comprises the following steps of firstly cleaning the silicon wafer by mixed solution of concentrated sulfuric acid and hydrogen peroxide solution by adopting the cleaning equipment, wherein the proportion by weight of the sulfuric acid to the hydrogen peroxide is (65-170):1, then, cleaning by deionized water, then, cleaning the silicon wafer by the hydrogen peroxide solution or salpeter solution so as to remove carbon residues and part of metallics and form a layer of oxidation film, cleaning by the deionized water, and finally, removing the oxidation film on the silicon wafer by the mixed solution of hydrochloric acid and hydrofluoric acid, and cleaning by the deionized water. According to the silicon wafer cleaning method for preparing the high-efficiency solar cell and the cleaning equipment provided by the invention, the hydrophobicity of the silicon wafer can be effectively improved, i.e. the cleaned silicon wafer is completely dehydrated after the oxidation film on the silicon wafer is removed.
Description
Technical field
The present invention relates to solar cell and manufacture field, particularly a kind of silicon wafer cleaning method for the preparation of efficient solar battery and cleaning equipment.
Background technology
For efficient solar battery, the surface treatment of silicon chip is very crucial, and the cleaning in early stage can be removed organic impurities and the metallic of silicon chip surface, thereby can effectively avoid in the high temperature techniques such as diffusion in the later stage, oxidation, activation introducing impurity or defect.
At integrated circuit (Integrated Circuit; Abbreviation IC) in industry, traditional RCA cleaning method, although splendid cleaning performance is arranged, there are the problems such as program is numerous and diverse, process window is young, the solution life cycle is short in the method.Moreover, when the solar energy industry is used RCA cleaning method cleaning silicon chip, its SC-1 solution has corrosiveness because being alkalescent to silicon chip, causes square resistance controllability very poor (square resistance rising) in the cleaning of cell piece after diffusion.Thereby, for the solar energy industry, the RCA ablution is not desirable cleaning method.
Also there is a kind of cleaning method SPM ablution of extensive use in the IC industry, it adopts the mixed solution of the concentrated sulfuric acid and hydrogenperoxide steam generator, wherein the mass percent of sulfuric acid and hydrogen peroxide is 15～30: 1, the purpose of hydrogenperoxide steam generator is mainly to decompose to produce bubble, strengthen the impurity elimination effect, each add (hydrogenperoxide steam generator stoste that hundreds of mL percent concentration is 30%) on a small quantity gets final product.This mixed solution can very effectively be removed organic matter and the part metals impurity on wafer (silicon chip) surface under the condition of heating.But existing SPM cleaning method mainly designs for the wafer of semicon industry, through polishing, very smooth due to crystal column surface, so there is not the problem of cleaning rear dehydration.But due to the solar energy industry when making solar cell, usually be all first to make matte (remove the damage layer, increase light absorption), if directly apply mechanically the SPM ablution of IC industry, can cause the silicon chip surface hydrophobicity poor, occur that surface hangs water or the phenomenon such as obvious washmarking trace is arranged, thereby do not reach the purpose of removing impurities on surface of silicon chip.
Therefore, the surface hydrophobic problem of matte silicon chip while how to provide a kind of silicon wafer cleaning method for the preparation of efficient solar battery and equipment to adopt SPM ablution cleaning silicon chip to solve, even the silicon chip after cleaning is dehydration fully after the deoxidation film, become industry technical problem urgently to be resolved hurrily.
Summary of the invention
The objective of the invention is to provide a kind of silicon wafer cleaning method for the preparation of efficient solar battery and cleaning equipment, the surface hydrophobic problem of matte silicon chip in the time of can solving SPM ablution cleaning silicon chip by described cleaning method and cleaning equipment, thus the cleanliness factor cleaned improved.
