CN107523880A - For the processing method of bad after Wool-making agent of bad processing and preparation method thereof after monocrystalline silicon making herbs into wool and monocrystalline silicon making herbs into wool - Google Patents

For the processing method of bad after Wool-making agent of bad processing and preparation method thereof after monocrystalline silicon making herbs into wool and monocrystalline silicon making herbs into wool Download PDF

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CN107523880A
CN107523880A CN201610446469.7A CN201610446469A CN107523880A CN 107523880 A CN107523880 A CN 107523880A CN 201610446469 A CN201610446469 A CN 201610446469A CN 107523880 A CN107523880 A CN 107523880A
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wool
bad
making herbs
monocrystalline silicon
making
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程寒松
李然
闫缓
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HANGZHOU JULI HYDROGEN ENERGY TECHNOLOGY Co Ltd
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HANGZHOU JULI HYDROGEN ENERGY TECHNOLOGY Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B33/00After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • C30B33/08Etching
    • C30B33/10Etching in solutions or melts

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  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

The present invention relates to Wool-making agent, disclose the Wool-making agent for bad processing after monocrystalline silicon making herbs into wool, including sodium hydroxide or potassium hydroxide and flocking additive, the weight/mass percentage composition of sodium hydroxide or potassium hydroxide is 0.5%~5%, the deionized water that flocking additive includes the low VOC that volumn concentration is 0.1%~8%, volumn concentration is 92%~99.9%.Also disclose its preparation method, and the processing method of bad after monocrystalline silicon making herbs into wool, bad after making herbs into wool is respectively placed in into ethanol, acetone and isopropanol to be cleaned by ultrasonic, bad after cleaning is placed in this kind of Wool-making agent, the mass loss of every very little silicon chip monolithic is 0.019g~0.044g, and matte controlled reflectivity system is 12%~14%.The present invention carries out making herbs into wool again to bad after etching and handled, and 95%~97%, silicon chip surface, without significant difference, the method increase the utilization rate of silicon chip, greatly save production cost the silicon chip yields after processing with normal silicon chip.

Description

For bad after Wool-making agent of bad processing and preparation method thereof after monocrystalline silicon making herbs into wool and monocrystalline silicon making herbs into wool Processing method
Technical field
The present invention relates to Wool-making agent, is related to the Wool-making agent for bad processing after monocrystalline silicon making herbs into wool, further relates to The method that this kind is used for the bad Wool-making agent handled after monocrystalline silicon making herbs into wool is made, and after monocrystalline silicon making herbs into wool not The processing method of good.
Background technology
Photovoltaic solar cell can realize opto-electronic conversion, and it produces electron hole pair by absorbing photon, And then potential can be produced at PN junction both ends, PN junction is connected with wire, electric current is formed, realizes light Can be to electric conversion of energy.
Effectively to utilize luminous energy, uniform matte generally is prepared on solar battery sheet surface, reduces the anti-of light Rate is penetrated, its production process includes making herbs into wool, diffusion, wet etching, plated film, printing-sintering, test etc., In actual production process, due to equipment or technological problemses, each operation can all produce the underproof silicon chip in part, Referred to as bad, cost can be caused to increase if directly scrapping processing by bad.During making herbs into wool, usually Occur that making herbs into wool is uneven, silicon chip turns white etc. bad, such silicon chip can reduce conversion efficiency, or even lead Cause to degrade or scrap so that production cost increase.This badness piece is handled, can typically be used again Making herbs into wool improves.
Currently for making herbs into wool is uneven, hickie, silicon chip turn white shinny etc. bad, majority is forged using high temperature After burning, then silicon chip is placed in making herbs into wool in alkali-Isopropanol Solvent, 10~20min of making herbs into wool time.The technological process is adopted With temperature programming calcining, time-consuming and requires harsher, follow-up making herbs into wool system reaction time length, and isopropyl Alcohol toxicity is larger, volatile, there is larger harm to environment.To solve the above problems, it need to develop new bad Piece processing method, on the basis of bad pile effects are improved, shorten the time, reduce cost.
