CN102921665A - Cleaning solution and cleaning method for silicon nitride film on surface of silicon chip - Google Patents
Cleaning solution and cleaning method for silicon nitride film on surface of silicon chip Download PDFInfo
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- CN102921665A CN102921665A CN2012103655468A CN201210365546A CN102921665A CN 102921665 A CN102921665 A CN 102921665A CN 2012103655468 A CN2012103655468 A CN 2012103655468A CN 201210365546 A CN201210365546 A CN 201210365546A CN 102921665 A CN102921665 A CN 102921665A
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- silicon chip
- cleaning fluid
- nitride film
- silicon nitride
- silicon
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 72
- 239000010703 silicon Substances 0.000 title claims abstract description 72
- 238000004140 cleaning Methods 0.000 title claims abstract description 71
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 47
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 33
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000012530 fluid Substances 0.000 claims description 50
- 239000002893 slag Substances 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 235000011194 food seasoning agent Nutrition 0.000 claims description 3
- 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
- 238000007605 air drying Methods 0.000 description 7
- 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
- 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
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 238000002360 preparation method Methods 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
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 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
- 230000007774 longterm Effects 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
- 239000002245 particle Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000002000 scavenging effect Effects 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 cleaning solution and a cleaning method for a silicon nitride film on the surface of a silicon chip. The method comprises the following step of: cleaning the silicon nitride film on the surface of the silicon chip by adopting the cleaning solution, wherein the cleaning solution contains potassium permanganate and hydrofluoric acid in a mass ratio of 1: (90-130). According to the technical scheme, the silicon nitride film on the surface of the unqualified silicon chip (a dreg falling chip or a rainbow chip) is cleaned by adopting the cleaning solution prepared by dissolving the potassium permanganate and the hydrofluoric acid in the mass ratio of 1: (90-130) into water, so that the silicon nitride film on the surface can be removed, the thickness of the silicon chip can also be ensured, and corrosion of the silicon chip is not affected by the length of the reaction time.
Description
Technical field
The present invention relates to the 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 the prior art, the main flow process of the production 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 Chemical Vapor 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 simultaneously the good ability that stops sodium ion, shelters metal and water vapor diffusion; Its chemical stability is also fine, and except hydrofluoric acid and hot phosphoric acid can slowly corrode, other acid was substantially inoperative with it.
Yet in the manufacture of solar cells process, the PECVD operation the defective cell piece of plated film outward appearance easily occurs owing to equipment or technique is unusual.As fall slag sheet, rainbow plate etc., wherein, fall that the slag sheet refers to since on the equipment silicon nitride particle of long-term deposition drop to silicon chip surface, cause being blocked by silicon nitride the silicon chip of the silicon nitride film that the position can not plate; Rainbow plate refers to because device transmission stops, the graphite boat of carrying silicon chip is stuck in the processing chamber, and the silicon chip of the silicon chip surface silicon nitride film uneven distribution of formation is because different silicon nitride deposit thickness can present different colors, therefore, this type of silicon chip is called rainbow plate.
In order to reduce production costs, special cleaning method is processed the purpose that reaches the secondary utilization thereby this type of cell piece need to be chosen employing before printing.At present, usually use following method that underproof silicon chip is cleared up: 1, with the silicon nitride film behind the hydrofluoric acid clean PECVD: use HF and pure water to regulate the cleaning fluid of suitable concentration, the silicon chip behind the plated film is carried out the soaking and washing striping.2, with silicon nitride film behind the phosphoric acid cleaning PECVD: use H
3PO
4Cleaning fluid with pure water adjusting suitable concentration carries out the soaking and washing striping to the silicon chip after behind the plated film.3, with silicon nitride film behind hydrofluoric acid and the nitric acid mixed liquor cleaning PECVD: use HF and HNO
3Mixed liquor is regulated the suitable concentration cleaning fluid, and silicon chip behind the PECVD is carried out the soaking and washing striping.But existing these cleaning methods can cause serious waste usually, this be because PECVD after defective silicon chip be divided into two kinds: 1, fall the slag sheet: about the even 80nm of whole plated film, part surface not plated film cause surperficial defective; 2, rainbow plate: monolithic membrane thickness unevenness thickness is at 75～200nm.Existing technique can be cleared up the defective silicon chip of the first and be recycled, and defective silicon chip behind the second plated film uses existing the 1st, 2 kind of scheme to process this type of silicon chip because thickness is uneven, causes and can't the secondary utilization cause waste.Use the 3rd kind of scheme to remove, but since in the 3rd the scheme herb liquid can corrode silicon chip, 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 fully the silicon nitride film of full wafer to be cleaned up, can cause the silicon chip uneven distribution can't the secondary utilization after the cleaning.
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 carry out the technical problem that silicon nitride film is removed to falling slag sheet or rainbow plate to solve cleaning method of the prior art.
