WO2012017947A1 - Aqueous processing solution for fixed abresive grain wire saw - Google Patents

Aqueous processing solution for fixed abresive grain wire saw Download PDF

Info

Publication number
WO2012017947A1
WO2012017947A1 PCT/JP2011/067457 JP2011067457W WO2012017947A1 WO 2012017947 A1 WO2012017947 A1 WO 2012017947A1 JP 2011067457 W JP2011067457 W JP 2011067457W WO 2012017947 A1 WO2012017947 A1 WO 2012017947A1
Authority
WO
WIPO (PCT)
Prior art keywords
water
mass
fixed abrasive
soluble
wire saw
Prior art date
Application number
PCT/JP2011/067457
Other languages
French (fr)
Japanese (ja)
Inventor
直樹 丸尾
康徳 沼田
高橋　宏明
Original Assignee
ユシロ化学工業株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by ユシロ化学工業株式会社 filed Critical ユシロ化学工業株式会社
Priority to KR1020137001523A priority Critical patent/KR101788901B1/en
Priority to SG2012096475A priority patent/SG186486A1/en
Priority to EP11814573.9A priority patent/EP2602058A4/en
Priority to CN201180036629.6A priority patent/CN103025486B/en
Publication of WO2012017947A1 publication Critical patent/WO2012017947A1/en

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28D—WORKING STONE OR STONE-LIKE MATERIALS
    • B28D5/00—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
    • B28D5/0058—Accessories specially adapted for use with machines for fine working of gems, jewels, crystals, e.g. of semiconductor material
    • B28D5/0076—Accessories specially adapted for use with machines for fine working of gems, jewels, crystals, e.g. of semiconductor material for removing dust, e.g. by spraying liquids; for lubricating, cooling or cleaning tool or work
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M173/00—Lubricating compositions containing more than 10% water
    • C10M173/02—Lubricating compositions containing more than 10% water not containing mineral or fatty oils
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06—Metal compounds
    • C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/02—Hydroxy compounds
    • C10M2207/021—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/022—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms containing at least two hydroxy groups
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/04—Ethers; Acetals; Ortho-esters; Ortho-carbonates
    • C10M2207/046—Hydroxy ethers
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
    • C10M2207/124—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms containing hydroxy groups; Ethers thereof
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/127—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids polycarboxylic
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/06—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to an acyloxy radical of saturated carboxylic or carbonic acid
    • C10M2209/062—Vinyl esters of saturated carboxylic or carbonic acids, e.g. vinyl acetate
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/104—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing two carbon atoms only
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/04—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2215/042—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms containing hydroxy groups; Alkoxylated derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2217/02—Macromolecular compounds obtained from nitrogen containing monomers by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2217/028—Macromolecular compounds obtained from nitrogen containing monomers by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a nitrogen-containing hetero ring
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01—Physico-chemical properties
    • C10N2020/04—Molecular weight; Molecular weight distribution
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01—Physico-chemical properties
    • C10N2020/055—Particles related characteristics
    • C10N2020/06—Particles of special shape or size
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/02—Pour-point; Viscosity index
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/04—Detergent property or dispersant property
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/22—Metal working with essential removal of material, e.g. cutting, grinding or drilling