The content of the invention
The present invention in view of the shortcomings of the prior art, discloses the making herbs into wool for bad processing after monocrystalline silicon making herbs into wool Agent, also disclose the method that this kind is used for the bad Wool-making agent handled after monocrystalline silicon making herbs into wool that makes, Yi Jidan The processing method of bad after crystal silicon making herbs into wool.The present invention proposes bad caused by existing making herbs into wool process The processing method of bad after a kind of fine-hair maring using monocrystalline silicon slice, this method can be entered in 5~10 minutes to bad Row making herbs into wool again, matte is uniform, surface is clean, and silicon chip yields is 95%~97%, using the processing method again Silicon chip reflectivity after making herbs into wool is 12%~14%.The application method can greatly save equipment cost and time cost. This method performs etching on bad surface, by controlling experiment condition (reaction temperature, time, making herbs into wool The parameters such as agent content), etch rate can be regulated and controled so that the making herbs into wool defect part of silicon chip surface passes through Wool-making agent Effect, etches uniform matte.
In order to solve the above-mentioned technical problem, the present invention is addressed by following technical proposals.
For the Wool-making agent of bad processing after monocrystalline silicon making herbs into wool, including sodium hydroxide or potassium hydroxide and making herbs into wool The weight/mass percentage composition of additive, sodium hydroxide or potassium hydroxide is 0.5%~5%, and flocking additive includes body It is 92%~99.9% to accumulate low VOC, volumn concentration that percentage composition is 0.1%~8% Deionized water.
Low content of volatile organic compounds is relatively low in the present invention, and main purpose is reduction reaction rate.The reason for this is that: First, reaction rate is slower, enables to the reaction on bad surface more gentle, ultimately forms uniform Matte, obtain the good silicon chip of making herbs into wool effect;Second, reaction rate is slower, can at utmost reduce bad The mass loss of piece so that bad again the quality after making herbs into wool still in the reasonable scope, do not influence follow-up work Sequence is normally carried out, and conference is crossed in mass loss causes silicon chip fragment rate increase in subsequent handling.Silicon after making herbs into wool Piece is sprayed, and acid cleaning process flow then can be entered together with normal silicon chip.
Preferably, low VOC is the low-grade aliphatic amine containing 3~7 carbon, contains 3~8 One or more in the polyalcohol of individual carbon, the carboxylic acid containing 3~14 carbon, the ethers containing 4~8 carbon. Low VOC in the present invention reacts with silicon chip surface plays the effect of masking, can lure Lead the generation of small crystal nucleus.
Preferably, the low-grade aliphatic amine containing 3~7 carbon be triethylamine, monoethanolamine, tetramethylethylenediamine, One or more in amylamine, tripropyl amine (TPA).Triethylamine, monoethanolamine, tetramethylethylenediamine, amylamine, 3 third Amine plays a part of masking in the reaction, silicon chip surface can be induced to generate small crystal nucleus, and be further development of Feature of interest.Wherein monoethanolamine and amylamine, boiling point is high, and volatilization is slow, can repeatedly use, and both water Dissolubility is good, and controllable scope is wide, and tripropyl amine (TPA) is a kind of stronger organic base of alkalescence, and promotion is played to making herbs into wool and is made With.
Preferably, the polyalcohol containing 3~8 carbon is ethylene glycol, glycerine, sorbierite, a contracting diethyl One or more in glycol, diethylene glycol, season pentanediol, isooctanol.It is polynary containing 3~8 carbon Alcohol is from ethylene glycol, glycerine, sorbierite, diglycol, diethylene glycol, season pentanediol, different Octanol, surface tension is reduced, reduce absorption of the hydrogen in reaction in silicon chip surface so that silicon wafer wool making is more equal Even, surface is cleaner.Ethylene glycol, glycerine, sorbierite, diglycol, diethylene glycol, season Pentanediol, isooctanol have hydrophilic radical hydroxyl, and its wetability and gas solubility performance are preferable, surface tension Small, the solid adhesion of liquid is bigger, is more easily wetted, it is possible to increase inorganic base to the infiltration rate of silicon chip surface from And increase substantially making herbs into wool efficiency and effect.The water solubility of ethylene glycol preferably, also can be mutual with most alcohols It is molten, the uniformity of solution can be improved.
