CN102921665B - The cleaning fluid of the silicon nitride film of silicon chip surface and sweep-out method - Google Patents
The cleaning fluid of the silicon nitride film of silicon chip surface and sweep-out method Download PDFInfo
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- CN102921665B CN102921665B CN201210365546.8A CN201210365546A CN102921665B CN 102921665 B CN102921665 B CN 102921665B CN 201210365546 A CN201210365546 A CN 201210365546A CN 102921665 B CN102921665 B CN 102921665B
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- Prior art keywords
- cleaning fluid
- silicon chip
- nitride film
- silicon nitride
- hydrofluoric acid
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 71
- 239000010703 silicon Substances 0.000 title claims abstract description 71
- 238000004140 cleaning Methods 0.000 title claims abstract description 66
- 239000012530 fluid Substances 0.000 title claims abstract description 53
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 42
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 28
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 18
- 239000002893 slag Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000007605 air drying Methods 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000005260 corrosion Methods 0.000 abstract description 5
- 230000007797 corrosion Effects 0.000 abstract description 5
- 230000035484 reaction time Effects 0.000 abstract description 3
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 8
- 230000002950 deficient Effects 0.000 description 7
- 238000009826 distribution Methods 0.000 description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 239000006117 anti-reflective coating Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- 235000011194 food seasoning agent Nutrition 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000003667 anti-reflective effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 235000008216 herbs Nutrition 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001039 wet etching Methods 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
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- Cleaning Or Drying Semiconductors (AREA)
Abstract
The invention discloses a kind of cleaning fluid and sweep-out method of silicon nitride film of silicon chip surface.The method comprises the following steps: adopt cleaning fluid to remove the silicon nitride film of silicon chip surface, wherein cleaning fluid contains potassium permanganate and the hydrofluoric acid that mass ratio is 1: 90 ~ 130.Apply technical scheme of the present invention, potassium permanganate and hydrofluoric acid is adopted to clean according to the silicon nitride film that the mass ratio cleaning fluid be mixed with soluble in water of 1: 90 ~ 130 is surperficial to underproof silicon chip (falling slag sheet or rainbow plate), not only can remove the silicon nitride film on surface, the thickness of silicon chip can also be ensured simultaneously, and the impact of reaction time length is not subject on the corrosion of silicon chip.
Description
Technical field
The present invention relates to solar cell preparing technical field, in particular to a kind of cleaning fluid and sweep-out method of silicon nitride film of silicon chip surface.
Background technology
In prior art, the production main flow of crystal silicon battery is generally: the deposition of making herbs into wool, diffusion, wet etching, antireflective coating, serigraphy and sintering.Wherein, the deposition of antireflective coating normally adopts PECVD (Plasma Enhanced ChemicalVapor Deposition, plasma reinforced chemical vapour deposition method) technique to form silicon nitride film.Silicon nitride (SI
3n
4) film is navy blue antireflective film-Si
3n
4film, it has remarkable anti-oxidant and insulating properties, has good stop sodium ion simultaneously, shelters the ability of metal and water vapor diffusion; Its chemical stability is also fine, and except hydrofluoric acid and hot phosphoric acid can slowly corrode, other acid is substantially inoperative with it.
But in manufacture of solar cells process, due to the exception of equipment or technique, easily there is the defective cell piece of plated film outward appearance in PECVD operation.As fallen slag sheet, rainbow plate etc., wherein, falling slag sheet refers to because the silicon nitride particle of long time sedimentation on equipment drops to silicon chip surface, causes the silicon chip being blocked the silicon nitride film that position can not plate by silicon nitride; Rainbow plate refers to because device transmission stops, the graphite boat of carrying silicon chip is stuck in processing chamber, and the silicon chip of the silicon chip surface silicon nitride film uneven distribution of formation, because different nitride deposition thickness can present different colors, therefore, this type of silicon chip is called rainbow plate.
