KR101788901B1 - Aqueous processing solution for fixed abrasive grain wire saw - Google Patents

Aqueous processing solution for fixed abrasive grain wire saw Download PDF

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KR101788901B1
KR101788901B1 KR1020137001523A KR20137001523A KR101788901B1 KR 101788901 B1 KR101788901 B1 KR 101788901B1 KR 1020137001523 A KR1020137001523 A KR 1020137001523A KR 20137001523 A KR20137001523 A KR 20137001523A KR 101788901 B1 KR101788901 B1 KR 101788901B1
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processing liquid
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KR20130095724A (en
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나오키 마루오
야스노리 누마타
히로아키 다카하시
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유시로 가가쿠 고교(주)
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
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    • B28D5/00—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
    • B28D5/0058—Accessories specially adapted for use with machines for fine working of gems, jewels, crystals, e.g. of semiconductor material
    • B28D5/0076—Accessories specially adapted for use with machines for fine working of gems, jewels, crystals, e.g. of semiconductor material for removing dust, e.g. by spraying liquids; for lubricating, cooling or cleaning tool or work
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    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/06—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to an acyloxy radical of saturated carboxylic or carbonic acid
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    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/104—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing two carbon atoms only
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    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/04—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
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    • C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
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    • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
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  • Oil, Petroleum & Natural Gas (AREA)
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Abstract

본 발명의 (A) 폴리비닐피롤리돈, 및 비닐피롤리돈을 포함하는 공중합물로부터 선택되는 적어도 1종류 이상의 수용성 고분자, 및 (B) 물을 함유하는 고정 지립 와이어 소용 수용성 가공액에 따르면, 칩이 혼입된 가공액의 증점을 억제할 수 있고, 가공액과 칩과의 반응을 억제하여 수소의 발생을 억제할 수 있고, 칩이 혼입된 가공액의 증점ㆍ겔화를 억제할 수 있다.According to the water-soluble working fluid for small-sized fixed abrasive wire containing at least one kind of water-soluble polymer selected from the group consisting of (A) polyvinyl pyrrolidone and a copolymer including vinyl pyrrolidone, and (B) water, It is possible to suppress the thickening of the processing liquid in which the chips are mixed and to inhibit the reaction between the processing liquid and the chip to suppress the generation of hydrogen and suppress the thickening and gelation of the processing liquid containing the chips.

Description

고정 지립 와이어 소용 수용성 가공액{AQUEOUS PROCESSING SOLUTION FOR FIXED ABRASIVE GRAIN WIRE SAW}{AQUEOUS PROCESSING SOLUTION FOR FIXED ABRASIVE GRAIN WIRE SAW}

본 발명은, 고정 지립 와이어 소(wire saw)용 수용성 가공액에 관한 것이며, 상세하게는 실리콘 웨이퍼를 고정 지립 와이어 소에 의해 절단 가공할 때에 사용하는 고정 지립 와이어 소용 수용성 가공액에 관한 것이다.TECHNICAL FIELD The present invention relates to a water-soluble working fluid for a wire saw, and more particularly to a water-soluble working fluid for use in cutting a silicon wafer with a fixed abrasive wire.

실리콘 웨이퍼의 제조 비용 감소를 도모하기 위해, 실리콘 웨이퍼의 절단 가공 기술의 향상이 중요해지고 있다. 실리콘 웨이퍼의 가공에 있어서는 유리 지립 방식에서의 와이어 소에 의한 절단이 주류를 이루고 있지만, 상기 유리 지립 방식의 가공에 있어서 이하의 다양한 문제가 있다.In order to reduce the manufacturing cost of the silicon wafer, it is important to improve the cutting processing technology of the silicon wafer. In the processing of silicon wafers, the cutting by the wire saw in the glass abrasive method is the mainstream, but there are the following various problems in the processing of the glass abrasive method.

(1) 가공액으로서, 오일제에 지립을 분산시킨 슬러리를 사용하기 때문에 유리 지립과 절단 부스러기와의 분리가 곤란하다. (2) 와이어 주행 속도에 제한이 있어 가공 능률 향상에 한계가 있다. (3) 절단 손실(kerf-loss)을 적게 하기 위해 와이어를 세선화한 경우에는, 가공 중에 단선이 일어나고, 수율이 저하된다. (4) 절단 손실을 적게 하기 위해 지립을 미립화한 경우에는, 슬러리 점도가 상승하고, 절단 손실을 많게 한다는 등 역효과의 문제가 지적되어 있다.(1) Since the slurry in which the abrasive grains are dispersed in the oil agent is used as the working fluid, it is difficult to separate the glass abrasive grains from the cutting debris. (2) There is a limitation in the wire running speed, which leads to limitations in improving the machining efficiency. (3) When the wire is thinned to reduce the kerf-loss, breakage occurs during processing, and the yield decreases. (4) In the case where the abrasive grains are atomized in order to reduce the cutting loss, it is pointed out that the slurry viscosity increases and the cutting loss is increased.

이러한 문제에 대하여, 최근 피아노선 등의 와이어 표면에 전착이나 레진 본드 등에 의해 다이아몬드 지립을 고정한 고정 지립 와이어 소가 개발되어 있다(특허문헌 1). 고정 지립 와이어 소를 이용하여 취성 재료를 가공하는 경우, 윤활, 냉각, 발생하는 칩(cut debris; 절단 부스러기)의 분산을 목적으로서 가공액을 이용한다. 상기 가공액으로서는, 인화성의 문제 등도 함께 생각하면, 수용성 가공액을 이용하는 것이 바람직하다. 그러나, 피삭재가 실리콘인 경우, 일반재에 비해 칩과 가공액과의 반응성이 높고, 실리콘 부스러기(칩)가 가공액 중의 수분 또는 알칼리와 반응하여 수소를 발생시키고, 인화될 우려가 있다. 따라서, 실리콘과의 반응성을 억제시킨 가공액인 것이 바람직하다. 이러한 관점에서 특허문헌 2에 개시된 바와 같은 가공액이 제안되어 있다.In response to such a problem, a fixed abrasive wire element in which diamond abrasive grains are fixed by electrodeposition, resin bond, or the like to a wire surface such as a piano wire has recently been developed (Patent Document 1). When a brittle material is processed by using a fixed abrasive wire element, the working fluid is used for the purpose of lubrication, cooling, and dispersion of generated chips (cut debris). It is preferable to use a water-soluble processing liquid as the above-mentioned processing liquid, considering the problem of flammability. However, when the workpiece is made of silicon, the reactivity between the chip and the processing liquid is higher than that of the general material, and silicon chips (chips) react with water or alkali in the processing liquid to generate hydrogen, and there is a fear that the substrate will be printed. Therefore, it is preferable that the treatment liquid is one which suppresses reactivity with silicon. From this point of view, a processing liquid as disclosed in Patent Document 2 has been proposed.