Definitions

  • the present invention relates to a water-soluble working fluid for a fixed abrasive wire saw, and more particularly to a water-soluble working fluid for a fixed abrasive wire saw that is used when a silicon wafer is cut with a fixed abrasive wire saw.
  • Patent Document 1 a fixed abrasive wire saw in which diamond abrasive grains are fixed to the surface of a wire such as a piano wire by electrodeposition or resin bond.
  • a working fluid is used for the purpose of lubrication, cooling, and dispersion of generated chips.
  • the working fluid it is preferable to use a water-soluble working fluid in consideration of flammability problems and the like.
  • the work material is silicon
  • the reactivity between the chips and the machining fluid is higher than that of general materials, and the silicon waste (chips) reacts with moisture or alkali in the machining fluid to generate hydrogen, There is a risk of ignition. Therefore, it is desirable that the processing liquid has reduced reactivity with silicon. From such a viewpoint, a machining fluid as shown in Patent Document 2 has been proposed.
  • the thickening and gelation of the working fluid cause the following problems. (1) The amount of oil introduced by the wire changes and the thickness variation increases (degradation of product quality). (2) Wire slip occurs and the wire is disconnected (decrease in yield). (3) Cleaning in the next process becomes difficult (removal of chips and oil between wafers is difficult). (4) The life of the oil agent is short, and the amount of additional liquid increases (cost increase).
  • the thickening of the machining fluid mixed with chips can be suppressed, the reaction between the machining fluid and chips can be suppressed, and the generation of hydrogen can be suppressed. It is an object of the present invention to provide a water-soluble machining liquid for a fixed abrasive wire saw that can be suppressed.
  • the increase in viscosity due to the mixing of Si chips occurs because the mixed Si chips are fine powder and the dispersibility of the Si chips is inferior.
  • the increase in the viscosity can be solved by adding a predetermined water-soluble polymer to the working fluid to improve the dispersibility of Si chips.
  • the machining fluid contains Si chips, the Si chips and the machining fluid may react to generate hydrogen.
  • thickening and gelation may occur by containing Si chips.
  • the above problems (3) and (4) can be solved by adding a predetermined water-soluble polymer to the working fluid.
  • the present inventors diligently studied the above-mentioned problems and completed the following invention.
  • the first aspect of the present invention is a fixed abrasive wire saw water containing (A) at least one water-soluble polymer selected from polyvinylpyrrolidone and a copolymer containing vinylpyrrolidone, and (B) water. It is a soluble processing fluid (hereinafter sometimes referred to as “the processing fluid of the present invention”).
  • the processing liquid of the present invention contains a predetermined water-soluble polymer as the component (A)
  • the processing liquid contains silicon powder
  • the dispersibility of the silicon powder can be improved.
  • An increase in the viscosity of the working fluid containing sucrose can be suppressed.
  • the weight average molecular weight of the component (A) is preferably 2,000 to 1,000,000.
  • the content of the component (A) is preferably 0.02% by mass or more and 7% by mass or less, based on 100% by mass of the entire water-soluble processing liquid for a fixed abrasive wire saw.
  • the water-soluble processing liquid for a fixed abrasive wire saw of the first invention further contains (C) an alkali salt of a polyvalent carboxylic acid.
  • the content of the component (C) is preferably 0.01% by mass or more and 10% by mass or less, based on 100% by mass of the entire water-soluble processing liquid for a fixed abrasive wire saw.
  • the water-soluble processing liquid for a fixed abrasive wire saw of the first invention further contains one or more selected from the group consisting of (D) glycols, glycol ethers, and polyoxyalkylene glycols.
  • the content of the component (D) is preferably 0.1% by mass or more and 95% by mass or less, based on 100% by mass of the entire water-soluble processing liquid for fixed abrasive wire saws.
  • the viscosity of the water-soluble processing liquid for fixed abrasive wire saw of the first invention is preferably 50 mPa ⁇ s or less at 25 ° C.
  • the viscosity of the working fluid itself is high, the viscosity of the working fluid containing silicon powder is further increased. Therefore, it is preferable that the viscosity of the machining liquid itself is not more than a predetermined value.
  • the viscosity of the working fluid formed by adding 10% by mass of silicon powder having an average particle size of 1.5 ⁇ m to the water-soluble working fluid for fixed abrasive wire saw of the first invention and stirring is 25 ° C. It is preferably 100 mPa ⁇ s or less.
  • the predetermined water-soluble polymer is contained, when the processing liquid contains silicon powder that is silicon chips, the silicon powder is processed. It can be dispersed in a liquid. Therefore, an increase in the viscosity of the processing liquid containing silicon powder can be suppressed.
  • the processing liquid of the present invention contains a predetermined water-soluble polymer, it is possible to suppress the generation of hydrogen by the reaction between the silicon powder and the processing liquid, and the processing liquid containing silicon powder. The thickening and gelation of the liquid can be suppressed.
  • the water-soluble processing liquid for a fixed abrasive wire saw of the present invention contains (A) at least one water-soluble polymer selected from polyvinylpyrrolidone and a copolymer containing vinylpyrrolidone, and (B) water. ing.
  • the processing liquid of the present invention contains at least one water-soluble polymer selected from polyvinylpyrrolidone and a copolymer containing vinylpyrrolidone as the component (A).
  • the water-soluble polymer in the processing liquid contains at least one water-soluble polymer selected from polyvinylpyrrolidone and a copolymer containing vinylpyrrolidone as the component (A).
  • the lower limit of the weight average molecular weight of the water-soluble polymer of component (A) by gel permeation chromatography / multi-angle laser light scattering detector method is preferably 2,000 or more, more preferably 8,000 or more, and the upper limit. However, it is preferably 1,000,000 or less, more preferably 700,000 or less, and still more preferably 500,000 or less. If the molecular weight is too small outside this range, the effect of adding the component (A) may not be exhibited. Conversely, if the molecular weight is too large, the aggregation and the viscosity of the processing liquid may be too high.
  • the content of the component (A) is preferably 0.02% by mass or more, more preferably 0.05% by mass or more, with the lower limit being preferably 0.02% by mass or more, based on the mass (100% by mass) of the entire water-soluble processing liquid for fixed abrasive wire saw More preferably, it is 0.2 mass% or more, and an upper limit becomes like this. Preferably it is 7 mass% or less, More preferably, it is 5 mass% or less, More preferably, it is 3 mass% or less. If the content of the component (A) is too small outside this range, the thickening suppressing effect and the hydrogen generation suppressing effect may be insufficient, and conversely if too large, the viscosity of the working fluid may be increased. is there.
  • the water-soluble polymer of component (A) is polyvinyl pyrrolidone or a copolymer containing vinyl pyrrolidone, and these may be used as a mixture of two or more.
  • the proportion of vinylpyrrolidone units is preferably 60 mol% or more based on the entire copolymer.
  • Examples of the monomer copolymerized with vinyl pyrrolidone include vinyl acetate.
  • the processing liquid of the present invention may further contain an alkali salt of a polyvalent carboxylic acid as the component (C).
  • an alkali salt of a polyvalent carboxylic acid as the component (C).
  • Examples of the polyvalent carboxylic acid include adipic acid, oxalic acid, dodecanedioic acid, citric acid, malic acid and the like.
  • Examples of the alkali include hydroxides of alkali metals such as potassium hydroxide and sodium hydroxide, amines such as triethanolamine, triisopropanolamine, ethylenediamine, and N- (2-aminoethyl) -2-aminoethanol.
  • the content of the component (C) is preferably 0.01% by mass or more, more preferably 0.1% by mass or more, and the upper limit is based on the mass (100% by mass) of the entire working fluid of the present invention. Is preferably 10% by mass or less, more preferably 2% by mass or less, and still more preferably 1% by mass or less. If the content of the component (C) is too small outside the above range, the effect of adding the component (C) becomes difficult to be exhibited. is there.
  • the processing liquid of the present invention may further contain one or more selected from the group consisting of glycols, glycol ethers, and polyoxyalkylene glycols as component (D).
  • component (D) By containing the component (D), there is an effect of imparting lubricity and wettability.
  • glycols examples include propylene glycol, diethylene glycol, ethylene glycol, butylene glycol and the like.
  • glycol ethers include alkyl ethers of the glycols, and examples of the alkyl group include a methyl group, an ethyl group, and a butyl group.
  • a part of the hydroxyl group of glycols may be an alkyl ether, or all may be an alkyl ether.
  • Specific examples of glycol ethers include diethylene glycol monoethyl ether, diethylene glycol diethyl ether, propylene glycol monoethyl ether, and the like.
  • polyoxyalkylene glycols examples include polyethylene glycol, polypropylene glycol, a copolymer of polyoxyethylene and polyoxypropylene, and the weight average molecular weight (in terms of polystyrene using gel permeation chromatography) is preferably 10,000. The following is more preferably 5000 or less, and still more preferably 400 or less.
  • the content of the component (D) is preferably 0.1% by mass or more, more preferably 0.5% by mass or more, and still more preferably, based on the mass (100% by mass) of the entire working fluid of the present invention. It is 1% by mass or more, more preferably 3% by mass or more, particularly preferably 10% by mass or more, and the upper limit is preferably 95% by mass or less, more preferably 90% by mass or less, and further preferably 80% by mass or less. If the content of the component (D) is too small outside the above range, the effect of adding the component (D) is not expressed, and conversely, if the content of the component (D) is too large, the cooling performance may be lowered. .
  • the working fluid of the present invention contains the above-described component (A), and in some cases, further contains (C) component and (D) component, and the balance is (B) water.
  • the type of water is not particularly limited, such as distilled water or tap water.
  • the processing liquid with much water content the processing liquid containing a silicon powder will thicken and it will be easy to gelatinize.
  • the processing liquid of the present invention contains silicon powder even in a composition having a high water content, for example, a composition in which water is 90% by mass or more based on the mass of the entire processing liquid. The thickening and gelation of the liquid can be suppressed.
  • the viscosity of the working fluid of the present invention is 25 ° C., preferably 50 mPa ⁇ s or less, more preferably 25 mPa ⁇ s or less, and still more preferably 20 mPa ⁇ s or less.
  • the viscosity of the working fluid (pseudo-use fluid) in which a predetermined silicon powder is dispersed in the working fluid of the present invention is 100 mPa ⁇ s, preferably 55 mPa ⁇ s or less, more preferably 50 mPa ⁇ s at 25 ° C. s or less, more preferably 45 mPa ⁇ s or less.
  • the viscosity of the pseudo use liquid is such that 10% by mass of silicon powder (particle diameter: 1.5 ⁇ m) is added to the processing liquid of the present invention, and after stirring and mixing, a stainless steel ball (diameter 2 mm) is added and stirred at 1000 rpm for 10 hours.
  • the pseudo-use liquid obtained by filtering the stainless steel balls was measured. If the viscosity of the processing liquid itself is too high, the viscosity of the pseudo-use liquid containing silicon powder inevitably increases. In addition, if the viscosity of the pseudo use liquid is too high, the problems described in the above problem column may occur.
  • the viscosities of the working liquid and the pseudo use liquid can be measured with a Brookfield viscometer.
  • the pH of the working fluid is preferably 5.0 or more and 9.0 or less. If the pH of the machining fluid is too low, there is a risk of corrosion of the iron material or wire that is touched by the machining fluid. Conversely, if the pH of the machining fluid is too high, the machining fluid reacts with the silicon powder to generate hydrogen. May occur.
  • the working fluid of the present invention may be used after diluting in water, but in that case as well, the pH of the diluted working fluid is preferably in the above range.
  • Examples 1 to 13 and Comparative Examples 1 to 5 have the compositions shown in Tables 1 to 3. It produced as follows. While measuring the pH of the produced processing liquid, the viscosity at 25 degreeC was measured with the Brookfield type viscometer. Furthermore, 10% by mass of silicon powder (average particle size of 1.5 m) was added to each processing liquid, and after stirring and mixing, stainless steel balls (diameter 2 mm) were added and stirred at 1000 rpm for 10 hours to form a pseudo use liquid. .
  • the viscosity (mPa ⁇ s, 25 ° C.) of the pseudo use liquid was measured with a Brookfield viscometer. Further, 10 ml of the pseudo use liquid was heated to 50 ° C., and the amount of hydrogen (ml) generated in 30 minutes was measured.
  • the weight average molecular weight of polyvinylpyrrolidone (PVP) was 9700 for PVP K-15, 70000 for PVP K-30, and 400000 for PVP K-60.
  • PVP / VA is a copolymer of vinyl pyrrolidone and vinyl acetate, the weight average molecular weight is 32,000, and the proportion of vinyl pyrrolidone in the copolymer is 70 mol%.
  • the pseudo-use fluid viscosity increases and exceeds 55 mPa ⁇ s.
  • the working fluids of the present invention (Examples 1 to 13) have a small viscosity change even in the pseudo-use fluid, and all are 45 mPa ⁇ s or less.
  • Examples 1 to 3 and Comparative Examples 1 and 2 are obtained by diluting the stock solution 10 times. Therefore, the composition of the stock solution is 10 times the amount of each compound.
  • Group I Group I is Examples 1 to 6 and Comparative Examples 1 to 3, which are examples of working fluids with a large amount of water.
  • the compositions with high water content (Comparative Examples 1 to 3) were all thickened and gelled. It did not become thick and did not thicken.
  • the hydrogen generation amount in Examples 1 to 6, hydrogen generation was 5 ml or less, while in Comparative Examples 1 to 3, the hydrogen generation amount was 15 ml or more, which was very large.
  • Group II Group II is Examples 7 to 12 and Comparative Example 4, in which the types and amounts of the component (C) and the component (D) were unified, and the component (A) was changed. From this, the thickening inhibitory effect of various polyvinylpyrrolidone (PVP) and a vinylpyrrolidone / vinyl acetate copolymer (PVP / VA) was shown. As for the hydrogen generation amount, when Examples 7 to 12 and Comparative Example 4 were compared, the processing liquid of the present invention containing polyvinylpyrrolidone and the like had a small amount of hydrogen generation.
  • Group III Group III is Example 13 and Comparative Example 5 and includes (D) component different from Group I and Group II. From this, the effect of thickening suppression by polyvinylpyrrolidone (PVP) was shown irrespective of the kind of (D) component. Further, when Example 13 and Comparative Example 5 were compared, Example 13 containing polyvinylpyrrolidone had a small amount of hydrogen generation. From the above, the processing liquid of the present invention containing at least one kind of water-soluble polymer selected from polyvinylpyrrolidone and a copolymer containing vinylpyrrolidone has an increased viscosity in a pseudo-use liquid in which silicon powder is dispersed. It was shown that it has the effect of suppressing hydrogen generation as well as suppression.
  • the water-soluble processing liquid for a fixed abrasive wire saw of the present invention can be used particularly suitably when a silicon wafer is cut using a fixed abrasive wire saw.