Preferably, the carboxylic acid containing 3~14 carbon be 3- methylpropanoic acids, Beta-alanine, citric acid, One or more in 4-Aminobutanoicacid, ethylenediamine tetra-acetic acid, ethanedioic acid.Citric acid is tricarboxylic acids, have compared with Strong hydrophilicity, wettability are good.
Preferably, the ethers containing 4~8 carbon is propylene glycol monomethyl ether, ethylene glycol ethyl ether, diethylene glycol second One or more in ether.Ethers containing 4~8 carbon is from propylene glycol monomethyl ether, ethylene glycol ethyl ether, diethyl Glycol ether, surface tension is reduced, reduce absorption of the hydrogen in reaction in silicon chip surface so that silicon wafer wool making Evenly, surface is cleaner.Wherein propylene glycol monomethyl ether, not only containing hydroxyl but also ether was contained, solubility property is excellent It is different so that solution component dispersiveness is more preferable, and surface tension is low, good to silicon chip wettability, can effectively take off Except the bubble of silicon chip surface, making herbs into wool reaction is promoted to carry out.
The method that this kind is used for the bad Wool-making agent handled after monocrystalline silicon making herbs into wool is made, preparing low volatility has Machine compound;Sodium hydrate aqueous solution or potassium hydroxide aqueous solution are prepared with deionized water, by sodium hydroxide water Solution or potassium hydroxide aqueous solution are heated to 65~80 DEG C, add low VOC, are well mixed, Obtain Woolen-making liquid.
The processing method of bad, comprises the following steps after monocrystalline silicon making herbs into wool:By bad after monocrystalline silicon making herbs into wool It is respectively placed in ethanol, acetone and isopropanol and is cleaned by ultrasonic;Bad after monocrystalline silicon making herbs into wool after cleaning is put In produced above for carrying out making herbs into wool in the Wool-making agent of bad processing after monocrystalline silicon making herbs into wool.The present invention is bad Silicon wafer suede that texturing method obtains uniformly, surface defect state it is few, add luminous absorptance surface area, subtract Few light reflection loss, significantly improves photoelectric transformation efficiency.Silicon chip surface after making herbs into wool of the present invention is clean, nothing Obvious flower piece, can effectively reduce silicon chip surface spot, water wave print the defects of.
Preferably, during making herbs into wool, for temperature control at 70~85 DEG C, the reaction time is 5~10min.Present invention system The suede time is short, only needs 5~10min, and relatively conventional IPA systems can shorten 5~13min, can further reduce Cost and lifting production capacity.
Compared with prior art, beneficial effects of the present invention are:
(1) the bad Wool-making agent handled after being used for monocrystalline silicon making herbs into wool of the invention, can effectively be reduced bad Shinny quantity that piece making herbs into wool is uneven, hickie, silicon chip turn white, the small organic molecule energy that the Woolen-making liquid contains Enough and monocrystalline silicon surface acts on, and effectively controls the progress of making herbs into wool reaction, on the one hand can induce the production of small crystal nucleus It is raw, feature of interest is further development of, on the other hand can improve permeability of the alkali to silicon face, so as to big Width improves making herbs into wool efficiency and effect, and the silicon chip yields after this method processing is effectively reduced 95%~97% Production cost.
(2) the bad texturing method yields of the present invention is high, is 95%~97%, reduces scrappage, saves About cost.
(3) silicon wafer suede that the bad texturing method of the present invention obtains uniformly, surface defect state it is few, add Luminous absorptance surface area, light reflection loss is reduced, significantly improves photoelectric transformation efficiency.
(4) silicon chip surface after making herbs into wool of the present invention is clean, without obvious flower piece, can effectively reduce silicon chip surface The defects of spot, water wave print.
(5) the making herbs into wool time of the present invention is short, only needs 5~10min, and relatively conventional IPA systems can shorten 5~13min, it can further reduce cost and lifting production capacity.
(6) corrosive liquid system boiling point of the invention is high, stability is good, and volatility is small during preparing matte, It can repeatedly use.
Brief description of the drawings
Fig. 1 is the SEM detection figure of the monocrystalline silicon piece after embodiment 7 is handled.
Embodiment
Embodiment 1
For the Wool-making agent of bad processing after monocrystalline silicon making herbs into wool, including sodium hydroxide and flocking additive, hydrogen The weight/mass percentage composition of sodium oxide molybdena is 0.5%, and flocking additive includes the low volatilization that volumn concentration is 0.1% Property organic compound, volumn concentration be 99.9% deionized water.