일본 특허 출원 제2001-054850호Japanese Patent Application No. 2001-054850 일본 특허 출원 제2003-082334호Japanese Patent Application No. 2003-082334

그러나, 최근 가공 정밀도를 향상시킴으로써 칩이 미세해지고, 특허문헌 2에 개시된 바와 같은 가공액에서는 충분한 안정성이 얻어지지 않는다는 것을 알 수 있었다. 특히, 칩이 혼입된 가공액의 점도가 상승하여, 다양한 문제가 발생한다는 것을 알 수 있었다. 또한, 수분을 다량으로 함유하여, pH가 알칼리성인 가공액의 경우에는 수소가 발생한다는 문제 뿐만 아니라, 증점, 겔화가 발생한다는 문제가 있었다.However, it has been found that by improving the processing precision in recent years, the chip becomes finer and sufficient stability can not be obtained in the processing liquid as disclosed in Patent Document 2. In particular, it has been found that the viscosity of the processing liquid containing the chips increases, resulting in various problems. Further, in the case of a processing liquid containing a large amount of water and having an alkaline pH, there has been a problem that not only hydrogen is generated but also thickening and gelation occur.

가공액의 증점, 겔화는, 하기의 문제를 발생한다.The thickening and gelation of the processing liquid cause the following problems.

(1) 와이어에 의해 반입되는 도입 유량이 변화되어, 두께 변동이 커진다(제품 품위의 열화).(1) The introduced flow rate introduced by the wire changes, and the thickness variation becomes large (deterioration of the product quality).

(2) 와이어 슬립이 발생하고, 와이어가 단선된다(수율의 저하).(2) Wire slip occurs and the wire is broken (reduction in yield).

(3) 후속 공정에서의 세정이 어려워진다(웨이퍼간의 칩, 오일제의 제거가 어려움).(3) Cleaning in a subsequent process becomes difficult (difficulty in removing chips and oil between wafers).

(4) 오일제의 수명이 짧고, 갱액량(更液量)이 증가한다(비용 증가).(4) The life of the oil agent is short, and the amount of the gangue solution is increased (the cost is increased).

따라서, 본 발명에서는, 칩이 혼입된 가공액의 증점을 억제할 수 있고, 가공액과 칩과의 반응을 억제하여 수소의 발생을 억제할 수 있고, 나아가 가공액의 증점ㆍ겔화를 억제할 수 있는 고정 지립 와이어 소용 수용성 가공액을 제공하는 것을 과제로 한다.Therefore, in the present invention, it is possible to suppress the thickening of the processing liquid containing the chips, suppress the reaction between the processing liquid and the chip, suppress the generation of hydrogen, and further suppress the thickening and gelation of the processing liquid And an object of the present invention is to provide a water-soluble working fluid for use with a fixed abrasive wire.

이상의 문제를 해결하기 위해 본 발명자들은 예의 검토하여, 이하의 사항을 발견하였다.In order to solve the above problems, the inventors of the present invention have made extensive studies and found the following.

(1) Si 칩의 혼입에 의한 점도의 상승은 혼입되는 Si 칩이 미분이기 때문에, 또한, Si 칩의 분산성이 떨어지기 때문에 발생한다.(1) The increase in the viscosity due to the incorporation of the Si chip is caused because the Si chip to be incorporated is a differential and also because the dispersibility of the Si chip is deteriorated.

(2) 상기 점도의 상승은 가공액에 소정의 수용성 고분자를 함유시키고, Si 칩의 분산성을 향상시킴으로써 해결할 수 있다.(2) The increase in the viscosity can be solved by containing a predetermined water-soluble polymer in the processing liquid and improving the dispersibility of the Si chip.

(3) 가공액에 Si 칩이 포함되어 있는 경우, Si 칩과 가공액이 반응하여, 수소가 발생하는 경우가 있다.(3) When the Si chip is contained in the processing liquid, the Si chip and the processing liquid may react with each other and hydrogen may be generated.

(4) 수분을 다량으로 함유하는 가공액의 경우에는, Si 칩을 함유함으로써 증점, 겔화가 발생하는 경우가 있다.(4) In the case of a processing liquid containing a large amount of water, the thickening and gelation may occur by containing Si chips.

(5) 상기 (3) 및 (4)의 문제는, 가공액에 소정의 수용성 고분자를 함유시킴으로써 해결할 수 있다.(5) The problems of (3) and (4) above can be solved by including a predetermined water-soluble polymer in the processing liquid.

본 발명자들은, 상기 문제에 대하여 예의 검토하여 이하의 발명을 완성시키기에 이르렀다.Means for Solving the Problems The inventors of the present invention have made extensive studies on the above problems and have completed the following inventions.

제1 본 발명은, (A) 폴리비닐피롤리돈, 및 비닐피롤리돈을 포함하는 공중합물로부터 선택되는 적어도 1종류 이상의 수용성 고분자, 및 (B) 물을 함유하는 고정 지립 와이어 소용 수용성 가공액(이하, 「본 발명의 가공액」이라 하는 경우가 있음)이다.The present invention relates to a water-soluble processing liquid for small-sized stationary graining wire comprising (A) at least one water-soluble polymer selected from polyvinyl pyrrolidone and a copolymer including vinyl pyrrolidone, and (B) (Hereinafter sometimes referred to as " processing liquid of the present invention ").

본 발명의 가공액은, (A) 성분으로서 소정의 수용성 고분자를 함유함으로써, 가공액 중에 실리콘 분말을 함유하는 경우 실리콘 분말의 분산성을 향상시킬 수 있으며, 실리콘 분말을 함유하는 가공액의 점도 상승을 억제할 수 있다. 또한, 가공액과 실리콘 분말이 반응하여 수소가 발생하는 것을 억제함과 함께, 실리콘 분말을 함유하는 가공액의 증점, 겔화를 억제할 수 있다.The processing liquid of the present invention contains a predetermined water-soluble polymer as the component (A), so that the dispersibility of the silicon powder can be improved when the processing liquid contains silicon powder, and the viscosity of the processing liquid containing the silicon powder Can be suppressed. In addition, it is possible to suppress the generation of hydrogen due to the reaction of the working fluid and the silicon powder, and to suppress the thickening and gelation of the working fluid containing the silicon powder.

