WO2011007590A1 - Water-soluble working fluid for fixed-abrasive wire saw - Google Patents
Water-soluble working fluid for fixed-abrasive wire saw Download PDFInfo
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- WO2011007590A1 WO2011007590A1 PCT/JP2010/052095 JP2010052095W WO2011007590A1 WO 2011007590 A1 WO2011007590 A1 WO 2011007590A1 JP 2010052095 W JP2010052095 W JP 2010052095W WO 2011007590 A1 WO2011007590 A1 WO 2011007590A1
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- carboxylic acid
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- 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
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- 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
- C10M2207/0225—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms containing at least two hydroxy groups used as base material
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- 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
- C10M2209/1045—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing two carbon atoms only used as base material
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- 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
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- 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 machining fluid for a fixed abrasive wire saw.
- the wire saw cutting method includes a free abrasive grain method and a fixed abrasive grain method.
- a slurry in which abrasive particles are dispersed in an oil is used as a processing liquid.
- Patent Document 1 discloses a fixed abrasive wire saw in which abrasive grains of 30 to 60 ⁇ m or less are fixed by resin bonding, and this is run at a linear speed of 1000 to 2500 m / min to cut a brittle material. This enables cutting with high efficiency.
- Patent Document 2 proposes a water-soluble processing liquid composition for a fixed abrasive wire saw containing (A) glycols. JP 2001-045450 A JP 2003-082334 A
- Patent Document 2 by incorporating glycols and optionally other components in the water-soluble processing liquid composition for fixed abrasive wire saws, it is suitable for cutting processing materials other than rare earth magnets and also for cutting silicon. It is said that it is suitable and the reaction with silicon can be suppressed.
- the stability of the processing liquid when silicon cutting waste is mixed which affects the silicon processability. It was found that there are cases where
- the present invention has been made in view of the above, and an object of the present invention is to provide a water-soluble processing liquid for a fixed abrasive wire saw that is excellent in silicon processability.
- the present inventors have obtained the following knowledge.
- the machining fluid has an appropriate viscosity. That is, when the viscosity is too low, the wire is cut, and when the viscosity is too high, the wire slips, and the processability of silicon becomes insufficient.
- the liquid property of the machining liquid becomes unstable and the liquid viscosity may increase.
- the present invention is a water-soluble processing liquid for a fixed abrasive wire saw, which contains (A) a glycol and water and has a viscosity at 25 ° C. of 3 mPa ⁇ s to 50 mPa ⁇ s.
- the viscosity at 25 ° C. is preferably 5 mPa ⁇ s or more and 25 mPa ⁇ s or less.
- viscosity means a viscosity measured by a B-type rotational viscometer.
- Contains glycols and water is a concept that the water-soluble processing liquid for a fixed abrasive wire saw of the present invention may be composed only of glycols and water, or may contain other components. .
- the pH of the working fluid is preferably adjusted to 5.0 or more and 7.5 or less, more preferably 5.5 or more and 6.5 or less.
- the (B) carboxylic acid preferably has 7 or less carbon atoms.
- the total of (A) glycols, (B) carboxylic acid, and (C) a compound that exhibits basicity when dissolved in water is 100% by mass. % By mass to 95% by mass, (B) 0.01% by mass to 60% by mass of carboxylic acid, and (C) 0.01% by mass to 60% by mass of a compound that is dissolved in water and exhibits basicity.
- (B) carboxylic acid and (C) a compound which is dissolved in water and exhibits basicity be contained in a total amount of 0.02% by mass to 60% by mass.
- the water-soluble working fluid for fixed abrasive wire saw of the present invention is suitably used for cutting of silicon material.
- the processing time is shortened and the cutting accuracy of the silicon wafer can be improved. Therefore, in the cutting process using a fixed abrasive wire saw, it is possible to provide a water-soluble processing liquid for a fixed abrasive wire saw that is particularly excellent in silicon processability.
- water-soluble processing liquid for fixed abrasive wire saw of the present invention contains (A) glycols and water, and optionally, (B) carboxylic acid and (C ) Compounds that are basic when dissolved in water and other components may be included. Hereinafter, each component will be described in detail.
- the water-soluble processing liquid of the present invention contains (A) glycols.
