CN103013711A - Cleaning solution and cleaning process for removing metal ion contamination of crystalline silicon wafer - Google Patents
Cleaning solution and cleaning process for removing metal ion contamination of crystalline silicon wafer Download PDFInfo
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- CN103013711A CN103013711A CN2013100139630A CN201310013963A CN103013711A CN 103013711 A CN103013711 A CN 103013711A CN 2013100139630 A CN2013100139630 A CN 2013100139630A CN 201310013963 A CN201310013963 A CN 201310013963A CN 103013711 A CN103013711 A CN 103013711A
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Abstract
The invention relates to the technical field of metal ion removal and cleaning of a crystalline silicon solar cell, and particularly relates to a cleaning solution and cleaning process for removing metal ion contamination of a crystalline silicon wafer. The cleaning solution comprises 1.0*10<-5>-1.0*10<-3> mol/L chelator, acid and deionized water, wherein the acid ensures that the pH value of the cleaning solution is 2-4. The cleaning process comprises the following steps: 1, cleaning a silicon wafer with one of an HF solution, an HF+H2O2+H2O solution and a BOE+H2O2+H2O solution at room temperature for 1-5 minutes; 2, cleaning the silicon wafer with deionized water; 3, cleaning with the cleaning solution at room temperature for 2-10 minutes; and 4, rinsing the silicon wafer with deionized water to remove residual acid on the surface of the silicon wafer. According to the invention, the cleaning solution is simple in formula, low in cost and favorable in effect of removing metal ion contamination of a crystalline silicon wafer; and the cleaning process is performed at room temperature, and is low in production cost and simple to operate.
Description
Technical field
The present invention relates to crystal-silicon solar cell and go to metal ion cleaning technique field, especially a kind of scavenging solution and cleaning thereof of removing the crystal silicon chip metal ion pollution.
Background technology
At present the solar level crystal silicon chip is because the manufacturing process problem of itself, caused that the crystal silicon chip surface has that a large amount of metallic impurity are residual, organic pollutant is residual, particulate matter is residual etc.Metallic impurity remain in silicon chip surface or enter in the wafer bulk can become the current carrier deathnium, reduce the silicon chip minority carrier life time, electrical property to solar cell has a huge impact, and causes the open circuit voltage of battery, short-circuit current to reduce, thereby reduces battery efficiency.
Removing at present crystal silicon chip goes the purging method of metal ion pollution to mainly contain:
(1) RCA standard cleaning method:
(1) SC-1:NH
4OH/H
2O
2/ H
230～80 ℃ of O are because H
2O
2Oxygenizement, silicon chip surface generates one deck SiO
2Film is wetting ability, can be cleaned liquid between silicon chip surface and the particle and soak into.Because the zone of oxidation of silicon chip surface and the Si on silicon chip top layer are by NH
4The OH corrosion, the particle that therefore is attached to silicon chip surface just falls into scavenging solution, thereby reaches the purpose of removing particle.
(2) SC-2: HCl/H
2O
2/ H
2The metal contaminations such as 65～85 ℃ of sodium for the removal silicon chip surface of O, iron, magnesium.
(3) SC-3: H
2SO
4/ H
2O
2120～150 ℃ of SC-3 have very strong oxidation capacity, can will be dissolved in the scavenging solution after the burning, and can generate CO to oxidation operation
2And H
2O.Can remove heavy organic contaminations and the part metals of silicon chip surface pollutes with the SC-3 cleaning silicon chip.
But RCA cleaning production cost is high, and rinse liquid temperature is high, has therefore limited its application in the solar cell manufacturing.
(2) HCl+HF washing out method:
20～25 ℃ of HF+HCl of HF+HCl:HF+HCl can remove the natural oxidizing layer of silicon chip surface, therefore, the metallic impurity that are attached on the natural oxidizing layer will be dissolved in the scavenging solution, can remove the Al of silicon chip surface, Fe, Zn, the metals such as Ni, HF+HCl also can be removed the metal hydroxides that is attached on the natural oxidizing layer.But this purging method can not thoroughly be removed metal ion.
