Working fluid
A machining fluid with polyoxyalkyleneamine and additional components addresses the issue of wire saw bending in multi-wire saw devices, enhancing cutting efficiency and productivity by preventing wire bending and maintaining lubricity and cleanliness.
Patent Information
- Application Number
- PCT/JP2025/024299
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2024-07-08
- Filing Date
- 2025-07-07
- Publication Date
- 2026-01-15
AI Technical Summary
Existing machining fluids used in multi-wire saw devices for cutting brittle materials like silicon ingots often result in wire saw bending, leading to reduced productivity due to insufficient sharpness and inability to keep up with the cutting process.
A machining fluid containing polyoxyalkyleneamine as an active ingredient, with specific base number and nitrogen atom content, along with optional epichlorohydrin-modified polyoxyalkylene compounds and alkynediol alkylene oxide adducts, is used to enhance the performance of the multi-wire saw device, preventing wire bending and ensuring efficient cutting.
The proposed machining fluid effectively prevents wire saw bending, maintains cutting efficiency, and ensures appropriate lubricity and cleanliness, thereby improving productivity and reducing material loss during the cutting process.
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Abstract
Description
Processing fluid
[0001] The present invention relates to machining fluids.
[0002] In the manufacture of semiconductor products, precise cutting of silicon ingots, a brittle material, is important. For silicon ingot cutting, wire sawing is generally used from the viewpoints of machining accuracy and productivity. Wire sawing is also used for machining materials such as ceramics, quartz, sapphire, and glass. Generally, wire sawing methods include a free abrasive method, in which free abrasive grains are supplied to the sliding contact between the wire and the workpiece, and a fixed abrasive method, in which abrasive grains are fixed to the wire surface. Both of these wire sawing methods use a coolant to improve cutting efficiency, suppress friction between the workpiece and the tool, reduce frictional heat generated during machining, extend tool life, and remove chips. Examples of coolant used for these applications include oil-based coolants primarily composed of mineral oil, animal and vegetable oil, or synthetic oil, and aqueous coolants made water-soluble by blending surfactant compounds. In recent years, water-soluble machining fluids have come to be used from the viewpoints of safety during work and environmental issues.
[0003] For example, Patent Document 1 discloses a water-soluble cutting fluid for silicon ingot slicing, characterized by containing as essential components a polyoxyalkylene adduct having a number average molecular weight of 500 or less and a specific structure, and a monovalent or divalent aliphatic carboxylic acid or a salt thereof having 4 to 10 carbon atoms (including the carbon in the carbonyl group).Patent Document 2 discloses a water-soluble working fluid composition for fixed abrasive wire saws used to cut rare earth magnets, characterized by containing specific amounts of glycols, carboxylic acids, compounds that dissolve in water and exhibit basicity, and water (however, the total of these components is 100 parts by weight). Patent Document 3 discloses a brittle material processing fluid containing at least one selected from the group consisting of alkynediols having an HLB value of 4 or more and 12 or less and alkylene oxide adducts of alkynediols having an HLB value of 4 or more and 12 or less, a nonionic surfactant which is an ethylene oxide adduct having an HLB value of 6 or more and the number of moles of ethylene oxide added in the molecular structure of 5 or more and which does not have a carbon-carbon triple bond, and a carboxylic acid, each in a specific content.
[0004] In both of the above wire sawing methods, a multi-wire saw machine is used to cut multiple wafers from an ingot at once. In a multi-wire saw machine, a wire is wound around each groove on two or more guide rollers, each groove having a plurality of grooves carved at regular intervals. Each wire is held parallel to the other with a constant tension. During cutting, the guide rollers are rotated, and a machining fluid discharged from a nozzle or the like is applied to the wire while the wire travels in one or both directions. The ingot is pressed against the wire to which the machining fluid is applied. The use of a multi-wire saw machine allows for efficient cutting, since a large number of wafers can be cut at once. Furthermore, the narrow cutting margin results in relatively little material loss during cutting, and the machine also has the advantage of being able to easily accommodate larger diameter ingots.
[0005] JP 2011-68884 A JP 2003-82335 A JP 2018-154762 A
[0006] However, when using a multi-wire saw device to cut out wafers, depending on the working fluid, the sharpness of the wire saw may be insufficient, and the wire saw may not be able to keep up with the cutting when the ingot is pressed down, resulting in the wire saw bending. When this problem occurs, measures must be taken, such as extending the ingot cutting time, which results in reduced productivity.
[0007] Therefore, an object of the present invention is to provide a machining fluid that can be used in a multi-wire saw device and has excellent performance in preventing the wire saw from bending.
