TW200918662A - Water-soluble cutting oil for isolation abrasive grain wire-saw, slurry and cutting method - Google Patents

Water-soluble cutting oil for isolation abrasive grain wire-saw, slurry and cutting method Download PDF

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Publication number
TW200918662A
TW200918662A TW097133391A TW97133391A TW200918662A TW 200918662 A TW200918662 A TW 200918662A TW 097133391 A TW097133391 A TW 097133391A TW 97133391 A TW97133391 A TW 97133391A TW 200918662 A TW200918662 A TW 200918662A
Authority
TW
Taiwan
Prior art keywords
water
cutting
oil
mass
brittle material
Prior art date
Application number
TW097133391A
Other languages
Chinese (zh)
Inventor
Eiji Niwa
Tsutomu Oi
Tomoko Nozu
Dai Mukai
Original Assignee
Kyodo Yushi
Noritake Co Ltd
Noritake Bonded Abrasive Co Ltd
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 Kyodo Yushi, Noritake Co Ltd, Noritake Bonded Abrasive Co Ltd filed Critical Kyodo Yushi
Publication of TW200918662A publication Critical patent/TW200918662A/en

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B57/00Devices for feeding, applying, grading or recovering grinding, polishing or lapping agents
    • B24B57/02Devices for feeding, applying, grading or recovering grinding, polishing or lapping agents for feeding of fluid, sprayed, pulverised, or liquefied grinding, polishing or lapping agents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B27/00Other grinding machines or devices
    • B24B27/06Grinders for cutting-off
    • B24B27/0633Grinders for cutting-off using a cutting wire
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M173/00Lubricating compositions containing more than 10% water
    • C10M173/02Lubricating compositions containing more than 10% water not containing mineral or fatty oils
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/02Hydroxy compounds
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/02Hydroxy compounds
    • C10M2207/021Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/022Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms containing at least two hydroxy groups
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/121Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
    • C10M2207/123Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms polycarboxylic
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/127Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids polycarboxylic
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2209/00Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/104Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing two carbon atoms only
    • C10M2209/1045Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing two carbon atoms only used as base material
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/32Wires, ropes or cables lubricants

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)
  • Processing Of Stones Or Stones Resemblance Materials (AREA)
  • Lubricants (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)

Abstract

An objective of the present invention is to provide a water-soluble cutting oil for isolation abrasive grain wire-saw, a cutting slurry containing the oil and a cutting method for brittle material using the slurry, with which a "cracking" problem of one part of wafer falling from slice stage can be avoided during cutting or after cutting and excellent cutting accuracy can be obtained when an isolation abrasive grain wire-saw is used to cut silicon wafer from ingot. The present invention provides a water-soluble cutting oil for isolation abrasive grain wire-saw, a cutting slurry containing the oil and abrasive, and a cutting method for brittle material using the slurry, the water-soluble cutting oil for isolation abrasive grain wire-saw containing (A) propylene glycol, (B) diethylene glycol, (C) dicarboxylic acid salt, (D) alkylene oxide additive of alkylene glycol, and (E) water, wherein the blending amount of (B) diethylene glycol with respect to the blending amount of (A) propylene glycol is 1.50 to 1.80 times.