(3) silicon single crystal rough polishing technique: utilize the alkaline solution of high density that monocrystalline silicon surface is corroded fast to certain thickness, some metallic impurity that can remove like this monocrystalline silicon surface are residual, particle residue, organic contamination are residual, but it is residual also to have a small amount of metal ion.
The shortcomings such as the above purging method exists production cost high, and the removal metal ion is not thorough.Therefore need searching a kind of simple to operate, remove effective scavenging solution and the cleaning thereof of crystal silicon chip metal ion pollution.
Summary of the invention
In order to overcome the deficiency of existing technology, the invention provides a kind of scavenging solution and cleaning thereof of removing the crystal silicon chip metal ion pollution.
The technical solution adopted for the present invention to solve the technical problems is: a kind of scavenging solution of removing the crystal silicon chip metal ion pollution, and composed of the following components: sequestrant 1.0 * 10
-5Mol/L-1.0 * 10
-3Mol/L makes scavenging solution pH value scope in the acid of 2-4, and deionized water.
According to another embodiment of the invention, comprise that further described sequestrant is one or more in ethylenediamine tetraacetic acid (EDTA), nitrilotriacetic acid(NTA), diethylene triaminepentaacetic acid(DTPA), the triethylenetetraaminehexaacetic acid.
According to another embodiment of the invention, comprise that further described acid is one or more among the BOE of the buffering etching solution (Buffered Oxide Etch, hereinafter referred BOE) of hydrochloric acid, hydrofluoric acid, acetic acid, 6:1 or 10:1.
A kind of cleaning of the scavenging solution of removing the crystal silicon chip metal ion pollution is as follows:
The first step: use HF solution, HF+H
2O
2+ H
2O solution or BOE+H
2O
2+ H
2A kind of at room temperature cleaning silicon chip 1-5 min in the O solution.HF acid solution mass concentration is 3%-10%, HF+H
2O
2+ H
2The by volume 1:1:5 preparation of O solution, BOE+H
2O
2+ H
2The by volume 1:1:5 preparation of O solution;
Second step: use the washed with de-ionized water silicon chip;
The 3rd step: use above-mentioned scavenging solution to clean 2-10min under the room temperature;
The 4th step: use the deionized water rinsing silicon chip, the acid that remains in silicon chip surface is washed.
The invention has the beneficial effects as follows:
(1) a kind of scavenging solution and cleaning thereof of removing the crystal silicon chip metal ion pollution of the present invention, the scavenging solution prescription is simple, and is with low cost, and it is effective to remove the crystal silicon chip metal ion pollution.
(2) a kind of scavenging solution and cleaning thereof of removing the crystal silicon chip metal ion pollution of the present invention, cleaning is at room temperature carried out, and production cost is low, and is simple to operate.
Embodiment
A kind of scavenging solution of removing the crystal silicon chip metal ion pollution, composed of the following components: sequestrant 1.0 * 10
-5Mol/L-1.0 * 10
-3Mol/L makes scavenging solution pH value scope in the acid of 2-4, and deionized water.Described sequestrant is one or more in ethylenediamine tetraacetic acid (EDTA), nitrilotriacetic acid(NTA), diethylene triaminepentaacetic acid(DTPA), the triethylenetetraaminehexaacetic acid.Described acid is one or more among the BOE of the BOE of hydrochloric acid, hydrofluoric acid, acetic acid, 6:1 or 10:1.
A kind of cleaning of the scavenging solution of removing the crystal silicon chip metal ion pollution is as follows:
The first step: use HF solution, HF+H
2O
2+ H
2O solution or BOE+H
2O
2+ H
2A kind of at room temperature cleaning silicon chip 1-5 min in the O solution.HF acid solution mass concentration is 3%-10%, HF+H
2O
2+ H
2The by volume 1:1:5 preparation of O solution, BOE+H
2O
2+ H
2The by volume 1:1:5 preparation of O solution.Main Function is that the silicon chip surface zone of oxidation is removed, and the silicon below the zone of oxidation is eroded about 5-20 nm, the metal ion on silicon chip top layer can be exposed to silicon chip surface like this.