Low VOC is triethylamine, monoethanolamine, tetramethylethylenediamine.
The above-mentioned method for the Wool-making agent of bad processing after monocrystalline silicon making herbs into wool is made, prepares low waves Hair property organic compound;Sodium hydrate aqueous solution is prepared with deionized water, sodium hydrate aqueous solution is heated to 65 DEG C, low VOC is added, is well mixed, obtains Woolen-making liquid.
The processing method of bad, comprises the following steps after monocrystalline silicon making herbs into wool:By bad after monocrystalline silicon making herbs into wool It is respectively placed in ethanol, acetone and isopropanol and is cleaned by ultrasonic;Bad after monocrystalline silicon making herbs into wool after cleaning is put It is used to carry out making herbs into wool after monocrystalline silicon making herbs into wool in the Wool-making agent of bad processing in produced above, during making herbs into wool, temperature Degree control is at 70 DEG C, reaction time 5min.Bad after making herbs into wool can enter subsequently together with normal silicon chip Acid cleaning process flow.
Gained silicon chip detects through metallographic microscope, and pyramid matte size is 1~2 micron, and uniform in size, Dispersed distribution, reflectivity 12%, the mass loss of every very little silicon chip monolithic is 0.019g, every cun of bad list Face corrosion thinning amount is 0.20 micron.
Embodiment 2
For the Wool-making agent of bad processing after monocrystalline silicon making herbs into wool, including sodium hydroxide and flocking additive, hydrogen The weight/mass percentage composition of sodium oxide molybdena is 5%, and flocking additive includes the low volatility that volumn concentration is 8% Organic compound, the deionized water that volumn concentration is 92%.
Low VOC is the low-grade aliphatic amine containing 3~7 carbon and polynary containing 3~8 carbon Alcohol.
Low-grade aliphatic amine containing 3~7 carbon is amylamine.Polyalcohol containing 3~8 carbon is ethylene glycol, third Triol, sorbierite.
The above-mentioned method for the Wool-making agent of bad processing after monocrystalline silicon making herbs into wool is made, prepares low waves Hair property organic compound;Sodium hydrate aqueous solution is prepared with deionized water, sodium hydrate aqueous solution is heated to 80 DEG C, low VOC is added, is well mixed, obtains Woolen-making liquid.
The processing method of bad, comprises the following steps after monocrystalline silicon making herbs into wool:By bad after monocrystalline silicon making herbs into wool It is respectively placed in ethanol, acetone and isopropanol and is cleaned by ultrasonic;Bad after monocrystalline silicon making herbs into wool after cleaning is put It is obtained for carrying out making herbs into wool, making herbs into wool in the Wool-making agent of bad processing after monocrystalline silicon making herbs into wool in claim 1 When, temperature control is at 85 DEG C, reaction time 10min.Bad after making herbs into wool can be together with normal silicon chip Into follow-up acid cleaning process flow.
Gained silicon chip detects through metallographic microscope, and pyramid matte size is 2~4 microns, and uniform in size, Dispersed distribution, reflectivity 14%, the mass loss of every very little silicon chip monolithic is 0.044g, every cun of bad list Face corrosion thinning amount is 0.46 micron.
Embodiment 3
For the Wool-making agent of bad processing after monocrystalline silicon making herbs into wool, including sodium hydroxide and flocking additive, hydrogen The weight/mass percentage composition of sodium oxide molybdena is 3%, and flocking additive includes the low volatility that volumn concentration is 0.2% Organic compound, the deionized water that volumn concentration is 99.8%.
Low VOC is the low-grade aliphatic amine containing 3~7 carbon, polynary containing 3~8 carbon Alcohol, the carboxylic acid containing 3~14 carbon and the ethers containing 4~8 carbon.
Low-grade aliphatic amine containing 3~7 carbon is triethylamine, amylamine, tripropyl amine (TPA).
Polyalcohol containing 3~8 carbon is diglycol, diethylene glycol, season pentanediol, isooctanol.