- glycols include ethylene glycol, propylene glycol, 1,4-butanediol, hexamethylene glycol, neopentyl glycol, diethylene glycol, triethylene glycol, dipropylene glycol, tripropylene glycol, polyethylene glycol, polypropylene glycol, polyethylene glycol And polypropylene glycol copolymers, and glycols such as polyoxyethylene and polyoxypropylene copolymers, glycol monoalkyls such as triethylene glycol monobutyl ether, triethylene glycol monomethyl ether, diethylene glycol monobutyl ether and tripropylene glycol monomethyl ether Ether, polyoxyethylene and polyoxypropylene Water-soluble glycols such as monoalkyl ethers of polymerization thereof.
- glycols exemplified above it is preferable to use propylene glycol, dipropylene glycol, diethylene glycol, triethylene glycol, polyethylene glycol or polypropylene glycol, and it is particularly preferable to use propylene glycol or polyethylene glycol. These can be used alone or in combination of two or more. Moreover, you may use as a copolymer which consists of said 2 or more types of component.
- the molecular weight of the glycols is preferably 70 to 100,000, more preferably 76 to 10,000. If the molecular weight is within this range, silicon processability can be further improved.
- the lower limit of (A) glycols is preferably 1% by mass or more, more preferably 5% by mass or more, further preferably 15% by mass or more, and further preferably 20%, based on the total processing liquid.
- the upper limit is preferably 95% by mass or less, more preferably 89% by mass or less, and still more preferably 85% by mass or less.
- the water-soluble processing liquid of the present invention contains the (A) glycols and water as long as the (A) glycols and the balance are composed of only water, but other additives and the like. These components may be contained. Moreover, it is preferable to further contain (B) a carboxylic acid or (C) a compound which is dissolved in water and exhibits basicity.
- the water-soluble processing liquid of the present invention preferably further contains (B) a carboxylic acid in addition to (A) glycols and water.
- a carboxylic acid having 7 or less carbon atoms is preferably used, a carboxylic acid having 2 to 6 carbon atoms is more preferably used, and a carboxylic acid having 6 carbon atoms is used. Particularly preferred.
- citric acid, succinic acid, lactic acid, malic acid, adipic acid, succinic acid, and acetic acid are preferably used, and citric acid and succinic acid are more preferably used, and citric acid is used. Is particularly preferred.
- the liquid stability can be suitably maintained when silicon cutting waste is mixed during the cutting process, and a water-soluble processing liquid having excellent silicon processability is obtained. be able to.
- the (B) carboxylic acid is preferably contained in an amount of 0.01% by mass or more and 60% by mass or less, and 0.05% by mass or more and 10% by mass or less based on the entire processing liquid. It is more preferable that the content is 0.1% by mass or more and 5% by mass or less.
- (C) Compound that exhibits basic properties when dissolved in water
- a basic compound hereinafter referred to as “(C) basic compound”
- (C) basic compound the compound containing an alkali metal element, an alkanolamine, an alkylamine, ammonia, etc. are mentioned, for example, These can be used individually by 1 type or in combination of 2 or more types. Among these, it is preferable to use a compound containing an alkali metal element.
- Examples of the compound containing an alkali metal element include sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium hydrogen carbonate and potassium hydrogen carbonate, and potassium hydroxide is particularly preferably used.
- the basic compound (C) is preferably contained in an amount of 0.01% by mass or more and 60% by mass or less, and 0.05% by mass or more and 10% by mass or less, based on the entire processing liquid. It is more preferably contained, and particularly preferably 0.1 to 5% by mass.
- (C) By making the content of the basic compound in this way, when silicon cutting waste is mixed, the liquid stability can be suitably maintained, and further, a water-soluble processing liquid having excellent silicon processability is obtained. Can do.
- (D) salt a salt formed from (B) carboxylic acid and (C) basic compound
- (D) salt a salt formed from (B) carboxylic acid and (C) basic compound
- (D) salts include alkali metal salts of carboxylic acids and amine salts of carboxylic acids.
- the total content of the (B) carboxylic acid and the (C) basic compound is 0.02% by mass or more and 60% by mass or less based on the entire processing liquid.