Second step: use the washed with de-ionized water silicon chip.Remove the residual acid solution of silicon chip surface.
The 3rd step: use above-mentioned scavenging solution to clean 2-10min under the room temperature.Above-mentioned scavenging solution component is:
Sequestrant 1.0 * 10
-5Mol/L-1.0 * 10
-3Mol/L
After acid added a certain amount of acid, the scavenging solution pH value was at 2-4
The deionized water surplus
Sequestrant is one or more in ethylenediamine tetraacetic acid (EDTA), nitrilotriacetic acid(NTA), diethylene triaminepentaacetic acid(DTPA), the triethylenetetraaminehexaacetic acid.
Acid is hydrochloric acid, hydrofluoric acid, acetic acid, BOE(6:1) or BOE(10:1) at least a.
Add acid solution H can be provided
+, when pH value was 2-4, sequestrant can form stable inner complex with many kinds of metal ions.
The 4th step: use the deionized water rinsing silicon chip, the acid that remains in silicon chip surface is washed.
The present invention is further illustrated below in conjunction with specific embodiment.But the present invention is not limited to following example.
Embodiment 1:
A kind of scavenging solution of removing the crystal silicon chip metal ion pollution, composed of the following components:
Sequestrant 1.0 * 10
-5Mol/L-1.0 * 10
-3Mol/L
BOE(6:1) with by volume 1:125 ratio preparation of water, the scavenging solution pH value is controlled at about 2-4
The deionized water surplus
Sequestrant is at least a in ethylenediamine tetraacetic acid (EDTA), nitrilotriacetic acid(NTA), diethylene triaminepentaacetic acid(DTPA), the triethylenetetraaminehexaacetic acid.
With above-mentioned scavenging solution the crystal silicon chip that has metallic pollution is carried out cleaning, step is as follows:
The first step: use BOE+H
2O
2+ H
2O solution is cleaning silicon chip 1-5 min at room temperature.BOE+H
2O
2+ H
2The by volume 1:1:5 preparation of O solution.
Second step: use the washed with de-ionized water silicon chip, remove the residual acid solution of silicon chip surface.
The 3rd step: use above-mentioned scavenging solution to clean 2-10min under the room temperature.
The 4th step: use the deionized water rinsing silicon chip.Remove the residual acid solution of silicon chip surface.
Through above-mentioned the crystal silicon chip that has metallic pollution is cleaned after, use annealing furnace in 700 degrees centigrade of lower nitrogen atmospheres, to be incubated 10 minutes, then use hydrofluoric acid to remove surface oxide layer, carry out again tincture of iodine passivation, use at last WCT-120 test silicon lamellar body minority carrier life time, with only use HF+HCl solution to clean after carry out again same subsequent disposal silicon chip compare test process and result such as table 1.
Table 1:
Embodiment 2:
A kind of scavenging solution of removing the crystal silicon chip metal ion pollution, composed of the following components:
Sequestrant 1.0 * 10
-5Mol/L-1.0 * 10
-3Mol/L
The by volume 1:3000 ratio preparation of HCl and water, the scavenging solution pH value is at 2-4
The deionized water surplus
Described sequestrant is at least a in ethylenediamine tetraacetic acid (EDTA), nitrilotriacetic acid(NTA), diethylene triaminepentaacetic acid(DTPA), the triethylenetetraaminehexaacetic acid.
To the technique that the crystal silicon chip that has metallic pollution cleans, contain following steps with above-mentioned scavenging solution:
The first step: use BOE+H
2O
2+ H
2O solution is cleaning silicon chip 1-5 min at room temperature.BOE+H
2O
2+ H
2The by volume 1:1:5 preparation of O solution.
Second step: use the washed with de-ionized water silicon chip, remove the residual acid solution of silicon chip surface.