Carboxylic acid containing 3~14 carbon be 3- methylpropanoic acids, Beta-alanine, citric acid, 4-Aminobutanoicacid, Ethylenediamine tetra-acetic acid, ethanedioic acid.
Ethers containing 4~8 carbon is propylene glycol monomethyl ether, ethylene glycol ethyl ether, diethylene glycol ether.
The above-mentioned method for the Wool-making agent of bad processing after monocrystalline silicon making herbs into wool is made, prepares low waves Hair property organic compound;Sodium hydrate aqueous solution is prepared with deionized water, sodium hydrate aqueous solution is heated to 70 DEG C, low VOC is added, is well mixed, obtains Woolen-making liquid.
The processing method of bad, comprises the following steps after monocrystalline silicon making herbs into wool:By bad after monocrystalline silicon making herbs into wool It is respectively placed in ethanol, acetone and isopropanol and is cleaned by ultrasonic;Bad after monocrystalline silicon making herbs into wool after cleaning is put It is obtained for carrying out making herbs into wool, making herbs into wool in the Wool-making agent of bad processing after monocrystalline silicon making herbs into wool in claim 1 When, temperature control is at 80 DEG C, reaction time 8min.Bad after making herbs into wool can enter together with normal silicon chip Enter follow-up acid cleaning process flow.
Gained silicon chip detects through metallographic microscope, and pyramid matte size is 2~3 microns, and uniform in size, Dispersed distribution, reflectivity 13%, the mass loss of every cun bad is 0.03g, every cun of bad one side corruption It is 0.31 micron to lose Reducing thickness.
Embodiment 4
For the Wool-making agent of bad processing after monocrystalline silicon making herbs into wool, including sodium hydroxide and flocking additive, hydrogen The weight/mass percentage composition of sodium oxide molybdena is 0.8%, and flocking additive includes the low volatilization that volumn concentration is 0.1% Property organic compound, volumn concentration be 99.9% deionized water.
Low VOC is the low-grade aliphatic amine containing 3~7 carbon, polynary containing 3~8 carbon Alcohol, the carboxylic acid containing 3~14 carbon and the ethers containing 4~8 carbon.
Low-grade aliphatic amine containing 3~7 carbon is monoethanolamine, amylamine, tripropyl amine (TPA).
Polyalcohol containing 3~8 carbon is ethylene glycol, sorbierite.
Carboxylic acid containing 3~14 carbon is citric acid, 4-Aminobutanoicacid, ethanedioic acid.
Ethers containing 4~8 carbon is propylene glycol monomethyl ether.
The above-mentioned method for the Wool-making agent of bad processing after monocrystalline silicon making herbs into wool is made, prepares low waves Hair property organic compound;Sodium hydrate aqueous solution is prepared with deionized water, sodium hydrate aqueous solution is heated to 68 DEG C, low VOC is added, is well mixed, obtains Woolen-making liquid.
The processing method of bad, comprises the following steps after monocrystalline silicon making herbs into wool:By bad after monocrystalline silicon making herbs into wool It is respectively placed in ethanol, acetone and isopropanol and is cleaned by ultrasonic;Bad after monocrystalline silicon making herbs into wool after cleaning is put It is obtained for carrying out making herbs into wool, making herbs into wool in the Wool-making agent of bad processing after monocrystalline silicon making herbs into wool in claim 1 When, temperature control is at 80 DEG C, reaction time 6min.Bad after making herbs into wool can enter together with normal silicon chip Enter follow-up acid cleaning process flow.
Gained silicon chip detects through metallographic microscope, and pyramid matte size is 2~3 microns, and uniform in size, Dispersed distribution, reflectivity 12.5%, the mass loss of every cun bad is 0.02g, every cun of bad one side Corrosion thinning amount is 0.31 micron.
Embodiment 5
For the Wool-making agent of bad processing after monocrystalline silicon making herbs into wool, including potassium hydroxide and flocking additive, hydrogen The weight/mass percentage composition of potassium oxide is 1%, and flocking additive includes the low volatility that volumn concentration is 0.2% Organic compound, the deionized water that volumn concentration is 99.8%.
Low VOC is the low-grade aliphatic amine containing 3~7 carbon, the ethers containing 4~8 carbon.
Low-grade aliphatic amine containing 3~7 carbon is triethylamine, monoethanolamine.
