CN102773933B - Chemical processing method of wire-cutting recovery liquids - Google Patents
Chemical processing method of wire-cutting recovery liquids Download PDFInfo
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- CN102773933B CN102773933B CN201110123660.5A CN201110123660A CN102773933B CN 102773933 B CN102773933 B CN 102773933B CN 201110123660 A CN201110123660 A CN 201110123660A CN 102773933 B CN102773933 B CN 102773933B
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Abstract
The invention discloses a chemical processing method of wire-cutting recovery liquids. The method comprises adding carboxylic acid polymers and alcohol amine substances into a wire-cutting recovery liquid. The wire-cutting recovery liquids can be directly applied in silicon wafer cutting after treated by additives, and performances equivalent to novel cutting liquids can be obtained, so that the utilization ratio of the recovery liquids is improved and the production cost is reduced.
Description
Technical field
The line cutting field that the invention belongs to Silicon Wafer, is specifically related to the recovery liquid reclaiming from the mortar of Silicon Wafer line cutting to carry out chemical treatment.
Background technology
Silicon chip is the basis of manufacturing solar cell, in silicon chip cutting process, metal wire is wrapped on guide roller, mortar is brought into cutting zone by metal wire, drive guide roller to do relative motion to silicon rod (ingot), silicon rod (ingot) is cut into certain thickness silicon chip.In this process, be brought into the amount of mortar and performance and determined the cut quality of silicon chip.Conventionally mortar is mainly made up of liquid cutting liquid (as polyethylene glycol) and solid-state silicon carbide micro-powder, wherein the silicon carbide micro-powder of high rigidity is main cutting medium, polyethylene glycol (PEG) is as the carrier of carborundum, silicon carbide micro-powder is dispersed in to the cutting surfaces of silico briquette, reduce the accumulation of mechanical stress in cutting process, and due to the higher thermal capacitance of polyethylene glycol, can take away a large amount of frictional heat that produce in cutting process, play cooling effect; Simultaneously the good mobility of polyethylene glycol, can take away the accessory substance producing in cutting process in time, as silica flour and metal impurities, avoids at silicon chip surface, because the gathering of large granular impurity causes silicon chip surface out-of-flatness, affecting the yields of silicon chip.
Cost proportion shared in mortar cutting on line technique is larger, in cutting process, need to constantly supplement new mortar, discharges waste mortar, and the main component of waste mortar is polyethylene glycol, silicon carbide micro-powder, silica flour and a small amount of metal fillings impurity.For these used waste mortars, silicon chip processing enterprise generally carries out recycling to it and reduces costs, and reduces the pollution to environment.But reclaim at present the polyethylene glycol obtaining, wherein still contain a small amount of silica flour and metal fillings impurity, and the existence of silica flour and metal fillings impurity while making to reuse wire cutting technology become unstable, silicon chip surface Quality Down, therefore, the polyethylene glycol that recovery obtains just can re-start use after generally need mixing by proper proportion with new polyethylene glycol, as disclosed in CN101623898A; Even if directly use, but the moisture reclaiming in liquid is had to requirement, and the water content that reclaims liquid is subject to various factors, restive and be extended to production.
Summary of the invention
In view of the problems referred to above of existing silicon chip line cutting recovery liquid, the invention provides a kind of line cutting and reclaim the chemical treatment method of liquid, after the inventive method is processed, line cutting is reclaimed liquid without mixing with new cutting liquid again, can directly apply completely, and can obtain the performance suitable with new cutting liquid, reclaim the utilization rate of liquid and reduce production costs thereby improve.
The object of this invention is to provide a kind of line cutting and reclaim the chemical treatment method of liquid, described method comprises that cutting on line reclaims the step that adds carboxylic acids polymer and alcamines material in liquid.
Term of the present invention " liquid is reclaimed in line cutting " refers to and uses centrifugal separation technology to reclaim the waste mortar that produces in line cutting process, the liquid part that recovery obtains is that liquid is reclaimed in line cutting, its composition overwhelming majority is polyethylene glycol, propane diols or isopropanol recovering liquid, still contains extremely silica flour and the metal fillings impurity of trace.The liquid part of this recovery can be used technology general in this area to process again, for example, adds hydrofluoric acid and is combined with silica flour, adds hydrochloric acid, and the inorganic acids such as nitric acid and metal reaction generate the methods such as water soluble salt, further to improve the purity that reclaims liquid.
According to the present invention one preferred embodiment, described method can also comprise the step that further adds alcohol ethers and/or phenylethylene polymer.
Term used in the present invention " polymer " refers to by many identical, and the compound that simple construction unit repeats to be formed by connecting by covalent bond, is the raw material of synthetic polymer.