- it is more preferably 0.1% by mass or more and 20% by mass or less, and particularly preferably 0.2% by mass or more and 10% by mass or less. If it does in this way, the silicon reactivity of a processing liquid can be suppressed, and it can be set as the processing liquid which is excellent in silicon stability while being excellent in liquid stability.
- the total of (A) glycols, (B) carboxylic acid, and (C) basic compound is 100% by mass
- the (A) glycols, (B) carboxylic acid, and (C) basic The proportion of the compound is (A) glycols of 30% by mass to 95% by mass, (B) carboxylic acid of 0.1% by mass to 5% by mass, and (C) basic compound of 0.1% by mass or more. It is preferable to mix so that 5 mass% or less and the remainder may be water.
- the amount of the (A) glycols, (B) carboxylic acid, and (C) basic compound is adjusted, and the pH of the processing liquid is preferably adjusted to 5.0 or more and 7.5 or less, In this way, when silicon cutting waste is mixed during the cutting process, the liquid stability can be suitably maintained, and it is particularly effective to obtain a water-soluble processing liquid that is excellent in silicon processability. .
- (E) Other components in addition to the above (A) glycols and water, and optionally included (B) carboxylic acid and (C) basic compound or (D) salt, (E) Other components may be contained.
- various additives that do not adversely affect the processed material such as corrosion and discoloration and do not affect the stability of the system after mixing are added within a range that does not affect the processing performance. be able to.
- a viscosity adjusting agent, a pH adjusting agent, an antifoaming agent, an antioxidant and the like can be added.
- known viscosity modifiers can be used without particular limitation, but those that are soluble in water are preferred.
- pH adjusters examples include inorganic bases (such as sodium hydroxide, potassium hydroxide and ammonia), organic bases (such as alkanolamine and alkylamine), inorganic acids (hydrochloric acid, sulfuric acid, etc.), organic acids ( The above carboxylic acids and the like can be used.
- inorganic bases such as sodium hydroxide, potassium hydroxide and ammonia
- organic bases such as alkanolamine and alkylamine
- inorganic acids hydroochloric acid, sulfuric acid, etc.
- organic acids organic acids
- the above carboxylic acids and the like can be used.
- antifoaming agent, antioxidant and the like known ones can be used without particular limitation, but these are also preferably soluble in water.
- the water-soluble processing liquid of the present invention contains the above components.
- the water-soluble working fluid of the present invention may be diluted with water as necessary according to the working environment of the cutting process. That is, a concentrated composition composed of the above-mentioned component (A) excluding water is mixed and prepared, and appropriately diluted with water at the time of on-site cutting processing work, to an appropriate water-soluble processing liquid according to the working environment and situation. It can also be used after adjusting. Further, a concentrated composition composed of the above-mentioned component (A) containing a certain amount of water may be mixed and prepared, and further diluted with water during the on-site cutting process.
- the water-soluble processing liquid of the present invention has a viscosity at the time of use in cutting (that is, when the processing liquid is used for cutting without being diluted, the viscosity of the processing liquid before dilution, or after the dilution is performed)
- the viscosity of the diluted working fluid is adjusted to be 3 mPa ⁇ s or more and 50 mPa ⁇ s or less at 25 ° C.
- “Viscosity” refers to the viscosity measured by a B-type rotary viscometer. The viscosity at 25 ° C.
- the water-soluble processing liquid is preferably 3 mPa ⁇ s to 50 mPa ⁇ s, more preferably 5 mPa ⁇ s to 30 mPa ⁇ s, and more preferably 5 mPa ⁇ s to 25 mPa ⁇ s. It is particularly preferred.
- the viscosity of the water-soluble processing liquid is within this range, when used for cutting with a fixed abrasive wire saw, a water-soluble processing liquid having particularly excellent silicon processability can be obtained.
- a viscosity it can adjust suitably with content of said (A) glycols, content of (B) carboxylic acid and (C) basic compound, and other additives (viscosity modifier) etc. .
- the water-soluble processing liquid of the present invention is preferably used so that the pH is adjusted to 5.0 or more and 7.5 or less.