Ethers containing 4~8 carbon is propylene glycol monomethyl ether.
The above-mentioned method for the Wool-making agent of bad processing after monocrystalline silicon making herbs into wool is made, prepares low waves Hair property organic compound;Potassium hydroxide aqueous solution is prepared with deionized water, potassium hydroxide aqueous solution is heated to 58 DEG C, low VOC is added, is well mixed, obtains Woolen-making liquid.
The processing method of bad, comprises the following steps after monocrystalline silicon making herbs into wool:By bad after monocrystalline silicon making herbs into wool It is respectively placed in ethanol, acetone and isopropanol and is cleaned by ultrasonic;Bad after monocrystalline silicon making herbs into wool after cleaning is put It is obtained for carrying out making herbs into wool, making herbs into wool in the Wool-making agent of bad processing after monocrystalline silicon making herbs into wool in claim 1 When, temperature control is at 82 DEG C, reaction time 9min.Bad after making herbs into wool can enter together with normal silicon chip Enter follow-up acid cleaning process flow.
Gained silicon chip detects through metallographic microscope, and pyramid matte size is 2~3 microns, and uniform in size, Dispersed distribution, reflectivity 12.7%, the mass loss of every cun bad is 0.035g, every cun of bad one side Corrosion thinning amount is 0.37 micron.
Embodiment 6
For the Wool-making agent of bad processing after monocrystalline silicon making herbs into wool, including potassium hydroxide and flocking additive, hydrogen The weight/mass percentage composition of potassium oxide is 2%, and flocking additive includes the low volatility that volumn concentration is 0.1% Organic compound, the deionized water that volumn concentration is 99.9%.
Low VOC is the low-grade aliphatic amine containing 3~7 carbon, polynary containing 3~8 carbon Alcohol and the ethers containing 4~8 carbon.
Low-grade aliphatic amine containing 3~7 carbon is triethylamine, monoethanolamine, tetramethylethylenediamine.
Polyalcohol containing 3~8 carbon is ethylene glycol.
Ethers containing 4~8 carbon is propylene glycol monomethyl ether.
The above-mentioned method for the Wool-making agent of bad processing after monocrystalline silicon making herbs into wool is made, prepares low waves Hair property organic compound;Potassium hydroxide aqueous solution is prepared with deionized water, potassium hydroxide aqueous solution is heated to 68 DEG C, low VOC is added, is well mixed, obtains Woolen-making liquid.
The processing method of bad, comprises the following steps after monocrystalline silicon making herbs into wool:By bad after monocrystalline silicon making herbs into wool It is respectively placed in ethanol, acetone and isopropanol and is cleaned by ultrasonic;Bad after monocrystalline silicon making herbs into wool after cleaning is put It is obtained for carrying out making herbs into wool, making herbs into wool in the Wool-making agent of bad processing after monocrystalline silicon making herbs into wool in claim 1 When, temperature control is at 80 DEG C, reaction time 6min.Bad after making herbs into wool can enter together with normal silicon chip Enter follow-up acid cleaning process flow.
Gained silicon chip detects through metallographic microscope, and pyramid matte size is 2~3 microns, and uniform in size, Dispersed distribution, reflectivity 12.9%, the mass loss of every cun bad is 0.038g, every cun of bad one side Corrosion thinning amount is 0.40 micron.
Embodiment 7
For after monocrystalline silicon making herbs into wool bad processing Wool-making agent, including volume fraction be 0.36% triethylamine, The ethylene glycol ethyl ether that the diglycol and volume fraction that volume fraction is 1.6% are 2.0%;Quality percentage Content is 0.5% potassium hydroxide.
The processing method of bad, comprises the following steps after monocrystalline silicon making herbs into wool:By (the monocrystalline silicon making herbs into wool of color spot piece Bad afterwards) sort out, it is ultrasonically treated respectively in ethanol, acetone, isopropanol, ultrasonic temperature is room Temperature, frequency 70kHz, scavenging period 8min, to remove the greasy dirt of silicon chip surface.It is bad after cleaning Piece can immerse carries out making herbs into wool for the Wool-making agent of bad processing after monocrystalline silicon making herbs into wool.The making herbs into wool time is 8min, Texturing slot temperature is 85 DEG C, and the equally distributed silicon chip of matte is prepared;Silicon chip after making herbs into wool is sprayed Processing, subsequent process flow are identical with normal silicon chip flow.