According to the present invention one preferred embodiment, liquid is reclaimed in the cutting of described line can be selected from polyethylene glycol, propane diols or isopropanol recovering liquid.Wherein the molecular weight of polyethylene glycol is generally less than 300.
Carboxylic acids polymer is for regulating line cutting to reclaim viscosity and the pH value of liquid.According to the present invention, one preferred embodiment, described carboxylic acids polymer is acrylic copolymer, can be selected from any one in maleic acid acrylic copolymer, acrylic acid-hydroxypropyl acrylate copolymer, acrylic acid-2-acrylamide-2-methyl propane sulfonic copolymer and acrylic acid-acrylate-phosphonic acids-sulfonate quadripolymer, the molecular weight of this acrylic copolymer should be less than 5000, the addition of carboxylic acids polymer can be line cutting reclaim liquid gross weight 0.1～2%, preferably 0.1～1%.
Reclaim the decentralization in liquid for strengthening silicon carbide powder cutting on line, can add for example alcamines dispersant of dispersant, alcamines material can reclaim for example polyethylene glycol generation esterification of liquid with line cutting, generate larger molecule, produce space steric effect, strengthen silicon carbide powder material cutting on line and reclaim the dispersiveness in liquid.According to the present invention one preferred embodiment, described alcamines material can be selected from any one in monoethanolamine, triethanolamine or triethanolamine oleate.The addition of alcamines material can be line cutting reclaim liquid gross weight 0.1～2%, preferably 0.1～1%.
Additive of the present invention can also contain surface active agent alcohol ether class surfactant, and such surfactant can, in wafer cutting process, strengthen silicon carbide powder and the dispersiveness of silica flour in cutting liquid, prevents particle agglomeration.According to the present invention one preferred embodiment, described alcohol ethers can be selected from as NPE, AEO or sodium sulfate of polyethenoxy ether of fatty alcohol.The addition of alcohol ethers can be line cutting reclaim liquid gross weight 0～2%, preferably 0.1～1%.
According to the present invention, one preferred embodiment, in order further to optimize dispersiveness and the suspension stability of cutting liquid, also can add phenylethylene polymer, the molecular weight of described phenylethylene polymer can be 2000-4000, the addition of phenylethylene polymer can reclaim 0～2% of liquid gross weight for line cutting, and preferable range is 0.1-1%.
According to the present invention one preferred embodiment, the total addition level of described carboxylic acids polymer, alcamines material and/or alcohol ethers and/or phenylethylene polymer can be the 0.5-8% that liquid gross weight is reclaimed in line cutting, preferably 1-5%.Various additives should add in a fixed order, to avoid irreversible particle coagulation, affect its dispersiveness and stability.
According to the present invention, one preferred embodiment, under agitation described reagent being joined to line cutting reclaims in liquid, the time interval that adds carboxylic acids polymer, alcamines material and/or alcohol ethers and/or phenylethylene polymer is 0.5-3 hour, preferably 1-3 hour.
The concrete steps that additive adds lambda line cutting recovery liquid are: at ambient temperature, first slowly add carboxylic acids polymer, in adition process, need to stir apparatus and do not stop to stir, after adding, still need to stir after 0.5-3 hour, add again alcamines dispersant, then continue to stir 0.5-3 hour.
More than add the line cutting of carboxylic acids polymer and alcamines additive to reclaim liquid, also can select to continue to add one or both in alcohol ether surfactants, phenylethylene polymer, the mode adding is as above-mentioned requirements, slowly add, do not stop to stir, the joining day of every kind of reagent is spaced apart 0.5-3 hour.
The line cutting of processing through mentioned reagent is reclaimed liquid after cutting is used recovery, can also re-start processing by above technical scheme, again recycles.
The chemical treatment method that liquid is reclaimed in line cutting of the present invention can obtain having the required excellent dispersiveness of cutting, the cutting liquid of thermal conductivity and mobility, after this cutting liquid and silicon carbide micro-powder (this silicon carbide micro-powder can be the silicon carbide micro-powder of brand-new silicon carbide micro-powder, recovery or both mixtures) mix by means known in the art, can directly apply to silicon chip cutting technique, and obtain the performance quite even more excellent with new cutting liquid, thereby improve the utilization rate of recovery liquid and reduce production costs.
Detailed description of the invention
Embodiment 1
600 kilograms of (Liaoning Fine Chemical Industry Co., Ltd. of liquid are reclaimed in the cutting of taking polyethylene glycol line, name of product KLsi-II, lot number 20110321F41), then slowly add 12 kilograms of maleic acid acrylic copolymers, do not stop to stir 1 hour, slowly add again 0.6 kilogram of monoethanolamine, continue to stir after 1 hour, obtain treated line cutting and reclaim liquid.
