WO2018169008A1 - Liquide de traitement pour matériau fragile - Google Patents

Liquide de traitement pour matériau fragile Download PDF

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Publication number
WO2018169008A1
WO2018169008A1 PCT/JP2018/010249 JP2018010249W WO2018169008A1 WO 2018169008 A1 WO2018169008 A1 WO 2018169008A1 JP 2018010249 W JP2018010249 W JP 2018010249W WO 2018169008 A1 WO2018169008 A1 WO 2018169008A1
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WO
WIPO (PCT)
Prior art keywords
mass
component
processing liquid
brittle material
material processing
Prior art date
Application number
PCT/JP2018/010249
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English (en)
Japanese (ja)
Inventor
友彦 北村
Original Assignee
出光興産株式会社
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 出光興産株式会社 filed Critical 出光興産株式会社
Priority to CN201880018018.0A priority Critical patent/CN110382673B/zh
Publication of WO2018169008A1 publication Critical patent/WO2018169008A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B27/00—Other grinding machines or devices
    • B24B27/06—Grinders for cutting-off
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B55/00—Safety devices for grinding or polishing machines; Accessories fitted to grinding or polishing machines for keeping tools or parts of the machine in good working condition
    • B24B55/02—Equipment for cooling the grinding surfaces, e.g. devices for feeding coolant
    • 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
    • B28D5/04—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor by tools other than rotary type, e.g. reciprocating tools
    • 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
    • C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
    • C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
    • C10M105/10—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M105/14—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms polyhydroxy
    • 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
    • C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
    • C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
    • C10M105/18—Ethers, e.g. epoxides
    • 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
    • C10M129/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
    • C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
    • C10M129/04—Hydroxy compounds
    • C10M129/06—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M129/08—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms containing at least 2 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
    • C10M145/00—Lubricating compositions characterised by the additive being a macromolecular compound containing oxygen
    • C10M145/18—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M145/24—Polyethers
    • C10M145/26—Polyoxyalkylenes
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting

Definitions

  • the present invention relates to a brittle material working fluid and a method for producing the brittle material working fluid.
  • wire saw processing is generally used for cutting silicon ingots from the viewpoint of processing accuracy and productivity.
  • Wire saw processing is also used for processing materials such as ceramics, quartz, sapphire, and glass.
  • a free abrasive grain method that performs processing while supplying free abrasive grains to a sliding portion between the wire and a workpiece, and a wire in which abrasive grains are fixed to the surface of the wire in advance
  • a fixed abrasive method in which processing is performed using
  • the fixed abrasive method is often used for the reason that the yield can be improved.
  • the processing fluid used in the above-mentioned applications includes an aqueous processing fluid containing mineral oil, animal and vegetable oils, synthetic oil, etc. as a main component and a compound having a surface active ability to provide water-soluble processing. Liquid. In recent years, a working fluid imparted with water solubility has been used from the viewpoint of safety during work and environmental problems.
  • Patent Document 1 discloses a water-soluble machining liquid composition for a fixed abrasive wire saw that is used for cutting work materials other than rare earth magnets, and contains glycols.
  • a liquid composition is disclosed.
  • Patent Document 2 discloses a water-soluble working fluid composition for fixed abrasive wire saws used for cutting rare earth magnets, which includes glycols, carboxylic acid, a compound that dissolves in water and exhibits basicity, water Are contained in a specific content (however, the total of these components is 100 parts by weight), and a water-soluble working liquid composition for a fixed abrasive wire saw is disclosed.
  • Patent Document 3 discloses an aqueous cutting fluid characterized by containing 0.01 to 20% by mass of acetylene glycol and / or its alkylene oxide adduct.
  • a multi-wire saw apparatus is used to cut out a plurality of silicon wafers from the above-described silicon ingot at a time.
  • the multi-wire saw device one wire is wound around each groove on two or more guide rollers having a plurality of grooves carved at a constant interval, and each wire is held in parallel with a constant tension.
  • each guide roller is rotated and the wire is run in one or both directions while the machining liquid discharged from the nozzle or the like is adhered to the wire, and the silicon ingot is pushed onto the wire to which the machining liquid is adhered. Cutting is applied.
  • the processing liquid used for the wire saw processing is put into a tank provided in the wire saw device, supplied from the tank to the processing chamber nozzle by a pump provided in the wire saw device, and discharged from the nozzle.
  • the machining fluid discharged from the nozzle is supplied aiming at the machining gap (gap between the wire and the silicon ingot), used for lubrication of the machining gap, etc., and then returns to the tank again.
  • the machining fluid circulates in the wire saw device.
  • the processing liquid may be violently scattered due to high-speed rotation of the guide roller accompanying the increase in the wire speed, which leads to bubbling of the processing liquid.
  • the processing liquid may flow down to a tank below the wire saw device, and the processing liquid in the tank may be foamed violently and overflow from the tank.
  • the problem that fine chips generated during the cutting process promote foaming of the processing liquid, and wire saws and cut wafers are significantly contaminated by the chips, and the load for cleaning them is large. There was a problem of becoming.
  • the present invention has been made in view of the above problems, and an object of the present invention is to provide a brittle material processing liquid that is excellent in antifoaming properties and contamination suppression effects.
  • the present inventors have one or more selected from the group consisting of water, acetylene glycol satisfying a specific condition and an alkylene oxide adduct of acetylene glycol, and no acetylene group satisfying the specific condition. It has been found that a brittle material processing liquid that contains a nonionic surfactant and the content ratio of these components satisfies a specific range can solve the above-mentioned problems.
  • Each embodiment of the present invention has been completed based on such knowledge. That is, according to each embodiment of the present invention, the following [1] or [2] is provided.