[0008] According to the present invention, the following items [1] to
[16] are provided. [1] A working fluid containing an active ingredient and water, wherein the active ingredient contains the following component (A): Component (A): a polyoxyalkyleneamine having a base number of 5.0 to 110 mg KOH / g and a nitrogen atom content of 0.10 to 3.0 mass%. [2] The working fluid according to [1], wherein the content of component (A) is 50 mass% or more based on the total amount of the active ingredient. [3] The working fluid according to [1] or [2], wherein component (A) is one or more selected from an alkylene oxide adduct of a monoamine and an alkylene oxide adduct of a polyamine. [4] The working fluid according to [3], wherein component (A) is an alkylene oxide adduct of a polyamine. [5] The processing fluid according to [4], wherein the alkylene oxide adduct of the polyamine is represented by the following general formula (I) and has a mass average molecular weight (Mw) of 500 to 10,000: [In the general formula (I), A 1 ~A 4 each independently represents an ethylene group or a propylene group; A 1 ~A 4When a plurality of are present, they may be the same or different. a, b, c, and d are the average values of the number of alkylene oxide units, and each independently is a number of 1 or more.] [6] The processing fluid according to [1] or [2], wherein the component (A) is represented by the following general formula (II): [In the general formula (II), X is an alkyl group having 1 to 4 carbon atoms or an aminoalkyl group having 1 to 4 carbon atoms. 5 and A 6 each independently represents an ethylene group or a propylene group; A 6 When a plurality of alkylene oxide units are present, they may be the same or different. e is the average value of the number of alkylene oxide units and is a number of 1 or more.] [7] The processing fluid according to [1] or [2], wherein the component (A) has a repeating unit represented by the following general formula (III): [In the general formula (III), A 7 each independently represents an ethylene group or a propylene group; A 8 each independently represents an ethylene group, a propylene group, or a butylene group; A 7 When a plurality of A are present, they may be the same or different, 8When a plurality of are present, they may be the same or different. f is the average value of the number of alkylene oxide units and is a number equal to or greater than 1.] [8] The working fluid according to any one of [1] to [7], wherein the active ingredient further contains the following component (B): Component (B): epichlorohydrin-modified polyoxyalkylene compound. [9] The working fluid according to [8], wherein the content of component (B) is 0.10 to 10.0 mass% based on the total amount of the active ingredients.
[10] The working fluid according to any one of [1] to [9], wherein the active ingredient further contains the following component (C): Component (C): alkylene oxide adduct of alkynediol.
[11] The working fluid according to
[10] , wherein the content of component (C) is 0.10 to 10.0 mass% based on the total amount of the active ingredients.
[12] The working fluid according to any one of [1] to
[11] , wherein the working fluid is used when cutting a workpiece made of a brittle material using a multi-wire saw device.
[13] The working fluid according to
[12] , wherein the wires constituting the multi-wire saw device are fixed abrasive wires.
[14] The working fluid according to
[12] or
[13] , wherein the brittle material is crystalline silicon, sapphire, silicon carbide, gallium nitride, neodymium magnet, quartz, or glass.
[15] The working fluid according to any one of
[12] to
[14] , wherein the wires constituting the multi-wire saw device have a strand diameter of 120 μm or less and a wire spacing of 1,100 μm or less.
[16] A method for producing a working fluid containing an active ingredient and water, comprising a step of mixing the active ingredient and the water, wherein the active ingredient contains the following component (A): Component (A): a polyoxyalkyleneamine having a base number of 5.0 to 110 mg KOH / g and a nitrogen atom content of 0.10 to 3.0 mass%.
[0009] According to the present invention, it is possible to provide a machining fluid that can be used in a multi-wire saw device and has excellent performance in preventing the wire saw from bending.
[0010] The upper and lower limits of the numerical ranges described herein can be arbitrarily combined. For example, when "A to B" and "C to D" are described as numerical ranges, the numerical ranges "A to D" and "C to B" are also included in the scope of the present invention. Furthermore, the numerical ranges described herein, "lower limit to upper limit," mean that the range is equal to or greater than the lower limit and equal to or less than the upper limit, unless otherwise specified. Furthermore, in this specification, numerical values in the examples are numerical values that can be used as upper or lower limits. Furthermore, in this specification, unless otherwise specified, "polyoxyalkyleneamine" refers to an amine compound having oxyalkylene units as repeating units, the molecular terminals of which may be hydroxyl groups or hydrocarbyloxy groups. Furthermore, the oxyalkylene units may be of one type or a combination of two or more types. The oxyalkylene units preferably have 2 to 4 carbon atoms. The origin of the oxyalkylene units is not particularly limited, and they may be derived from alkylene oxides or diols. Specific examples of alkylene oxides include ethylene oxide, propylene oxide (PO), oxetane, 1,2-butylene oxide, 2,3-butylene oxide, 1,3-butylene oxide, and tetrahydrofuran.
[0011] [Mode of Machining Fluid] The machining fluid of this embodiment contains an active ingredient and water. The active ingredient contains the following component (A): Component (A): a polyoxyalkyleneamine having a base number of 5.0 to 110 mgKOH / g and a nitrogen atom content of 0.10 to 3.0 mass %.
[0012] The present inventors have conducted extensive research to solve the above problems, and as a result have found that a machining fluid containing the above components can solve the above problems. After further research, the present inventors have completed the present invention.
[0013] The active ingredients contained in the machining fluid of this embodiment are described in detail below. <Component (A)> Component (A) is a polyoxyalkyleneamine having a base number of 5.0 to 110 mgKOH / g and a nitrogen atom content of 0.10 to 3.0 mass%, and is an amine compound containing oxyalkylene units. The molecular terminals of the polyoxyalkyleneamine may be hydroxyl groups or hydrocarbyloxy groups, but hydroxyl groups are preferred. The polyoxyalkyleneamine may contain one type of oxyalkylene unit or two or more types. When two or more types are combined, the addition of the multiple types of oxyalkylene units may be either random addition or block addition, or a mixture of random addition and block addition may be used, but a block addition copolymer is preferred.