The 3rd step: use above-mentioned scavenging solution to clean 2-10min under the room temperature.
The 4th step: use the deionized water rinsing silicon chip.Remove the residual acid solution of silicon chip surface.
Through above-mentioned the crystal silicon chip that has metallic pollution is cleaned after, use annealing furnace in 700 degrees centigrade of lower nitrogen atmospheres, to be incubated 10 minutes, then use hydrofluoric acid to remove surface oxide layer, carry out again tincture of iodine passivation, use at last WCT-120 test silicon lamellar body minority carrier life time, with only use HF+HCl solution to clean after carry out again same subsequent disposal silicon chip compare test process and result such as table 2.
Table 2:
Embodiment 3:
A kind of scavenging solution of removing the crystal silicon chip metal ion pollution, composed of the following components:
Sequestrant 1.0 * 10
-5Mol/L-1.0 * 10
-3Mol/L
The by volume 1:3000 ratio preparation of HF and water, the scavenging solution pH value is at 2-4
The deionized water surplus
Described sequestrant is at least a in ethylenediamine tetraacetic acid (EDTA), nitrilotriacetic acid(NTA), diethylene triaminepentaacetic acid(DTPA), the triethylenetetraaminehexaacetic acid.
To the technique that the crystal silicon chip that has metallic pollution cleans, contain following steps with above-mentioned scavenging solution:
The first step: use BOE+H
2O
2+ H
2O solution is cleaning silicon chip 1-5 min at room temperature.BOE+H
2O
2+ H
2The by volume 1:1:5 preparation of O solution.
Second step: use the washed with de-ionized water silicon chip, remove the residual acid solution of silicon chip surface.
The 3rd step: use above-mentioned scavenging solution to clean 2-10min under the room temperature.
The 4th step: use the deionized water rinsing silicon chip, remove the residual acid solution of silicon chip surface.
Through above-mentioned the crystal silicon chip that has metallic pollution is cleaned after, use annealing furnace in 700 degrees centigrade of lower nitrogen atmospheres, to be incubated 10 minutes, then use hydrofluoric acid to remove surface oxide layer, carry out again tincture of iodine passivation, use at last WCT-120 test silicon lamellar body minority carrier life time, with only use HF+HCl solution to clean after carry out again same subsequent disposal silicon chip compare test process and result such as table 3.
Table 3:
Cleaning fluid composition of the present invention is simple, and cost is low, and it is effective to remove the crystal silicon chip metal ion pollution, to the crystal silicon chip not damaged; It is high to clean crystal silicon chip efficient, and cleaning performance is good, economic security, process stabilization; Be worthy of popularization in related industries.
Claims (4)
1. a scavenging solution of removing the crystal silicon chip metal ion pollution is characterized in that, and is composed of the following components: sequestrant 1.0 * 10
-5Mol/L-1.0 * 10
-3Mol/L makes scavenging solution pH value scope in the acid of 2-4, and deionized water.
2. a kind of scavenging solution of removing the crystal silicon chip metal ion pollution according to claim 1, it is characterized in that described sequestrant is one or more in ethylenediamine tetraacetic acid (EDTA), nitrilotriacetic acid(NTA), diethylene triaminepentaacetic acid(DTPA), the triethylenetetraaminehexaacetic acid.
3. a kind of scavenging solution of removing the crystal silicon chip metal ion pollution according to claim 1 is characterized in that, described acid is one or more in the buffering etching solution of the buffering etching solution of hydrochloric acid, hydrofluoric acid, acetic acid, 6:1 or 10:1.
4. according to claim 1,2 or 3 described a kind of cleanings of removing the scavenging solution of crystal silicon chip metal ion pollution, it is characterized in that cleaning step is as follows:
The first step: use HF solution, HF+H
2O
2+ H
2O solution or buffering etching solution+H
2O
2+ H
2A kind of at room temperature cleaning silicon chip 1-5 min in the O solution; HF acid solution mass concentration is 3%-10%, HF+H
2O
2+ H
2The by volume 1:1:5 preparation of O solution, buffering etching solution+H
2O
2+ H
2The by volume 1:1:5 preparation of O solution;
Second step: use the washed with de-ionized water silicon chip;
The 3rd step: use above-mentioned scavenging solution to clean 2-10min under the room temperature;
The 4th step: use the deionized water rinsing silicon chip, the acid that remains in silicon chip surface is washed.