  • the content of the component (A) is 0.010% by mass or more and 0.200% by mass or less based on 100% by mass of the total amount of the brittle material processing liquid
  • the content of the component (B) is 0.020% by mass or more and 0.500% by mass or less based on 100% by mass of the total amount of the brittle material processing liquid
  • the content of the component (A) and the component (B) A brittle material processing liquid in which the ratio [A / B] is 0.05 to 2.00 in terms of
  • a method for producing a brittle material processing liquid The content of the component (A) is 0.010% by mass or more and 0.200% by mass or less based on 100% by mass of the total amount of the brittle material processing liquid, The content of the component (B) is 0.020% by mass or more and 0.500% by mass or less based on 100% by mass of the total amount of the brittle material processing liquid, and the content of the component (A) and the component (B) The method for producing a brittle material processing liquid according to the
  • the brittle material processing fluid contains water, the following component (A) and component (B), and contains component (A).
  • the amount is 0.010% by mass or more and 0.200% by mass or less based on the total amount of 100% by mass of the brittle material processing liquid
  • Content of component (B) is 0.020% by mass or more and 0.500% by mass or less based on 100% by mass of the total amount of brittle material processing liquid
  • content of component (A) and component (B) The ratio [A / B] is 0.05 to 2.00 in terms of mass ratio.
  • a nonionic surfactant that is an ethylene oxide adduct having an ethylene oxide addition mole number of 5 or more in the molecular structure and does not have an acetylene group. It is inferior in antifoaming property and pollution control effect.
  • the “HLB value” means a value of HLB (Hydrophilic-Lipophilic Balance) calculated by the Griffin method.
  • the lower limit value and upper limit value which were described in steps can be combined independently, respectively.
  • the description of the lower limit value “preferably 10 or more, more preferably 20 or more, more preferably 30 or more” and “preferably 90 or less, more preferably 80 or less, more preferably 60 or less”. Therefore, the preferable range can be set to “10 or more and 60 or less” by combining “preferable lower limit value (10)” and “more preferable upper limit value (60)”.
  • the “more preferable lower limit value (30)” and the “preferable upper limit value (90)” can be combined to set the preferable range to “30 or more and 90 or less”.
  • preferably 10 to 90, more preferably 20 to 80, still more preferably 30 to 60 can be used as “10 to 60”.
  • 10 to 90 is simply described as a preferable numerical range, it represents a range of 10 to 90.
  • each component contained in the processing liquid will be described.
  • Component (A) is at least one selected from the group consisting of acetylene glycol having an HLB value of 4 to 12 and an alkylene oxide adduct of acetylene glycol having an HLB value of 4 to 12.
  • HLB value of the component (A) is less than 4, the solubility of the component (A) in water is poor. Moreover, the defoaming property of the said processing liquid and the contamination inhibitory effect will deteriorate that the HLB value of the said component (A) is more than 12.
  • the HLB value is preferably 4 or more and 10 or less, more preferably 4 or more and 9 or less, and still more preferably 4 or more and 8 or less.
  • alkylene oxide hereinafter also simply referred to as“ AO ”) adduct refers to not only a compound to which a single alkylene oxide is added, but also a plurality of alkylene oxides, In addition, a compound to which a polyalkylene oxide is added is also included.
  • EO ethylene oxide
  • PO propylene oxide
  • Examples of the acetylene glycol include compounds represented by the following general formula (1).
  • R 1 to R 4 each independently represents an alkyl group having 1 to 5 carbon atoms.
  • Specific examples of the alkyl group having 1 to 5 carbon atoms that can be taken by R 1 to R 4 are methyl group, ethyl group, n-propyl group, isopropyl group, n-butyl group, isobutyl group, sec-butyl.
  • R 1 and R 3 are preferably an isobutyl group or a 3-methylbutyl group.
  • R 2 and R 4 are preferably methyl groups.
  • the compound represented by the general formula (1) is preferably a compound having a structure in which R 1 and R 3 are the same as each other or a structure in which R 2 and R 4 are the same as each other, more preferably Is a compound having a structure in which R 1 and R 3 are identical to each other, and R 2 and R 4 are identical to each other.
  • the alkylene oxide adduct of acetylene glycol is preferably an alkylene oxide adduct of the compound represented by the general formula (1) in which AO is added to each hydroxyl group of the compound represented by the general formula (1). More preferably, an alkylene oxide adduct of the compound represented by the general formula (1) to which EO and / or PO is added, and more preferably an alkylene of the compound represented by the general formula (1) to which EO is added. It is an oxide adduct.
  • the suitable aspect of the acetylene glycol which forms the alkylene oxide adduct of the said acetylene glycol is the same as the suitable aspect of the compound represented by the aforementioned general formula (1).
  • the structure derived from EO for example, ethyleneoxy group or poly (oxyethylene) structure
  • the structure derived from PO for example, propyleneoxy group or poly (oxypropylene) structure
  • the structures may be bonded to each other in a random type, may be bonded in a block type, and preferably is a block type.