[0014] Specifically, component (A) is required to have a base number of 5.0 to 110 mgKOH / g as measured by the perchloric acid method in accordance with JIS K 2501:2003, and when the base number is within this range, the wire saw will have excellent anti-warping performance. The base number of component (A) is preferably 8.0 to 105 mgKOH / g, and more preferably 12.0 to 100 mgKOH / g.
[0015] Furthermore, component (A) must have a nitrogen atom content of 0.10 to 3.0 mass%, and within this range, the wire saw will have excellent anti-warping performance. The nitrogen atom content of component (A) is preferably 0.20 to 2.80 mass%, more preferably 0.30 to 2.70 mass%.
[0016] Component (A) is preferably one or more compounds selected from the group consisting of alkylene oxide adducts of monoamines and alkylene oxide adducts of polyamines, and more preferably alkylene oxide adducts of polyamines. The alkylene oxide adducts of polyamines are preferably represented by the following general formula (I) and have a mass average molecular weight (Mw) of 500 to 10,000: [In the general formula (I), A 1 ~A 4each independently represents an ethylene group or a propylene group; A 1 ~A 4 When a plurality of groups are present, they may be the same or different. a, b, c, and d are the average values of the numbers of alkylene oxide units, and each is independently a number of 0 or more.
[0017] In the general formula (I), a, b, c, and d are the average values of the numbers of alkylene oxide units, and each independently represents a number equal to or greater than 0. From the viewpoint of solubility in the base oil and suppressing cloudiness of the working fluid to improve its appearance, a, b, c, and d are each independently preferably a number from 1 to 11, more preferably a number from 1 to 8, and even more preferably a number from 1 to 5.
[0018] As the component (A), a compound represented by the following general formula (II) is also preferably used.
[0019] [In the general formula (II), X is an alkyl group having 1 to 4 carbon atoms or an aminoalkyl group having 1 to 4 carbon atoms. 5 and A 6 each independently represents an ethylene group or a propylene group; A 6 When a plurality of groups are present, they may be the same or different. e is the average value of the number of alkylene oxide units and is a number of 1 or more.
[0020] In the above general formula (II), e is the average value of the number of alkylene oxide units and is a number equal to or greater than 1. From the viewpoint of improving the lubricity between the workpiece and the abrasive grains and of suppressing cloudiness of the machining fluid to improve its appearance, e is preferably a number from 1 to 50, more preferably a number from 1 to 48, and even more preferably a number from 1 to 45. Furthermore, X in the above general formula (II) is preferably an aminoalkyl group having 1 to 4 carbon atoms.
[0021] As the component (A), a compound having a repeating unit represented by the following general formula (III) is also preferably used.
[0022] [In the general formula (III), A 7each independently represents an ethylene group or a propylene group; A 8 each independently represents an ethylene group, a propylene group, or a butylene group; A 7 When a plurality of A are present, they may be the same or different, 8 When a plurality of groups are present, they may be the same or different. f is the average number of alkylene oxide units and is a number of 1 or more.
[0023] In the general formula (III), f is the average value of the number of alkylene oxide units and is a number equal to or greater than 1. From the viewpoints of improving the lubricity between the workpiece and the abrasive grains and suppressing cloudiness of the machining fluid to improve the appearance, f is preferably a number from 1 to 50, more preferably a number from 1 to 48, and even more preferably a number from 1 to 45.
[0024] From the viewpoint of lubricity, the mass average molecular weight of the component (A) is preferably 300 or more, more preferably 400 or more, even more preferably 500 or more, and particularly preferably 600 or more. Furthermore, from the viewpoint of reducing the stickiness of the processing fluid, the mass average molecular weight of the component (A) is preferably 10,000 or less, more preferably 8,000 or less, even more preferably 6,000 or less, and particularly preferably 5,000 or less. The upper and lower limits of these numerical ranges can be arbitrarily combined. Specifically, the mass average molecular weight of the component (A) is preferably 300 to 10,000, more preferably 400 to 8,000, even more preferably 500 to 6,000, and particularly preferably 600 to 5,000.
[0025] The suitable ranges of the mass average molecular weight of those represented by general formulas (I) and (II) and those having a repeating unit represented by general formula (III) are the same as those for component (A). Component (A) is preferably one or more selected from the group consisting of those represented by general formula (I), those represented by general formula (II), and those having a repeating unit represented by general formula (III).
[0026] The content of component (A) is preferably 50% by mass or more, more preferably 60% by mass or more, even more preferably 70% by mass or more, and particularly preferably 80% by mass or more, based on the total amount of the active ingredients. The content of component (A) is 100% by mass or less, and may be 99% by mass or less.