제1 본 발명에 있어서, 상기 (A) 성분의 중량 평균 분자량은 2,000 내지 1,000,000인 것이 바람직하다.In the first aspect of the present invention, the weight average molecular weight of the component (A) is preferably 2,000 to 1,000,000.

제1 본 발명에 있어서, 상기 (A) 성분의 함유량은 고정 지립 와이어 소용 수용성 가공액 전체의 질량을 100 질량％로 하여, 0.02 질량％ 이상 7 질량％ 이하로 하는 것이 바람직하다.In the first aspect of the present invention, the content of the component (A) is preferably 0.02 mass% or more and 7 mass% or less based on 100 mass% of the total mass of the water-soluble working fluid for fixed abrasive wire.

제1 본 발명의 고정 지립 와이어 소용 수용성 가공액은, (C) 다가 카르복실산의 알칼리염을 더 함유하는 것이 바람직하다. 상기 (C) 성분의 함유량은, 고정 지립 와이어 소용 수용성 가공액 전체의 질량을 100 질량％로 하여, 0.01 질량％ 이상 10 질량％ 이하인 것이 바람직하다. 본 발명의 가공액은, (C) 성분으로서 다가 카르복실산의 알칼리염을 함유함으로써 분산성, 세정성, 내부식성을 부여하는 것이 용이해진다.The water-soluble working liquid for immobilizing a fixed abrasive wire of the first invention preferably further contains (C) an alkali salt of a polycarboxylic acid. The content of the component (C) is preferably 0.01% by mass or more and 10% by mass or less based on 100% by mass of the total amount of the water-soluble processing liquid for small-diameter fixed-wiring wires. The working fluid of the present invention contains an alkaline salt of a polycarboxylic acid as the component (C), thereby making it easy to impart dispersibility, cleaning property and corrosion resistance.

제1 본 발명의 고정 지립 와이어 소용 수용성 가공액은, (D) 글리콜류, 글리콜에테르류, 및 폴리옥시알킬렌글리콜류로 이루어지는 군으로부터 선택되는 1종 이상을 더 함유하는 것이 바람직하다. 상기 (D) 성분의 함유량은, 고정 지립 와이어 소용 수용성 가공액 전체의 질량을 100 질량％로 하여, 0.1 질량％ 이상 95 질량％ 이하인 것이 바람직하다.The water-soluble working fluid for small-diameter fixed abrasive wire of the first invention of the present invention preferably further contains at least one kind selected from the group consisting of (D) glycols, glycol ethers, and polyoxyalkylene glycols. The content of the component (D) is preferably 0.1% by mass or more and 95% by mass or less based on 100% by mass of the total amount of the water-soluble processing liquid for small-diameter fixed-wiring wires.

제1 본 발명의 고정 지립 와이어 소용 수용성 가공액의 점도는, 25 ℃에서 50 mPaㆍs 이하인 것이 바람직하다. 가공액 자체의 점도가 높으면, 실리콘 분말을 함유하는 가공액의 점도는 더욱 높아진다. 따라서, 가공액 자체의 점도는 소정의 값 이하인 것이 바람직하다.The viscosity of the water-soluble working liquid for immobilizing a fixed abrasive wire of the first aspect of the present invention is preferably 50 mPa s or less at 25 캜. If the viscosity of the processing liquid itself is high, the viscosity of the processing liquid containing the silicon powder becomes higher. Therefore, the viscosity of the processing liquid itself is preferably a predetermined value or less.

제1 본 발명의 고정 지립 와이어 소용 수용성 가공액에, 평균 입경 1.5 ㎛의 실리콘 분말을 10 질량％ 첨가하여 교반하여 형성한 가공액(의사 사용액)의 점도는, 25 ℃에서 100 mPaㆍs 이하인 것이 바람직하다. 소정의 실리콘 분말을 함유하는 의사 사용액의 점도가 높으면, 상기 과제의 란에 기재한 여러 문제가 발생할 우려가 있다.The viscosity of a working fluid (physiological solution) formed by adding 10 mass% of silicon powder having an average particle diameter of 1.5 탆 to the water-soluble working fluid for fixed abrasive wire of the first invention of the present invention and stirring the mixture is 100 mPa s or less at 25 캜 desirable. If the viscosity of the physiological solution containing a predetermined amount of silicon powder is high, various problems described in the column of the above-mentioned problems may occur.

본 발명의 고정 지립 와이어 소용 수용성 가공액에 따르면, 소정의 수용성 고분자를 함유하고 있기 때문에, 상기 가공액이 실리콘칩인 실리콘 분말을 함유하는 경우 상기 실리콘 분말을 가공액 중에 분산시킬 수 있다. 따라서, 실리콘 분말을 함유하는 가공액의 점도 상승을 억제할 수 있다. 또한, 본 발명의 가공액은, 소정의 수용성 고분자를 함유하고 있기 때문에 실리콘 분말과 가공액이 반응하여 수소를 발생하는 것을 억제할 수 있으며, 실리콘 분말을 함유하는 가공액의 증점, 겔화를 억제할 수 있다.According to the water-soluble working fluid for fixed abrasive wire of the present invention, since the water-soluble polymer contains a predetermined water-soluble polymer, the silicon powder can be dispersed in the working fluid when the working fluid contains silicon powder as a silicon chip. Therefore, it is possible to suppress the viscosity increase of the processing liquid containing the silicon powder. Further, since the processing liquid of the present invention contains a predetermined water-soluble polymer, generation of hydrogen by reaction between the silicon powder and the processing liquid can be suppressed, and the processing liquid containing silicon powder can be prevented from thickening and gelation .

<고정 지립 와이어 소용 수용성 가공액><Water-soluble processing liquid for fixed abrasive wire>

본 발명의 고정 지립 와이어 소용 수용성 가공액은, (A) 폴리비닐피롤리돈, 및 비닐피롤리돈을 포함하는 공중합물로부터 선택되는 적어도 1종류 이상의 수용성 고분자, 및 (B) 물을 함유하고 있다.The water-soluble working liquid for immobilizing a fixed abrasive wire of the present invention contains (A) at least one water-soluble polymer selected from polyvinyl pyrrolidone and a copolymer including vinyl pyrrolidone, and (B) water .