- the pH is preferably 5.5 or more and 6.5 or less. If the pH is within this range, the reaction between silicon and the processing liquid can be suppressed and the processing liquid can be stabilized even when silicon is mixed in the processing liquid as cutting waste after cutting. Can do. Therefore, an increase in the viscosity of the working fluid and a decrease in the life of the working fluid can be suppressed, and a water-soluble working fluid that is further excellent in silicon processability can be obtained.
- About adjustment of pH it can adjust suitably with content of said (A) glycols, content of (B) carboxylic acid and (C) basic compound, and other additives (pH adjuster) etc. .
- the material to be cut was processed using the multi-cutting machine. Specifically, as shown in FIG. 1, 10 grooves are formed in the material to be cut by the working fluid according to Examples 1 to 5, Comparative Examples 1 and 2 or Reference Examples 1 and 2, and the single wire saw cutting machine. The total depth of cut in the 10 grooves was used as an evaluation index. The working fluid was discharged toward the wire before and after the cut portion of the material to be cut. The results are shown in Table 3.
- the present invention can be suitably used as a water-soluble processing liquid for a fixed abrasive wire saw that can accurately cut a silicon material using a fixed abrasive wire saw during the manufacture of a silicon wafer.
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Abstract
Description
(1)切断加工時のワイヤにかかる負荷等を適切に調節し、ワイヤの破断やワイヤの滑りを抑制することで、シリコンの加工性を向上させることができるものと考えられる。ワイヤの破断やワイヤ滑りを抑制する観点で、加工液の種々のパラメータを検討した結果、加工液には適正粘度が存在することを知見した。すなわち、粘度が低すぎるとワイヤの切断が発生し、粘度が高すぎるとワイヤの滑りが発生し、シリコンの加工性が十分でなくなる。
(2)シリコン切り屑が混入した場合において、加工液の液性状が不安定となって液粘度が上昇する場合があることを知見した。液粘度が上昇すると、上記のようにワイヤの滑りが生じ、加工性の低下が懸念される他、液寿命の低下も懸念される。
(3)シリコン切り屑が混入した場合において、加工液の液性状を安定させるためには、シリコンと加工液との反応を抑制することが効果的であると考えられる。シリコンとの反応を抑制する観点で、加工液の種々のパラメータを検討した結果、加工液には適正pHが存在することを知見した。すなわち、所定範囲のpHとすることにより、シリコンとの反応をさらに抑制することができる。これにより、加工液の液性状を安定化でき、液粘度を適正に維持できるので、シリコン加工性を向上させることができるとともに、液寿命の低下を抑制することができる。
(4)加工液粘度やpHの調整について検討した結果、加工液中に酸及び塩基を添加することが好ましいことを知見した。特に酸成分として、カルボン酸、好ましくは炭素数7以下のカルボン酸を添加することで、シリコン加工性をさらに向上させることができる。 As a result of intensive studies to solve the above problems, the present inventors have obtained the following knowledge.
(1) It is considered that the workability of silicon can be improved by appropriately adjusting the load applied to the wire during the cutting process and suppressing the breakage of the wire and the slipping of the wire. As a result of examining various parameters of the machining fluid from the viewpoint of suppressing wire breakage and wire slip, it was found that the machining fluid has an appropriate viscosity. That is, when the viscosity is too low, the wire is cut, and when the viscosity is too high, the wire slips, and the processability of silicon becomes insufficient.
(2) It has been found that when silicon chips are mixed, the liquid property of the machining liquid becomes unstable and the liquid viscosity may increase. When the liquid viscosity rises, the wire slips as described above, and there is a concern that the workability may be lowered, and the liquid life may be shortened.
(3) In the case where silicon chips are mixed, it is considered effective to suppress the reaction between silicon and the processing liquid in order to stabilize the liquid property of the processing liquid. As a result of examining various parameters of the working fluid from the viewpoint of suppressing the reaction with silicon, it was found that the working fluid has an appropriate pH. That is, the reaction with silicon can be further suppressed by setting the pH within a predetermined range. Thereby, since the liquid property of a process liquid can be stabilized and a liquid viscosity can be maintained appropriately, a silicon workability can be improved and the fall of a liquid life can be suppressed.