Abstract

It is possible to control thickening of the processing solution contaminated by scraps by means of at least one water-soluble polymer selected from a copolymer containing (A) polyvinylpyrrolidone and vinylpyrrolidone and in addition by means of a aqueous processing solution for fixed abrasive grain wire saw containing (B) water. It is also possible to control the reaction between processing solution and scraps as well as the generation of hydrogen. Even further, it is possible to control the thickening and gelation of processing solution contaminated by scraps.

Description

固定砥粒ワイヤソー用水溶性加工液Water-soluble machining fluid for fixed abrasive wire saws
　本発明は、固定砥粒ワイヤソー用水溶性加工液に関し、詳細には、シリコンウエハを固定砥粒ワイヤソーにより切断加工する際に使用する、固定砥粒ワイヤソー用水溶性加工液に関する。 The present invention relates to a water-soluble working fluid for a fixed abrasive wire saw, and more particularly to a water-soluble working fluid for a fixed abrasive wire saw that is used when a silicon wafer is cut with a fixed abrasive wire saw.
　シリコンウエハの製造コスト低減を図るため、シリコンウエハの切断加工技術の向上が重要となっている。シリコンウエハの加工においては、遊離砥粒方式でのワイヤソーによる切断が主流であるが、該遊離砥粒方式の加工において、以下の様々な問題がある。 In order to reduce the manufacturing cost of silicon wafers, it is important to improve silicon wafer cutting technology. In the processing of silicon wafers, cutting with a wire saw in the free abrasive grain method is the mainstream, but in the processing of the free abrasive grain method, there are various problems as follows.
　（１）加工液として、油剤に砥粒を分散させたスラリーを使用するため遊離砥粒と切断屑との分離が困難である。（２）ワイヤ走行速度に制限があり加工能率向上に限界がある。（３）カーフロスを少なくするためにワイヤを細線化した場合は、加工中に断線が起き、歩留まりが低下する。（４）カーフロスを少なくするために砥粒を微粒化した場合は、スラリー粘度が上昇し、カーフロスを多くさせるなど逆効果の問題が指摘されている。 (1) Since a slurry in which abrasive grains are dispersed in an oil agent is used as a working fluid, it is difficult to separate free abrasive grains and cutting waste. (2) There is a limit to the wire traveling speed and there is a limit to improving the machining efficiency. (3) When the wire is thinned to reduce kerf loss, disconnection occurs during processing, and the yield decreases. (4) When abrasive grains are atomized to reduce kerf loss, the problem of adverse effects has been pointed out, such as an increase in slurry viscosity and an increase in kerf loss.
　このような問題に対し、最近、ピアノ線等のワイヤ表面に、電着やレジンボンド等によりダイヤモンド砥粒を固定した固定砥粒ワイヤソーが開発されている（特許文献１）。固定砥粒ワイヤソーを用いて脆性材料を加工する場合、潤滑、冷却、発生する切り屑の分散を目的として加工液を用いる。該加工液としては、引火性の問題等も合わせて考えれば、水溶性加工液を用いることが好ましい。しかし、被削材がシリコンの場合、一般材に比べて切り屑と加工液との反応性が高く、シリコン屑（切り屑）が加工液中の水分あるいはアルカリと反応して水素を発生させ、引火する恐れがある。したがって、シリコンとの反応性が抑制させた加工液であることが望ましい。このような観点から特許文献２に示すような加工液が提案されている。 Recently, a fixed abrasive wire saw in which diamond abrasive grains are fixed to the surface of a wire such as a piano wire by electrodeposition or resin bond has been developed (Patent Document 1). When processing a brittle material using a fixed abrasive wire saw, a working fluid is used for the purpose of lubrication, cooling, and dispersion of generated chips. As the working fluid, it is preferable to use a water-soluble working fluid in consideration of flammability problems and the like. However, when the work material is silicon, the reactivity between the chips and the machining fluid is higher than that of general materials, and the silicon waste (chips) reacts with moisture or alkali in the machining fluid to generate hydrogen, There is a risk of ignition. Therefore, it is desirable that the processing liquid has reduced reactivity with silicon. From such a viewpoint, a machining fluid as shown in Patent Document 2 has been proposed.
特願２００１－０５４８５０Japanese Patent Application 2001-054850 特願２００３－０８２３３４Japanese Patent Application No. 2003-082334
　しかしながら、近年加工精度を向上させることで、切り屑が細かくなり、特許文献２で示すような加工液では、十分な安定性が得られないことが分かった。特に、切り屑が混入した加工液の粘度が上昇し、様々な問題が生じることが分かった。また、水分を多量に含有しｐＨがアルカリ性の加工液の場合は、水素が発生する問題だけでなく、増粘、ゲル化が生じるという問題があった。 However, in recent years, it has been found that, by improving the machining accuracy, the chips become finer, and with the machining fluid as shown in Patent Document 2, sufficient stability cannot be obtained. In particular, it has been found that the viscosity of the machining fluid mixed with chips increases and various problems occur. In addition, in the case of a processing liquid containing a large amount of water and having an alkaline pH, there is a problem that not only hydrogen is generated but also thickening and gelation occur.
　加工液の増粘、ゲル化は、下記の問題を生じる。
（１）ワイヤによって持ち込まれる導入油量が変化し、厚みばらつきが大きくなる（製品品位の劣化）。
（２）ワイヤすべりが発生し、ワイヤが断線する（歩留まりの低下）。
（３）次工程での洗浄が難しくなる（ウエハ間の切り屑、油剤の除去が難しい）。
（４）油剤の寿命が短く、更液量が増える（コスト増加）。 The thickening and gelation of the working fluid cause the following problems.
(1) The amount of oil introduced by the wire changes and the thickness variation increases (degradation of product quality).
(2) Wire slip occurs and the wire is disconnected (decrease in yield).
(3) Cleaning in the next process becomes difficult (removal of chips and oil between wafers is difficult).
(4) The life of the oil agent is short, and the amount of additional liquid increases (cost increase).
　よって、本発明では、切り屑が混入した加工液の増粘を抑制でき、加工液と切り屑との反応を抑制して水素の発生を抑制でき、さらに、加工液の増粘・ゲル化を抑制できる、固定砥粒ワイヤソー用水溶性加工液を提供することを課題とする。 Therefore, in the present invention, the thickening of the machining fluid mixed with chips can be suppressed, the reaction between the machining fluid and chips can be suppressed, and the generation of hydrogen can be suppressed. It is an object of the present invention to provide a water-soluble machining liquid for a fixed abrasive wire saw that can be suppressed.
　以上の問題を解決すべく、本発明者らは鋭意検討し、以下の事項を見出した。
（１）Ｓｉ切り屑の混入による粘度の上昇は、混入するＳｉ切り屑が微粉であるため、また、Ｓｉ切り屑の分散性が劣るため、起こる。
（２）上記粘度の上昇は、加工液に所定の水溶性高分子を含有させて、Ｓｉ切り屑の分散性を向上させることで解決できる。
（３）加工液にＳｉ切り屑が含まれている場合、Ｓｉ切り屑と加工液とが反応して、水素が発生する場合がある。
（４）水分を多量に含有する加工液の場合は、Ｓｉ切り屑を含有することで、増粘、ゲル化が生じる場合がある。
（５）上記（３）および（４）の問題は、加工液に所定の水溶性高分子を含有させることで解決することができる。 In order to solve the above problems, the present inventors diligently studied and found the following matters.
(1) The increase in viscosity due to the mixing of Si chips occurs because the mixed Si chips are fine powder and the dispersibility of the Si chips is inferior.
(2) The increase in the viscosity can be solved by adding a predetermined water-soluble polymer to the working fluid to improve the dispersibility of Si chips.
(3) When the machining fluid contains Si chips, the Si chips and the machining fluid may react to generate hydrogen.
(4) In the case of a working fluid containing a large amount of moisture, thickening and gelation may occur by containing Si chips.
(5) The above problems (3) and (4) can be solved by adding a predetermined water-soluble polymer to the working fluid.
　本発明者らは、上記問題について鋭意検討して、以下の発明を完成するに至った。
　第１の本発明は、（Ａ）ポリビニルピロリドン、および、ビニルピロリドンを含む共重合物から選ばれる少なくとも一種類以上の水溶性高分子、ならびに、（Ｂ）水を含有する、固定砥粒ワイヤソー用水溶性加工液（以下、「本発明の加工液」と言う場合がある。）である。 The present inventors diligently studied the above-mentioned problems and completed the following invention.
The first aspect of the present invention is a fixed abrasive wire saw water containing (A) at least one water-soluble polymer selected from polyvinylpyrrolidone and a copolymer containing vinylpyrrolidone, and (B) water. It is a soluble processing fluid (hereinafter sometimes referred to as “the processing fluid of the present invention”).