  • Component (A) includes 2,5,8,11-tetramethyl-6-dodecin-5,8-diol, 5,8-dimethyl-6-dodecin-5,8-diol, 2,4,7, 9-tetramethyl-5-dodecin-4,7-diol, 8-hexadecin-7,10-diol, 7-tetradecine-6,9-diol, 2,3,6,7-tetramethyl-4-octyne 3,6-diol, 3,6-diethyl-4-octyne-3,6-diol, 2,5-dimethyl-3-hexyne-2,5-diol, 2,4,7,9-tetramethyl-5
  • An acetylene glycol represented by the general formula (1) such as decyne-4,7-diol and 3,6-dimethyl-4-octyne-3,6-diol; and an acetylene represented by the
  • alkylene oxide examples include EO and / or PO. Of these, 2,5,8,11-tetramethyl-6-dodecin-5,8-diol, 5,8-dimethyl-6-dodecin-5,8-diol, 2,4,7, 9-tetramethyl-5-dodecin-4,7-diol, 8-hexadecin-7,10-diol, 7-tetradecine-6,9-diol, 2,3,6,7-tetramethyl-4-octyne 3,6-diol, 3,6-diethyl-4-octyne-3,6-diol, 2,5-dimethyl-3-hexyne-2,5-diol, 2,4,7,9-tetramethyl-5
  • One or more alkylene oxide adducts selected from the group consisting of decyne-4,7-diol and 3,6-dimethyl-4-octyne-3,6-d
  • Content of a component (A) is 0.010 mass% or more and 0.200 mass% or less on the basis of 100 mass% of the whole quantity of the said processing liquid.
  • the content of the component (A) is preferably 0.015% by mass or more, more preferably 0.020% by mass or more, and still more preferably 0.05% by mass or more based on the total amount of the processing liquid of 100% by mass. It is 040% by mass or more, and preferably 0.150% by mass or less, more preferably 0.100% by mass or less, and still more preferably 0.070% by mass or less.
  • Component (B) is an ethylene oxide adduct having an HLB value of 6 or more, an added mole number of ethylene oxide in the molecular structure of 5 or more, and a nonionic surfactant having no acetylene group. .
  • the processing liquid contains the component (B) so as to satisfy the content ratio [A / B], so that the processing liquid is excellent in antifoaming property and contamination suppression effect.
  • the number of moles of EO added to the component (B) is less than 5, the effect of suppressing contamination of the processing liquid is deteriorated.
  • the EO addition mole number is preferably 6 or more, more preferably 7 or more, still more preferably 10 or more, and still more preferably 20 or more.
  • the upper limit of the EO addition mole number is not particularly limited, but is preferably 40 or less, more preferably 35 or less, and still more preferably 30 or less, from the viewpoint of obtaining a better defoaming property and contamination suppressing effect of the processing liquid. It is.
  • the solubility to the water of a component (B) is inferior that the HLB value of the said component (B) is less than 6. From such a viewpoint, the HLB value is preferably 7 or more, more preferably 8 or more.
  • the upper limit of the HLB value of the component (B) is not particularly limited, but is preferably 20 or less, more preferably 15 or less, and still more preferably from the viewpoint of further improving the antifoaming property and the contamination suppressing effect of the processing liquid. 10 or less.
  • component (B) examples include a copolymer of ethylene oxide and alkylene oxide, an ester derivative of polyethylene glycol, and an ether derivative of polyethylene glycol.
  • Component (B) is preferably selected from the group consisting of block copolymers of EO and AO (ie, polyoxyethylene polyoxyalkylene block copolymers), polyoxyethylene alkyl ethers and polyoxyethylene alkylene alkyl ethers.
  • block copolymers of EO and AO ie, polyoxyethylene polyoxyalkylene block copolymers
  • polyoxyethylene alkyl ethers ie, polyoxyethylene alkyl ethers
  • polyoxyethylene alkylene alkyl ethers ie, polyoxyethylene alkylene alkyl ethers
  • One or more types more preferably a block copolymer of EO and AO.
  • the copolymer of EO and AO is a copolymer of EO and AO, which will be described later.
  • the addition mode of EO and AO may be either random addition or block addition, and random addition and block addition. Addition may be mixed, but a block-added copolymer is preferable, and a pluronic-type copolymer is more preferable.
  • the AO include alkylene oxides having 3 or 4 carbon atoms, such as propylene oxide (PO), oxetane, 1,2-butylene oxide, 2,3-butylene oxide, 1,3-butylene oxide, and tetrahydrofuran. Can be mentioned.
  • the copolymer of EO and AO is more preferably a copolymer of EO and PO, still more preferably a block copolymer of EO and PO, and still more preferably a triblock of EO and PO.
  • the number average molecular weight (Mn) of the structural portion derived from AO is preferably 500 or more, more preferably 1,000 or more, and further preferably 1,500 or more. And preferably 5,000 or less, more preferably 3,000 or less, and still more preferably 2,000 or less.
  • the polyoxyethylene alkyl ether is preferably an EO adduct of a higher alcohol.
  • the higher alcohol include aliphatic alcohols having 6 to 24 carbon atoms.
  • the carbon number of the higher alcohol is preferably 8 or more, more preferably 10 or more, still more preferably 12 or more, and is preferably 20 or less, more preferably 18 or less, and still more preferably 16 or less.
  • the aliphatic alcohol is preferably a primary alcohol or a secondary alcohol, and more preferably a primary alcohol. Further, it may be linear, branched or cyclic.
  • aliphatic alcohol examples include octanol, 2-ethylhexanol, nonanol, decanol, undecyl alcohol, lauryl alcohol, tridecyl alcohol, isotridecyl alcohol, myristyl alcohol, pentadecyl alcohol, palmityl alcohol, heptadecanol.
  • Saturated fatty alcohols such as stearyl alcohol, isostearyl alcohol, nonadecyl alcohol, eicosanol; octenyl alcohol, decenyl alcohol, dodecenyl alcohol, tridecenyl alcohol, tetradecenyl alcohol, palmitoleyl alcohol, Unsaturated aliphatic alcohols such as oleyl alcohol, gadrel alcohol, linoleyl alcohol; ethyl cyclohexyl alcohol, propyl cyclohexyl Alcohol, octylcyclohexyl alcohol, nonylcyclohexyl alcohol, cyclic aliphatic alcohols, such as adamantyl alcohol.