For achieving the above object, the invention provides a kind of silicon wafer cleaning method for the preparation of efficient solar battery, the method comprises the following steps: a, the mixed solution by the concentrated sulfuric acid and hydrogenperoxide steam generator are cleaned silicon chip, the quality proportioning of sulfuric acid and hydrogen peroxide is 65～170: 1, cleaning temperature is 100～125 ℃, and scavenging period is 5～30min; B, by deionized water, described silicon chip is cleaned; C, by hydrogenperoxide steam generator or salpeter solution, silicon chip is cleaned, the quality proportioning of described hydrogen peroxide and water is 1: 3～10, the quality proportioning of described nitric acid and water is 1: 2～5, and described cleaning temperature is 60～80 ℃, and described scavenging period is 5～20min; D, by deionized water, described silicon chip is cleaned; E, the mixed solution by hydrochloric acid and hydrofluoric acid are cleaned silicon chip, and described hydrogen chloride and hydrofluoric quality proportioning are 1～3: 1, and described cleaning temperature is 15～25 ℃, and described scavenging period is 30～90s; F, by deionized water, described silicon chip is cleaned.
In a preferred embodiment, the cleaning fluid of described correspondence is arranged in corresponding rinse bath, and described silicon chip is cleaned in corresponding rinse bath by the mode of immersion or hydro-peening.
In a preferred embodiment, in step a, the mass percent concentration of described concentrated sulfuric acid stoste is 98.3%, and the mass percent concentration of described hydrogenperoxide steam generator stoste is 30%, and the quality proportioning of described sulfuric acid, hydrogen peroxide and water is 65～170: 1: 3～6.
In further preferred embodiment, the quality proportioning of described sulfuric acid, hydrogen peroxide and water is 70: 1: 3.5, and cleaning temperature is 122 ℃, and scavenging period is 10min.
In a preferred embodiment, in step c, the mass percent concentration of described hydrogenperoxide steam generator stoste is 30%, and the quality proportioning of described hydrogen peroxide and water is 1: 5, and described cleaning temperature is 65 ℃, and described scavenging period is 10min; Described salpeter solution stock solution quality percent concentration is 47%, and the quality proportioning of described nitric acid and water is 1: 3, and described cleaning temperature is 65 ℃, and described scavenging period is 10min.
In a preferred embodiment, in step e, the mass percent concentration of described hydrochloric acid and hydrofluoric acid stoste is respectively 37% and 49%, and the quality proportioning of hydrogen chloride, hydrogen fluoride and water is 4: 5: 50, and described cleaning temperature is 25 ℃, and described scavenging period is 50s.
In a preferred embodiment, in step c, described hydrogenperoxide steam generator or salpeter solution, for removing the residual and part metals particle of the carbon of the concentrated sulfuric acid after processing, form layer oxide film at silicon chip surface simultaneously, in step e, described oxide-film is removed by hydrofluoric acid.
The present invention also provides a kind of cleaning equipment for the above-mentioned silicon wafer cleaning method for the preparation of efficient solar battery, and this cleaning equipment comprises the first rinse bath, the first rinsing bowl, the second rinse bath, the second rinsing bowl, the 3rd rinse bath and the 3rd rinsing bowl; The mixed solution that cleaning fluid in described the first rinse bath is the concentrated sulfuric acid and hydrogenperoxide steam generator, the quality proportioning of described sulfuric acid and hydrogen peroxide is 65～170: 1, cleaning fluid in described the second rinse bath is hydrogenperoxide steam generator or salpeter solution, the quality proportioning of described hydrogen peroxide and water is 1: 3～10, and the quality proportioning of described nitric acid and water is 1: 2～5; The mixed solution that cleaning fluid in described the 3rd rinse bath is hydrochloric acid and hydrofluoric acid, described hydrogen chloride and hydrofluoric quality proportioning are 1～3: 1.
In a preferred embodiment, the quality proportioning of sulfuric acid, hydrogen peroxide and water described in the first rinse bath is 65～170: 1: 3～6; When described in the second rinse bath, cleaning fluid is hydrogenperoxide steam generator, the quality proportioning of described hydrogen peroxide and water is 1: 5, and when described in the second rinse bath, cleaning fluid is salpeter solution, the quality proportioning of nitric acid and water is 1: 3; Described in the 3rd rinse bath, the quality proportioning of hydrogen chloride, hydrogen fluoride and water is 4: 5: 50.
In further preferred embodiment, described in described the first rinse bath, the quality proportioning of sulfuric acid, hydrogen peroxide and water is 70: 1: 3.5.