Description

200918662 九、發明說明: •【發明所屬之技術領域】 本發明係有關:游離磨粒線鋸用水溶性加工油劑、磨 ’·漿、使用該磨漿之切斷方法。更詳言之,本發明係有關: '在將脆性材料以線鋸切斷加工時,使用於調製含有對被切 斷材料所供給之油劑與游離磨粒之磨漿之水溶性加工油 劑、含有該油劑與游離磨粒之磨漿、使用該磨漿之脆性材 料之切斷方法。 【先前技術】 在硬度高之脆性材料之切斷加工上,從加工效率、加 工精度之觀點來看,近年來廣泛地使用以游離磨粒之線 鑛、刀鑛(帶雜)。此時,一般係使用將磨粒與油劑混合並 調整而成之液體(磨漿)。 目前提案有例如:含有⑷從.由多元醇、多元醇縮合 物、及多元醇衍生物所成群組中選出至少一種的化合物、 ⑻芳香族多域酸鹽、⑹烧二醇之環氧燒加成物以及水 之水溶性切斷加工用油劑(專利文獻n。 在使用游離磨粒線鑛進行石夕等脆性材料之切斷加工 日:’從鑄錠切取石夕晶時為了降低切損(Kerf kss)之目的, 最近正逐漸將磨劑之粒度從朝向# 1500、# 2500 使其變得更微細。此時,當進行切斷時或切斷後,易產生 部分晶片從切片台掉落之「破裂」現象。 [專利文獻1]日本特開2006_96951號公報 【發明内容】 320544 6 200918662 ' (發明欲解決的課題) - 本發明之目的係提供:無上述「破裂」之問題,而且 可传到切斷精度優良之游離磨粒線鑛用水溶性加工油劑。 ‘夕;& ΐ發明之其他目的係提供:含有上述油劑與游離磨粒 • 之磨漿。 本發明之另一目的係提供 性材料之切斷加工方法。 :使用上述油劑、磨漿之脆 (解決課題的手段) .明人等為了解決上述課題而致力研究後結果發 現·右在含有丙二醇、二乙二醇、二羧酸鹽、烷二醇之環 氧烧加成物以及水之油劑中,二乙二醇之比例增加,則剝 離測試之卿毅會降低,而「破裂」發生之可能性降低, 相反地若丙二醇之比例增加,則切斷性會提高;以及經由 調整烧二醇之環氧烧加成物之添加量,可顯著地減少「破 髮」毛生’遂完成本發明。 本發明係提供下述所示之游離磨粒線鋸用水溶性加工 油劑、磨漿、使用該磨漿之切斷方法者。 1.:種游離磨粒線鋸用水溶性加工油劑,係含有(α)丙二 醇、、(β)二乙二醇、(c)二羧酸鹽、(D)烷二醇之環氧烷 加成物以及(Ε)水之游離磨粒線鋸用水溶性加工 其中, ’由州’ 為 相對於(Α)丙二醇之調配量,(Β)二乙二醇之調配量 5〇至1. 80倍。 里 2.如上述1之游離磨粒線鋸用水溶性加工油劑,其中,含 320544 7 200918662 有(A)丙二醇30至33質量%、(幻二乙二醇托至 1%、(C)一羧酸鹽0. 5至1〇質量%、⑼烷二醇之; 烷加成物2至10質量%、(E)水5至22. 5質量%。 1 3. 如上述1或2之游離磨粒線鋸用水溶性加工油气,1 中’⑹二叛酸鹽係碳數8至20之二雜烧醇胺之鹽: 4. 如上述1至3中^ -項之游離磨粒線㈣水溶性加工二由 劑,其中,(D)烷二醇之環氧烷加成物之分子量 至 5000。 ’、 °° 5. —種切斷加工用磨漿,係含有上述丨至4中任—項之游 離磨粒線鋸用水溶性加工油劑及磨粒者。、1 6· -種脆性材料之加工方法,係使用上述5之磨漿切斷跪 性材料者。 7·如上述6之方法,其中,脆性材料係石夕系脆性材料。 8. 一種石夕系跪性材料,係依上述6或7之脆性材料之加工 方法加 工而成。 (發明的效果) i本發明之(B)二乙二醇之調配量相對於(A)丙二醇之調 配量,特定比例之水溶性加H與制在前述特定比 例之範圍外之油劑之情形相比,磨漿巾之磨粒之分散安定 性、對切斷用線鋸之磨粒附著性(沾黏性)、剝離性、切斷 2優m輯效率高,且切斷加1面之精度優良。 ’在切斷加工後去除磨漿之洗淨步驟中,也無須使用 冷肩專即可輕易以水洗淨,且也無須擔心著火性,並且即 使磨衆飛散、附著堆積於切斷加工機之表面或地板等上, 320544 8 200918662 也可簡單地清掃’因此不會使作 -高生產性。 而有助於提 【實施方式】 '本發明之油劑中,相對於(A)丙二醇之調配 -乙二酵之調配量係15〇至18〇倍。若在此 (B)一 產生部分晶片從切片台掉落之「破列 ,則易 線鑛之磨粒附著性(沾黏性)會有“二對切斷用 本發明之油劑中,成分(A)之丙二醇人旦、。 【質量《佳。若未達30質量%,則對 3里=至33 性(沾黏性)會有逐漸變差之傾向 ^之曰磨粒附著 有「破裂」易於發生之傾向。超過33…,則會 本發明之油劑中,成分⑻之 59質量%為佳。若未達45 —知之3 1以45至 生之傾向,若超過59質量%、,則°對=有「破裂」易於發 性(沾黏性)會有逐漸變差之傾向。刀斷用線鑛之磨粒附著 使用於本發明中之成分( 時,有助於磨粒之分散性、再分散當製成磨裝 性等。本發明中所使用之二羧酸粒對線錯之附著 數8至20之二幾酸與碳數2至12之;^ 舉例如:碳 以芳香族二羧酸為佳,具體而言可兴之之鹽。二羧酸 對駄酸。麵胺之具體例可舉例^^^:酸、異_、 :乙私胺、單異丙醇胺、二異、:乙%胺、 基乙醇鞍、1乙基乙醇胺等。 〜、丙醇胺、單甲 使用於本發明中之二竣酸鹽對於水之溶解度係在2〇 32( 200918662 °C時1在5^_水以上者為佳。絲達5^灣水, 則一缓酸鹽容易析出而不佳。 本發明之油劑中,二綾酸鹽之含量以〇·5至1〇質量% ,為佳、以〇_5至5質量%較佳、以〇5至2質量%最佳、。若 未達〇· 5質量%,則提高磨製中之磨粒之分散性之效果會不 足,而且即使超過10質量%,則因分散性之提高效果已餘 和,而在經濟面上為不利。 本㈣中所使用之成分⑻之^醇之環氧烧加成物 可舉例如:乙二醇及/劣王__含 哔夂/或丙一知之裱氧乙烷及/或環氧丙 烷加成物。加成莫耳數以5至100為佳、以10至8〇更佳, 分子量以500至5000為佳、以1〇〇〇至2〇〇〇更佳。 上述烧二醇之環氧烧加成物對於水之溶解度以在5g /100g水以上者為佳。 曰本發明之油劑中’成分(D)之烷二醇之環氧烷加成物之 3里以2至10貝置%為佳、以3至1〇質量%更佳。若含量 未達2質量% ’則提高磨粒對於、㈣之附著性之效果低,而 即使超過10質量%,卻因效果已飽和而不經濟。 