  • Unsaturated aliphatic alcohols such as oleyl alcohol, gadrel alcohol, linoleyl alcohol; ethyl cyclohexyl alcohol, propyl cyclohexyl Alcohol, octy
  • the polyoxyethylene alkylene alkyl ether is preferably an EO and AO adduct of a higher alcohol.
  • the higher alcohol is the same as that described for the polyoxyethylene alkyl ether.
  • AO other than EO include alkylene oxides having 3 or 4 carbon atoms, such as 1,2-propylene oxide, 1,3-propylene oxide, 1,2-butylene oxide, and 2,3-butylene oxide. 1,3-butylene oxide and tetrahydrofuran.
  • the polyoxyethylene alkyl ether and the polyoxyethylene alkylene alkyl ether can be synthesized by adding EO and / or AO to the higher alcohol, but the addition of EO and AO to the higher alcohol is known.
  • a component (B) may be used individually by 1 type, and may be used in combination of 2 or more type.
  • Content of a component (B) is 0.020 mass% or more and 0.500 mass% or less on the basis of 100 mass% of the whole quantity of the said processing liquid.
  • the content of the component (B) is preferably 0.030% by mass or more, more preferably 0.035% by mass or more, and still more preferably 0.00% by mass, based on the total amount of the machining fluid of 100% by mass. It is 060% by mass or more, and preferably 0.200% by mass or less, more preferably 0.175% by mass or less, and further preferably 0.120% by mass or less.
  • content ratio [A / B] of a component (A) and a component (B) in the said process liquid is 0.05 or more and 2.00 or less by mass ratio.
  • the content ratio is less than 0.05, the antifoaming property and the contamination suppressing effect of the processing liquid are deteriorated.
  • the content ratio exceeds 2.00, the antifoaming property and the contamination suppressing effect of the processing liquid are deteriorated.
  • the content ratio [A / B] is preferably 0.10 or more, more preferably 0.15 or more, still more preferably 0.20 or more, and preferably by mass ratio. 0.90 or less, more preferably 0.80 or less, and still more preferably 0.75 or less.
  • the water is not particularly limited, and purified water such as distilled water and ion exchange water (deionized water); tap water; industrial water; and the like can be used, preferably purified water, more preferably ion exchange water ( Deionized water).
  • purified water such as distilled water and ion exchange water (deionized water); tap water; industrial water; and the like
  • purified water more preferably ion exchange water ( Deionized water).
  • the water content is based on the total amount of the machining fluid of 100% by mass, Preferably it is 50.000 mass% or more, More preferably, it is 75.000 mass% or more, More preferably, it is 95.000 mass% or more, More preferably, it is 96.000 mass% or more, More preferably, it is 96.500 mass% or more It is. And from a viewpoint of ensuring the amount of active ingredients in the processing fluid, it is preferably 99.970 mass% or less, more preferably 99.930 mass% or less, and still more preferably 99.900 mass% or less.
  • the “active ingredient” refers to all ingredients excluding water from the processing liquid.
  • the working fluid is composed of a polyhydric alcohol and a polyhydric alcohol derivative as the component (C) in addition to the aforementioned component (A), component (B) and water. It is preferable to contain at least one alcohol component selected from the group.
  • component (C) examples include ethylene glycol, propylene glycol, 1,4-butanediol, hexamethylene glycol, neopentyl glycol, diethylene glycol, triethylene glycol, dipropylene glycol, tripropylene glycol, glycerin, and ester derivatives thereof. , These ether derivatives; polyethylene glycol, polypropylene glycol and the like.
  • Component (C) is preferably one or more selected from the group consisting of ethylene glycol, propylene glycol, dipropylene glycol, diethylene glycol, polyethylene glycol, glycerin, their ester derivatives and their ether derivatives, more preferably ethylene glycol , One or more selected from the group consisting of diethylene glycol, polyethylene glycol, glycerin, their ester derivatives and their ether derivatives, more preferably selected from the group consisting of diethylene glycol, glycerin, their ester derivatives, and their ether derivatives One or more.
  • a component (C) may be used individually by 1 type, and may be used in combination of 2 or more type.
  • the content of the component (C) is preferably 0.010 based on the total amount of the processing liquid of 100% by mass from the viewpoint of improving water retention in the processing liquid.
  • % By mass, more preferably 0.030% by mass or more, more preferably 0.060% by mass or more, still more preferably 1.000% by mass or more, from the viewpoint of obtaining an effect commensurate with the content, Preferably it is 5.000 mass% or less, More preferably, it is 4.000 mass% or less, More preferably, it is 3.500 mass% or less, More preferably, it is 1.500 mass% or less.
  • the content ratio [C / A] of the component (A) and the component (C) in the working fluid is preferably 1.00 or more by mass ratio.
  • it is 1.20 or more, more preferably 1.40 or more, still more preferably 5.00 or more, and preferably 300 or less, more preferably 250 or less, still more preferably 230 or less, and even more preferably 10 0.0 or less.
  • the content ratio [C / B] of the component (B) and the component (C) in the working fluid is preferably 0.20 or more by mass ratio.
  • it is 0.30 or more, more preferably 0.50 or more, still more preferably 5.00 or more, and preferably 100 or less, more preferably 90.0 or less, still more preferably 87.0 or less, more More preferably, it is 10.0 or less.
  • the processing fluid further contains other additives as long as the object of the present invention is not impaired. You may contain.
  • Other additives include surfactants other than components (A) and (B), pH adjusters, antifoaming agents, metal deactivators, bactericides / preservatives, rust inhibitors, antioxidants, and the like. It is done. These additives may be used alone or in combination of two or more. Moreover, in these additives, 1 or more types chosen from the group which consists of surfactant other than a component (A) and (B) and a pH adjuster are preferable.