　本発明の加工液は、（Ａ）成分として所定の水溶性高分子を含有することにより、加工液中にシリコン粉を含有する場合において、シリコン粉の分散性を向上させることができ、シリコン粉を含有する加工液の粘度上昇を抑制することができる。また、加工液とシリコン粉とが反応し水素を発生するのを抑制すると共に、シリコン粉を含有する加工液の増粘、ゲル化を抑制することができる。 When the processing liquid of the present invention contains a predetermined water-soluble polymer as the component (A), when the processing liquid contains silicon powder, the dispersibility of the silicon powder can be improved. An increase in the viscosity of the working fluid containing sucrose can be suppressed. In addition, it is possible to suppress the reaction between the processing liquid and the silicon powder to generate hydrogen, and to suppress the thickening and gelation of the processing liquid containing the silicon powder.
　第１の本発明において、前記（Ａ）成分の重量平均分子量は、２，０００～１，０００，０００であることが好ましい。 In the first aspect of the present invention, the weight average molecular weight of the component (A) is preferably 2,000 to 1,000,000.
　第１の本発明において、前記（Ａ）成分の含有量は、固定砥粒ワイヤソー用水溶性加工液全体の質量を１００質量％として、０．０２質量％以上７質量％以下とすることが好ましい。 In the first aspect of the present invention, the content of the component (A) is preferably 0.02% by mass or more and 7% by mass or less, based on 100% by mass of the entire water-soluble processing liquid for a fixed abrasive wire saw.
　第１の本発明の固定砥粒ワイヤソー用水溶性加工液は、さらに、（Ｃ）多価カルボン酸のアルカリ塩を含有することが好ましい。前記（Ｃ）成分の含有量は、固定砥粒ワイヤソー用水溶性加工液全体の質量を１００質量％として、０．０１質量％以上１０質量％以下であることが好ましい。本発明の加工液は、（Ｃ）成分として多価カルボン酸のアルカリ塩を含有することにより、分散性、洗浄性、耐腐食性を付与することが容易となる。 It is preferable that the water-soluble processing liquid for a fixed abrasive wire saw of the first invention further contains (C) an alkali salt of a polyvalent carboxylic acid. The content of the component (C) is preferably 0.01% by mass or more and 10% by mass or less, based on 100% by mass of the entire water-soluble processing liquid for a fixed abrasive wire saw. By containing the alkali salt of polyvalent carboxylic acid as the component (C), the working fluid of the present invention can easily impart dispersibility, cleanability and corrosion resistance.
　第１の本発明の固定砥粒ワイヤソー用水溶性加工液は、さらに、（Ｄ）グリコール類、グリコールエーテル類、および、ポリオキシアルキレングリコール類からなる群から選ばれる一種以上を含有することが好ましい。前記（Ｄ）成分の含有量は、固定砥粒ワイヤソー用水溶性加工液全体の質量を１００質量％として、０．１質量％以上９５質量％以下であることが好ましい。 It is preferable that the water-soluble processing liquid for a fixed abrasive wire saw of the first invention further contains one or more selected from the group consisting of (D) glycols, glycol ethers, and polyoxyalkylene glycols. The content of the component (D) is preferably 0.1% by mass or more and 95% by mass or less, based on 100% by mass of the entire water-soluble processing liquid for fixed abrasive wire saws.
　第１の本発明の固定砥粒ワイヤソー用水溶性加工液の粘度は、２５℃で５０ｍＰａ・ｓ以下であることが好ましい。加工液自体の粘度が高いと、シリコン粉を含有する加工液の粘度はさらに高くなる。よって、加工液自体の粘度は所定の値以下であることが好ましい。 The viscosity of the water-soluble processing liquid for fixed abrasive wire saw of the first invention is preferably 50 mPa · s or less at 25 ° C. When the viscosity of the working fluid itself is high, the viscosity of the working fluid containing silicon powder is further increased. Therefore, it is preferable that the viscosity of the machining liquid itself is not more than a predetermined value.
　第１の本発明の固定砥粒ワイヤソー用水溶性加工液に、平均粒子径１．５μｍのシリコン粉を１０質量％添加し撹拌して形成した加工液（擬似使用液）の粘度は、２５℃で１００ｍＰａ・ｓ以下であることが好ましい。所定のシリコン粉を含有する擬似使用液の粘度が高いと、上記課題の欄に記載した諸問題が発生する虞がある。 The viscosity of the working fluid (pseudo-use fluid) formed by adding 10% by mass of silicon powder having an average particle size of 1.5 μm to the water-soluble working fluid for fixed abrasive wire saw of the first invention and stirring is 25 ° C. It is preferably 100 mPa · s or less. When the viscosity of the pseudo use liquid containing the predetermined silicon powder is high, there is a possibility that various problems described in the column of the above problem may occur.
　本発明の固定砥粒ワイヤソー用水溶性加工液によると、所定の水溶性高分子を含有していることから、該加工液がシリコン切り屑であるシリコン粉を含有する場合において、該シリコン粉を加工液中に分散させることができる。よって、シリコン粉を含有する加工液の粘度上昇を抑制することができる。また、本発明の加工液は、所定の水溶性高分子を含有していることから、シリコン粉と加工液とが反応して水素を発生するのを抑制でき、また、シリコン粉を含有する加工液の増粘、ゲル化を抑制できる。 According to the water-soluble processing liquid for fixed abrasive wire saw of the present invention, since the predetermined water-soluble polymer is contained, when the processing liquid contains silicon powder that is silicon chips, the silicon powder is processed. It can be dispersed in a liquid. Therefore, an increase in the viscosity of the processing liquid containing silicon powder can be suppressed. In addition, since the processing liquid of the present invention contains a predetermined water-soluble polymer, it is possible to suppress the generation of hydrogen by the reaction between the silicon powder and the processing liquid, and the processing liquid containing silicon powder. The thickening and gelation of the liquid can be suppressed.
　＜固定砥粒ワイヤソー用水溶性加工液＞
　本発明の固定砥粒ワイヤソー用水溶性加工液は、（Ａ）ポリビニルピロリドン、および、ビニルピロリドンを含む共重合物から選ばれる少なくとも一種類以上の水溶性高分子、ならびに、（Ｂ）水を含有している。 <Water-soluble machining fluid for fixed abrasive wire saws>
The water-soluble processing liquid for a fixed abrasive wire saw of the present invention contains (A) at least one water-soluble polymer selected from polyvinylpyrrolidone and a copolymer containing vinylpyrrolidone, and (B) water. ing.
　（（Ａ）成分）
　本発明の加工液は、（Ａ）成分として、ポリビニルピロリドン、および、ビニルピロリドンを含む共重合物から選ばれる少なくとも一種類以上の水溶性高分子を含有している。該水溶性高分子を加工液に含有させることにより、シリコン粉を含有してなる加工液中において、該シリコン粉の分散性を向上させることができる。このため、シリコン粉を含有してなる加工液の粘度の上昇を抑制することができる。また、シリコン粉と加工液との反応を抑制し、シリコン粉を含有してなる加工液において水素が発生するのを抑制できる。さらに、シリコン粉を含有してなる加工液の増粘、ゲル化を抑制することができる。 ((A) component)
The processing liquid of the present invention contains at least one water-soluble polymer selected from polyvinylpyrrolidone and a copolymer containing vinylpyrrolidone as the component (A). By containing the water-soluble polymer in the processing liquid, the dispersibility of the silicon powder can be improved in the processing liquid containing the silicon powder. For this reason, the raise of the viscosity of the processing liquid containing a silicon powder can be suppressed. Further, the reaction between the silicon powder and the processing liquid can be suppressed, and generation of hydrogen in the processing liquid containing the silicon powder can be suppressed. Furthermore, thickening and gelation of the working fluid containing silicon powder can be suppressed.
　ゲルパーミエーションクロマトグラフィー／多角度レーザー光散乱検出器法による（Ａ）成分の水溶性高分子の重量平均分子量は下限が、好ましくは２，０００以上、より好ましくは８，０００以上であり、上限が、好ましくは１，０００，０００以下、より好ましくは７００，０００以下、さらに好ましくは５００，０００以下である。該範囲を外れて分子量が小さすぎると、（Ａ）成分を入れる効果が発現されなくなる虞があり、逆に、分子量が大きすぎると凝集や加工液の粘度が高くなりすぎる虞がある。 The lower limit of the weight average molecular weight of the water-soluble polymer of component (A) by gel permeation chromatography / multi-angle laser light scattering detector method is preferably 2,000 or more, more preferably 8,000 or more, and the upper limit. However, it is preferably 1,000,000 or less, more preferably 700,000 or less, and still more preferably 500,000 or less. If the molecular weight is too small outside this range, the effect of adding the component (A) may not be exhibited. Conversely, if the molecular weight is too large, the aggregation and the viscosity of the processing liquid may be too high.
　（Ａ）成分の含有量は、固定砥粒ワイヤソー用水溶性加工液全体の質量を基準（１００質量％）として、下限が好ましくは０．０２質量％以上、より好ましくは０．０５質量％以上、さらに好ましくは０．２質量％以上であり、上限が好ましくは７質量％以下、より好ましくは５質量％以下、さらに好ましくは３質量％以下である。該範囲を外れて（Ａ）成分の含有量が少なすぎると増粘の抑制効果、水素発生抑制効果が不十分になる虞があり、逆に、多すぎると加工液の粘度が高くなる虞がある。 The content of the component (A) is preferably 0.02% by mass or more, more preferably 0.05% by mass or more, with the lower limit being preferably 0.02% by mass or more, based on the mass (100% by mass) of the entire water-soluble processing liquid for fixed abrasive wire saw More preferably, it is 0.2 mass% or more, and an upper limit becomes like this. Preferably it is 7 mass% or less, More preferably, it is 5 mass% or less, More preferably, it is 3 mass% or less. If the content of the component (A) is too small outside this range, the thickening suppressing effect and the hydrogen generation suppressing effect may be insufficient, and conversely if too large, the viscosity of the working fluid may be increased. is there.