[0027] <Component (B) and Component (C)> From the viewpoint of improving cleanability, the machining fluid of the present embodiment preferably further contains at least one selected from the group consisting of the following component (B) or the following component (C): Component (B): epichlorohydrin-modified polyoxyalkylene compound Component (C): alkylene oxide adduct of alkynediol
[0028] <Component (B)> Component (B) can be a compound obtained by contacting an epichlorohydrin-unmodified polyoxyalkylene compound with epichlorohydrin to modify or polymerize it, but it may also be a compound having an oxyalkylene unit derived from the polymerization site of epichlorohydrin, which is obtained by adding epichlorohydrin to an alcohol and polymerizing it, or a compound having an oxyalkylene unit as the copolymerization site of alkylene oxide and epichlorohydrin, which is obtained by polymerizing an alkylene oxide and epichlorohydrin to an alcohol.
[0029] As described above, component (B) is a modified product with epichlorohydrin, and therefore typically contains chlorine atoms. The content of chlorine atoms in component (B) is, for example, 10,000 ppm by mass or less, 8,000 ppm by mass or less, 5,000 ppm by mass or less, 3,000 ppm by mass or less, 2,000 ppm by mass or less, 1,000 ppm by mass or less, or 700 ppm by mass or less.
[0030] The content of component (B) is preferably 0.10 to 10.0 mass %, more preferably 0.20 to 9.0 mass %, and particularly preferably 0.50 to 8.0 mass %, based on the total amount of the active ingredients.
[0031] <Component (C)> The processing fluid of the present embodiment preferably further contains the following component (C): Component (C): Alkynediol alkylene oxide adduct
[0032] The component (C) is an alkylene oxide adduct of an alkynediol, and its production method is not particularly limited. Examples of the alkynediol include compounds represented by the following general formula (1):
[0033]
[0034] In general formula (1), R 1 ~R 4 R each independently represents a hydrogen atom or an alkyl group having 1 to 6 carbon atoms. 1 ~R 4 is preferably an alkyl group having 1 to 5 carbon atoms. 1 ~R 4 Specific examples of alkyl groups having 1 to 6 carbon atoms that can be selected as R include methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, sec-butyl, tert-butyl, n-pentyl, 1-methylbutyl, 2-methylbutyl, 3-methylbutyl, 1,1-dimethylpropyl, 1,2-dimethylpropyl, and 2,2-dimethylpropyl groups. 1 and R 3 is preferably an isobutyl group or a 3-methylbutyl group. 2 and R 4 is preferably a methyl group. In addition, the compound represented by general formula (1) preferably contains R 1 and R 3 are identical to each other or R 2 and R 4 are compounds having the same structure, and more preferably R 1 and R 3 are identical to each other, and R 2 and R 4 are compounds having the same structure as each other.
[0035] Furthermore, as component (C), preferred examples include alkylene oxide adducts of compounds represented by general formula (1) in which AO is added to each hydroxyl group of the compound represented by general formula (1), more preferred examples include alkylene oxide adducts of compounds represented by general formula (1) in which EO and / or PO are added to each hydroxyl group of the compound represented by general formula (1), and even more preferred examples include ethylene oxide adducts of compounds represented by general formula (1) in which EO is added to each hydroxyl group of the compound represented by general formula (1). Note that when the compound contains a structure in which a structure derived from EO (e.g., an ethyleneoxy group or a poly(oxyethylene) structure) and a structure derived from PO (e.g., a propyleneoxy group or a poly(oxypropylene) structure) are bonded, the respective structures may be bonded to each other in a random manner or in a block manner, preferably in a block manner.
[0036] Specific examples of the alkynediol include 2,5,8,11-tetramethyl-6-dodecyne-5,8-diol, 5,8-dimethyl-6-dodecyne-5,8-diol, 2,4,7,9-tetramethyl-5-dodecyne-4,7-diol, 8-hexadecyne-7,10-diol, 7-tetradecyne-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-decyne-4,7-diol, and 3,6-dimethyl-4-octyne-3,6-diol.
[0037] Component (C) is preferably 2,5,8,11-tetramethyl-6-dodecyne-5,8-diol, 5,8-dimethyl-6-dodecyne-5,8-diol, 2,4,7,9-tetramethyl-5-dodecyne-4,7-diol, 8-hexadecyne-7,10-diol, 7-tetradecyne-6,9-diol, 2,3,6,7-tetramethyl-4-octyne-3,6-diol, 3,6-diethyl-4-octyne-3,6-diol, 2, alkylene oxide adducts of one or more alkynediols selected from the group consisting of 5-dimethyl-3-hexyne-2,5-diol, 2,4,7,9-tetramethyl-5-decyne-4,7-diol, and 3,6-dimethyl-4-octyne-3,6-diol; more preferably 2,5,8,11-tetramethyl-6-dodecyne-5,8-diol, 5,8-dimethyl-6-dodecyne-5,8-diol, 2,4,7,9-tetramethyl-5 2,4,7,9-tetramethyl-5-decyne-4,7-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-decyne-4,7-diol, and 3,6-dimethyl-4-octyne-3,6-diol. more preferably, one or more selected from the group consisting of an ethylene oxide adduct of 2,5,8,11-tetramethyl-6-dodecyne-5,8-diol and an ethylene oxide adduct of 2,4,7,9-tetramethyl-5-decyne-4,7-diol; and still more preferably, an ethylene oxide adduct of 2,5,8,11-tetramethyl-6-dodecyne-5,8-diol.