  • surfactants other than components (A) and (B) include anionic surfactants, cationic surfactants, nonionic surfactants other than components (A) and (B), and amphoteric surfactants. It is done.
  • anionic surfactant include alkyl benzene sulfonate and alpha olefin sulfonate.
  • cationic surfactant include quaternary ammonium salts such as alkyltrimethylammonium salts, dialkyldimethylammonium salts, and alkyldimethylbenzylammonium salts.
  • Nonionic surfactants other than components (A) and (B) include, for example, acetylene glycol having an HLB value of less than 4 and greater than 12, an alkylene oxide adduct of acetylene glycol having an HLB value of less than 4 and greater than 12, and molecules An ethylene oxide adduct in which the number of moles of ethylene oxide in the structure is less than 5, and a nonionic surfactant having no acetylene group, and an ethylene oxide adduct having an HLB of less than 6.
  • Nonionic surfactants having no acetylene group for example, polyoxyethylene alkyl ethers other than components (A) and (B), ethers such as polyoxyethylene alkylphenyl ethers other than components (A) and (B), Amides such as fatty acid alkanolamides).
  • amphoteric surfactants include alkyl betaines as betaines.
  • nonionic surfactants such as ethers other than components (A) and (B), more preferably acetylene glycol having an HLB value of less than 4 and more than 12, and an HLB value of less than 4 and more than 12
  • the pH adjuster is mainly used to adjust the pH of the processing liquid.
  • the pH adjuster include various acid components and base components, and the pH of the processing liquid can be appropriately adjusted by adjusting the content ratio of these components.
  • the acid component and the base component can react with each other to form a salt. Therefore, when an acid component and a base component are used as a pH adjuster, when a reaction product of the acid component and the base component exists in the processing liquid, as described above, the reaction product of the acid component and the base component is contained.
  • Each content of the acid component and the base component contributing to the reaction calculated from the amount can also be calculated. Moreover, it can replace with the said reaction material in that case, and can be considered that the said acid component and base component before reaction are contained.
  • Examples of the acid component used as a pH adjuster include various fatty acids such as lauric acid, stearic acid, oleic acid, linoleic acid, linolenic acid, neodecanoic acid, isononanoic acid, capric acid, and isostearic acid; acetic acid, malic acid, and citric acid.
  • fatty acids such as lauric acid, stearic acid, oleic acid, linoleic acid, linolenic acid, neodecanoic acid, isononanoic acid, capric acid, and isostearic acid
  • acetic acid malic acid, and citric acid
  • Examples thereof include carboxylic acids such as acids; polymer acids such as polyacrylic acid and salts thereof; and inorganic acids such as phosphoric acid.
  • fatty acids are preferable, fatty acids having 12 or less carbon atoms such as neodecanoic acid, isononanoic acid, capric acid, and dodecanedioic acid are more preferable, and a group consisting of neodecanoic acid, isononanoic acid, capric acid, and dodecanedioic acid. One or more selected are more preferable.
  • Examples of the base component used as a pH adjuster include monoethanolamine, diethanolamine, triethanolamine, monoisopropanolamine, diisopropanolamine, triisopropanolamine, tri-n-propanolamine, tri-n-butanolamine, Isobutanolamine, tri-tert-butanolamine, N-methylethanolamine, N-ethylethanolamine, N-butylethanolamine, N-cyclohexylethanolamine, N-methyldiethanolamine, N-ethyldiethanolamine, N-cyclohexyldiethanolamine, Alkanolamines such as N, N-dimethylethanolamine and N, N-diethylethanolamine; methylamine, dimethylamine, ethylamine , Diethylamine, propylamine, alkyl amines such as dipropylamine; and the ammonia.
  • tertiary amines are preferable, and at least one selected from the group consisting of triethanolamine, triisopropanolamine, N-methyldiethanolamine, and N-cyclohexyldiethanolamine is more preferable.
  • Examples of the antifoaming agent include silicone oil, fluorosilicone oil, and fluoroalkyl ether.
  • Examples of the metal deactivator include imidazoline, pyrimidine derivatives, thiadiazole, and benzotriazole.
  • Examples of the disinfectant / preservative include p-oxybenzoates (parabens), benzoic acid, salicylic acid, sorbic acid, dehydroacetic acid, p-toluenesulfonic acid and salts thereof, and phenoxyethanol.
  • Examples of the rust inhibitor include alkylbenzene sulfonate, dinonyl naphthalene sulfonate, alkenyl succinate, and polyhydric alcohol esters other than component (C).
  • Examples of the antioxidant include phenolic antioxidants and amine antioxidants.
  • the total content of other additives in the processing liquid is preferably 0.001% by mass or more, more preferably 0, based on the total amount of the processing liquid of 100% by mass. 0.002% by mass or more, more preferably 0.010% by mass or more, and preferably 0.200% by mass or less, more preferably 0.150% by mass or less, still more preferably 0.130% by mass or less, more More preferably, it is 0.100 mass% or less, More preferably, it is 0.050 mass% or less.
  • the ratio ((other additives) / A) between the amount of the other additives and the content of the component (A) in the processing liquid is preferably a mass ratio. 0.01 or more, more preferably 0.05 or more, still more preferably 0.10 or more, still more preferably 0.20 or more, and preferably 10.0 or less, more preferably 9.00 or less, further Preferably it is 5.00 or less, More preferably, it is 1.00 or less, More preferably, it is 0.50 or less.