In order to reduce production cost, this type of cell piece needs to choose the special cleaning method of employing before printing and carries out processing thus reach the object of secondary utilization.At present, following method is usually used to clear up underproof silicon chip: 1, with the silicon nitride film after hydrofluoric acid clean PECVD: to use HF and pure water to regulate the cleaning fluid of suitable concentration, carry out soaking and washing striping to the silicon chip after plated film.2, with silicon nitride film after phosphoric acid cleaning PECVD: use H
3pO
4regulate the cleaning fluid of suitable concentration with pure water, soaking and washing striping is carried out to the silicon chip after after plated film.3, with silicon nitride film after hydrofluoric acid and nitric acid mixed liquor cleaning PECVD: use HF and HNO
3mixed liquor regulates suitable concentration cleaning fluid, carries out soaking and washing striping to silicon chip after PECVD.But these cleaning methods existing can cause serious waste usually, this is because defective silicon chip is divided into two kinds after PECVD: 1, fall slag sheet: even about the 80nm of overall plated film, the surface that the non-plated film of part surface causes is defective; 2, rainbow plate: monolithic membrane thickness unevenness thickness is at 75 ~ 200nm.Existing technique can be cleared up the first defective silicon chip and be recycled, and after the second plated film, defective silicon chip, 2 kind scheme existing 1st because thickness inequality uses cannot process this type of silicon chip, causes to utilize and cause waste by secondary.Use the 3rd kind of scheme to remove, but can corrode silicon chip due to scheme herb liquid in the 3rd, the uneven distribution of rainbow plate silicon nitride film simultaneously, the silicon nitride film corrosion rate of the different thickness of liquid is different.In order to be cleaned up by the silicon nitride film of full wafer completely, silicon chip uneven distribution after cleaning, can be caused to utilize by secondary.
Summary of the invention
The present invention aims to provide a kind of cleaning fluid and sweep-out method of silicon nitride film of silicon chip surface, can not effectively to the technical problem falling slag sheet or rainbow plate and carry out silicon nitride film removing to solve cleaning method of the prior art.
To achieve these goals, according to an aspect of the present invention, a kind of sweep-out method of silicon nitride film of silicon chip surface is provided.The method comprises the following steps: adopt cleaning fluid to remove the silicon nitride film of silicon chip surface, wherein cleaning fluid contains potassium permanganate and the hydrofluoric acid that mass ratio is 1: 90 ~ 130.
Further, cleaning fluid contains potassium permanganate and the hydrofluoric acid that mass ratio is 1: 120.
Further, the mass percentage 1% ~ 10% of potassium permanganate in cleaning fluid, the mass percentage of hydrofluoric acid is 40% ~ 80%.
Further, silicon chip, for falling slag sheet, adopts cleaning fluid at room temperature to soak 0.4 ~ 1 hour falling slag sheet.
Further, cleaning fluid is adopted to soak 0.5 hour to falling slag sheet.
Further, silicon chip is rainbow plate, adopts cleaning fluid at room temperature to soak 3.5 ~ 4.5 hours rainbow plate.
Further, cleaning fluid is adopted to soak 4 hours to rainbow plate.
Further, comprise further after adopting cleaning fluid to remove the silicon nitride film of silicon chip surface: adopt pure water to carry out flushing twice to silicon chip, then with hot-air seasoning, drying is carried out to the silicon chip removing silicon nitride film.
According to another aspect of the present invention, provide a kind of removing liquid for removing silicon chip surface silicon nitride film, in this cleaning fluid, the mass percentage of potassium permanganate is 1% ~ 10%, and the percent mass of hydrofluoric acid is containing 40% ~ 80%.
Apply technical scheme of the present invention, potassium permanganate and hydrofluoric acid is adopted to clean according to the silicon nitride film that the mass ratio cleaning fluid be mixed with soluble in water of 1: 90 ~ 130 is surperficial to underproof silicon chip (falling slag sheet or rainbow plate), not only can remove the silicon nitride film on surface, the thickness of silicon chip can also be ensured simultaneously, and the impact of reaction time length is not subject on the corrosion of silicon chip.
Detailed description of the invention
It should be noted that, when not conflicting, the embodiment in the present invention and the feature in embodiment can combine mutually.The present invention is described in detail below in conjunction with embodiment.