　（Ａ）成分の水溶性高分子は、ポリビニルピロリドン、または、ビニルピロリドンを含む共重合体であり、これらは二種以上を混合して使用してもよい。ビニルピロリドンを含む共重合体は、ビニルピロリドン単位の割合が、共重合体全体を基準として、好ましくは６０モル％以上である。ビニルピロリドンと共重合させるモノマーとしては、酢酸ビニルが挙げられる。 The water-soluble polymer of component (A) is polyvinyl pyrrolidone or a copolymer containing vinyl pyrrolidone, and these may be used as a mixture of two or more. In the copolymer containing vinylpyrrolidone, the proportion of vinylpyrrolidone units is preferably 60 mol% or more based on the entire copolymer. Examples of the monomer copolymerized with vinyl pyrrolidone include vinyl acetate.
　（（Ｃ）成分）
　本発明の加工液は、さらに、（Ｃ）成分として、多価カルボン酸のアルカリ塩を含有していてもよい。（Ｃ）成分を添加し、その添加量を調整することにより、分散性、洗浄性や耐腐食性を付与するという効果がある。 ((C) component)
The processing liquid of the present invention may further contain an alkali salt of a polyvalent carboxylic acid as the component (C). By adding the component (C) and adjusting the addition amount, there is an effect of imparting dispersibility, cleanability and corrosion resistance.
　多価カルボン酸としては、アジピン酸、シュウ酸、ドデカン二酸、クエン酸、リンゴ酸等が挙げられる。アルカリとしては、水酸化カリウム、水酸化ナトリウム等のアルカリ金属の水酸化物、トリエタノールアミン、トリイソプロパノールアミン、エチレンジアミン、Ｎ－（２－アミノエチル）－２－アミノエタノール等のアミンが挙げられる。 Examples of the polyvalent carboxylic acid include adipic acid, oxalic acid, dodecanedioic acid, citric acid, malic acid and the like. Examples of the alkali include hydroxides of alkali metals such as potassium hydroxide and sodium hydroxide, amines such as triethanolamine, triisopropanolamine, ethylenediamine, and N- (2-aminoethyl) -2-aminoethanol.
　（Ｃ）成分の含有量は、本発明の加工液全体の質量を基準（１００質量％）として、下限が好ましくは０．０１質量％以上、より好ましくは０．１質量％以上であり、上限が好ましくは１０質量％以下、より好ましくは２質量％以下、さらに好ましくは１質量％以下である。上記範囲を外れて（Ｃ）成分の含有量が少なすぎると、（Ｃ）成分を添加する効果が発揮されにくくなり、逆に、多すぎると増粘、ゲル化や原液からの析出の虞がある。 The content of the component (C) is preferably 0.01% by mass or more, more preferably 0.1% by mass or more, and the upper limit is based on the mass (100% by mass) of the entire working fluid of the present invention. Is preferably 10% by mass or less, more preferably 2% by mass or less, and still more preferably 1% by mass or less. If the content of the component (C) is too small outside the above range, the effect of adding the component (C) becomes difficult to be exhibited. is there.
　（（Ｄ）成分）
　本発明の加工液は、さらに、（Ｄ）成分として、グリコール類、グリコールエーテル類、および、ポリオキシアルキレングリコール類からなる群から選ばれる一種以上を含有していてもよい。（Ｄ）成分を含有することにより、潤滑性、湿潤性を付与するという効果がある。 ((D) component)
The processing liquid of the present invention may further contain one or more selected from the group consisting of glycols, glycol ethers, and polyoxyalkylene glycols as component (D). By containing the component (D), there is an effect of imparting lubricity and wettability.
　グリコール類としては、プロピレングリコール、ジエチレングリコール、エチレングリコール、ブチレングリコール等が挙げられる。グリコールエーテル類としては、前記グリコール類のアルキルエーテルが挙げられ、アルキル基としては、メチル基、エチル基、ブチル基などが挙げられる。なお、グリコール類のヒドロキシ基の一部がアルキルエーテルとなっていてもよいし、すべてがアルキルエーテルとなっていてもよい。グリコールエーテル類の具体例としては、ジエチレングリコールモノエチルエーテル、ジエチレングリコールジエチルエーテル、プロピレングリコールモノエチルエーテル等が挙げられる。 Examples of glycols include propylene glycol, diethylene glycol, ethylene glycol, butylene glycol and the like. Examples of the glycol ethers include alkyl ethers of the glycols, and examples of the alkyl group include a methyl group, an ethyl group, and a butyl group. In addition, a part of the hydroxyl group of glycols may be an alkyl ether, or all may be an alkyl ether. Specific examples of glycol ethers include diethylene glycol monoethyl ether, diethylene glycol diethyl ether, propylene glycol monoethyl ether, and the like.
　ポリオキシアルキレングリコール類としては、ポリエチレングリコール、ポリプロピレングリコール、ポリオキシエチレンとポリオキシプロピレンの共重合体等が挙げられ、重量平均分子量（ゲルパーミエーションクロマトグラフィーを用いたポリスチレン換算）が、好ましくは１００００以下、より好ましくは５０００以下、さらに好ましくは４００以下のものを用いる。 Examples of the polyoxyalkylene glycols include polyethylene glycol, polypropylene glycol, a copolymer of polyoxyethylene and polyoxypropylene, and the weight average molecular weight (in terms of polystyrene using gel permeation chromatography) is preferably 10,000. The following is more preferably 5000 or less, and still more preferably 400 or less.
　（Ｄ）成分の含有量は、本発明の加工液全体の質量を基準（１００質量％）として、下限が好ましくは０．１質量％以上、より好ましくは０．５質量％以上、さらに好ましくは１質量％以上、さらに好ましくは３質量％以上、特に好ましくは１０質量％以上であり、上限が好ましくは９５質量％以下、より好ましくは９０質量％以下、さらに好ましくは８０質量％以下である。上記範囲を外れて（Ｄ）成分の含有量が少なすぎると（Ｄ）成分を入れる効果が発現されなくなり、逆に、（Ｄ）成分の含有量が多すぎると冷却性が低下する虞がある。 The content of the component (D) is preferably 0.1% by mass or more, more preferably 0.5% by mass or more, and still more preferably, based on the mass (100% by mass) of the entire working fluid of the present invention. It is 1% by mass or more, more preferably 3% by mass or more, particularly preferably 10% by mass or more, and the upper limit is preferably 95% by mass or less, more preferably 90% by mass or less, and further preferably 80% by mass or less. If the content of the component (D) is too small outside the above range, the effect of adding the component (D) is not expressed, and conversely, if the content of the component (D) is too large, the cooling performance may be lowered. .
　本発明の加工液は、上記した（Ａ）成分を含有し、場合によっては、さらに、（Ｃ）成分および（Ｄ）成分を含有しており、残部は（Ｂ）水となっている。水としては、蒸留水、水道水等、その種類は特に限定されない。なお、（Ｂ）水の含有量が多い加工液では、シリコン粉を含有する加工液が増粘し、ゲル化しやすい。これに対し、本発明の加工液では、水の含有量が多い組成、例えば、加工液全体の質量を基準として、水が９０質量％以上となるような組成においても、シリコン粉を含有する加工液の増粘・ゲル化を抑制することができる。 The working fluid of the present invention contains the above-described component (A), and in some cases, further contains (C) component and (D) component, and the balance is (B) water. The type of water is not particularly limited, such as distilled water or tap water. In addition, in (B) the processing liquid with much water content, the processing liquid containing a silicon powder will thicken and it will be easy to gelatinize. In contrast, the processing liquid of the present invention contains silicon powder even in a composition having a high water content, for example, a composition in which water is 90% by mass or more based on the mass of the entire processing liquid. The thickening and gelation of the liquid can be suppressed.
　＜加工液の性状＞
　本発明の加工液の粘度は、２５℃で、好ましくは５０ｍＰａ・ｓ以下であり、より好ましくは２５ｍＰａ・ｓ以下、さらに好ましくは２０ｍＰａ・ｓ以下である。また、本発明の加工液に、所定のシリコン粉を分散させた加工液（擬似使用液）の粘度は、２５℃で、１００ｍＰａ・ｓ、好ましくは５５ｍＰａ・ｓ以下であり、より好ましくは５０ｍＰａ・ｓ以下であり、さらに好ましくは４５ｍＰａ・ｓ以下である。該擬似使用液の粘度は、本発明の加工液にシリコン粉（粒子径：１．５μｍ）を１０質量％添加し、撹拌混合後、ステンレス鋼球（直径２ｍｍ）を入れ、１０００ｒｐｍで１０時間撹拌し、該ステンレス鋼球を濾別して得られた擬似使用液について測定したものである。上記した加工液自体の粘度が高すぎると、シリコン粉を含有する擬似使用液の粘度も必然的に高くなる。また、擬似使用液の粘度が高すぎると、上記課題の欄において述べた諸問題が発生する虞がある。なお、加工液および擬似使用液の粘度は、ブルックフィールド型粘度計にて測定することができる。 <Properties of machining fluid>
The viscosity of the working fluid of the present invention is 25 ° C., preferably 50 mPa · s or less, more preferably 25 mPa · s or less, and still more preferably 20 mPa · s or less. Moreover, the viscosity of the working fluid (pseudo-use fluid) in which a predetermined silicon powder is dispersed in the working fluid of the present invention is 100 mPa · s, preferably 55 mPa · s or less, more preferably 50 mPa · s at 25 ° C. s or less, more preferably 45 mPa · s or less. The viscosity of the pseudo use liquid is such that 10% by mass of silicon powder (particle diameter: 1.5 μm) is added to the processing liquid of the present invention, and after stirring and mixing, a stainless steel ball (diameter 2 mm) is added and stirred at 1000 rpm for 10 hours. The pseudo-use liquid obtained by filtering the stainless steel balls was measured. If the viscosity of the processing liquid itself is too high, the viscosity of the pseudo-use liquid containing silicon powder inevitably increases. In addition, if the viscosity of the pseudo use liquid is too high, the problems described in the above problem column may occur. The viscosities of the working liquid and the pseudo use liquid can be measured with a Brookfield viscometer.