  • the processing liquid contains other additives, water, component (A) and component (B), and if necessary, contained in the processing liquid
  • the total content of the component (C) is preferably 98.000% by mass or more, more preferably 99.000% by mass or more, and still more preferably 99.800% by mass or more, based on the total amount of the processing fluid of 100% by mass. , More preferably 99.900% by mass or more, and preferably 100% by mass or less, more preferably 99.999% by mass or less, still more preferably 99.998% by mass or less, and still more preferably 99.950. It is below mass%.
  • the total content (active ingredient amount) of (C) and other additives is preferably 0.030% by mass or more, more preferably 0.080% by mass or more, and still more preferably, based on the total amount of the processing liquid of 100% by mass. Is 0.100% by mass or more, and preferably 5.500% by mass or less, more preferably 3.500% by mass or less, further preferably 2.000% by mass or less, and still more preferably 1.000% by mass. Hereinafter, it is more preferably 0.500% by mass or less.
  • the pH of the working fluid is preferably 4 or more and 9 or less. It is preferable that the pH of the processing liquid is 4 or more because corrosion of the wire, processing apparatus, and the like can be suppressed. Moreover, it is preferable that the pH of the processing liquid is 9 or less because, for example, a large amount of hydrogen can be suppressed from chips when processing silicon or the like. From such a viewpoint, the pH of the processing liquid is more preferably 4 or more and 8 or less, and further preferably 5 or more and 8 or less.
  • the manufacturing method of the brittle material processing liquid is: At least with water, (A): one or more selected from the group consisting of an acetylene glycol having an HLB value of 4 to 12 and an alkylene oxide adduct of acetylene glycol having an HLB value of 4 to 12, and (B): nonionic surfactant having an HLB value of 6 or more, an ethylene oxide adduct having an addition mole number of ethylene oxide in the molecular structure of 5 or more, and having no acetylene group, A method for producing a brittle material processing liquid,
  • the content of the component (A) is 0.010% by mass or more and 0.200% by mass or less based on 100% by mass of the total amount of the brittle material processing liquid
  • the content of the component (B) is 0.020% by mass or more and 0.500% by mass or less based on 100% by mass of the total amount of the brittle material processing liquid, and the content of the component
  • component (A) and component (B) are blended sequentially or simultaneously with water.
  • the component (B) may be blended and the mixture may be blended in water.
  • water, a component (A), and a component (B) may be mix
  • the blending order, blending method and the like of each component to be blended are not particularly limited.
  • water, a component (A), a component (B), a component (C), and other additives are respectively the same as what was mentioned above in the column of a brittle material processing liquid, The suitable aspect is also the same. Therefore, the detailed description is abbreviate
  • the preferred blending amount of water, component (A), component (B), component (C), and other additives and the preferred blending ratio between the components are also listed in the column of brittle material processing liquid, respectively. Since it is the same as each content and each content ratio in the said process liquid mentioned above, the detailed description is abbreviate
  • the brittle material processing liquid can be suitably used when wire sawing a workpiece made of a brittle material such as a silicon ingot using the wire saw described above, preferably a fixed abrasive wire saw. That is, the processing liquid can be suitably used when processing a workpiece made of a brittle material using a wire.
  • the brittle material include crystalline silicon, sapphire, gallium nitride, silicon carbide, neodymium magnet, zirconia, graphite, niobic acid, tantalate, quartz and glass.
  • the processing liquid can be more suitably used when processing crystalline silicon, sapphire, silicon carbide, neodymium magnet, crystal, or glass from the viewpoint of the contamination suppression effect, and processes crystalline silicon, sapphire, or silicon carbide. In this case, it can be used more suitably.
  • the brittle material processing liquid may be obtained, for example, by diluting a concentrated liquid obtained by reducing the amount of water in the processing liquid and concentrating it two to 700 times with water. That is, when the above-described processing is performed, the concentrated liquid of the processing liquid or the composition or stock solution for the processing liquid having the same composition as the concentrated liquid (hereinafter also simply referred to as “concentrated liquid”) is doubled with water. It can be diluted to 700 times or less and used as the brittle material processing liquid. Moreover, the said processing liquid can be concentrated so that it may become the concentrate shown below, and it can also be used as an aspect suitable for storage, transportation, etc.
  • the “concentrated liquid” is not limited to a concentrated liquid obtained by reducing the amount of water from the processing liquid as described above, but is prepared on the assumption that the processing liquid is diluted with water. Of the prepared composition or stock solution.
  • the concentrate for example, water and, (A): one or more selected from the group consisting of an acetylene glycol having an HLB value of 4 to 12 and an alkylene oxide adduct of acetylene glycol having an HLB value of 4 to 12, and (B): nonionic surfactant having an HLB value of 6 or more, an ethylene oxide adduct having an addition mole number of ethylene oxide in the molecular structure of 5 or more, and having no acetylene group, Including
  • the content of the component (A) is preferably 0.200% by mass or more, and preferably 30.000% by mass or less, based on 100% by mass of the total concentrated liquid of the brittle material processing liquid.
  • the content of the component (B) is preferably 0.300% by mass or more, and preferably 90.000% by mass or less, more preferably 75.000% by mass, based on 100% by mass of the total concentrated liquid of the brittle material processing liquid. %, And the content ratio [A / B] of the component (A) and the component (B) is 0.05 to 2.00 in terms of mass ratio. It is done.
  • the concentrate further contains component (C), preferably 5.000% by mass or more, more preferably 10.000% by mass or more, and preferably 95.000% by mass based on the total amount of the concentrate 100% by mass. % Or less.
  • the concentrated solution contains other additives in addition to water, component (A), component (B), and component (C) contained as necessary, as long as the object of the present invention is not impaired. It may be.