Gained silicon chip detects through metallographic microscope, and pyramid matte size is 3~4 microns, and uniform in size, Dispersed distribution, reflectivity 12.9%, Si wafer quality loss is 0.18g after making herbs into wool, and bad single-sided corrosion subtracts Thin amount is 1.9 microns.
Embodiment 8
For after monocrystalline silicon making herbs into wool bad processing Wool-making agent, including volume fraction be 1.08% tripropyl amine (TPA), The ethylenediamine tetra-acetic acid that the sorbierite and volume fraction that volume fraction is 1.5% are 3.8%;Weight/mass percentage composition For 1.2% sodium hydroxide.
The processing method of bad, comprises the following steps after monocrystalline silicon making herbs into wool:By (the monocrystalline silicon making herbs into wool of color spot piece Bad afterwards) sort out, it is ultrasonically treated respectively in ethanol, acetone, isopropanol, ultrasonic temperature is room Temperature, frequency 80kHz, scavenging period 10min, to remove the greasy dirt of silicon chip surface;After cleaning not The good Wool-making agent progress making herbs into wool that can be immersed for bad processing after monocrystalline silicon making herbs into wool.The making herbs into wool time is 7min, Texturing slot temperature is 80 DEG C, and the equally distributed silicon chip of matte is prepared;Silicon chip after making herbs into wool is sprayed Processing, subsequent process flow are identical with normal silicon chip flow.
Gained silicon chip detects through metallographic microscope, and pyramid matte size is 2~3 microns, and uniform in size, Dispersed distribution, reflectivity 13.4%, Si wafer quality loss is 0.19g after making herbs into wool, and bad single-sided corrosion subtracts Thin amount is 1.99 microns.
Embodiment 9
For the Wool-making agent of bad processing after monocrystalline silicon making herbs into wool, including it is 0.70% that Woolen-making liquid, which includes volume fraction, Tetramethylethylenediamine, volume fraction be 2.3% season pentanediol and volume fraction be 4.8% diethylene glycol Ether;Weight/mass percentage composition is 4.5% sodium hydroxide.
The processing method of bad, comprises the following steps after monocrystalline silicon making herbs into wool:By (the monocrystalline silicon making herbs into wool of color spot piece Bad afterwards) sort out, it is ultrasonically treated respectively in ethanol, acetone, isopropanol, ultrasonic temperature is room Temperature, frequency 70kHz, scavenging period 8min, to remove the greasy dirt of silicon chip surface.It is bad after cleaning Piece can immerse carries out making herbs into wool for the Wool-making agent of bad processing after monocrystalline silicon making herbs into wool.The making herbs into wool time is 5min, Texturing slot temperature is 70 DEG C, and the equally distributed silicon chip of matte is prepared;Silicon chip after making herbs into wool is sprayed Processing, subsequent process flow are identical with normal silicon chip flow;
Gained silicon chip detects through metallographic microscope, and pyramid matte size is 1~2 micron, and uniform in size, Dispersed distribution, reflectivity 12.7%, Si wafer quality loss is 0.21g after making herbs into wool, and bad single-sided corrosion subtracts Thin amount is 2.20 microns.
Embodiment 10
For the Wool-making agent of bad processing after monocrystalline silicon making herbs into wool, including it is 1.01% that Woolen-making liquid, which includes volume fraction, Amylamine, volume fraction be 5.8% ethylene glycol, volume fraction be 0.78% citric acid and volume fraction For 3.9% ethylene glycol ethyl ether;Weight/mass percentage composition is 2% sodium hydroxide.
The processing method of bad, comprises the following steps after monocrystalline silicon making herbs into wool:By (the monocrystalline silicon making herbs into wool of color spot piece Bad afterwards) sort out, it is ultrasonically treated respectively in ethanol, acetone, isopropanol, ultrasonic temperature is room Temperature, frequency 80kHz, scavenging period 5min, to remove the greasy dirt of silicon chip surface.It is bad after cleaning Piece can immerse carries out making herbs into wool for the Wool-making agent of bad processing after monocrystalline silicon making herbs into wool.The making herbs into wool time is 10min, Texturing slot temperature is 75 DEG C, and the equally distributed silicon chip of matte is prepared;Silicon chip after making herbs into wool is sprayed Processing, subsequent process flow are identical with normal silicon chip flow.