適於使用本發明之油劑進行切斷加工之被加工材料之 例子可舉例如:在電子產業領域中所廣泛制之跪性材 料,具體例可舉例如:石夕(單曰曰曰、多晶)、録碎等之半導體; 氧化铭、氧化鍅等之陶竞;石#玻璃、石夕酸玻璃等之破璃。 當脆性材料為矽系時,油劑之邱以5至9為佳。此時,鹼 性物質以使用有機驗性物質較使用無機驗性物質為佳。 別是,以驗性温和之三乙醇胺、三異丙醇腔等三級燒醇胺 320544 10 200918662 為佳。 - 使用於本發明之油劑中之水可使用超純水'蒸餘水、 •離子交換水、自來水、城市用水、工業用水等任一者,水 ,之含量以5至22.5質量%為佳。若水之含量超過22.5質量 % ’則磨漿之黏度過低而會有切斷加工性能降低的情形。此 外若未達5質量%,則在切斷加工時因產生熱而使磨漿中 之水刀(油劑中之水分)蒸發,會使油劑本身產生著火性而 有喪失水溶性油劑之特性之虞。 f - 本發明之油劑可經由使成分(^)至(E)在適當之溫度條 件下(例如.40至70 C左右)混合溶解而輕易製造。此時, 依需要,也可適當添加而使其含有界面活性劑(陰離子系、 非離子系)、水洛性增黏劑、防腐劑、防霉劑、非鐵金屬防 鏽劑、pH緩衝劑等。 本發明之油劑通常將油劑與磨粒G列如Gc,綠色碳化 矽磨粒)以質量比為油劑:磨粒=1. 〇 :"至u: u(例 如.1. 0.0. 9)混合後做為脆性材料之切斷加工用磨漿使用。 (實施例) 。以下,藉由實施例及比較例,進一步詳細說明本發明 之水溶性油劑,但本發明並不受此等所限定。 1.油劑之性狀測定方法 (a) pH測定 將各油劑以離子交換水稀釋成2倍後,依jis_z_88〇2 玻璃電極法測定。 2.磨漿之性狀測試法 320544 11 200918662 將各油劑之磨漿(以質量比為油劑:Gc#i_磨粒 1.0 : 0.9)依下述之測試條件、測試方法進行測定。 (a)磨粒分散安定性測試 並在室溫放置 將各油劑之磨漿裝入l〇〇ml之量筒中 12小時後’以肉眼觀察磨粒分散安定性。 評估係按照下述基準。 〇:分離油分量未達10ml X :分離油分量超過10ml (b)磨粒對線之附著性測試 將線於裝容器内之磨漿中浸潰5秒後拿起,並以垂直 之狀態下放置10'秒後,以顯微鏡觀察並評估。 評估係按照下述基準。 〇:磨粒良好地附著於線上 X :少許磨粒附著於線上而幾乎未附著 (C)剝離性測試 將矽晶(Silicon Wafer,直徑:3英吋’厚度:〇8_) 浸潰於各油劑之磨漿中後,垂直放置15分鐘。接著,使此 等2片晶片之重疊位置稍微錯開,使其呈現水平並載置法 碼後,使其互相重疊16小時。16小時後,將互相重疊之2 片晶片以長尾夾垂直地吊掛,在1片晶片上以每次^运分 階段地載置法碼後,記錄重疊之晶片剝離時之载重。刀 評估係按照下述基準。 〇:剝離載重在1 〇g以下(不易破裂) X :剝離載重在2〇g以上(易破裂) 320544 12 200918662 ' (d)切斷性測試 以3英吋鑄錠切斷用線鋸進行切斷。 切斷裝置:多線鋸MS-34(Takatori公司製) 1 切斷材料:單晶矽鑄旋 •材料尺寸:Φ3英吋X6〇mmL 線徑:0. 14mm 線之線速度· 200nun/min 新線供給量:8m/min 彎曲係值 評估係測定加工面之彎曲(Warp ;即起伏) 小者表示加工精度良好。 評估 7//m以下:合格(〇) 超過7/z m :不合格(x) 综合評估 合格(〇):全部皆為〇之情形 【不合格(X):有X之情形 結果如表1及2所示。 320544 13 200918662 [表l ]200918662 IX. Description of the invention: • Technical field to which the invention pertains The present invention relates to a water-soluble processing oil agent for a free abrasive wire saw, a grinding slurry, and a cutting method using the same. More specifically, the present invention relates to: 'When a brittle material is cut by a wire saw, it is used to prepare a water-soluble processing oil containing a refining agent for the oil agent and the free abrasive grains supplied to the material to be cut. And a method for cutting the slurry of the oil agent and the free abrasive grains, and the brittle material using the slurry. [Prior Art] In the cutting process of a brittle material having a high hardness, in view of processing efficiency and processing accuracy, wire ore and knife ore (with impurities) of free abrasive grains have been widely used in recent years. In this case, a liquid (grinding) in which abrasive grains are mixed with an oil agent and adjusted is generally used. The present proposal includes, for example, a compound containing (4) a compound selected from the group consisting of a polyol, a polyol condensate, and a polyol derivative, (8) an aromatic