  • the content of water in the concentrated solution is preferably 0.100% by mass or more and less than 50000% by mass based on the total amount of the concentrated solution of 100% by mass.
  • water, a component (A), a component (B), a component (C), and other additives are respectively the same as what was mentioned above in the column of a brittle material processing liquid,
  • the suitable Since the aspect is also the same, detailed description thereof is omitted.
  • a component (A), a component (B), a component (C), and another additive The said concentrate is 2 with water.
  • each of the components is contained so as to satisfy the range of suitable contents of each component described above in the column of brittle material processing liquid.
  • the above-mentioned working fluids described above in the column of brittle material working fluid are also respectively used for suitable content ratios among water, component (A), component (B), component (C), and other additives. It is the same as the content ratio between each component in the inside, and the detailed description thereof is omitted.
  • the concentrated liquid can be used as a composition or a stock solution for preparing the processing liquid by mainly diluting with water. That is, as a method of using a concentrated liquid of brittle material processing liquid according to an embodiment of the present invention, for example, water and, (A): one or more selected from the group consisting of an acetylene glycol having an HLB value of 4 to 12 and an alkylene oxide adduct of acetylene glycol having an HLB value of 4 to 12, and (B): nonionic surfactant having an HLB value of 6 or more, an ethylene oxide adduct having an addition mole number of ethylene oxide in the molecular structure of 5 or more, and having no acetylene group, Including
  • the content of the component (A) is preferably 0.200% by mass or more, and preferably 30.000% by mass or less based on 100% by mass of the total amount of the concentrate.
  • the content of component (B) is preferably 0.300% by mass or more, and preferably 90.000% by mass or less, more preferably 75.000% by mass or less, based on 100% by mass of the total concentrate.
  • the content ratio [A / B] of a component (A) and a component (B) is 0.05 or more and 2.00 or less by mass ratio,
  • the concentrated liquid of a brittle material processing liquid The content of the component (A) is 0.010% by mass or more and 0.200% by mass or less based on 100% by mass of the total amount of the brittle material processing liquid,
  • the content of the component (B) is 0.020% by mass or more and 0.500% by mass or less based on 100% by mass of the total amount of the brittle material processing liquid, and the content of the component (A) and the component (B)
  • the brittle material working fluid is prepared by diluting with water so that the ratio [A / B] is 0.05 or more and 2.00 or less by mass ratio, This is a method for
  • the concentrated liquid and the processing liquid used in the method of use may each independently contain one or more selected from the group consisting of the component (C) and other additives as necessary.
  • water, a component (A), a component (B), a component (C), and other additives are respectively the same as what was mentioned above in the column of a brittle material processing liquid, The suitable aspect is also the same. Therefore, the detailed description is abbreviate
  • a component (A), a component (B), a component (C), and other additives in the concentrate used by the said usage method the content ratio between each component, and those suitable ranges Since each is the same as each content and each content ratio in the concentrated liquid described above, detailed description thereof is omitted.
  • the content of water, the component (A), the component (B), the component (C), and other additives in the working fluid used in the method of use, the content ratio between the components, and their preferred ranges Are the same as the respective contents and ratios described above in the column of brittle material processing liquid, and detailed description thereof will be omitted.
  • the concentrated liquid and the processing liquid are the same as the above-described concentrated liquid and the processing liquid, respectively, and the preferred embodiments including the respective components contained therein are also the same. Omitted.
  • water, the component (A), the component (B), the component (C), and other additives contained in the concentrated liquid and the processing liquid are the same as those described above in the column of the brittle material processing liquid. Since the preferred embodiment is the same, detailed description thereof is omitted.
  • the suitable content of each component of water, a component (A), a component (B), a component (C), and other additives and the content ratio between each component are also each in the column of a brittle material processing liquid. This is the same as the content ratio between the components in the processing liquid described above, and a detailed description thereof will be omitted.
  • the brittle material processing method is a method of processing a workpiece made of the brittle material such as a silicon ingot using the processing liquid.
  • the machining fluid is used by supplying the machining fluid to the workpiece and bringing it into contact with the workpiece.
  • the machining fluid lubricates between the workpiece and a processing tool such as the wire saw. Furthermore, it is used for removal of chips (chips), rust prevention of workpieces, cooling of tools and workpieces, and the like.
  • Specific examples of the processing of the brittle material performed using the processing liquid include various processing such as cutting, grinding, punching, polishing, drawing, drawing, rolling, and the like. Among them, cutting and grinding are preferable, and cutting is more preferable.
  • the brittle material as the workpiece include the materials described above. Note that, as described above, the processing liquid is preferably used as one used for cutting a silicon ingot.
  • the wire saw processing method of both the free abrasive grain method and the fixed abrasive grain method cuts a plurality of silicon wafers from the silicon ingot at a time.
  • one wire is wound around each groove on two or more guide rollers having a plurality of grooves carved at a constant interval, and each wire is held in parallel with a constant tension.
  • each guide roller is rotated and the wire is run in one or both directions while the machining liquid discharged from the nozzle or the like is adhered to the wire, and the silicon ingot is pushed onto the wire to which the machining liquid is adhered. Cutting is applied.
  • processing may be performed while applying a processing liquid to a workpiece itself such as a silicon ingot as necessary.
  • the processing liquid used for processing is stored in a tank or the like, and is transported from there to the aforementioned processing chamber nozzle by piping or the like.
  • the machining fluid used at the time of cutting is collected in a used machining fluid receiving tank or the like below the cutting device.
  • the processing liquid is more preferably used as a processing liquid used in such a brittle material processing method.