[0038] Component (C) may be used singly or in combination of two or more. Component (C) is preferably one or more selected from the group consisting of alkylene oxide adducts of alkynediols having an HLB value of 4 to 12.
[0039] The content of component (C) is preferably 0.10 to 10.0 mass %, more preferably 0.05 to 3.0 mass %, and even more preferably 0.5 to 2.0 mass %, based on the total amount of the active ingredients.
[0040] <Other Components> The active ingredient may contain components other than component (A), component (B), and component (C) (hereinafter also referred to as "other components") to the extent that the object of the present invention is not impaired. Examples of other components include additives such as surfactants other than the compounds corresponding to component (A), component (B), or component (C), pH adjusters, water retention improvers, antifoaming agents, metal deactivators, bactericides / preservatives, rust inhibitors, and antioxidants. One type of other component may be used alone, or two or more types may be used in combination.
[0041] Surfactants other than compounds corresponding to component (A), component (B), or component (C) include polyoxyalkylene compounds other than component (A), component (B), or component (C), anionic surfactants, cationic surfactants, nonionic surfactants other than polyoxyalkylene compounds, and amphoteric surfactants. Polyoxyalkylene compounds other than component (A), component (B), or component (C) are compounds having oxyalkylene units as repeating units, whose molecular terminals may be hydroxyl groups or hydrocarbyloxy groups. Examples of anionic surfactants include alkylbenzene sulfonates and alpha-olefin sulfonates. Examples of cationic surfactants include quaternary ammonium salts such as alkyltrimethylammonium salts, dialkyldimethylammonium salts, and alkyldimethylbenzylammonium salts. Examples of nonionic surfactants other than polyoxyalkylene compounds include amides such as fatty acid alkanolamides. Examples of amphoteric surfactants include betaine-based alkylbetaines.
[0042] pH adjusters are primarily used to adjust the pH of machining fluids. Examples of pH adjusters include various acid components and base components. Adjusting the content ratio of these components allows the appropriate adjustment of the pH of the machining fluid. The acid component and base component may react with each other to form a salt. Therefore, when an acid component and a base component are used as pH adjusters, if a reaction product of the acid component and the base component is present in the machining fluid, the respective contents of the acid component and the base component that contributed to the reaction can be calculated from the contents of the reaction product of the acid component and the base component, as described above. In this case, the machining fluid can be considered to contain the acid component and the base component before the reaction, instead of the reaction product.
[0043] Examples of acid components used as pH adjusters 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; carboxylic acids such as acetic acid, malic acid, and citric acid; polymeric acids such as polyacrylic acid and salts thereof; and inorganic acids such as phosphoric acid. Among these, fatty acids are preferred, and fatty acids having 12 or less carbon atoms such as neodecanoic acid, isononanoic acid, capric acid, and dodecanedioic acid are more preferred, with one or more selected from the group consisting of neodecanoic acid, isononanoic acid, capric acid, and dodecanedioic acid being even more preferred.
[0044] Examples of the base component used as a pH adjuster include alkanolamines such as monoethanolamine, diethanolamine, triethanolamine, monoisopropanolamine, diisopropanolamine, triisopropanolamine, tri-n-propanolamine, tri-n-butanolamine, triisobutanolamine, tri-tert-butanolamine, N-methylethanolamine, N-ethylethanolamine, N-butylethanolamine, N-cyclohexylethanolamine, N-methyldiethanolamine, N-ethyldiethanolamine, N-cyclohexyldiethanolamine, N,N-dimethylethanolamine, and N,N-diethylethanolamine; alkylamines such as methylamine, dimethylamine, ethylamine, diethylamine, propylamine, and dipropylamine; and ammonia. Among these, tertiary amines are preferred, and at least one selected from the group consisting of triethanolamine, triisopropanolamine, N-methyldiethanolamine, and N-cyclohexyldiethanolamine is more preferred.
[0045] Examples of water retention enhancers include ethylene glycol, propylene glycol, 1,4-butanediol, hexamethylene glycol, neopentyl glycol, diethylene glycol, triethylene glycol, dipropylene glycol, tripropylene glycol, glycerin, ester derivatives thereof, ether derivatives thereof, polyethylene glycol, polypropylene glycol, etc. Antifoaming agents include, for example, silicone oil, fluorosilicone oil, polyether polysiloxane, and fluoroalkyl ether. Metal deactivators include, for example, imidazoline, pyrimidine derivatives, thiadiazole, and benzotriazole. Bactericides and preservatives include, for example, paraoxybenzoic acid esters (parabens), as well as benzoic acid, salicylic acid, sorbic acid, dehydroacetic acid, p-toluenesulfonic acid, and salts thereof, and phenoxyethanol. Rust inhibitors include, for example, alkylbenzenesulfonate, dinonylnaphthalenesulfonate, alkenylsuccinic acid esters, and polyhydric alcohol esters. Examples of antioxidants include phenolic antioxidants and amine antioxidants.
[0046] When the working fluid of the present embodiment contains other components, the total content of the other components may be 0.10% by mass or more, 0.20% by mass or more, or 0.30% by mass or more, based on the total amount of the active ingredients, or 30.00% by mass or less, 20.00% by mass or less, 10.00% by mass or less, 5.00% by mass or less, or 3.00% by mass or less.