(4) As a result of examining the adjustment of the working fluid viscosity and pH, it was found that it is preferable to add an acid and a base to the working fluid. In particular, by adding a carboxylic acid, preferably a carboxylic acid having 7 or less carbon atoms, as an acid component, the silicon processability can be further improved.
本発明は、(A)グリコール類及び水を含有し、25℃における粘度が3mPa・s以上50mPa・s以下である、固定砥粒ワイヤソー用水溶性加工液である。本発明において、25℃における上記粘度が5mPa・s以上25mPa・s以下であることが好ましい。 This invention is made | formed based on the said knowledge, and takes the following structures. That is,
The present invention is a water-soluble processing liquid for a fixed abrasive wire saw, which contains (A) a glycol and water and has a viscosity at 25 ° C. of 3 mPa · s to 50 mPa · s. In the present invention, the viscosity at 25 ° C. is preferably 5 mPa · s or more and 25 mPa · s or less.
「グリコール類及び水を含有し」とは、本発明の固定砥粒ワイヤソー用水溶性加工液が、グリコール類及び水のみからなっていてもよいし、他の成分を含んでいてもよい概念である。 In the present invention, “viscosity” means a viscosity measured by a B-type rotational viscometer.
“Contains glycols and water” is a concept that the water-soluble processing liquid for a fixed abrasive wire saw of the present invention may be composed only of glycols and water, or may contain other components. .
本発明の水溶性加工液には、(A)グリコール類が含有される。グリコール類としては、例えば、エチレングリコール、プロピレングリコール、1,4-ブタンジオール、ヘキサメチレングリコール、ネオペンチルグリコール、ジエチレングリコール、トリエチレングリコール、ジプロピレングリコール、トリプロピレングリコール、ポリエチレングリコール、ポリプロピレングリコール、ポリエチレングリコールとポリプロピレングリコールの共重合物、及びポリオキシエチレンとポリオキシプロピレンの共重合物等のグリコール、トリエチレングリコールモノブチルエーテル、トリエチレングリコールモノメチルエーテル、ジエチレングリコールモノブチルエーテル及びトリプロピレングリコールモノメチルエーテル等のグリコールモノアルキルエーテル、ポリオキシエチレンとポリオキシプロピレン共重合物のモノアルキルエーテル等の水溶性グリコール類が挙げられる。上記例示したグリコール類のうち、プロピレングリコール、ジプロピレングリコール、ジエチレングリコール、トリエチレングリコール、ポリエチレングリコール又はポリプロピレングリコールを用いることが好ましく、特にプロピレングリコール、又はポリエチレングリコールを用いることが好ましい。これらは1種単独であるいは2種以上を組み合わせて用いることができる。また、上記2種以上の成分からなる共重合体として用いてもよい。上記グリコール類の分子量は好ましくは70~100,000、より好ましくは76~10,000である。分子量がこの範囲にあれば、シリコン加工性を一層向上させることができる。 (A) Glycols The water-soluble processing liquid of the present invention contains (A) glycols. Examples of glycols include ethylene glycol, propylene glycol, 1,4-butanediol, hexamethylene glycol, neopentyl glycol, diethylene glycol, triethylene glycol, dipropylene glycol, tripropylene glycol, polyethylene glycol, polypropylene glycol, polyethylene glycol And polypropylene glycol copolymers, and glycols such as polyoxyethylene and polyoxypropylene copolymers, glycol monoalkyls such as triethylene glycol monobutyl ether, triethylene glycol monomethyl ether, diethylene glycol monobutyl ether and tripropylene glycol monomethyl ether Ether, polyoxyethylene and polyoxypropylene Water-soluble glycols such as monoalkyl ethers of polymerization thereof. Of the glycols exemplified above, it is preferable to use propylene glycol, dipropylene glycol, diethylene glycol, triethylene glycol, polyethylene glycol or polypropylene glycol, and it is particularly preferable to use propylene glycol or polyethylene glycol. These can be used alone or in combination of two or more. Moreover, you may use as a copolymer which consists of said 2 or more types of component. The molecular weight of the glycols is preferably 70 to 100,000, more preferably 76 to 10,000. If the molecular weight is within this range, silicon processability can be further improved.