((A) 성분)(Component (A))

본 발명의 가공액은, (A) 성분으로서 폴리비닐피롤리돈, 및 비닐피롤리돈을 포함하는 공중합물로부터 선택되는 적어도 1종류 이상의 수용성 고분자를 함유하고 있다. 이 수용성 고분자를 가공액에 함유시킴으로써, 실리콘 분말을 함유하여 이루어지는 가공액 중에서 상기 실리콘 분말의 분산성을 향상시킬 수 있다. 그 때문에, 실리콘 분말을 함유하여 이루어지는 가공액의 점도의 상승을 억제할 수 있다. 또한, 실리콘 분말과 가공액과의 반응을 억제하여, 실리콘 분말을 함유하여 이루어지는 가공액에 있어서 수소가 발생하는 것을 억제할 수 있다. 또한, 실리콘 분말을 함유하여 이루어지는 가공액의 증점, 겔화를 억제할 수 있다.The working fluid of the present invention contains at least one water-soluble polymer selected from a copolymer including polyvinyl pyrrolidone and vinyl pyrrolidone as the component (A). By including the water-soluble polymer in the working fluid, the dispersibility of the silicon powder in the working fluid containing the silicon powder can be improved. Therefore, an increase in the viscosity of the processing liquid containing the silicon powder can be suppressed. Further, the reaction between the silicon powder and the working fluid can be suppressed, and hydrogen generation in the working fluid containing the silicon powder can be suppressed. Further, the thickening and gelation of the processing liquid containing the silicon powder can be suppressed.

겔 투과 크로마토그래피/다각도 레이저 광 산란 검출기법에 의한 (A) 성분의 수용성 고분자의 중량 평균 분자량은 하한이 바람직하게는 2,000 이상, 보다 바람직하게는 8,000 이상이고, 상한이 바람직하게는 1,000,000 이하, 보다 바람직하게는 700,000 이하, 더욱 바람직하게는 500,000 이하이다. 상기 범위를 벗어나 분자량이 지나치게 작으면, (A) 성분을 넣는 효과가 발현되지 않게 될 우려가 있고, 반대로 분자량이 지나치게 크면 응집이나 가공액의 점도가 지나치게 높아질 우려가 있다.The weight average molecular weight of the water-soluble polymer as the component (A) by the gel permeation chromatography / polygonal laser light scattering detection technique is preferably 2,000 or more, more preferably 8,000 or more, and the upper limit is preferably 1,000,000 or less Preferably 700,000 or less, and more preferably 500,000 or less. If the molecular weight is excessively smaller than the above range, the effect of adding the component (A) may not be exhibited. Conversely, if the molecular weight is too large, the viscosity of the aggregation or the processing liquid may become excessively high.

(A) 성분의 함유량은, 고정 지립 와이어 소용 수용성 가공액 전체의 질량을 기준(100 질량％)으로 하여, 하한이 바람직하게는 0.02 질량％ 이상, 보다 바람직하게는 0.05 질량％ 이상, 더욱 바람직하게는 0.2 질량％ 이상이고, 상한이 바람직하게는 7 질량％ 이하, 보다 바람직하게는 5 질량％ 이하, 더욱 바람직하게는 3 질량％ 이하이다. 상기 범위를 벗어나 (A) 성분의 함유량이 지나치게 적으면 증점의 억제 효과, 수소 발생 억제 효과가 불충분해질 우려가 있고, 반대로 지나치게 많으면 가공액의 점도가 높아질 우려가 있다.The content of the component (A) is preferably 0.02% by mass or more, more preferably 0.05% by mass or more, still more preferably 0.05% by mass or more, still more preferably 0.05% Is not less than 0.2 mass%, and the upper limit thereof is preferably not more than 7 mass%, more preferably not more than 5 mass%, further preferably not more than 3 mass%. If the content of the component (A) is too small outside the above range, the effect of inhibiting the thickening and the hydrogen generation may be insufficient.

(A) 성분의 수용성 고분자는, 폴리비닐피롤리돈, 또는 비닐피롤리돈을 포함하는 공중합체이며, 이들은 2종 이상을 혼합하여 사용할 수도 있다. 비닐피롤리돈을 포함하는 공중합체는, 비닐피롤리돈 단위의 비율이 공중합체 전체를 기준으로 하여 바람직하게는 60 몰％ 이상이다. 비닐피롤리돈과 공중합시키는 단량체로서는, 아세트산비닐을 들 수 있다.The water-soluble polymer of component (A) is a copolymer containing polyvinylpyrrolidone or vinylpyrrolidone, and they may be used in a mixture of two or more. In the copolymer containing vinylpyrrolidone, the proportion of vinylpyrrolidone units is preferably at least 60 mol% based on the entire copolymer. As the monomer copolymerizing with vinyl pyrrolidone, vinyl acetate can be mentioned.

((C) 성분)(Component (C)) [

본 발명의 가공액은, (C) 성분으로서 다가 카르복실산의 알칼리염을 더 함유하고 있을 수도 있다. (C) 성분을 첨가하여, 그의 첨가량을 조정함으로써, 분산성, 세정성이나 내부식성을 부여한다는 효과가 있다.The working liquid of the present invention may further contain an alkaline salt of a polycarboxylic acid as the component (C). (C) is added, and the amount of the component (C) is adjusted so as to impart dispersibility, cleaning property and corrosion resistance.

다가 카르복실산으로서는, 아디프산, 옥살산, 도데칸디오산, 시트르산, 말산 등을 들 수 있다. 알칼리로서는, 수산화칼륨, 수산화나트륨 등의 알칼리 금속의 수산화물, 트리에탄올아민, 트리이소프로판올아민, 에틸렌디아민, N-(2-아미노에틸)-2-아미노에탄올 등의 아민을 들 수 있다.Examples of the polycarboxylic acid include adipic acid, oxalic acid, dodecanedioic acid, citric acid, malic acid and the like. Examples of the alkali include hydroxides of alkali metals such as potassium hydroxide and sodium hydroxide, and amines such as triethanolamine, triisopropanolamine, ethylenediamine and N- (2-aminoethyl) -2-aminoethanol.