[0047] <Water> The machining fluid of the present embodiment contains water. The water is not particularly limited, and purified water such as distilled water or ion-exchanged water (deionized water); tap water; industrial water; etc. can be used, with purified water or ion-exchanged water (deionized water) being preferred, and ion-exchanged water (deionized water) being more preferred.
[0048] The water content is adjusted appropriately depending on the usage of the working fluid. For example, when the working fluid of this embodiment is used to process a workpiece (e.g., cutting a brittle material with a multi-wire saw), the water content in the working fluid (hereinafter also referred to as the "water content of the first embodiment") is preferably 95.000% by mass or more, more preferably 97.500% by mass or more, even more preferably 99.500% by mass or more, and particularly preferably 99.600% by mass or more, based on the total amount of the working fluid (100% by mass), from the viewpoint of improving the flame retardancy of the working fluid and enhancing safety, and from the viewpoint of reducing the viscosity of the working fluid and improving handleability. Furthermore, from the viewpoint of ensuring the amount of active ingredients in the working fluid, the water content is preferably 99.910% by mass or less, more preferably 99.900% by mass or less, even more preferably 99.890% by mass or less, even more preferably 99.880% by mass or less, and particularly preferably 99.870% by mass or less. The machining fluid of this embodiment may be concentrated by reducing the amount of water in the machining fluid from the viewpoint of transportation efficiency and storage efficiency. For example, the machining fluid may be a concentrated product obtained by reducing the amount of water in the machining fluid and concentrating it 20 to 2,000 times. Then, when it is used (when machining a workpiece), it may be diluted 20 to 2,000 times with water.
[0049] (Content of Component (A)) When the water content of the working fluid of this embodiment is the water content of the first aspect described above, the content of component (A) is preferably 0.0100 mass% or more, based on 100 mass% of the total amount of the working fluid. A content of component (A) of 0.0100 mass% or more can achieve a good compositional balance of the working fluid, making it easier to improve the effects of the present invention. From the viewpoint of further improving the effects of the present invention, the content of component (A) is preferably 0.0150 mass% or more, more preferably 0.0200 mass% or more, and even more preferably 0.0250 mass% or more, based on 100 mass% of the total amount of the working fluid. Furthermore, from the viewpoint of the solubility of component (A) in water, the content of component (A) is preferably 0.500 mass% or less, more preferably 0.100 mass% or less, even more preferably 0.0800 mass% or less, and even more preferably 0.0700 mass% or less, based on the total amount of the working fluid.
[0050] [Method for Producing Machining Fluid] The method for producing the machining fluid of this embodiment is not particularly limited. For example, the method for producing the machining fluid of this embodiment is a method for producing a machining fluid containing an active ingredient and water, comprising a step of mixing the active ingredient with the water, wherein the active ingredient contains the following component (A): Component (A): a polyoxyalkyleneamine having a base number of 5.0 to 110 mg KOH / g and a nitrogen atom content of 0.10 to 3.0 mass %.
[0051] In the manufacturing method of the working fluid of this embodiment, one or more components selected from component (B), component (C), and other components may be further mixed. The order in which component (A), component (B), component (C), and other components are mixed is not particularly limited. For example, component (A), component (B), component (C), and one or more components selected from component (B), component (C), and other components may be mixed sequentially or simultaneously with water. Alternatively, component (A) and one or more components selected from component (B), component (C), and other components may be mixed in advance and the resulting mixture may be mixed with water. Note that component (A), component (B), component (C), water, and other components are each the same as those described above, and preferred embodiments thereof are also the same, so detailed description thereof is omitted. Furthermore, the preferred amounts and preferred ratios of component (A), component (B), component (C), water, and other components are the same as those described above, and therefore detailed description thereof is omitted.
[0052] [Uses of the machining fluid] The machining fluid of this embodiment can prevent wire breakage even when the wires are thinned and the wire spacing is narrowed in a multi-wire saw device, and has appropriate lubricity and excellent cleanliness. Therefore, the machining fluid of this embodiment can be suitably used when cutting a workpiece made of a brittle material using a multi-wire saw device. Fixed abrasive wires can be suitably used as the wires constituting the multi-wire saw device. Note that the machining fluid of this embodiment can be used not only for cutting using a multi-wire saw device, but also for cutting using a single-wire saw device. The wires constituting the single-wire saw device may be fixed abrasive wires.
[0053] Examples of brittle materials include crystalline silicon, sapphire, gallium nitride, silicon carbide, neodymium magnet, quartz crystal, and glass. The machining fluid of the present embodiment is particularly suitable for cutting crystalline silicon, sapphire, or silicon carbide.
[0054] [Method for Machining Brittle Materials] The working fluid of this embodiment can prevent wire breakage even when the wires are thinned and the wire spacing is narrowed in a multi-wire saw device, and has appropriate lubricity and excellent cleanliness. Therefore, the working fluid of this embodiment provides a method for cutting a workpiece made of a brittle material using a multi-wire saw device. Fixed abrasive wires can be suitably used as the wires constituting the multi-wire saw device. Note that the working fluid of this embodiment also provides a method for cutting a workpiece made of a brittle material using a single-wire saw device.