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|---|---|---|---|
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|---|---|---|---|
| CN2013100139630A CN103013711A (en) | 2013-01-15 | 2013-01-15 | Cleaning solution and cleaning process for removing metal ion contamination of crystalline silicon wafer |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105449045A (en) * | 2015-12-29 | 2016-03-30 | 常州比太科技有限公司 | Surface micro corrosion cleaning method applicable for crystal silicon wafer after RIE (Reactive Ion Etching) texturing |
| CN107123608A (en) * | 2017-06-19 | 2017-09-01 | 浙江晶科能源有限公司 | A kind of solar cell processing procedure metal ion pollution detection method and device |
| CN107369619A (en) * | 2016-05-12 | 2017-11-21 | 中芯国际集成电路制造(上海)有限公司 | A kind of semiconductor devices and preparation method, electronic installation |
| CN108384667A (en) * | 2018-02-28 | 2018-08-10 | 浙江晶科能源有限公司 | A kind of silicon chip cleaning liquid and silicon wafer cleaning method |
| CN108735575A (en) * | 2017-04-18 | 2018-11-02 | 上海新昇半导体科技有限公司 | Wafer processing method |
| CN109326505A (en) * | 2018-08-27 | 2019-02-12 | 上海申和热磁电子有限公司 | A kind of method and device for improving silicon wafer and finally cleaning metal degree |
| CN111540670A (en) * | 2020-05-11 | 2020-08-14 | 广州粤芯半导体技术有限公司 | Wet cleaning method for wafer and manufacturing method for semiconductor device |
| CN113956925A (en) * | 2021-11-10 | 2022-01-21 | 重庆臻宝实业有限公司 | Metal ion cleaning agent for semiconductor material |
| CN114806747A (en) * | 2022-04-28 | 2022-07-29 | 安徽富乐德科技发展股份有限公司 | Wafer cleaning water and method for cleaning wafer |
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| CN105449045B (en) * | 2015-12-29 | 2017-03-22 | 江西比太科技有限公司 | Surface micro corrosion cleaning method applicable for crystal silicon wafer after RIE (Reactive Ion Etching) texturing |
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| CN108384667A (en) * | 2018-02-28 | 2018-08-10 | 浙江晶科能源有限公司 | A kind of silicon chip cleaning liquid and silicon wafer cleaning method |
| CN109326505A (en) * | 2018-08-27 | 2019-02-12 | 上海申和热磁电子有限公司 | A kind of method and device for improving silicon wafer and finally cleaning metal degree |
| CN111540670A (en) * | 2020-05-11 | 2020-08-14 | 广州粤芯半导体技术有限公司 | Wet cleaning method for wafer and manufacturing method for semiconductor device |
| CN111540670B (en) * | 2020-05-11 | 2023-10-24 | 粤芯半导体技术股份有限公司 | Wet cleaning method for wafer and manufacturing method for semiconductor device |
| CN113956925A (en) * | 2021-11-10 | 2022-01-21 | 重庆臻宝实业有限公司 | Metal ion cleaning agent for semiconductor material |
| CN113956925B (en) * | 2021-11-10 | 2023-06-23 | 重庆臻宝科技股份有限公司 | Metal ion cleaning agent for semiconductor material |
| CN114806747A (en) * | 2022-04-28 | 2022-07-29 | 安徽富乐德科技发展股份有限公司 | Wafer cleaning water and method for cleaning wafer |
| CN115975738A (en) * | 2022-12-12 | 2023-04-18 | 嘉兴市小辰光伏科技有限公司 | Additive for reducing acid consumption in cleaning acid tank and application |
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Application publication date: 20130403 |