(C) 성분의 함유량은, 본 발명의 가공액 전체의 질량을 기준(100 질량％)으로 하여, 하한이 바람직하게는 0.01 질량％ 이상, 보다 바람직하게는 0.1 질량％ 이상이고, 상한이 바람직하게는 10 질량％ 이하, 보다 바람직하게는 2 질량％ 이하, 더욱 바람직하게는 1 질량％ 이하이다. 상기 범위를 벗어나 (C) 성분의 함유량이 지나치게 적으면, (C) 성분을 첨가하는 효과가 발휘되기 어려워지고, 반대로 지나치게 많으면 증점, 겔화나 원액으로부터의 석출의 우려가 있다.The content of the component (C) is preferably 0.01 mass% or more, more preferably 0.1 mass% or more, and the upper limit is preferably 100 mass% or less, Is 10 mass% or less, more preferably 2 mass% or less, and further preferably 1 mass% or less. If the content of the component (C) is excessively small outside the above range, the effect of adding the component (C) becomes difficult to exhibit. On the other hand, if it is excessively large, there is a fear of thickening, gelation or precipitation from the raw liquid.

((D) 성분)(Component (D))

본 발명의 가공액은, (D) 성분으로서 글리콜류, 글리콜에테르류, 및 폴리옥시알킬렌글리콜류로 이루어지는 군으로부터 선택되는 1종 이상을 더 함유하고 있을 수도 있다. (D) 성분을 함유함으로써, 윤활성, 습윤성을 부여한다는 효과가 있다.The working fluid of the present invention may further contain at least one component selected from the group consisting of glycols, glycol ethers, and polyoxyalkylene glycols as the component (D). (D), it has an effect of imparting lubricity and wettability.

글리콜류로서는, 프로필렌글리콜, 디에틸렌글리콜, 에틸렌글리콜, 부틸렌글리콜 등을 들 수 있다. 글리콜에테르류로서는 상기 글리콜류의 알킬에테르를 들 수 있고, 알킬기로서는 메틸기, 에틸기, 부틸기 등을 들 수 있다. 또한, 글리콜류의 히드록시기의 일부가 알킬에테르로 되어 있을 수도 있고, 전부가 알킬에테르로 되어 있을 수도 있다. 글리콜에테르류의 구체예로서는, 디에틸렌글리콜모노에틸에테르, 디에틸렌글리콜디에틸에테르, 프로필렌글리콜모노에틸에테르 등을 들 수 있다.Examples of the glycols include propylene glycol, diethylene glycol, ethylene glycol, and butylene glycol. Examples of the glycol ethers include alkyl ethers of the above-mentioned glycols. Examples of the alkyl groups include methyl, ethyl and butyl. In addition, some of the hydroxyl groups of the glycols may be alkyl ethers, or all of them may be alkyl ethers. Specific examples of glycol ethers include diethylene glycol monoethyl ether, diethylene glycol diethyl ether, propylene glycol monoethyl ether and the like.

폴리옥시알킬렌글리콜류로서는, 폴리에틸렌글리콜, 폴리프로필렌글리콜, 폴리옥시에틸렌과 폴리옥시프로필렌의 공중합체 등을 들 수 있으며, 중량 평균 분자량(겔 투과 크로마토그래피를 이용한 폴리스티렌 환산)이 바람직하게는 10000 이하, 보다 바람직하게는 5000 이하, 더욱 바람직하게는 400 이하인 것을 이용한다.Examples of the polyoxyalkylene glycols include polyethylene glycol, polypropylene glycol, and copolymers of polyoxyethylene and polyoxypropylene. The weight average molecular weight (in terms of polystyrene using gel permeation chromatography) is preferably 10,000 or less More preferably 5000 or less, further preferably 400 or less.

(D) 성분의 함유량은, 본 발명의 가공액 전체의 질량을 기준(100 질량％)으로 하여, 하한이 바람직하게는 0.1 질량％ 이상, 보다 바람직하게는 0.5 질량％ 이상, 더욱 바람직하게는 1 질량％ 이상, 더욱 바람직하게는 3 질량％ 이상, 특히 바람직하게는 10 질량％ 이상이고, 상한이 바람직하게는 95 질량％ 이하, 보다 바람직하게는 90 질량％ 이하, 더욱 바람직하게는 80 질량％ 이하이다. 상기 범위를 벗어나 (D) 성분의 함유량이 지나치게 적으면 (D) 성분을 넣는 효과가 발현되지 않게 되고, 반대로 (D) 성분의 함유량이 지나치게 많으면 냉각성이 저하될 우려가 있다.The content of the component (D) is preferably not less than 0.1% by mass, more preferably not less than 0.5% by mass, further preferably not less than 1% by mass, based on the total mass of the processing liquid of the present invention (100% More preferably not less than 95% by mass, more preferably not less than 90% by mass, further preferably not more than 80% by mass, to be. If the content of the component (D) is too small, the effect of adding the component (D) is not exhibited. If the content of the component (D) is excessively large, the cooling property may be deteriorated.

본 발명의 가공액은 상기한 (A) 성분을 함유하고, 경우에 따라서는 (C) 성분 및 (D) 성분을 더 함유하고 있으며, 잔부는 (B) 물로 되어 있다. 물로서는, 증류수, 수돗물 등, 그의 종류는 특별히 한정되지 않는다. 또한, (B) 물의 함유량이 많은 가공액에서는, 실리콘 분말을 함유하는 가공액이 증점되고, 겔화되기 쉽다. 이에 비해, 본 발명의 가공액에서는 물의 함유량이 많은 조성, 예를 들면 가공액 전체의 질량을 기준으로서 물이 90 질량％ 이상이 된 조성에 있어서도, 실리콘 분말을 함유하는 가공액의 증점ㆍ겔화를 억제할 수 있다.The working fluid of the present invention contains the above-mentioned component (A), and in some cases, the component (C) and the component (D) are further contained, and the balance is (B) water. As the water, distilled water, tap water and the like are not particularly limited. Further, in the case of the (B) processing liquid having a large water content, the processing liquid containing the silicon powder is thickened and is likely to gel. On the contrary, in the processing liquid of the present invention, even in a composition having a high water content, for example, a composition in which water is 90 mass% or more based on the mass of the entire processing liquid, the processing liquid containing silicon powder is subjected to the thickening and gelation .