[0055] <Multi-wire Saw Device> The multi-wire saw device mentioned in the present embodiment regarding the use of the machining fluid and the method for machining brittle materials will now be described. A multi-wire saw device used in cutting processes, for example, has two or more guide rollers with multiple grooves carved at regular intervals, with one wire wound around each groove, and each wire held parallel with a constant tension. During cutting, the guide rollers are rotated, and machining fluid ejected from a nozzle or the like is applied to the wire while the wire travels in one or both directions. A silicon ingot is pressed against the wire to which the machining fluid is applied to perform cutting. If necessary, machining may also be performed while the machining fluid is applied to the workpiece itself, such as a silicon ingot. The machining fluid used in cutting is stored in a tank or the like and transported from there to the aforementioned machining chamber nozzle via piping or the like. The machining fluid used during cutting is collected in a used machining fluid receiving tank or the like located below the cutting device. In some cases, the machining fluid may be circulated within the device and reused.
[0056] The spacing between the wires used in processing the brittle material is set appropriately depending on the thickness required for the wafers to be cut out, but is preferably 1,100 μm or less, for example, and is preferably 100 μm or more.
[0057] The present invention will be specifically described with reference to the following examples, although the present invention is not limited to the following examples.
[0058] [Methods for Measuring Various Physical Properties] The properties of the raw materials used in each example and each comparative example were measured according to the procedures shown below.
[0059] (1) Mass-average molecular weight The mass-average molecular weight (Mw) was measured by gel permeation chromatography (GPC). GPC was performed using two "TSKgel (registered trademark) SuperMultipore HZ-M" columns manufactured by Tosoh Corporation, tetrahydrofuran as an eluent, and a refractive index detector. The mass-average molecular weight (Mw) was determined using polystyrene as a standard sample.
[0060] (2) HLB Value The HLB value of component (C) was calculated by the Griffin method.
[0061] [Examples 1 to 8, Comparative Examples 1 to 6] The components listed below were mixed to prepare machining fluids having the compositions shown in Table 1, and the evaluations described below were carried out. The numerical units for the blended compositions in Table 1 are "mass %." Details of each component used to prepare the machining fluids having the compositions shown in Table 1 are described below.
[0062] <Component (A)> "Polyoxyalkyleneamine 1": base number 26.4 mgKOH / g, nitrogen atom content 0.66% by mass, mass average molecular weight (Mw) = 1,600, cloud point of 1% by mass aqueous solution = 18°C, and represented by the general formula (I) above. "Polyoxyalkyleneamine 2": base number 17.9 mgKOH / g, nitrogen atom content 0.44% by mass, mass average molecular weight (Mw) = 2,700, cloud point of 1% by mass aqueous solution = 68°C, and represented by the general formula (I) above. "Polyoxyalkyleneamine 3": base number 23.5 mgKOH / g, nitrogen atom content 0.60% by mass, mass average molecular weight (Mw) = 1,900, cloud point of 1% by mass aqueous solution = 30°C, and represented by the general formula (I) above. "Polyoxyalkyleneamine 4": a polyoxyalkyleneamine having a base number of 96.0 mg KOH / g, a nitrogen atom content of 2.50% by mass, a mass average molecular weight (Mw) of 600, and represented by the general formula (II) in which X is a methyl group. "Polyoxyalkyleneamine 5": a polyoxyalkyleneamine having a base number of 57.6 mg KOH / g, a nitrogen atom content of 1.50% by mass, a mass average molecular weight (Mw) of 1,000, and represented by the general formula (II) in which X is a methyl group. "Polyoxyalkyleneamine 6": a polyoxyalkyleneamine having a base number of 54.3 mg KOH / g, a nitrogen atom content of 1.40% by mass, a mass average molecular weight (Mw) of 2,000, and represented by the general formula (II) in which X is an aminopropyl group. "Polyoxyalkyleneamine 7": base number 15.8 mgKOH / g, nitrogen atom content 0.40 mass%, mass average molecular weight (Mw) = 1,900, having a repeating unit represented by the general formula (III)
[0063] <Component (A')> "EO-PO block polymer 1": polyoxyethylene-polyoxypropylene block polymer, CAS number: 9003-11-6, base number less than 0.1 mg KOH / g, nitrogen atom content less than 5 ppm by mass, mass average molecular weight (Mw) = 4,300 "EO-PO block polymer 2": polyoxyethylene-polyoxypropylene block polymer, CAS number: 9003-11-6, base number less than 0.1 mg KOH / g, nitrogen atom content less than 5 ppm by mass, mass average molecular weight (Mw) = 2,200 "Polyoxyalkyleneamine 8": polyetheramine, CAS number: 65605-36-9, base number 117 mg KOH / g, nitrogen atom content 3.10% by mass, mass average molecular weight (Mw) = 900 "Triisopropanolamine": CAS number: 122-20-3
[0064] <Component (B)> "Epichlorohydrin modified product" Epichlorohydrin modified product of EO adduct of alcohol having 9 to 11 carbon atoms, chlorine atom content: 565 ppm by mass
[0065] <Component (C)> "Alkynediol EO adduct" EO adduct of 2,5,8,11-tetramethyl-6-dodecyne-5,8-diol (EO adduct of alkynediol, HLB = 8)
[0066] <Water> ・Ion-exchanged water
[0067] [Evaluation] The machining fluids of the Examples and Comparative Examples were diluted 200 times and the following evaluations were carried out.