According to a kind of typical embodiment of the present invention, the sweep-out method of silicon nitride film comprises the following steps: adopt cleaning fluid to remove the silicon nitride film of silicon chip surface, wherein cleaning fluid contains potassium permanganate and the hydrofluoric acid that mass ratio is 1: 90 ~ 130.Adopt potassium permanganate and hydrofluoric acid to remove according to the silicon nitride film that the mass ratio cleaning fluid be mixed with soluble in water of 1: 90 ~ 130 is surperficial to underproof silicon chip (falling slag sheet or rainbow plate), only do not react in silicon chip in silicon nitride reaction because potassium permanganate has oxidisability.For cleaning rainbow plate, uneven distribution due to the silicon nitride film of silicon chip surface causes the generation main cause of defective rainbow plate, use the present invention not only can remove the silicon nitride film on surface, the thickness of silicon chip can also be ensured simultaneously, be not subject to the impact in reaction time to silicon slice corrosion.Current existing technique, major part adopts nitric acid in the mixed liquor of HF, and wherein nitric acid also has and has oxidisability, but also reacts with silicon chip simultaneously.Due to the uneven distribution of silicon nitride film on rainbow plate, the place cleaning that film is thin can continue corrosion of silicon after removing, and the uneven distribution of silicon chip after causing whole silicon nitride film to be removed, affects secondary and utilize.Preferably, described cleaning fluid contains potassium permanganate and the hydrofluoric acid that mass ratio is 1: 120.
Adopt cleaning fluid of the present invention, can carry out the adjustment of concentration according to the thickness etc. of the silicon nitride film that will remove, preferably, in cleaning fluid, the mass percentage of potassium permanganate is 1% ~ 10%, and the mass percentage of hydrofluoric acid is 40% ~ 80%.Certainly, the prolongation soak time that the cleaning fluid of low concentration can be suitable, during the concentration height of cleaning fluid, shortening soak time that can be suitable, according to a kind of typical embodiment of the present invention, adopts cleaning fluid at room temperature to soak 0.4 ~ 1 hour falling slag sheet.Preferably, cleaning fluid is adopted to soak 0.5 hour to falling slag sheet.According to a kind of typical embodiment of the present invention, cleaning fluid is adopted at room temperature to soak 3.5 ~ 4.5 hours rainbow plate.Preferably, cleaning fluid is adopted to soak 4 hours to rainbow plate.
After adopting the silicon nitride film of technical scheme of the present invention to defective silicon chip (falling slag sheet or rainbow plate) to remove, the method that this leader can be adopted usually to adopt further is cleared up silicon nitride film, preferably, comprising further after employing cleaning fluid removes the silicon nitride film of described silicon chip surface adopts pure water to carry out flushing twice to silicon chip, then carries out drying with hot-air seasoning to the silicon chip removing silicon nitride film.Heated-air drying advantage is: 1, remove clean to silicon chip liquid residue; 2, drying time is short.
Beneficial effect of the present invention is further illustrated below in conjunction with embodiment.
Embodiment 1
1) preparation of cleaning fluid: by potassium permanganate and hydrofluoric acid according to 1: 90 mass ratio be soluble in waterly mixed with cleaning fluid, the mass percentage of hydrofluoric acid is 80%;
2) slag sheet will be fallen insert in film magazine, put into the cleaning fluid prepared;
3) soak 30 minutes under room temperature;
4) silicon chip purified rinse water is taken out 2 times;
5) heated-air drying is adopted by silicon chip through row heated-air drying.
Embodiment 2
1) preparation of cleaning fluid: by potassium permanganate and hydrofluoric acid according to 1: 120 mass ratio be soluble in waterly mixed with cleaning fluid, the mass percentage of hydrofluoric acid is 40%;
2) rainbow plate is inserted in film magazine, put into the cleaning fluid prepared;
3) soak 4 hours under room temperature;
4) silicon chip purified rinse water is taken out 2 times;
5) heated-air drying is adopted by silicon chip through row heated-air drying.
Embodiment 3
1) preparation of cleaning fluid: by potassium permanganate and hydrofluoric acid according to 1: 120 mass ratio be soluble in waterly mixed with cleaning fluid, the mass percentage of hydrofluoric acid is 60%;
2) slag sheet will be fallen insert in film magazine, put into the cleaning fluid prepared;
3) soak 60 minutes under room temperature;
4) silicon chip purified rinse water is taken out 2 times;
5) heated-air drying is adopted by silicon chip through row heated-air drying.
Secondary utilizes the standard of silicon chip:
1, surface does not have foreign matter to remain, and surface is all in former silicon chip color.
2, after cleaning, silicon wafer thickness comparatively cleans front silicon wafer thickness minimizing < 15%, and silicon chip thin and thick uniformity tolerances is less than 20um.Utilize said method to carry out the cleaning of rainbow plate, result is as shown in table 1.