With quality proportioning low hydrophobic properties of the surface poor compare that can cause matte silicon chip of sulfuric acid in prior art with hydrogen peroxide, the present invention by the quality proportioning of sulfuric acid and hydrogen peroxide from 15～30 of prior art: 1 brings up to 65～170: 1, thereby improve the hydrophobic properties of the surface of matte silicon chip.
With clean and compare by sulfuric acid and mixed solution of hydrogen peroxide in prior art, silicon wafer cleaning method for the preparation of efficient solar battery of the present invention and cleaning equipment are also being removed the residual and part metals particle of carbon and are forming layer oxide film by hydrogenperoxide steam generator or salpeter solution thereafter, then remove described oxide-film by the mixed solution of hydrochloric acid and hydrofluoric acid, therefore can effectively improve the hydrophobic performance of silicon chip, even the dehydration fully after the deoxidation film of the silicon chip after cleaning.
The accompanying drawing explanation
The composition structural representation that Fig. 1 is the equipment of the Wafer Cleaning for the preparation of efficient solar battery of the present invention;
The flow chart that Fig. 2 is the silicon wafer cleaning method for the preparation of efficient solar battery of the present invention;
Fig. 3 is through the cleaning method shown in Fig. 2 of the present invention and the minority carrier life time contrast of silicon chip after other cleaning methods clean;
The electrical property of the minority carrier life time that Fig. 4 is silicon chip after the cleaning method shown in Fig. 2 of the present invention cleans and made solar cell.
Specific embodiments
Describe purpose of the present invention and effect in detail below in conjunction with specific embodiment and accompanying drawing.
Referring to Fig. 1, the equipment of the Wafer Cleaning for the preparation of efficient solar battery of the present invention comprises the first rinse bath 1, the first rinsing bowl 2, the second rinse bath 3, the second rinsing bowl 4, the 3rd rinse bath 5 and the 3rd rinsing bowl 6.The cleaning fluid of described correspondence is arranged in corresponding rinse bath, deionized water is arranged in corresponding rinsing bowl, described silicon chip is cleaned in corresponding rinse bath and rinsing bowl by the mode of immersion or hydro-peening, described cleaning setting can also be provided with the mechanical device automatically silicon chip shifted between each groove, this is the industry known techniques, does not repeat them here.
The mixed solution that cleaning fluid in described the first rinse bath 1 is the concentrated sulfuric acid and hydrogenperoxide steam generator, the quality proportioning of described sulfuric acid and hydrogen peroxide is 65～170: 1, the quality proportioning of described sulfuric acid, hydrogen peroxide and water is 65～170: 1: 3～6.In the first embodiment of cleaning equipment of the present invention, described in described the first rinse bath, the quality proportioning of sulfuric acid, hydrogen peroxide and water is 70: 1: 3.5.
Cleaning fluid in described the second rinse bath 3 is hydrogenperoxide steam generator or salpeter solution, and the quality proportioning of described hydrogen peroxide and water is 1: 3～10, and the quality proportioning of described nitric acid and water is 1: 2～5.In the first embodiment of cleaning equipment of the present invention, the cleaning fluid in described the second rinse bath 2 is hydrogenperoxide steam generator, and the quality proportioning of described hydrogen peroxide and water is 1: 5.In other embodiment of cleaning equipment of the present invention, the cleaning fluid in described the second rinse bath 2 is salpeter solution, and the quality proportioning of described nitric acid and water is 1: 3.
The mixed solution that cleaning fluid in described the 3rd rinse bath 5 is hydrochloric acid and hydrofluoric acid, described hydrogen chloride and hydrofluoric quality proportioning are 1～3: 1.In the first embodiment of cleaning equipment of the present invention, described in described the 3rd rinse bath 5, the quality proportioning of hydrogen chloride, hydrogen fluoride and water is 4: 5: 50.
Deionization resistivity of water in described the first rinsing bowl 2, the second rinsing bowl 4 and the 3rd rinsing bowl 6 is greater than 10M Ω.