[0068] <Wire deflection prevention performance of wire saw> Using a Takatori "WSD-K2" processing machine, Asahi Diamond Industrial Co., Ltd. fixed abrasive wire (φ0.10 mm) as the cutting wire, and diluted solutions of the processing fluids prepared in Examples 1 to 8 and Comparative Examples 1 to 6, silicon ingots were cut out under the following conditions: (Processing conditions) Maximum wire linear speed: 700 m / min Wire tension: 15 N Cutting speed: 0.5 mm / min
[0069] Here, when a silicon ingot is lowered from above the wire and pressed against the wire to perform cutting, if the cutting cannot keep up with the speed of the silicon ingot's descent, the wire will follow the silicon ingot being pressed down. Therefore, the difference between the wire's initial position and the wire's position during cutting of the silicon ingot was taken as the wire deflection amount, and was evaluated according to the following evaluation criteria. (Evaluation criteria) A: Deflection amount 8.00 mm or less B: Deflection amount more than 8.00 mm and 8.50 mm or less C: Deflection amount more than 8.50 mm
[0070] The composition of each machining fluid and the evaluation results are shown in Table 1.
[0071] From Table 1, the following can be seen. The diluted solutions of the machining fluids of Examples 1 to 8, which contain component (A) as the active ingredient, showed small amounts of wire deflection, indicating efficient cutting of the silicon ingot. In contrast, the diluted solutions of the machining fluids of Comparative Examples 1 to 6 showed large amounts of wire deflection, indicating poor efficiency in cutting the silicon ingot.
Claims
1. A machining fluid containing an active ingredient and water, wherein the active ingredient contains the following component (A): Component (A): a polyoxyalkyleneamine having a base number of 5.0 to 110 mg KOH / g and a nitrogen atom content of 0.10 to 3.0 mass%.
2. The machining fluid according to claim 1, wherein the content of component (A) is 50 mass% or more based on the total amount of the active ingredients.
3. The machining fluid according to claim 1 or 2, wherein the component (A) is at least one selected from the group consisting of alkylene oxide adducts of monoamines and alkylene oxide adducts of polyamines.
4. The machining fluid according to claim 3, wherein component (A) is an alkylene oxide adduct of polyamine.
5. The processing fluid according to claim 4, wherein the alkylene oxide adduct of polyamine is represented by the following general formula (I) and has a mass average molecular weight (Mw) of 500 to 10,000: [In the general formula (I), A 1 ~A 4 each independently represents an ethylene group or a propylene group; A 1 ~A 4 When a plurality of groups are present, they may be the same or different. a, b, c, and d are the average values of the numbers of alkylene oxide units, and each independently is a number of 1 or more.
6. The machining fluid according to claim 1 or 2, wherein the component (A) is represented by the following general formula (II): [In the general formula (II), X is an alkyl group having 1 to 4 carbon atoms or an aminoalkyl group having 1 to 4 carbon atoms. 5 and A 6 each independently represents an ethylene group or a propylene group; A 6 When a plurality of groups are present, they may be the same or different. e is the average value of the number of alkylene oxide units and is a number of 1 or more.
7. The machining fluid according to claim 1 or 2, wherein the component (A) has a repeating unit represented by the following general formula (III): [In the general formula (III), A 7 each independently represents an ethylene group or a propylene group; A 8 each independently represents an ethylene group, a propylene group, or a butylene group; A 7 When a plurality of A are present, they may be the same or different, 8 When a plurality of groups are present, they may be the same or different. f is the average number of alkylene oxide units and is a number of 1 or more.
8. The machining fluid according to any one of claims 1 to 7, wherein the active ingredient further contains the following component (B): Component (B): an epichlorohydrin-modified polyoxyalkylene compound.
9. The machining fluid according to claim 8, wherein the content of component (B) is 0.10 to 10.0 mass % based on the total amount of the active ingredients.
10. The working fluid according to any one of claims 1 to 9, wherein the active ingredient further contains the following component (C): Component (C): an alkylene oxide adduct of an alkynediol.
11. The machining fluid according to claim 10, wherein the content of component (C) is 0.10 to 10.0 mass % based on the total amount of the active ingredients.
12. The machining fluid according to any one of claims 1 to 11, which is used when cutting a workpiece made of a brittle material using a multi-wire saw device.
13. The machining fluid according to claim 12, wherein the wires constituting the multi-wire saw device are fixed abrasive wires.
14. The working fluid according to claim 12 or 13, wherein the brittle material is crystalline silicon, sapphire, silicon carbide, gallium nitride, neodymium magnet, quartz, or glass.
15. The machining fluid according to any one of claims 12 to 14, wherein the wires constituting the multi-wire saw device have a strand diameter of 120 μm or less and the spacing between the wires is 1,100 μm or less.
16. A method for producing a machining fluid containing an active ingredient and water, comprising a step of mixing the active ingredient with water, wherein the active ingredient contains the following component (A): Component (A): a polyoxyalkyleneamine having a base number of 5.0 to 110 mg KOH / g and a nitrogen atom content of 0.10 to 3.0 mass%.
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