Table 1
The data explanation of table 1, current technique does not possess the ability of cleaning rainbow plate, the present invention mainly has outstanding effect for the cleaning of rainbow plate, and adopt cleaning method of the present invention to clean for a long time can not to impact former silicon chip, the infringement of scavenging period to silicon chip need not be considered, can recycling.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (1)
1. a sweep-out method for the silicon nitride film of silicon chip surface, is characterized in that, described sweep-out method comprises the following steps:
1) preparation of cleaning fluid: potassium permanganate and hydrofluoric acid are mixed with described cleaning fluid according to the mass ratio of 1:90 is soluble in water, and the mass percentage of hydrofluoric acid is 80%;
2) slag sheet will be fallen insert in film magazine, put into described cleaning fluid;
3) soak 30 minutes under room temperature;
4) silicon chip purified rinse water is taken out 2 times;
5) adopt heated-air drying that silicon chip is carried out heated-air drying;
Or described sweep-out method comprises the following steps:
1) preparation of cleaning fluid: potassium permanganate and hydrofluoric acid are mixed with described cleaning fluid according to the mass ratio of 1:120 is soluble in water, and the mass percentage of hydrofluoric acid is 40%;
2) rainbow plate is inserted in film magazine, put into described cleaning fluid;
3) soak 4 hours under room temperature;
4) silicon chip purified rinse water is taken out 2 times;
5) adopt heated-air drying that silicon chip is carried out heated-air drying;
Or described sweep-out method comprises the following steps:
1) preparation of cleaning fluid: potassium permanganate and hydrofluoric acid are mixed with described cleaning fluid according to the mass ratio of 1:120 is soluble in water, and the mass percentage of hydrofluoric acid is 60%;
2) slag sheet will be fallen insert in film magazine, put into described cleaning fluid;
3) soak 60 minutes under room temperature;
4) silicon chip purified rinse water is taken out 2 times;
5) adopt heated-air drying that silicon chip is carried out heated-air drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210365546.8A CN102921665B (en) | 2012-09-27 | 2012-09-27 | The cleaning fluid of the silicon nitride film of silicon chip surface and sweep-out method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210365546.8A CN102921665B (en) | 2012-09-27 | 2012-09-27 | The cleaning fluid of the silicon nitride film of silicon chip surface and sweep-out method |
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| Publication Number | Publication Date |
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| CN102921665A CN102921665A (en) | 2013-02-13 |
| CN102921665B true CN102921665B (en) | 2015-08-05 |
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| CN103715304B (en) * | 2013-12-24 | 2016-09-07 | 天津英利新能源有限公司 | A kind of method realizing the process of aberration sheet based on wet etching machine |
| CN109848122A (en) * | 2018-12-29 | 2019-06-07 | 晶能光电（江西）有限公司 | The cleaning method of SiC panel surface AlN film layer |
| CN113637536A (en) * | 2021-08-10 | 2021-11-12 | 江苏凯威特斯半导体科技有限公司 | Strong oxidant cleaning solution and cleaning method for wafer boat in semiconductor production |
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| US7045073B2 (en) * | 2002-12-18 | 2006-05-16 | Intel Corporation | Pre-etch implantation damage for the removal of thin film layers |
| US7446051B2 (en) * | 2003-09-09 | 2008-11-04 | Csg Solar Ag | Method of etching silicon |
| WO2006096904A1 (en) * | 2005-03-16 | 2006-09-21 | Newsouth Innovations Pty Limited | Photolithography method for contacting thin-film semiconductor structures |
| KR100706822B1 (en) * | 2005-10-17 | 2007-04-12 | 삼성전자주식회사 | Composition for removing an insulation material, method of removing an insulation layer and method of recycling a substrate using the same |
| CN102151669B (en) * | 2010-11-26 | 2012-06-20 | 安阳市凤凰光伏科技有限公司 | Processing method of coating film crushed materials of solar silicon cell |
| CN102163549A (en) * | 2011-01-27 | 2011-08-24 | 巨力新能源股份有限公司 | Treating fluid for bad chip after crystalline silicon film coating and treating method thereof |
| CN102306687B (en) * | 2011-09-28 | 2012-12-05 | 湖南红太阳新能源科技有限公司 | Crystalline silica solar energy cell PECVD rainbow film reworking method |
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