<가공액의 성상>&Lt; Characteristics of machining liquid &

본 발명의 가공액의 점도는 25 ℃에서 바람직하게는 50 mPaㆍs 이하이고, 보다 바람직하게는 25 mPaㆍs 이하, 더욱 바람직하게는 20 mPaㆍs 이하이다. 또한, 본 발명의 가공액에 소정의 실리콘 분말을 분산시킨 가공액(의사 사용액)의 점도는 25 ℃에서 100 mPaㆍs, 바람직하게는 55 mPaㆍs 이하이고, 보다 바람직하게는 50 mPaㆍs 이하이고, 더욱 바람직하게는 45 mPaㆍs 이하이다. 상기 의사 사용액의 점도는, 본 발명의 가공액에 실리콘 분말(입경: 1.5 ㎛)을 10 질량％ 첨가하고, 교반 혼합한 후, 스테인리스강구(직경 2 mm)를 넣고, 1000 rpm으로 10시간 동안 교반하고, 상기 스테인리스강구를 여과 분별하여 얻어진 의사 사용액에 대하여 측정한 것이다. 상기한 가공액 자체의 점도가 지나치게 높으면, 실리콘 분말을 함유하는 의사 사용액의 점도도 필연적으로 높아진다. 또한, 의사 사용액의 점도가 지나치게 높으면, 상기 과제의 란에서 설명한 여러 문제가 발생할 우려가 있다. 또한, 가공액 및 의사 사용액의 점도는 브룩필드(Brookfield)형 점도계로 측정할 수 있다.The viscosity of the working liquid of the present invention at 25 캜 is preferably 50 mPa s or less, more preferably 25 mPa s or less, and further preferably 20 mPa s or less. The viscosity of the working fluid (pseudo solution) in which a predetermined amount of silicon powder is dispersed in the working fluid of the present invention is 100 mPa s, preferably 55 mPa s, more preferably 50 mPa 쨌 s Or less, and more preferably 45 mPa s or less. The viscosity of the doctor's solution was determined by adding 10 mass% of silicon powder (particle diameter: 1.5 占 퐉) to the working solution of the present invention, mixing with stirring, adding a stainless steel ball (diameter: 2 mm), stirring at 1000 rpm for 10 hours , And the stainless steel balls were measured for the doctor's service liquid obtained by filtration. If the viscosity of the processing liquid itself is excessively high, the viscosity of the liquid for the doctor's use containing the silicon powder inevitably becomes high. In addition, if the viscosity of the physician's solution is too high, various problems described in the column of the above-mentioned problem may occur. In addition, the viscosity of the working solution and the physiological solution can be measured with a Brookfield viscometer.

가공액의 pH는, 바람직하게는 5.0 이상 9.0 이하이다. 가공액의 pH가 지나치게 낮은 경우에는, 상기 가공액이 닿는 철재 또는 와이어의 부식이 발생할 우려가 있으며, 반대로 가공액의 pH가 지나치게 높은 경우에는, 가공액과 실리콘 분말이 반응하여 수소가 발생할 우려가 있다. 본 발명의 가공액은 물에 희석하여 사용할 수도 있지만, 이 경우에도 희석 후의 가공액의 pH는 상기 범위인 것이 바람직하다.The pH of the processing liquid is preferably 5.0 or more and 9.0 or less. If the pH of the processing liquid is excessively low, there is a possibility that corrosion of the iron or wire that the processing liquid touches may occur. Conversely, if the pH of the processing liquid is excessively high, have. The working solution of the present invention may be diluted with water. In this case, however, it is preferable that the pH of the diluted working solution is in the above range.

[실시예][Example]

<실시예 1 내지 13, 비교예 1 내지 5>&Lt; Examples 1 to 13 and Comparative Examples 1 to 5 >

본 발명의 고정 지립 와이어 소용 수용성 가공액(실시예 1 내지 13) 및 본 발명 이외의 고정 지립 와이어 소용 수용성 가공액(비교예 1 내지 5)을 표 1 내지 3에 나타낸 바와 같은 조성이 되도록 제작하였다. 제작한 가공액의 pH를 측정함과 함께, 브룩필드형 점도계로 25 ℃에서의 점도를 측정하였다.(Examples 1 to 13) of the present invention and water-soluble working fluids (Comparative Examples 1 to 5) for immobilizing fixed abrasive wires other than the present invention (Comparative Examples 1 to 5) were prepared so as to have compositions as shown in Tables 1 to 3 . The pH of the fabricated liquid was measured and the viscosity at 25 캜 was measured with a Brookfield viscometer.

또한, 각 가공액에 실리콘 분말(평균 입자계 1.5 m)을 10 질량％ 첨가하고, 교반 혼합한 후, 스테인리스강구(직경 2 mm)를 넣고, 1000 rpm으로 10시간 동안 교반하여 의사 사용액을 형성하였다. 상기 의사 사용액으로부터, 철망(50 메쉬)으로 스테인리스강구를 여과 분별한 후, 브룩필드형 점도계로 상기 의사 사용액의 점도(mPaㆍs, 25 ℃)를 측정하였다. 또한, 의사 사용액 10 ml를 50 ℃로 가열하고, 30분간에 발생하는 수소량(ml)을 측정하였다.10% by mass of silicon powder (average particle size 1.5 m) was added to each of the working solutions, stirred and mixed, and then stainless steel balls (diameter: 2 mm) were added and stirred at 1000 rpm for 10 hours to form a physiological solution . The stainless steel ball was separated from the physician solution by a wire mesh (50 mesh) by filtration, and then the viscosity (mPa · s, 25 ° C) of the physiological solution was measured with a Brookfield viscometer. In addition, 10 ml of the physician solution was heated to 50 占 폚, and the amount of hydrogen (ml) generated in 30 minutes was measured.

또한, 폴리비닐피롤리돈(PVP)의 중량 평균 분자량은 PVP K-15가 9700이고, PVP K-30이 70000이고, PVP K-60이 400000이었다. 또한, PVP/VA는 비닐피롤리돈과 아세트산비닐과의 공중합체이고, 중량 평균 분자량이 32,000, 공중합체 중의 비닐피롤리돈의 비율이 70 몰％이다.The weight average molecular weight of polyvinyl pyrrolidone (PVP) was 9700 for PVP K-15, 70000 for PVP K-30 and 400000 for PVP K-60. PVP / VA is a copolymer of vinyl pyrrolidone and vinyl acetate, and has a weight average molecular weight of 32,000 and a vinyl pyrrolidone ratio of 70 mol% in the copolymer.

Figure 112013005524633-pct00001
Figure 112013005524633-pct00001

Figure 112013005524633-pct00002
Figure 112013005524633-pct00002

Figure 112013005524633-pct00003
Figure 112013005524633-pct00003

비교예의 가공액에서는 모두 의사 사용액 점도가 상승하고, 55 mPaㆍs를 초과하였다. 이에 비해, 본 발명의 가공액(실시예 1 내지 13)은 의사 사용액에 있어서도 점도 변화가 작고, 모두 45 mPaㆍs 이하이다.In the case of the working liquid of the comparative example, the viscosity of the physically active liquid increased and exceeded 55 mPa 占 퐏. On the other hand, the processed liquids of the present invention (Examples 1 to 13) show little change in viscosity even in a physiological solution and are all 45 mPa.s or less.