　加工液のｐＨは、好ましくは５．０以上９．０以下である。加工液のｐＨが低すぎる場合は、該加工液が触れる鉄材またはワイヤの腐食が起こる虞があり、逆に、加工液のｐＨが高すぎる場合は、加工液とシリコン粉とが反応して水素が発生する虞がある。本発明の加工液は、水に希釈して使用してもよいが、その場合も、希釈後の加工液のｐＨは上記範囲であることが好ましい。 The pH of the working fluid is preferably 5.0 or more and 9.0 or less. If the pH of the machining fluid is too low, there is a risk of corrosion of the iron material or wire that is touched by the machining fluid. Conversely, if the pH of the machining fluid is too high, the machining fluid reacts with the silicon powder to generate hydrogen. May occur. The working fluid of the present invention may be used after diluting in water, but in that case as well, the pH of the diluted working fluid is preferably in the above range.
　＜実施例１～１３、比較例１～５＞
　本発明の固定砥粒ワイヤソー用水溶性加工液（実施例１～１３）及び本発明以外の固定砥粒ワイヤソー用水溶性加工液（比較例１～５）を表１～３に示すような組成となるように作製した。作製した加工液のｐＨを測定すると共に、ブルックフィールド型粘度計にて、２５℃での粘度を測定した。
　更に、各加工液にシリコン粉（平均粒子系１．５ｍ）を１０質量％添加し、撹拌混合後、ステンレス鋼球（直径２ｍｍ）を入れ、１０００ｒｐｍで１０時間撹拌して擬似使用液を形成した。該擬似使用液から、金網（５０メッシュ）でステンレス鋼球をろ別した後、ブルックフィールド型粘度計にて、該擬似使用液の粘度（ｍＰａ・ｓ、２５℃）を測定した。また、擬似使用液１０ｍｌを５０℃に加熱し、３０分間に発生する水素量（ｍｌ）を測定した。 <Examples 1 to 13 and Comparative Examples 1 to 5>
The water-soluble processing liquid for fixed abrasive wire saws of the present invention (Examples 1 to 13) and the water-soluble processing liquid for fixed abrasive wire saws of the present invention (Comparative Examples 1 to 5) have the compositions shown in Tables 1 to 3. It produced as follows. While measuring the pH of the produced processing liquid, the viscosity at 25 degreeC was measured with the Brookfield type viscometer.
Furthermore, 10% by mass of silicon powder (average particle size of 1.5 m) was added to each processing liquid, and after stirring and mixing, stainless steel balls (diameter 2 mm) were added and stirred at 1000 rpm for 10 hours to form a pseudo use liquid. . After the stainless steel balls were filtered from the pseudo use liquid with a metal mesh (50 mesh), the viscosity (mPa · s, 25 ° C.) of the pseudo use liquid was measured with a Brookfield viscometer. Further, 10 ml of the pseudo use liquid was heated to 50 ° C., and the amount of hydrogen (ml) generated in 30 minutes was measured.
　なお、ポリビニルピロリドン（ＰＶＰ）の重量平均分子量は、ＰＶＰ　Ｋ－１５が９７００であり、ＰＶＰ　Ｋ－３０が７００００であり、ＰＶＰ　Ｋ－６０が４０００００であった。また、ＰＶＰ／ＶＡは、ビニルピロリドンと酢酸ビニルとの共重合体であり、重量平均分子量が３２，０００、共重合体中のビニルピロリドンの割合が７０モル％である。 The weight average molecular weight of polyvinylpyrrolidone (PVP) was 9700 for PVP K-15, 70000 for PVP K-30, and 400000 for PVP K-60. PVP / VA is a copolymer of vinyl pyrrolidone and vinyl acetate, the weight average molecular weight is 32,000, and the proportion of vinyl pyrrolidone in the copolymer is 70 mol%.
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000002
Figure JPOXMLDOC01-appb-T000002
Figure JPOXMLDOC01-appb-T000003
Figure JPOXMLDOC01-appb-T000003
　比較例の加工液では、いずれも擬似使用液粘度が上昇し、５５ｍＰａ・ｓを超えている。これに対し、本発明の加工液（実施例１～１３）は、擬似使用液においても粘度変化が小さく、いずれも４５ｍＰａ・ｓ以下である。 In all of the working fluids of the comparative examples, the pseudo-use fluid viscosity increases and exceeds 55 mPa · s. In contrast, the working fluids of the present invention (Examples 1 to 13) have a small viscosity change even in the pseudo-use fluid, and all are 45 mPa · s or less.
　実施例１～３、比較例１、２は原液を１０倍に希釈したものである。したがって、原液の組成は、各化合物が１０倍量である。 Examples 1 to 3 and Comparative Examples 1 and 2 are obtained by diluting the stock solution 10 times. Therefore, the composition of the stock solution is 10 times the amount of each compound.
　（グループＩ）
　グループＩは、実施例１～６、および、比較例１～３であり、水分量が多い加工液の例である。比較例の加工液で、水分量の多い組成（比較例１～３）は、いずれも増粘・ゲル化したが、ＰＶＰを添加した本発明の加工液（実施例１～６）は、ゲル化せず、ほとんど増粘しなかった。
　また、水素発生量に関しては、実施例１～６では水素発生が５ｍｌ以下であるのに対し、比較例１～３では水素発生量が１５ｍｌ以上であり非常に多かった。 (Group I)
Group I is Examples 1 to 6 and Comparative Examples 1 to 3, which are examples of working fluids with a large amount of water. In the comparative working fluid, the compositions with high water content (Comparative Examples 1 to 3) were all thickened and gelled. It did not become thick and did not thicken.
Regarding the hydrogen generation amount, in Examples 1 to 6, hydrogen generation was 5 ml or less, while in Comparative Examples 1 to 3, the hydrogen generation amount was 15 ml or more, which was very large.
　（グループＩＩ）
　グループＩＩは、実施例７～１２、および、比較例４であり、（Ｃ）成分および（Ｄ）成分の種類および量を統一させ、（Ａ）成分について変化させたものである。これより、各種ポリビニルピロリドン（ＰＶＰ）、ビニルピロリドン／酢酸ビニル共重合体（ＰＶＰ／ＶＡ）の増粘抑制効果が示された。
　また、水素発生量に関しては、実施例７～１２と比較例４とを比べると、ポリビニルピロリドン等を含む本発明の加工液は水素発生量が少なかった。 (Group II)
Group II is Examples 7 to 12 and Comparative Example 4, in which the types and amounts of the component (C) and the component (D) were unified, and the component (A) was changed. From this, the thickening inhibitory effect of various polyvinylpyrrolidone (PVP) and a vinylpyrrolidone / vinyl acetate copolymer (PVP / VA) was shown.
As for the hydrogen generation amount, when Examples 7 to 12 and Comparative Example 4 were compared, the processing liquid of the present invention containing polyvinylpyrrolidone and the like had a small amount of hydrogen generation.
　（グループＩＩＩ）
　グループＩＩＩは、実施例１３と比較例５であり、グループＩ、グループＩＩと異なる（Ｄ）成分を含むものである。これより（Ｄ）成分の種類を問わずポリビニルピロリドン（ＰＶＰ）による増粘抑制の効果が示された。
  また実施例１３と比較例５を比較すると、ポリビニルピロリドンを含む実施例１３は水素発生量が少なかった。
　以上より、ポリビニルピロリドン、および、ビニルピロリドンを含む共重合物から選ばれる少なくとも一種類以上の水溶性高分子を含む本発明の加工液は、シリコン粉を分散させた擬似使用液において、粘度上昇を抑制すると共に水素発生を抑制する効果があることが示された。 (Group III)
Group III is Example 13 and Comparative Example 5 and includes (D) component different from Group I and Group II. From this, the effect of thickening suppression by polyvinylpyrrolidone (PVP) was shown irrespective of the kind of (D) component.
Further, when Example 13 and Comparative Example 5 were compared, Example 13 containing polyvinylpyrrolidone had a small amount of hydrogen generation.
From the above, the processing liquid of the present invention containing at least one kind of water-soluble polymer selected from polyvinylpyrrolidone and a copolymer containing vinylpyrrolidone has an increased viscosity in a pseudo-use liquid in which silicon powder is dispersed. It was shown that it has the effect of suppressing hydrogen generation as well as suppression.
　以上、現時点において、もっとも、実践的であり、かつ、好ましいと思われる実施形態に関連して本発明を説明したが、本発明は、本願明細書中に開示された実施形態に限定されるものではなく、請求の範囲および明細書全体から読み取れる発明の要旨或いは思想に反しない範囲で適宜変更可能であり、そのような変更を伴う固定砥粒ワイヤソー用水溶性加工液もまた本発明の技術的範囲に包含されるものとして理解されなければならない。 While the present invention has been described in connection with embodiments that are presently the most practical and preferred, the present invention is not limited to the embodiments disclosed herein. However, the present invention can be changed as appropriate without departing from the spirit or concept of the invention that can be read from the claims and the entire specification, and a water-soluble working fluid for a fixed abrasive wire saw accompanying such a change is also within the technical scope of the present invention. Must be understood as encompassed by.
　本発明の固定砥粒ワイヤソー用水溶性加工液は、固定砥粒ワイヤソーを用いてシリコンウエハを切断する際に特に好適に使用することができる。 The water-soluble processing liquid for a fixed abrasive wire saw of the present invention can be used particularly suitably when a silicon wafer is cut using a fixed abrasive wire saw.