Referring to Fig. 2, in conjunction with referring to Fig. 1, carry out the method for Wafer Cleaning by the equipment of the Wafer Cleaning for the preparation of efficient solar battery of the present invention and at first carry out step S20, the mixed solution by the concentrated sulfuric acid and hydrogenperoxide steam generator is cleaned silicon chip; At first in the first rinse bath 1, configure the mixed solution of the concentrated sulfuric acid and hydrogenperoxide steam generator, the mass percent concentration of described concentrated sulfuric acid stoste is 98.3%, the mass percent concentration of described hydrogenperoxide steam generator stoste is 30%, and in the solution configured, the quality proportioning of sulfuric acid, hydrogen peroxide and water is 65～170: 1: 3～6; Then by artificial or mechanical transfer mode, silicon chip is placed in the first rinse bath and is cleaned, cleaning temperature is 100～125 ℃, and scavenging period is 5～30min.In the first embodiment of cleaning method of the present invention, the quality proportioning of described sulfuric acid, hydrogen peroxide and water is 70: 1: 3.5, and described cleaning temperature is 122 ℃, and scavenging period is 10min.
Then continue step S21, by deionized water, described silicon chip is cleaned, described deionization resistivity of water is greater than 10M Ω, and silicon chip completing steps S20 cleaned by the mode of water cutter hydro-peening is cleaned, and washing time is 3～5min.
Then continue step S22, by hydrogenperoxide steam generator or salpeter solution, silicon chip is cleaned, at first in the second rinse bath 3, configure hydrogenperoxide steam generator or salpeter solution, the mass percent concentration of described hydrogenperoxide steam generator stoste is 30%, and the described hydrogen peroxide of the second rinse bath 3 be equipped with and the quality proportioning of water are 1: 3～10; Described salpeter solution stock solution quality percent concentration is 47%, and the described nitric acid of the second rinse bath 3 be equipped with and the quality proportioning of water are 1: 2～5; After in the second rinse bath 3, being equipped with hydrogenperoxide steam generator or salpeter solution, described silicon chip is arranged in the second rinse bath 3 and is cleaned by artificial or mechanical transfer mode, described cleaning temperature is 60～80 ℃, and described scavenging period is 5～20min.In this step, described hydrogenperoxide steam generator or salpeter solution can effectively be removed the residual and part metals particle of the carbon of the concentrated sulfuric acid after processing, and form layer oxide film at silicon chip surface simultaneously.In the first embodiment of cleaning method of the present invention, this step is cleaned silicon chip by hydrogenperoxide steam generator, and the quality proportioning of described hydrogen peroxide and water is 1: 5, and described cleaning temperature is 65 ℃, and described scavenging period is 10min.In other embodiment of cleaning method of the present invention, this step is cleaned silicon chip by salpeter solution, and the quality proportioning of described nitric acid and water is 1: 3, and described cleaning temperature is 65 ℃, and described scavenging period is 10min.
Then continue step S23, by deionized water, described silicon chip is cleaned, described deionization resistivity of water is greater than 10M Ω, and silicon chip completing steps S22 cleaned by the mode of water cutter hydro-peening is cleaned, and washing time is 3～5min.
Then continue step S24, mixed solution by hydrochloric acid and hydrofluoric acid is cleaned silicon chip, at first in the 3rd rinse bath 5, configure the mixed solution of hydrochloric acid and hydrofluoric acid, the mass percent concentration of described hydrochloric acid and hydrofluoric acid stoste is respectively 37% and 49%, and hydrogen chloride described in the cleaning fluid be equipped with and hydrofluoric quality proportioning are 1～3: 1; Silicon chip is arranged in the 3rd rinse bath 5 silicon chip is cleaned by artificial or mechanical transfer mode, and described cleaning temperature is 15～25 ℃, and described scavenging period is 30～90s.In the first embodiment of cleaning method of the present invention, in this step, the quality proportioning of hydrogen chloride, hydrogen fluoride and water is 4: 5: 50, and described cleaning temperature is 25 ℃, and described scavenging period is 50s.In this step, step S22 is removed by hydrofluoric acid at the formed oxide-film of silicon chip surface.