실시예 1 내지 3, 비교예 1, 2는 원액을 10배로 희석한 것이다. 따라서, 원액의 조성은 각 화합물이 10배량이다.In Examples 1 to 3 and Comparative Examples 1 and 2, the stock solution was diluted 10-fold. Therefore, the composition of the stock solution is 10 times the amount of each compound.

(그룹 I)(Group I)

그룹 I은 실시예 1 내지 6, 및 비교예 1 내지 3이며, 수분량이 많은 가공액의 예이다. 비교예의 가공액이며, 수분량이 많은 조성(비교예 1 내지 3)은, 모두 증점ㆍ겔화되었지만, PVP를 첨가한 본 발명의 가공액(실시예 1 내지 6)은 겔화되지 않고, 거의 증점되지 않았다.Group I is Examples 1 to 6 and Comparative Examples 1 to 3, and is an example of a processing liquid having a large amount of water. The compositions (Comparative Examples 1 to 3) which were the working liquids of Comparative Examples and Comparative Examples 1 to 3 were all thickened and gelated, but the processed liquid of the present invention (Examples 1 to 6) to which PVP had been added did not gel and hardly thickened .

또한, 수소 발생량에 대해서는, 실시예 1 내지 6에서는 수소 발생이 5 ml 이하인 데 비해, 비교예 1 내지 3에서는 수소 발생량이 15 ml 이상으로 매우 많았다.With respect to the amount of hydrogen generation, hydrogen generation was 5 ml or less in Examples 1 to 6, and hydrogen generation amount in Comparative Examples 1 to 3 was 15 ml or more.

(그룹 II)(Group II)

그룹 II는 실시예 7 내지 12, 및 비교예 4이며, (C) 성분 및 (D) 성분의 종류 및 양을 통일시키고, (A) 성분에 대하여 변화시킨 것이다. 이로부터, 각종 폴리비닐피롤리돈(PVP), 비닐피롤리돈/아세트산비닐 공중합체(PVP/VA)의 증점 억제 효과가 나타났다.Group II is Examples 7 to 12 and Comparative Example 4, and the kinds and amounts of the components (C) and (D) are unified and changed with respect to the component (A). From this, the effect of inhibiting the thickening of various polyvinylpyrrolidone (PVP) and vinylpyrrolidone / vinyl acetate copolymer (PVP / VA) was shown.

또한, 수소 발생량에 대해서는, 실시예 7 내지 12와 비교예 4를 비교하면, 폴리비닐피롤리돈 등을 포함하는 본 발명의 가공액은 수소 발생량이 적었다.Further, as for the amount of hydrogen generation, when comparing Examples 7 to 12 and Comparative Example 4, the processing liquid of the present invention including polyvinylpyrrolidone and the like produced less hydrogen.

(그룹 III)(Group III)

그룹 III은 실시예 13과 비교예 5이며, 그룹 I, 그룹 II와 상이한 (D) 성분을 포함하는 것이다. 이로부터 (D) 성분의 종류를 막론하고 폴리비닐피롤리돈(PVP)에 의한 증점 억제의 효과가 나타났다.Group III is Example 13 and Comparative Example 5, and includes the components (D) different from Group I and Group II. From this, the effect of inhibiting the thickening by polyvinylpyrrolidone (PVP) regardless of the kind of the component (D) was shown.

또한, 실시예 13과 비교예 5를 비교하면, 폴리비닐피롤리돈을 포함하는 실시예 13은 수소 발생량이 적었다.In comparison between Example 13 and Comparative Example 5, in Example 13 including polyvinylpyrrolidone, the amount of hydrogen generation was small.

이상으로부터, 폴리비닐피롤리돈, 및 비닐피롤리돈을 포함하는 공중합물로부터 선택되는 적어도 1종류 이상의 수용성 고분자를 포함하는 본 발명의 가공액은, 실리콘 분말을 분산시킨 의사 사용액에 있어서, 점도 상승을 억제함과 함께 수소 발생을 억제하는 효과가 있다는 것이 나타났다.From the above, it can be seen that the processing liquid of the present invention comprising at least one kind of water-soluble polymer selected from polyvinylpyrrolidone and copolymers including vinylpyrrolidone has a viscosity increase And suppress the generation of hydrogen.

이상, 현시점에서 가장 실천적이면서도 바람직하다고 생각되는 실시 형태와 관련하여 본 발명을 설명했지만, 본 발명은, 본원 명세서 중에 개시된 실시 형태로 한정되는 것은 아니며, 특허청구범위 및 명세서 전체로부터 이해되는 발명의 요지 또는 사상에 반하지 않는 범위에서 적절하게 변경 가능하고, 그와 같은 변경을 수반하는 고정 지립 와이어 소용 수용성 가공액도 또한 본 발명의 기술적 범위에 포함되는 것으로서 이해되어야 한다.While the present invention has been described with reference to the embodiment which is presently considered to be the most practical and preferred at present, the present invention is not limited to the embodiments disclosed in the specification, but may be embodied in the gist of the invention And the water-soluble working liquid for the fixed abrasive wire accompanied by such changes should also be understood as being included in the technical scope of the present invention.

본 발명의 고정 지립 와이어 소용 수용성 가공액은, 고정 지립 와이어 소를 이용하여 실리콘 웨이퍼를 절단할 때에 특히 바람직하게 사용할 수 있다.INDUSTRIAL APPLICABILITY The water-soluble working liquid for immobilizing a fixed abrasive wire of the present invention can be particularly preferably used for cutting a silicon wafer using a fixed abrasive wire.