Claims (9)

  1. （Ａ）ポリビニルピロリドン、および、ビニルピロリドンを含む共重合物から選ばれる少なくとも一種類以上の水溶性高分子、ならびに、（Ｂ）水を含有する固定砥粒ワイヤソー用水溶性加工液。 (A) at least one water-soluble polymer selected from polyvinylpyrrolidone and a copolymer containing vinylpyrrolidone, and (B) a water-soluble working solution for a fixed abrasive wire saw, which contains water.
  2. 前記（Ａ）成分の重量平均分子量が、２，０００～１，０００，０００である、請求項１に記載の固定砥粒ワイヤソー用水溶性加工液。 The water-soluble processing liquid for a fixed abrasive wire saw according to claim 1, wherein the component (A) has a weight average molecular weight of 2,000 to 1,000,000.
  3. 前記（Ａ）成分の含有量が、固定砥粒ワイヤソー用水溶性加工液全体の質量を１００質量％として、０．０２質量％以上７質量％以下である、請求項１または２に記載の固定砥粒ワイヤソー用水溶性加工液。 The fixed abrasive according to claim 1 or 2, wherein the content of the component (A) is 0.02% by mass or more and 7% by mass or less, based on 100% by mass of the entire water-soluble processing liquid for a fixed abrasive wire saw. Water-soluble machining fluid for grain wire saws.
  4. さらに、（Ｃ）多価カルボン酸のアルカリ塩を含有する、請求項１～３のいずれかに記載の固定砥粒ワイヤソー用水溶性加工液。 The water-soluble machining liquid for a fixed abrasive wire saw according to any one of claims 1 to 3, further comprising (C) an alkali salt of a polyvalent carboxylic acid.
  5. 前記（Ｃ）成分の含有量が、固定砥粒ワイヤソー用水溶性加工液全体の質量を１００質量％として、０．０１質量％以上１０質量％以下である、請求項４に記載の固定砥粒ワイヤソー用水溶性加工液。 5. The fixed abrasive wire saw according to claim 4, wherein the content of the component (C) is 0.01% by mass or more and 10% by mass or less, based on 100% by mass of the entire water-soluble processing liquid for the fixed abrasive wire saw. Water-soluble processing fluid.
  6. さらに、（Ｄ）グリコール類、グリコールエーテル類、および、ポリオキシアルキレングリコール類からなる群から選ばれる一種以上を含有する、請求項１～５のいずれかに記載の固定砥粒ワイヤソー用水溶性加工液。 The water-soluble machining fluid for fixed abrasive wire saws according to any one of claims 1 to 5, further comprising (D) one or more selected from the group consisting of glycols, glycol ethers, and polyoxyalkylene glycols. .
  7. 前記（Ｄ）成分の含有量が、固定砥粒ワイヤソー用水溶性加工液全体の質量を１００質量％として、０．１質量％以上９５質量％以下である、請求項６に記載の固定砥粒ワイヤソー用水溶性加工液。 7. The fixed abrasive wire saw according to claim 6, wherein the content of the component (D) is 0.1% by mass or more and 95% by mass or less based on 100% by mass of the entire water-soluble processing liquid for the fixed abrasive wire saw. Water-soluble processing fluid.
  8. 加工液の粘度が２５℃で５０ｍＰａ・ｓ以下である、請求項１～７のいずれかに記載の固定砥粒ワイヤソー用水溶性加工液。 The water-soluble processing liquid for a fixed abrasive wire saw according to any one of claims 1 to 7, wherein the viscosity of the processing liquid is 50 mPa · s or less at 25 ° C.
  9. 前記加工液に、平均粒子径１．５μｍのシリコン粉を１０質量％添加し撹拌して形成した擬似使用液の粘度が、２５℃で１００ｍＰａ・ｓ以下である、請求項１～８のいずれかに記載の固定砥粒ワイヤソー用水溶性加工液。 The viscosity of a pseudo use liquid formed by adding 10% by mass of silicon powder having an average particle diameter of 1.5 μm to the working liquid and stirring is 100 mPa · s or less at 25 ° C. The water-soluble processing liquid for fixed abrasive wire saws described in 1.
PCT/JP2011/067457 2010-08-03 2011-07-29 Aqueous processing solution for fixed abresive grain wire saw WO2012017947A1 (en)