本発明の水溶性加工液には、(A)グリコール類及び水に加えて、さらに(B)カルボン酸が含有されることが好ましい。(B)カルボン酸としては、炭素数が7以下のカルボン酸を用いることが好ましく、炭素数が2以上6以下のカルボン酸を用いることがさらに好ましく、炭素数が6のカルボン酸を用いることが特に好ましい。(B)カルボン酸の具体例としては、クエン酸、コハク酸、乳酸、リンゴ酸、アジピン酸、蓚酸、酢酸を用いることが好ましくクエン酸、コハク酸を用いることがより好ましく、クエン酸を用いることが特に好ましい。これらは、1種単独であるいは2種以上を組み合わせて用いることができる。炭素数が7以下のカルボン酸を用いることで、切断加工中、シリコン切断屑が混入した場合に、液安定性を好適に維持することができ、さらにシリコン加工性に優れる水溶性加工液とすることができる。 (B) Carboxylic acid The water-soluble processing liquid of the present invention preferably further contains (B) a carboxylic acid in addition to (A) glycols and water. (B) As the carboxylic acid, a carboxylic acid having 7 or less carbon atoms is preferably used, a carboxylic acid having 2 to 6 carbon atoms is more preferably used, and a carboxylic acid having 6 carbon atoms is used. Particularly preferred. As specific examples of (B) carboxylic acid, citric acid, succinic acid, lactic acid, malic acid, adipic acid, succinic acid, and acetic acid are preferably used, and citric acid and succinic acid are more preferably used, and citric acid is used. Is particularly preferred. These can be used alone or in combination of two or more. By using a carboxylic acid having a carbon number of 7 or less, the liquid stability can be suitably maintained when silicon cutting waste is mixed during the cutting process, and a water-soluble processing liquid having excellent silicon processability is obtained. be able to.
本発明の水溶性加工液が(A)グリコール類に加えて(B)カルボン酸を含有する形態においては、さらに、(C)水に溶解して塩基性を示す化合物(以下、「(C)塩基性化合物」という。)が含有されることが好ましい。(C)塩基性化合物としては、例えば、アルカリ金属元素を含有する化合物、アルカノールアミン、アルキルアミン及びアンモニア等が挙げられ、これらは、1種単独であるいは2種以上を組み合わせて用いることができる。この中でも、アルカリ金属元素を含有する化合物を用いることが好ましい。アルカリ金属元素を含有する化合物としては、水酸化ナトリウム、水酸化カリウム、炭酸ナトリウム、炭酸カリウム、炭酸水素ナトリウム及び炭酸水素カリウム等を挙げることができ、特に水酸化カリウムを用いることが好ましい。 (C) Compound that exhibits basic properties when dissolved in water In a form in which the water-soluble processing liquid of the present invention contains (B) a carboxylic acid in addition to (A) glycols, (C) it dissolves in water. It is preferable that a basic compound (hereinafter referred to as “(C) basic compound”) is contained. (C) As a basic compound, the compound containing an alkali metal element, an alkanolamine, an alkylamine, ammonia, etc. are mentioned, for example, These can be used individually by 1 type or in combination of 2 or more types. Among these, it is preferable to use a compound containing an alkali metal element. Examples of the compound containing an alkali metal element include sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium hydrogen carbonate and potassium hydrogen carbonate, and potassium hydroxide is particularly preferably used.