Liquid is reclaimed in above-mentioned line cutting and silicon carbide micro-powder (trade name: silicon carbide micro-powder, Yangzhong Jiaming Solar Energy New Material Co., Ltd., lot number: SD110420-33) mixes, and after mixing, can directly apply in line cutting production.
Embodiment 2
600 kilograms of (Liaoning Fine Chemical Industry Co., Ltd. of liquid are reclaimed in the cutting of taking polyethylene glycol line, name of product KLsi-II, lot number 20110321F41), then slowly add 0.6 kilogram of acrylic acid-hydroxypropyl acrylate copolymer, do not stop to stir 3 hours, slowly add again 12 kilograms of monoethanolamines, continue to stir after 3 hours, obtain treated line cutting and reclaim liquid.
Above-mentioned line cutting is reclaimed liquid and is mixed with silicon carbide micro-powder, after mixing, can directly apply in line cutting production.
Embodiment 3
600 kilograms of (Liaoning Fine Chemical Industry Co., Ltd. of liquid are reclaimed in the cutting of taking polyethylene glycol line, name of product KLsi-II, lot number 20110321F41), then slowly add 6 kilograms of acrylic acid-2-acrylamide-2-methyl propane sulfonic copolymers, do not stop to stir 2 hours, more slowly add 6 kilograms of triethanolamines, stir after 2 hours, slowly add again 0.6 kilogram of NPE, continue to stir after 2 hours, obtain treated line cutting and reclaim liquid.
Above-mentioned line cutting is reclaimed liquid and is mixed with silicon carbide micro-powder, after mixing, can directly apply in line cutting production.
Embodiment 4
600 kilograms of (Liaoning Fine Chemical Industry Co., Ltd. of liquid are reclaimed in the cutting of taking polyethylene glycol line, name of product KLsi-II, lot number 20110321F41), then slowly add 0.6 kilogram of maleic acid acrylic copolymer, do not stop to stir 2 hours, slowly add again 6 kilograms of triethanolamine oleates, stir after 2 hours, slowly add again 6 kilograms of AEOs, stir after 2 hours, slowly add again 0.6 kilogram of phenylethylene polymer, continue to stir after 2 hours, obtain treated line cutting and reclaim liquid.
After the cutting of above-mentioned line is reclaimed liquid and mixed, can directly apply in line cutting production.
Embodiment 5
600 kilograms of (Liaoning Fine Chemical Industry Co., Ltd. of liquid are reclaimed in the cutting of taking polyethylene glycol line, name of product KLsi-II, lot number 20110321F41), then slowly add 6 kilograms of acrylic acid-acrylate-phosphonic acids-sulfonate quadripolymers, do not stop to stir 2 hours, slowly add again 0.6 kilogram of triethanolamine oleate, stir after 2 hours, slowly add again 0.6 kilogram of sodium sulfate of polyethenoxy ether of fatty alcohol (AES), stir after 2 hours, slowly add again 6 kilograms of phenylethylene polymers, continue to stir after 2 hours, obtain treated line cutting and reclaim liquid.
After the cutting of above-mentioned line is reclaimed liquid and mixed, can directly apply in line cutting production.
Embodiment 6
Get the cutting of propane diols line and reclaim liquid (Cologne, Liaoning Fine Chemical Co., Ltd) 600 kilograms, then slowly add 3 kilograms of maleic acid acrylic copolymers, do not stop to stir 2 hours, slowly add again 3 kilograms of triethanolamine oleates, stir after 2 hours, more slowly add 3 kilograms of sodium sulfate of polyethenoxy ether of fatty alcohol (AES), stir after 2 hours, slowly add again 3 kilograms of phenylethylene polymers, continue to stir after 2 hours, obtain treated line cutting and reclaim liquid.
After the cutting of above-mentioned line is reclaimed liquid and mixed, can directly apply in line cutting production.
Embodiment 7
Get the cutting of isopropyl alcohol line and reclaim liquid (Cologne, Liaoning Fine Chemical Co., Ltd) 600 kilograms, then slowly add 3 kilograms of maleic acid acrylic copolymers, do not stop to stir 3 hours, slowly add again 3 kilograms of triethanolamine oleates, stir after 2 hours, more slowly add 3 kilograms of sodium sulfate of polyethenoxy ether of fatty alcohol (AES), stir after 2 hours, slowly add again 3 kilograms of phenylethylene polymers, continue to stir after 2 hours, obtain treated line cutting and reclaim liquid.
After the cutting of above-mentioned line is reclaimed liquid and mixed, can directly apply in line cutting production.