Priority Applications (4)

Application Number Priority Date Filing Date Title
KR1020137001523A KR101788901B1 (en) 2010-08-03 2011-07-29 Aqueous processing solution for fixed abrasive grain wire saw
SG2012096475A SG186486A1 (en) 2010-08-03 2011-07-29 Aqueous processing solution for fixed abrasive grain wire saw
EP11814573.9A EP2602058A4 (en) 2010-08-03 2011-07-29 Aqueous processing solution for fixed abresive grain wire saw
CN201180036629.6A CN103025486B (en) 2010-08-03 2011-07-29 Water-soluble working fluid for fixed-abrasive wire saw

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2010174673A JP5420498B2 (en) 2010-08-03 2010-08-03 Water-soluble machining fluid for fixed abrasive wire saws
JP2010-174673 2010-08-03

Publications (1)

Publication Number Publication Date
WO2012017947A1 true WO2012017947A1 (en) 2012-02-09

Family

ID=45559447

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2011/067457 WO2012017947A1 (en) 2010-08-03 2011-07-29 Aqueous processing solution for fixed abresive grain wire saw

Country Status (7)

Country Link
EP (1) EP2602058A4 (en)
JP (1) JP5420498B2 (en)
KR (1) KR101788901B1 (en)
CN (1) CN103025486B (en)
SG (1) SG186486A1 (en)
TW (1) TWI522457B (en)
WO (1) WO2012017947A1 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012115099A1 (en) * 2011-02-23 2012-08-30 ユシロ化学工業株式会社 Water-soluble working fluid for fixed abrasive grain wire saw
WO2014003157A1 (en) * 2012-06-29 2014-01-03 出光興産株式会社 Aqueous processing liquid

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6819619B2 (en) * 2018-01-22 2021-01-27 信越半導体株式会社 Work cutting method and wire saw
CN110497546A (en) * 2019-08-26 2019-11-26 哈尔滨商业大学 The method and apparatus of free-consolidation abrasive compound multiline cut silicon chips

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6243482A (en) * 1985-08-21 1987-02-25 Sanyo Chem Ind Ltd Abrasion working fluid
JPH10259396A (en) * 1997-03-21 1998-09-29 Neos Co Ltd Water-soluble cutting fluid for wire saw
JP2001054850A (en) 1999-08-11 2001-02-27 Osaka Diamond Ind Co Ltd Hard brittle material cutting method by means of fixed abrasive grain wire saw
JP2003082334A (en) 2001-09-06 2003-03-19 Yushiro Chem Ind Co Ltd Water-soluble work liquid composition for abrasive train fixed wire saw
JP2008161992A (en) * 2006-12-28 2008-07-17 Asahi Diamond Industrial Co Ltd Cutting method for processed member and manufacturing method for wafer

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1057478A (en) * 1990-06-22 1992-01-01 薛志纯 Metal working fluid
US5401428A (en) * 1993-10-08 1995-03-28 Monsanto Company Water soluble metal working fluids
JP2000296455A (en) * 1999-04-09 2000-10-24 Tokyo Seimitsu Co Ltd Fixed abrasive grain multi-wire saw
JP2002096251A (en) * 1999-09-17 2002-04-02 Sumitomo Special Metals Co Ltd Cutting method and cutting apparatus for rare earth alloys
JP2001138205A (en) * 1999-11-08 2001-05-22 Sumitomo Special Metals Co Ltd Method and apparatus for cutting rare earth alloy
JP2002167589A (en) * 2000-11-30 2002-06-11 Nippon Shokubai Co Ltd Metal working oil
TW575660B (en) * 2001-09-07 2004-02-11 Dai Ichi Kogyo Seiyaku Co Ltd Nonflammable water-based cutting fluid composition and nonflammable water-based cutting fluid
JP4874853B2 (en) * 2007-04-09 2012-02-15 Ｄｏｗａホールディングス株式会社 Cutting method of sintered rare earth magnet alloy
JP5253765B2 (en) * 2007-07-05 2013-07-31 株式会社Ａｄｅｋａ Additive for dicing cutting water and cutting method using the same
US8157876B2 (en) * 2007-07-31 2012-04-17 Cabot Microelectronics Corporation Slurry composition containing non-ionic polymer and method for use
US20090149359A1 (en) * 2007-12-10 2009-06-11 Hundley Lloyd E Formulation of a metal working fluid

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6243482A (en) * 1985-08-21 1987-02-25 Sanyo Chem Ind Ltd Abrasion working fluid
JPH10259396A (en) * 1997-03-21 1998-09-29 Neos Co Ltd Water-soluble cutting fluid for wire saw
JP2001054850A (en) 1999-08-11 2001-02-27 Osaka Diamond Ind Co Ltd Hard brittle material cutting method by means of fixed abrasive grain wire saw
JP2003082334A (en) 2001-09-06 2003-03-19 Yushiro Chem Ind Co Ltd Water-soluble work liquid composition for abrasive train fixed wire saw
JP2008161992A (en) * 2006-12-28 2008-07-17 Asahi Diamond Industrial Co Ltd Cutting method for processed member and manufacturing method for wafer

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of EP2602058A4 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012115099A1 (en) * 2011-02-23 2012-08-30 ユシロ化学工業株式会社 Water-soluble working fluid for fixed abrasive grain wire saw
WO2014003157A1 (en) * 2012-06-29 2014-01-03 出光興産株式会社 Aqueous processing liquid
JP2014009313A (en) * 2012-06-29 2014-01-20 Idemitsu Kosan Co Ltd Aqueous working fluid
CN104395448A (en) * 2012-06-29 2015-03-04 出光兴产株式会社 Aqueous processing fluid
US20150133354A1 (en) * 2012-06-29 2015-05-14 Idemitsu Kosan Co., Ltd. Aqueous processing liquid

Also Published As

Publication number Publication date
JP2012035336A (en) 2012-02-23
EP2602058A4 (en) 2014-12-24
KR101788901B1 (en) 2017-10-20
TWI522457B (en) 2016-02-21
TW201211235A (en) 2012-03-16
KR20130095724A (en) 2013-08-28
CN103025486A (en) 2013-04-03
SG186486A1 (en) 2013-02-28
EP2602058A1 (en) 2013-06-12
CN103025486B (en) 2016-03-30
JP5420498B2 (en) 2014-02-19

Similar Documents

Publication Publication Date Title
JP5639996B2 (en) Processing fluid for brittle materials and processing fluid for hard materials
JP4481898B2 (en) Water-based abrasive dispersion medium composition
TWI413681B (en) Slurry composition containing non-ionic polymer and method for use
JP6039935B2 (en) Aqueous processing fluid
JP5679642B2 (en) Water-soluble machining fluid for fixed abrasive wire saws
CN1760307B (en) Polishing composition and polishing method using the same
TWI521057B (en) Water-soluble working fluid for fixed abrasive grain wire saw
JP5420498B2 (en) Water-soluble machining fluid for fixed abrasive wire saws
WO2019131448A1 (en) Polishing composition
TWI613188B (en) Water-soluble cutting fluid for fixed honing granule saw, cutting method using the same, and substrate for electronic material obtained therefrom
JP6232480B2 (en) Aqueous processing fluid
WO2012026437A1 (en) Silicon wafer processing solution and silicon wafer processing method
JP7361467B2 (en) polishing composition
JP2008246668A (en) Aqueous abrasive particle dispersion medium composite, processing aqueous slurry, and processing method using them
CN105602522B (en) A kind of linear cutting mortar and preparation method thereof
EP4083152A1 (en) Polishing composition
JP2021105145A (en) Composition for polishing, and method of polishing silicon wafer
KR20130067809A (en) Aqueous sawing fluid composition

Legal Events

Date Code Title Description
WWE Wipo information: entry into national phase

Ref document number: 201180036629.6

Country of ref document: CN

121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 11814573

Country of ref document: EP

Kind code of ref document: A1

WWE Wipo information: entry into national phase

Ref document number: 12013500021

Country of ref document: PH

ENP Entry into the national phase

Ref document number: 20137001523

Country of ref document: KR

Kind code of ref document: A

WWE Wipo information: entry into national phase

Ref document number: 2011814573

Country of ref document: EP

NENP Non-entry into the national phase

Ref country code: DE