本発明の水溶性加工液において、上記(A)グリコール類及び水、並びに、任意に含まれる(B)カルボン酸及び(C)塩基性化合物若しくは(D)塩の他に、(E)その他の成分が含まれていてもよい。例えば、加工材料に対して腐食、変色等の悪影響を及ぼさず、且つ、混合後の系の安定性に影響を及ぼさないような種々の添加剤を、加工性能に影響を及ぼさない範囲で添加することができる。例えば、粘度調整剤、pH調整剤、消泡剤、酸化防止剤等を添加することができる。粘度調整剤としては、公知の粘度調整剤を特に限定することなく用いることができるが、水に可溶なものが好ましい。また、pH調整剤としては、無機塩基(前記の水酸化ナトリウム、水酸化カリウム、アンモニア等)、有機塩基(前記のアルカノールアミン、アルキルアミン等)、無機酸(塩酸、硫酸等)、有機酸(前記のカルボン酸等)を用いることができる。消泡剤、酸化防止剤等については、公知のものを特に限定することなく用いることができるが、これらも水に可溶であることが好ましい。 (E) Other components In the water-soluble processing liquid of the present invention, in addition to the above (A) glycols and water, and optionally included (B) carboxylic acid and (C) basic compound or (D) salt, (E) Other components may be contained. For example, various additives that do not adversely affect the processed material such as corrosion and discoloration and do not affect the stability of the system after mixing are added within a range that does not affect the processing performance. be able to. For example, a viscosity adjusting agent, a pH adjusting agent, an antifoaming agent, an antioxidant and the like can be added. As the viscosity modifier, known viscosity modifiers can be used without particular limitation, but those that are soluble in water are preferred. Examples of pH adjusters include inorganic bases (such as sodium hydroxide, potassium hydroxide and ammonia), organic bases (such as alkanolamine and alkylamine), inorganic acids (hydrochloric acid, sulfuric acid, etc.), organic acids ( The above carboxylic acids and the like can be used. As the antifoaming agent, antioxidant and the like, known ones can be used without particular limitation, but these are also preferably soluble in water.
プロピレングリコール(PG、和光純薬社製プロピレングリコール)、ポリエチレングリコール200(PEG200、和光純薬社製ポリエチレングリコール200、平均分子量180~200)、ポリエチレングリコール300(PEG300、和光純薬社製ポリエチレングリコール300、平均分子量300)、水、クエン酸(和光純薬社製クエン酸)、コハク酸(和光純薬社製コハク酸)及び水酸化カリウム(和光純薬社製水酸化カリウム)について、表1で示される組成となるように混合し、加工液を作製した。また、各加工液について、25℃粘度及びpHを測定した。尚、表1中の粘度は株式会社東京計器製B型回転粘度計(回転数60rpm)を用いて測定した。 (Preparation of water-soluble machining fluid for fixed abrasive wire saws)
Propylene glycol (PG, propylene glycol manufactured by Wako Pure Chemical Industries), polyethylene glycol 200 (PEG 200, polyethylene glycol 200 manufactured by Wako Pure Chemical Industries, average molecular weight 180-200), polyethylene glycol 300 (PEG 300, polyethylene glycol 300 manufactured by Wako Pure Chemical Industries, Ltd.) , Average molecular weight 300), water, citric acid (citric acid manufactured by Wako Pure Chemical Industries, Ltd.), succinic acid (succinic acid manufactured by Wako Pure Chemical Industries, Ltd.) and potassium hydroxide (potassium hydroxide manufactured by Wako Pure Chemical Industries, Ltd.) The processing liquid was prepared by mixing so as to have the composition shown. Moreover, about each process liquid, 25 degreeC viscosity and pH were measured. The viscosities in Table 1 were measured using a B-type rotational viscometer (rotation speed: 60 rpm) manufactured by Tokyo Keiki Co., Ltd.
被切断材として、25mm角の多結晶シリコンインゴットを用いた。また、固定砥粒ワイヤソーとしては、シングルワイヤソー型切断機(東鋼機械製作所製)を用いた。当該マルチ切断機の運転条件は、表2に表される条件とした。 (Evaluation of performance: cutting of polycrystalline silicon)
As a material to be cut, a 25 mm square polycrystalline silicon ingot was used. Moreover, as the fixed abrasive wire saw, a single wire saw type cutting machine (manufactured by Toko Machinery Co., Ltd.) was used. The operating conditions of the multi-cutting machine were the conditions shown in Table 2.
結果を表3に示す。 The material to be cut was processed using the multi-cutting machine. Specifically, as shown in FIG. 1, 10 grooves are formed in the material to be cut by the working fluid according to Examples 1 to 5, Comparative Examples 1 and 2 or Reference Examples 1 and 2, and the single wire saw cutting machine. The total depth of cut in the 10 grooves was used as an evaluation index. The working fluid was discharged toward the wire before and after the cut portion of the material to be cut.
The results are shown in Table 3.