Then continue step S25, by deionized water, described silicon chip is cleaned, described deionization resistivity of water is greater than 10M Ω, and silicon chip completing steps S24 cleaned by the mode of water cutter hydro-peening is cleaned, and washing time is 3～5min.
Referring to Fig. 3, it has shown respectively 10 is one group three groups of silicon chips adopt respectively the RCA cleaning method, the minority carrier life time of silicon chip after the first embodiment of cleaning method of the present invention and common nitration mixture cleaning method (usually using the mixed solution of hydrofluoric acid and nitric acid) clean, the curve of the minority carrier life time of the silicon chip that three kinds of cleaning methods clean is respectively C1, C2 and C3, can obviously find out that from figure the minority carrier life time that cleaning method silicon chip of the present invention is corresponding obviously is better than by the silicon chip minority carrier life time of common nitration mixture cleaning method gained, only slightly be worse than the silicon chip minority carrier life time of RCA cleaning method gained.But cleaning method of the present invention does not exist the existing square resistance of RCA cleaning method to be difficult to the problems such as control and complex process and life cycle is short.
It should be noted that, the minority carrier life time of silicon chip as herein described is not directly surveyed its minority carrier life time to the silicon chip after cleaning, but silicon chip is carried out effective minority carrier life time of the silicon chip that records after surface passivation after Wafer Cleaning, " minority carrier life time of silicon chip " as herein described refers to " effective minority carrier life time of silicon chip after surface passivation ", and passivating film can adopt silica or silicon nitride etc.
In addition, the open-circuit voltage curve C 4 of the minority carrier life time curve C 5 of the silicon chip from the cleaning method of the present invention shown in Fig. 4 cleans and made solar cell silicon wafer can be found out, the minority carrier life time of the silicon chip after cleaning method of the present invention cleans all is more than or equal to 292 μ s, and the equal large and 684mV of corresponding open-circuit voltage Voc.
In sum, silicon wafer cleaning method for the preparation of efficient solar battery of the present invention and cleaning equipment are first cleaned silicon chip by the mixed solution of the concentrated sulfuric acid and hydrogenperoxide steam generator, by deionized water, cleaned afterwards, then by hydrogenperoxide steam generator or salpeter solution, silicon chip is cleaned to remove the residual and part metals particle of carbon and form layer oxide film and by washed with de-ionized water, finally the mixed solution by hydrochloric acid and hydrofluoric acid is to remove the oxide-film on described silicon chip and to be cleaned by the deionized water sheet.The present invention can effectively improve the hydrophobic performance of silicon chip, even the dehydration fully after the deoxidation film of the silicon chip after cleaning.
Claims (10)
1. the silicon wafer cleaning method for the preparation of efficient solar battery, it is characterized in that, the method comprises the following steps: a, the mixed solution by the concentrated sulfuric acid and hydrogenperoxide steam generator are cleaned silicon chip, the quality proportioning of sulfuric acid and hydrogen peroxide is 65～170: 1, cleaning temperature is 100～125 ℃, and scavenging period is 5～30min; B, by deionized water, described silicon chip is cleaned; C, by hydrogenperoxide steam generator or salpeter solution, silicon chip is cleaned, the quality proportioning of described hydrogen peroxide and water is 1: 3～10, the quality proportioning of described nitric acid and water is 1: 2～5, and described cleaning temperature is 60～80 ℃, and described scavenging period is 5～20min; D, by deionized water, described silicon chip is cleaned; E, the mixed solution by hydrochloric acid and hydrofluoric acid are cleaned silicon chip, and described hydrogen chloride and hydrofluoric quality proportioning are 1～3: 1, and described cleaning temperature is 15～25 ℃, and described scavenging period is 30～90s; F, by deionized water, described silicon chip is cleaned.
2. the silicon wafer cleaning method for the preparation of efficient solar battery according to claim 1, is characterized in that, the cleaning fluid of described correspondence is arranged in corresponding rinse bath, and described silicon chip is cleaned in corresponding rinse bath by the mode of immersion or hydro-peening.
3. the silicon wafer cleaning method for the preparation of efficient solar battery according to claim 1, it is characterized in that, in step a, the mass percent concentration of described concentrated sulfuric acid stoste is 98.3%, the mass percent concentration of described hydrogenperoxide steam generator stoste is 30%, and the quality proportioning of described sulfuric acid, hydrogen peroxide and water is 65～170: 1: 3～6.