Experimental example 1:
Following table is the 100% recovery polyethylene glycol of processing through embodiment of the present invention 1-7, with undressed 100% recovery polyethylene glycol and 100% brand-new polyethylene glycol, after mixing at equal pace with the silicon carbide micro-powder of same type, the effect comparison under same line cutting technique Parameter Conditions.What wherein cutter number characterized is the cutting times of every a collection of metal wire before broken string, what average silicon wafer thickness deviation TTV characterized is the flatness of silicon chip surface after cutting, what cutting qualification rate characterized is that the silicon chip that cutting obtains meets qualified ratio, these parameters all with the quality of mortar: dispersiveness, mobility and cooling are relevant.
Adopt the handled line cutting of technical scheme of the present invention to reclaim liquid, the successful that cutting obtains is better than undressed recovery liquid, almost identical with the result of brand-new cutting liquid.
Claims (10)
1. a chemical treatment method for liquid is reclaimed in line cutting, and described method comprises that cutting on line reclaims the step that adds carboxylic acids polymer and alcamines material in liquid;
Described method also comprises the step that adds alcohol ethers and phenylethylene polymer;
Described alcohol ethers is selected from NPE, AEO or sodium sulfate of polyethenoxy ether of fatty alcohol;
The total addition level of described carboxylic acids polymer, alcamines material, alcohol ethers and phenylethylene polymer is the 1-5% that liquid gross weight is reclaimed in line cutting;
Under agitation described carboxylic acids polymer, alcamines material, alcohol ethers and phenylethylene polymer being joined to line cutting reclaims in liquid.
2. chemical treatment method as claimed in claim 1, is characterized in that: the addition of described carboxylic acids polymer and alcamines material is the 0.1-1% that liquid gross weight is reclaimed in line cutting.
3. chemical treatment method as claimed in claim 1, is characterized in that: the addition of described alcohol ethers and/or phenylethylene polymer is the 0.1-1% that liquid gross weight is reclaimed in line cutting.
4. chemical treatment method as claimed in claim 1, is characterized in that: described line cutting is reclaimed liquid and is selected from polyethylene glycol, propane diols or isopropanol recovering liquid.
5. chemical treatment method as claimed in claim 1, it is characterized in that: described carboxylic acids polymer is acrylic copolymer, be selected from any one in maleic acid acrylic copolymer, acrylic acid-hydroxypropyl acrylate copolymer, acrylic acid-2-acrylamide-2-methyl propane sulfonic copolymer and acrylic acid-acrylate-phosphonic acids-sulfonate quadripolymer.
6. chemical treatment method as claimed in claim 5, is characterized in that: the molecular weight of described acrylic copolymer is less than 5000.
7. chemical treatment method as claimed in claim 1, is characterized in that: described alcamines material is selected from any one in monoethanolamine, triethanolamine or triethanolamine oleate.
8. chemical treatment method as claimed in claim 1, is characterized in that: the molecular weight of described phenylethylene polymer is 2000～4000.
9. chemical treatment method as claimed in claim 1, is characterized in that: the time interval that adds described carboxylic acids polymer, alcamines material, alcohol ethers and phenylethylene polymer is 1-3 hour.
10. the chemical treatment method as described in as arbitrary in claim 1 to 9, is characterized in that: carboxylic acids polymer added before alcamines material.
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| CN105462677A (en) * | 2014-09-10 | 2016-04-06 | 新郑市宝德高技术有限公司 | Cutting fluid recovery method |
| CN107098346A (en) * | 2017-06-18 | 2017-08-29 | 郑州东林润光伏材料科技有限公司 | A kind of recovery method of silicon carbide micro-powder |
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| JP2003041240A (en) * | 2001-05-23 | 2003-02-13 | Fujimi Inc | Cutting grain, cutting composition containing the same, and method for producing silicon wafer using the composition |
| CN101113029B (en) * | 2006-07-26 | 2010-09-29 | 金柏林 | Treatment recovery method for monocrystalline silicon cutting waste liquor |
| CN100478412C (en) * | 2007-02-06 | 2009-04-15 | 中国科学院上海微系统与信息技术研究所 | Chemical mechanical polishing pulp for sapphire substrate underlay |
| CN101368126A (en) * | 2007-08-16 | 2009-02-18 | 江苏海迅实业集团股份有限公司 | Liquid coolant for cutting wire-electrode |
| US7985719B2 (en) * | 2008-04-28 | 2011-07-26 | Ward Irl E | Cutting and lubricating composition for use with a wire cutting apparatus |
| CN101623898B (en) * | 2009-04-28 | 2012-02-15 | 江西赛维Ldk太阳能高科技有限公司 | Chemical recovery method for mortar in wire cutting technology |
| JP5571795B2 (en) * | 2009-10-16 | 2014-08-13 | ダウ グローバル テクノロジーズ エルエルシー | Aqueous cutting fluid for use with diamond wire saws |
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