To achieve these goals, according to an aspect of the present invention, provide a kind of sweep-out method of silicon nitride film of silicon chip surface.The method may further comprise the steps: adopt cleaning fluid to remove the silicon nitride film of silicon chip surface, wherein to contain mass ratio be 1: 90～130 potassium permanganate and hydrofluoric acid to cleaning fluid.
Further, to contain mass ratio be 1: 120 potassium permanganate and hydrofluoric acid to cleaning fluid.
Further, the quality percentage composition 1%～10% of potassium permanganate in the cleaning fluid, the quality percentage composition of hydrofluoric acid is 40%～80%.
Further, silicon chip adopts cleaning fluid at room temperature to soak 0.4～1 hour falling the slag sheet for falling the slag sheet.
Further, adopt cleaning fluid to soak 0.5 hour falling the slag sheet.
Further, silicon chip is rainbow plate, adopts cleaning fluid at room temperature rainbow plate to be soaked 3.5～4.5 hours.
Further, adopt cleaning fluid that rainbow plate was soaked 4 hours.
Further, after adopting cleaning fluid to remove the silicon nitride film of silicon chip surface, further comprise: adopt pure water that silicon chip is washed twice, then with hot-air seasoning the silicon chip of removing silicon nitride film is carried out drying.
According to another aspect of the present invention, provide a kind of removing liquid for removing the silicon chip surface silicon nitride film, the quality percentage composition of potassium permanganate is 1%～10% in this cleaning fluid, and the quality percentage of hydrofluoric acid contains 40%～80%.
Use technical scheme of the present invention, adopt potassium permanganate and hydrofluoric acid to clean according to the silicon nitride film of 1: 90～130 the mass ratio cleaning fluid that is mixed with soluble in water to underproof silicon chip (falling slag sheet or rainbow plate) surface, not only can remove the silicon nitride film on surface, simultaneously can also guarantee the thickness of silicon chip, and the corrosion of silicon chip is not subjected to the impact of reaction time length.
The specific embodiment
Need to prove, in the situation that do not conflict, embodiment and the feature among the embodiment among the present invention can make up mutually.Describe the present invention in detail below in conjunction with embodiment.
A kind of typical embodiment according to the present invention, the sweep-out method of silicon nitride film may further comprise the steps: adopt cleaning fluid to remove the silicon nitride film of silicon chip surface, wherein to contain mass ratio be 1: 90～130 potassium permanganate and hydrofluoric acid to cleaning fluid.Adopt potassium permanganate and hydrofluoric acid according to 1: 90～130 the mass ratio cleaning fluid that is mixed with soluble in water the silicon nitride film on underproof silicon chip (falling slag sheet or rainbow plate) surface to be removed, only do not react in silicon chip in silicon nitride reaction because potassium permanganate has oxidisability.For cleaning rainbow plate, because the uneven distribution of 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, can also guarantee the thickness of silicon chip simultaneously, be not subjected to the impact in reaction time to silicon slice corrosion.Present existing technique, major part are to adopt nitric acid in the mixed liquor of HF, and wherein nitric acid also has and has oxidisability, but also reacts with silicon chip simultaneously.Because the uneven distribution of silicon nitride film on the rainbow plate can continue corrosion of silicon after the place cleaning that film is thin is removed, and causes whole silicon nitride films to remove the uneven distribution of rear silicon chip, affects the secondary utilization.Preferably, to contain mass ratio be 1: 120 potassium permanganate and hydrofluoric acid to described cleaning fluid.
Adopt cleaning fluid of the present invention, can carry out according to thickness of the silicon nitride film that will remove etc. the adjusting of concentration, preferably, the quality percentage composition of potassium permanganate is 1%～10% in the cleaning fluid, and the quality percentage composition of hydrofluoric acid is 40%～80%.Certainly, the prolongation soak time that the cleaning fluid of low concentration can be suitable, when the concentration of cleaning fluid is high, shortening soak time that can be suitable, a kind of typical embodiment according to the present invention adopts cleaning fluid at room temperature to soak 0.4～1 hour falling the slag sheet.Preferably, adopt cleaning fluid to soak 0.5 hour falling the slag sheet.A kind of typical embodiment according to the present invention adopts cleaning fluid at room temperature rainbow plate to be soaked 3.5～4.5 hours.Preferably, adopt cleaning fluid that rainbow plate was soaked 4 hours.
After adopting technical scheme of the present invention that the silicon nitride film of defective silicon chip (falling slag sheet or rainbow plate) is removed, the method that can adopt this leader usually to adopt is further cleared up silicon nitride film, preferably, adopt pure water that silicon chip is washed twice adopting cleaning fluid further to comprise after removing the silicon nitride film of described silicon chip surface, then with hot-air seasoning the silicon chip of removal silicon nitride film is carried out drying.The heated-air drying advantage is: 1, the silicon chip liquid residue is removed clean; 2, drying time is short.