Gained silicon chip detects through metallographic microscope, and pyramid matte size is 3~4 microns, and uniform in size, Dispersed distribution, reflectivity 13.6%, Si wafer quality loss is 0.29g after making herbs into wool, every cun of bad one side corruption It is 0.31 micron to lose Reducing thickness.
In a word, presently preferred embodiments of the present invention is the foregoing is only, it is all to be made according to scope of the present invention patent Equivalent changes and modifications, should all belong to the covering scope of patent of the present invention.

Claims (9)

1. the Wool-making agent for bad processing after monocrystalline silicon making herbs into wool, it is characterised in that:Including sodium hydroxide or hydrogen-oxygen The weight/mass percentage composition of change potassium and flocking additive, sodium hydroxide or potassium hydroxide is 0.5%~5%, and making herbs into wool adds Add agent include volumn concentration be 0.1%~8% low VOC, volumn concentration be 92%~99.9% deionized water.
2. the bad Wool-making agent handled according to claim 1 after being used for monocrystalline silicon making herbs into wool, it is characterised in that: Low VOC be the low-grade aliphatic amine containing 3~7 carbon, the polyalcohol containing 3~8 carbon, Carboxylic acid containing 3~14 carbon, the one or more in the ethers containing 4~8 carbon.
3. the bad Wool-making agent handled according to claim 2 after being used for monocrystalline silicon making herbs into wool, it is characterised in that: Low-grade aliphatic amine containing 3~7 carbon is triethylamine, monoethanolamine, tetramethylethylenediamine, amylamine, tripropyl amine (TPA) In one or more.
4. the bad Wool-making agent handled according to claim 2 after being used for monocrystalline silicon making herbs into wool, it is characterised in that: Polyalcohol containing 3~8 carbon is ethylene glycol, glycerine, sorbierite, diglycol, a contracting second two One or more in alcohol, season pentanediol, isooctanol.
5. the bad Wool-making agent handled according to claim 2 after being used for monocrystalline silicon making herbs into wool, it is characterised in that: Carboxylic acid containing 3~14 carbon is 3- methylpropanoic acids, Beta-alanine, citric acid, 4-Aminobutanoicacid, second two One or more in amine tetraacethyl, ethanedioic acid.
6. the bad Wool-making agent handled according to claim 2 after being used for monocrystalline silicon making herbs into wool, it is characterised in that: Ethers containing 4~8 carbon is propylene glycol monomethyl ether, ethylene glycol ethyl ether, one kind in diethylene glycol ether or several Kind.
7. make the bad processing after being used for monocrystalline silicon making herbs into wool described in claim 1 or 2 or 3 or 4 or 5 or 6 Wool-making agent method, it is characterised in that:Prepare low VOC;Hydrogen is prepared with deionized water Aqueous solution of sodium oxide or potassium hydroxide aqueous solution, sodium hydrate aqueous solution or potassium hydroxide aqueous solution are heated to 65~80 DEG C, low VOC is added, is well mixed, obtains Woolen-making liquid.
8. the processing method of bad after monocrystalline silicon making herbs into wool, it is characterised in that:Comprise the following steps:By monocrystalline silicon system Bad is respectively placed in ethanol, acetone and isopropanol and is cleaned by ultrasonic after suede;By the monocrystalline silicon making herbs into wool after cleaning Bad is placed in made from claim 7 for being carried out after monocrystalline silicon making herbs into wool in the Wool-making agent of bad processing afterwards Making herbs into wool.
9. the processing method of bad after the monocrystalline silicon making herbs into wool described in claim 8, it is characterised in that:During making herbs into wool, temperature At 70~85 DEG C, the reaction time is 5~10min for degree control.
CN201610446469.7A 2016-06-20 2016-06-20 For the processing method of bad after Wool-making agent of bad processing and preparation method thereof after monocrystalline silicon making herbs into wool and monocrystalline silicon making herbs into wool Pending CN107523880A (en)

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