4. the silicon wafer cleaning method for the preparation of efficient solar battery according to claim 3, is characterized in that, the quality proportioning of described sulfuric acid, hydrogen peroxide and water is 70: 1: 3.5, and cleaning temperature is 122 ℃, and scavenging period is 10min.
5. the silicon wafer cleaning method for the preparation of efficient solar battery according to claim 1, it is characterized in that, in step c, the mass percent concentration of described hydrogenperoxide steam generator stoste is 30%, the quality proportioning of described hydrogen peroxide and water is 1: 5, described cleaning temperature is 65 ℃, and described scavenging period is 10min; Described salpeter solution stock solution quality percent concentration is 47%, and the quality proportioning of described nitric acid and water is 1: 3, and described cleaning temperature is 65 ℃, and described scavenging period is 10min.
6. the silicon wafer cleaning method for the preparation of efficient solar battery according to claim 1, it is characterized in that, in step e, the mass percent concentration of described hydrochloric acid and hydrofluoric acid stoste is respectively 37% and 49%, the quality proportioning of hydrogen chloride, hydrogen fluoride and water is 4: 5: 50, described cleaning temperature is 25 ℃, and described scavenging period is 50s.
7. the silicon wafer cleaning method for the preparation of efficient solar battery according to claim 1, it is characterized in that, in step c, described hydrogenperoxide steam generator or salpeter solution are for removing the residual and part metals particle of the carbon of the concentrated sulfuric acid after processing, form layer oxide film at silicon chip surface simultaneously, in step e, described oxide-film is removed by hydrofluoric acid.
8. the cleaning equipment for the described silicon wafer cleaning method for the preparation of efficient solar battery of claim 1 to 7 any one, it is characterized in that, this cleaning equipment comprises the first rinse bath, the first rinsing bowl, the second rinse bath, the second rinsing bowl, the 3rd rinse bath and the 3rd rinsing bowl; The mixed solution that cleaning fluid in described the first rinse bath is the concentrated sulfuric acid and hydrogenperoxide steam generator, the quality proportioning of described sulfuric acid and hydrogen peroxide is 65～170: 1, cleaning fluid in described the second rinse bath is hydrogenperoxide steam generator or salpeter solution, the quality proportioning of described hydrogen peroxide and water is 1: 3～10, and the quality proportioning of described nitric acid and water is 1: 2～5; The mixed solution that cleaning fluid in described the 3rd rinse bath is hydrochloric acid and hydrofluoric acid, described hydrogen chloride and hydrofluoric quality proportioning are 1～3: 1.
9. the equipment of the Wafer Cleaning for the preparation of efficient solar battery according to claim 8, is characterized in that, the quality proportioning of sulfuric acid, hydrogen peroxide and water described in the first rinse bath is 65～170: 1: 3～6; When described in the second rinse bath, cleaning fluid is hydrogenperoxide steam generator, the quality proportioning of described hydrogen peroxide and water is 1: 5, and when described in the second rinse bath, cleaning fluid is salpeter solution, the quality proportioning of nitric acid and water is 1: 3; Described in the 3rd rinse bath, the quality proportioning of hydrogen chloride, hydrogen fluoride and water is 4: 5: 50.
10. the equipment of the Wafer Cleaning for the preparation of efficient solar battery according to claim 9, is characterized in that, described in described the first rinse bath, the quality proportioning of sulfuric acid, hydrogen peroxide and water is 70: 1: 3.5.
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| CN106952805A (en) * | 2017-04-11 | 2017-07-14 | 东方日升新能源股份有限公司 | A kind of graphite boat cleaning |
| CN111468462A (en) * | 2019-01-23 | 2020-07-31 | 山东浪潮华光光电子股份有限公司 | Method for removing ceramic disc carbide layer for L ED thinning paster |
| CN114226327A (en) * | 2021-12-17 | 2022-03-25 | 富乐德科技发展（天津）有限公司 | Cleaning method for removing composite sediment deposited on surface of ceramic substrate |
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