比較例1、2については、ワイヤが破断又は十分な切り込み深さが得られず、シリコン加工性が十分でなかった。また、比較例1、2については、Si混入後においても、加工液粘度は適正範囲外のままであった。
一方、参考例1については、十分な切り込み深さが得られたものの、加工液pHを7.8と高くしたことにより、シリコン混入後、加工液とシリコンとの反応が生じ、液安定性が低下して、粘度が適切な範囲から外れる結果となった。また、参考例2については、シリコン混入後においても、適切な粘度を維持でき、液安定性が得られたものの、加工液pHを4.3と低くしたことにより、十分な切り込み深さが得られず、加工後ワイヤが破断した。これより、加工液粘度の他、加工液pHについても、シリコン加工性の維持に重要な因子となることが分かった。 As shown in Table 3, all of Examples 1 to 5 according to the present invention had a large depth of cut, good cutting ability, and excellent silicon processability. Moreover, even after silicon mixing, an appropriate viscosity could be maintained, a decrease in liquid life was suppressed, and silicon processability could be improved.
In Comparative Examples 1 and 2, the wire was not broken or sufficient cutting depth was not obtained, and the silicon processability was not sufficient. In Comparative Examples 1 and 2, the working fluid viscosity remained outside the proper range even after Si was mixed.
On the other hand, for Reference Example 1, although a sufficient depth of cut was obtained, the reaction between the processing liquid and silicon occurred after mixing with silicon by increasing the processing liquid pH to 7.8. As a result, the viscosity deviated from the appropriate range. In Reference Example 2, an appropriate viscosity could be maintained even after mixing with silicon, and liquid stability was obtained, but a sufficient depth of cut was obtained by reducing the processing liquid pH to 4.3. The wire broke after processing. From this, it was found that the processing fluid pH as well as the processing fluid viscosity is an important factor for maintaining the silicon processability.
Claims (6)
- (A)グリコール類及び水を含有し、25℃における粘度が3mPa・s以上50mPa・s以下である、固定砥粒ワイヤソー用水溶性加工液。 (A) A water-soluble processing liquid for a fixed abrasive wire saw, which contains glycols and water and has a viscosity at 25 ° C. of 3 mPa · s to 50 mPa · s.
- pHが5.0以上7.5以下に調整されてなる、請求の範囲第1項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 pH is adjusted to 5.0 or more and 7.5 or less.
- さらに、(B)カルボン酸と(C)水に溶解して塩基性を示す化合物とを含有してなる、請求の範囲第1項又は第2項に記載の固定砥粒ワイヤソー用水溶性加工液。 Furthermore, the water-soluble processing liquid for fixed-abrasive wire saws of Claim 1 or 2 formed by containing (B) carboxylic acid and (C) the compound which melt | dissolves in water and shows basicity.
- 前記(B)カルボン酸の炭素数が7以下である、請求の範囲第3項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 3, wherein the carboxylic acid (B) has 7 or less carbon atoms.
- 前記(A)グリコール類と、前記(B)カルボン酸と、前記(C)水に溶解して塩基性を示す化合物と、の合計を100質量%として、前記(A)グリコール類が5質量%以上95質量%以下、前記(B)カルボン酸が0.01質量%以上60質量%以下、前記(C)水に溶解して塩基性を示す化合物が0.01質量%以上60質量%以下含有されるとともに、前記(B)カルボン酸と前記(C)水に溶解して塩基性を示す化合物とが合計で、0.02質量%以上60質量%以下含有され、残部が水である請求の範囲第3項又は第4項に記載の固定砥粒ワイヤソー用水溶性加工液。 The total amount of the (A) glycols, the (B) carboxylic acid, and the (C) compound showing basicity when dissolved in water is 100% by mass, and the (A) glycols is 5% by mass. 95% by mass or less, (B) 0.01% by mass or more and 60% by mass or less of the carboxylic acid, and (C) 0.01% by mass or more and 60% by mass or less of the compound which shows basicity when dissolved in water. And (B) the carboxylic acid and (C) the compound that is dissolved in water and exhibits basicity is contained in a total amount of 0.02% by mass or more and 60% by mass or less, and the balance is water. The water-soluble machining liquid for a fixed abrasive wire saw according to the item 3 or 4 in the range.
- シリコン材の切断加工に用いられる、請求の範囲第1項~第5項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 5, which is used for cutting a silicon material.
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