Further specify beneficial effect of the present invention below in conjunction with embodiment.
Embodiment 1
1) preparation of cleaning fluid: according to 1: 90 the mass ratio cleaning fluid that is mixed with soluble in water, the quality percentage composition of hydrofluoric acid is 80% with potassium permanganate and hydrofluoric acid;
2) will fall the slag sheet and insert in the film magazine, put into the cleaning fluid for preparing;
3) soaked 30 minutes under the room temperature;
4) take out silicon chip purified rinse water 2 times;
5) adopt heated-air drying with silicon chip through the row heated-air drying.
Embodiment 2
1) preparation of cleaning fluid: according to 1: 120 the mass ratio cleaning fluid that is mixed with soluble in water, the quality percentage composition of hydrofluoric acid is 40% with potassium permanganate and hydrofluoric acid;
2) rainbow plate is inserted in the film magazine, put into the cleaning fluid for preparing;
3) soaked 4 hours under the room temperature;
4) take out silicon chip purified rinse water 2 times;
5) adopt heated-air drying with silicon chip through the row heated-air drying.
Embodiment 3
1) preparation of cleaning fluid: according to 1: 120 the mass ratio cleaning fluid that is mixed with soluble in water, the quality percentage composition of hydrofluoric acid is 60% with potassium permanganate and hydrofluoric acid;
2) will fall the slag sheet and insert in the film magazine, put into the cleaning fluid for preparing;
3) soaked 60 minutes under the room temperature;
4) take out silicon chip purified rinse water 2 times;
5) adopt heated-air drying with silicon chip through the row heated-air drying.
Secondary utilizes the standard of silicon chip:
1, the surface does not have foreign matter residual, and the surface all is former silicon chip color.
2, clean rear silicon wafer thickness and clean front silicon wafer thickness minimizing＜15%, the even tolerance of silicon chip thin and thick is less than 20um.Utilize said method to carry out the cleaning of rainbow plate, the result is as shown in table 1.
Table 1
The data declaration of table 1, present technique does not possess the ability of cleaning rainbow plate, the present invention mainly is that the cleaning for rainbow plate has outstanding effect, and adopt the long-time cleaning of cleaning method of the present invention can not impact former silicon chip, need not consider that scavenging period, can recycling to the infringement of silicon chip.
The above is the preferred embodiments of the present invention only, is not limited to the present invention, and 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 modification of doing, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. the sweep-out method of the silicon nitride film of a silicon chip surface is characterized in that, may further comprise the steps:
Adopt cleaning fluid to remove the silicon nitride film of described silicon chip surface, it is 1: 90～130 potassium permanganate and hydrofluoric acid that wherein said cleaning fluid contains mass ratio.
2. sweep-out method according to claim 1 is characterized in that, it is 1: 120 potassium permanganate and hydrofluoric acid that described cleaning fluid contains mass ratio.
3. sweep-out method according to claim 1 is characterized in that, the quality percentage composition 1%～10% of potassium permanganate in the described cleaning fluid, and the quality percentage composition of described hydrofluoric acid is 40%～80%.
4. sweep-out method according to claim 1 is characterized in that, described silicon chip is for falling the slag sheet,
Adopt described cleaning fluid at room temperature to fall the slag sheet and soaked 0.4～1 hour described.
5. sweep-out method according to claim 4 is characterized in that, adopts described cleaning fluid to fall the slag sheet and soaked 0.5 hour described.
6. sweep-out method according to claim 1 is characterized in that, described silicon chip is rainbow plate, adopts described cleaning fluid at room temperature described rainbow plate to be soaked 3.5～4.5 hours.
7. sweep-out method according to claim 6 is characterized in that, adopts described cleaning fluid that described rainbow plate was soaked 4 hours.
8. sweep-out method according to claim 1 is characterized in that, further comprises remove the silicon nitride film of described silicon chip surface at described employing cleaning fluid after:
Adopt pure water that described silicon chip is washed twice, then with hot-air seasoning the described silicon chip of removing silicon nitride film is carried out drying.
9. removing liquid of be used for removing the silicon chip surface silicon nitride film, it is characterized in that, it is 1: 90～130 potassium permanganate and hydrofluoric acid that described cleaning fluid contains mass ratio, the quality percentage composition of potassium permanganate is 1%～10% in the described cleaning fluid, and the quality percentage of described hydrofluoric acid contains 40%～80%.
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| 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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Cited By (3)
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| CN103715304A (en) * | 2013-12-24 | 2014-04-09 | 天津英利新能源有限公司 | Method for treating chromatic aberration piece through 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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| 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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| CN102921665B (en) | 2015-08-05 |
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