  • the processing liquid is further used as a processing liquid used in a processing method of cutting a silicon wafer from a silicon ingot with a fixed abrasive wire. It is preferably used and more preferably used by a processing method of cutting a silicon wafer from a silicon ingot using a multi-wire apparatus using a fixed abrasive wire saw.
  • the brittle material processing apparatus is a processing apparatus that uses the brittle material processing liquid according to an embodiment of the present invention, preferably a multi-wire cutting apparatus, and more preferably a fixed abrasive.
  • the “processing apparatus using a brittle material processing liquid according to an embodiment of the present invention” can also be referred to as “a processing apparatus filled with a brittle material processing liquid according to an embodiment of the present invention”.
  • the circulation rate was adjusted so that the flow rate of the working fluid at this time was 1.3 L / min.
  • the liquid level after 5 minutes from the start of circulation was measured.
  • the liquid level is compared with the unit “mL” using the scale of the graduated cylinder.
  • the liquid level height increases, that is, the value of “mL” increases. Therefore, the smaller the liquid level height value “mL”, the better the defoaming property.
  • Tables 1 and 2 The obtained results are shown in Tables 1 and 2 below.
  • Liquid level: fine powder A blend of fine powder (“graphite powder”, manufactured by Wako Pure Chemical Industries, Ltd., special grade) so as to have a concentration of 13 mass% in the evaluation liquid was prepared as an evaluation liquid.
  • liquid level height was measured by the method similar to the measuring method of the liquid level height "without fine powder", and the defoaming property of the processing liquid at the time of fine powder mixing was evaluated. The obtained results are shown in Tables 1 and 2 below.
  • Examples 1 to 9 Comparative Examples 1 to 9
  • Each component was blended so as to have the composition shown in Tables 1 and 2 below to prepare a brittle material processing liquid. According to the said evaluation method, the brittle material processing liquid of each Example and a comparative example was evaluated. The obtained results are shown in Tables 1 and 2 below.
  • each component shown in following Table 1 and 2 represents the following compounds, respectively.
  • Surfactant 5 block copolymer of
  • each of the brittle material working fluids of Examples 1 to 9 contains the component (A) and the component (B) and satisfies the predetermined content ratio [A / B]. It was confirmed that the foam was excellent in defoaming property, and there was little contamination due to the adhesion of fine powder, and the anti-contamination effect was excellent. On the other hand, as shown in Table 2, since the brittle material processing liquids of Comparative Examples 1, 4, 8 and 9 do not satisfy the predetermined content ratio [A / B], all of them are inferior in antifoaming properties. It was confirmed that there were many stains due to adhesion of fine powder.
  • the brittle material processing liquids of Comparative Examples 2, 3 and 5 do not contain the component (B), and the brittle material processing liquids of Comparative Examples 6 and 7 do not contain the component (A). For this reason, it was confirmed that all of them were inferior in antifoaming properties and that there were many stains due to adhesion of fine powder.
  • the brittle material processing liquid of Comparative Example 5 uses an EO adduct of a higher alcohol having an EO addition mole number of less than 5.
  • the brittle material working fluid of Comparative Example 6 uses an EO adduct of acetylene glycol having an HLB value exceeding 12.
  • the processing liquid is less foamed during processing and has excellent defoaming properties. Was confirmed. Further, it was confirmed that the contamination on the apparatus and the cut silicon wafer was slight and easy to clean.
  • the brittle material processing liquid according to one embodiment of the present invention is excellent in antifoaming properties. Therefore, for example, when cutting a workpiece made of a brittle material such as a silicon ingot, foaming of the processing liquid can be suppressed, and the processing liquid overflows from the tank that receives the processing liquid due to foaming. It is possible to prevent adverse effects such as a soaking (occurrence of overflow) failure or a reduction in processing accuracy caused by foaming. In addition, the brittle material processing liquid according to one embodiment of the present invention is excellent in the contamination suppressing effect.
  • the brittle material working fluid according to an embodiment of the present invention is preferably used as a material for cutting brittle materials such as silicon ingots, and more preferably, fixed abrasive.
  • a grain wire is used as a coolant for cutting a silicon wafer from a silicon ingot.

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Abstract

La présente invention concerne un liquide de traitement pour matériau fragile qui contient de l'eau, (A) une ou plusieurs substances choisies dans le groupe constitué des glycols d'acétylène présentant une valeur HLB égale à 4 à 12 (bornes incluses) et des produits d'addition avec l'oxyde d'alkylène des glycols d'acétylène présentant une valeur HLB égale à 4 à 12 (bornes incluses), et (B) un tensioactif non ionique qui est un produit d'addition avec l'oxyde d'éthylène présentant une valeur HLB égale ou supérieure à 6 et à la structure moléculaire duquel a été ajouté un nombre de moles d'oxyde d'éthylène égal ou supérieur à 5, et qui ne possède pas de groupe acétylène. La teneur en composant (A) varie de 0,010 % en masse à 0,200 % en masse (bornes incluses) pour 100 % en masse du total du liquide de traitement pour matériau fragile ; la teneur en composant (B) varie de 0,020 % en masse à 0,500 % en masse (bornes incluses) pour 100 % en masse du total du liquide de traitement pour matériau fragile ; et le rapport entre la teneur en composant (A) et la teneur en composant (B), à savoir (A)/(B), varie de 0,05 à 2,00 (bornes incluses) en termes de rapport pondéral. La présente invention concerne également un procédé de production de ce liquide de traitement pour matériau fragile.
PCT/JP2018/010249 2017-03-17 2018-03-15 Liquide de traitement pour matériau fragile WO2018169008A1 (fr)

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JP2003183548A (ja) * 2001-12-18 2003-07-03 Nisshin Chem Ind Co Ltd インキ吸収剤組成物
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