Claims (9)

(A) 폴리비닐피롤리돈, 및 비닐피롤리돈을 포함하는 공중합물로부터 선택되는 적어도 1종류 이상의 수용성 고분자,
(B) 물,
(C) 다가 카르복실산의 알칼리염, 및
(D) 글리콜류, 글리콜에테르류, 및 폴리옥시알킬렌글리콜류로 이루어지는 군으로부터 선택되는 1종 이상
을 함유함과 동시에, 유리 지립을 포함하지 않는 고정 지립 와이어 소(wire saw)용 수용성 가공액이며,
상기 (A) 성분의 함유량이 고정 지립 와이어 소용 수용성 가공액 전체의 질량을 100 질량％로 하여, 0.02 질량％ 이상 7 질량％ 이하이고,
상기 (C) 성분의 함유량이 고정 지립 와이어 소용 수용성 가공액 전체의 질량을 100 질량％로 하여, 0.01 질량％ 이상 10 질량％ 이하이고,
상기 (D) 성분의 함유량이 고정 지립 와이어 소용 수용성 가공액 전체의 질량을 100 질량％로 하여, 0.1 질량％ 이상 95 질량％ 이하인 고정 지립 와이어 소용 수용성 가공액.(A) at least one water-soluble polymer selected from polyvinyl pyrrolidone, and copolymers comprising vinyl pyrrolidone,
(B) water,
(C) an alkali salt of a polycarboxylic acid, and
(D) at least one compound selected from the group consisting of glycols, glycol ethers, and polyoxyalkylene glycols
And is a water-soluble working fluid for a fixed abrasive wire wire saw which does not contain glass abrasive grains,
Wherein the content of the component (A) is 0.02 mass% or more and 7 mass% or less based on 100 mass% of the total mass of the water-soluble working fluid for fixed abrasive wire,
Wherein the content of the component (C) is 0.01% by mass or more and 10% by mass or less based on 100% by mass of the total amount of the water-soluble working fluid for fixed-
Wherein the content of the component (D) is 0.1% by mass or more and 95% by mass or less based on 100% by mass of the total amount of the water-soluble working liquid for fixed abrasive wire. 제1항에 있어서, 상기 (A) 성분의 중량 평균 분자량이 2,000 내지 1,000,000인 고정 지립 와이어 소용 수용성 가공액.The water-soluble working fluid according to claim 1, wherein the component (A) has a weight average molecular weight of from 2,000 to 1,000,000. 제1항 또는 제2항에 있어서, 상기 (A) 성분의 함유량이 고정 지립 와이어 소용 수용성 가공액 전체의 질량을 100 질량％로 하여, 0.2 질량％ 이상 7 질량％ 이하인 고정 지립 와이어 소용 수용성 가공액.A water-soluble processing liquid for small-sized fixed-abrasive wire according to claim 1 or 2, wherein the content of the component (A) is 0.2% by mass or more and 7% by mass or less based on 100% by mass of the entire water- . 제1항 또는 제2항에 있어서, 가공액의 점도가 25 ℃에서 50 mPaㆍs 이하인 고정 지립 와이어 소용 수용성 가공액.3. The water-soluble machining liquid according to claim 1 or 2, wherein the viscosity of the working fluid is 50 mPa.s or less at 25 DEG C. 제1항 또는 제2항에 있어서, 상기 가공액에 평균 입경 1.5 ㎛의 실리콘 분말을 10 질량％ 첨가하여 교반하여 형성한 의사 사용액의 점도가 25 ℃에서 100 mPaㆍs 이하인 고정 지립 와이어 소용 수용성 가공액.The process according to any one of claims 1 to 5, further comprising the step of adding a silicon powder having an average particle diameter of 1.5 탆 in an amount of 10 mass% liquid. 삭제delete 삭제delete 삭제delete 삭제delete
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Families Citing this family (4)

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Publication number Priority date Publication date Assignee Title
JP2012172117A (en) * 2011-02-23 2012-09-10 Yushiro Chemical Industry Co Ltd Water-soluble working fluid for fixed abrasive grain wire saw
JP6039935B2 (en) * 2012-06-29 2016-12-07 出光興産株式会社 Aqueous processing fluid
JP6819619B2 (en) * 2018-01-22 2021-01-27 信越半導体株式会社 Work cutting method and wire saw
CN110497546A (en) * 2019-08-26 2019-11-26 哈尔滨商业大学 The method and apparatus of free-consolidation abrasive compound multiline cut silicon chips

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000296455A (en) 1999-04-09 2000-10-24 Tokyo Seimitsu Co Ltd Fixed abrasive grain multi-wire saw
KR100494296B1 (en) * 2001-09-07 2005-06-10 다이이치 고교 세이야쿠 가부시키가이샤 nonflammable water-based cutting fluid composition and nonflammable water-based cutting fluid
JP2009013301A (en) * 2007-07-05 2009-01-22 Adeka Corp Additive for dicing cutting water and cutting work method using its additive

Family Cites Families (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6243482A (en) * 1985-08-21 1987-02-25 Sanyo Chem Ind Ltd Abrasion working fluid
CN1057478A (en) * 1990-06-22 1992-01-01 薛志纯 Metal working fluid
US5401428A (en) * 1993-10-08 1995-03-28 Monsanto Company Water soluble metal working fluids
JP3869520B2 (en) * 1997-03-21 2007-01-17 株式会社ネオス Water-soluble cutting fluid for wire saw
JP2001054850A (en) 1999-08-11 2001-02-27 Osaka Diamond Ind Co Ltd Hard brittle material cutting method by means of fixed abrasive grain wire saw
JP2002096251A (en) * 1999-09-17 2002-04-02 Sumitomo Special Metals Co Ltd Cutting method and cutting apparatus for rare earth alloys
JP2001138205A (en) * 1999-11-08 2001-05-22 Sumitomo Special Metals Co Ltd Method and apparatus for cutting rare earth alloy
JP2002167589A (en) * 2000-11-30 2002-06-11 Nippon Shokubai Co Ltd Metal working oil
JP4497767B2 (en) 2001-09-06 2010-07-07 ユシロ化学工業株式会社 Water-soluble machining fluid composition for fixed abrasive wire saw
JP2008161992A (en) * 2006-12-28 2008-07-17 Asahi Diamond Industrial Co Ltd Cutting method for processed member and manufacturing method for wafer
JP4874853B2 (en) * 2007-04-09 2012-02-15 Ｄｏｗａホールディングス株式会社 Cutting method of sintered rare earth magnet alloy
US8157876B2 (en) * 2007-07-31 2012-04-17 Cabot Microelectronics Corporation Slurry composition containing non-ionic polymer and method for use
US20090149359A1 (en) * 2007-12-10 2009-06-11 Hundley Lloyd E Formulation of a metal working fluid

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000296455A (en) 1999-04-09 2000-10-24 Tokyo Seimitsu Co Ltd Fixed abrasive grain multi-wire saw
KR100494296B1 (en) * 2001-09-07 2005-06-10 다이이치 고교 세이야쿠 가부시키가이샤 nonflammable water-based cutting fluid composition and nonflammable water-based cutting fluid
JP2009013301A (en) * 2007-07-05 2009-01-22 Adeka Corp Additive for dicing cutting water and cutting work method using its additive

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