poly-domain acid salt, and (6) an epoxidized diol. An oil for water-soluble cutting processing of an adduct and water (Patent Document n. Cutting of a brittle material such as Shixia using a free abrasive granule: "When cutting a stone from an ingot, in order to reduce the cut For the purpose of damage (Kerf kss), the particle size of the abrasive is gradually becoming finer from #1500 and #2500. At this time, when cutting or cutting, some wafers are easily removed from the slicing table. [Patent Document 1] Japanese Laid-Open Patent Publication No. 2006-96951 [Abstract] 320544 6 200918662 ' (Problems to be solved by the invention) - The object of the present invention is to provide a problem that the above-mentioned "breaking" is not caused, and It can be transferred to a water-soluble processing oil for free abrasive granules with excellent cutting precision. The other purpose of the invention is to provide a refining slurry containing the above oil agent and free abrasive particles. Purpose The cutting method of the material: The use of the above-mentioned oil agent, the brittleness of the refining (the means to solve the problem). In order to solve the above problems, Ming and others have made research and found that the right is containing propylene glycol, diethylene glycol, and In the case of an epoxidized adduct of a carboxylate, an alkylene glycol, and an oil of water, the ratio of diethylene glycol increases, and the peeling test will decrease, and the possibility of "breaking" will decrease. When the ratio of propylene glycol is increased, the cutting property is improved; and by adding the amount of the epoxidized adduct of the diol, the "breaking hair" can be remarkably reduced. The present invention has been completed. The water-soluble processing oil agent for free abrasive wire saw shown below, the refining method, and the cutting method using the refining agent. 1. A water-soluble processing oil agent for a free abrasive wire saw, which contains (α) propylene glycol. , (β) diethylene glycol, (c) dicarboxylate, (D) alkylene oxide adduct of alkanediol, and water-soluble processing of free abrasive wire saw of (Ε) water, ' is the amount of (Β) diethylene glycol relative to the amount of (Α) propylene glycol The dosage of 5 to 1.80 times. 2. The water-soluble processing oil agent for the free abrasive wire saw according to the above 1, wherein 320 540 7 200918662 has (A) propylene glycol 30 to 33% by mass, (magic diethylene 5质量百分比。 Alcohol to 1%, (C) monocarboxylic acid salt 0.5 to 1% by mass, (9) alkanediol; alkane adduct 2 to 10% by mass, (E) water 5 to 22.5% by mass. 1 3. The free abrasive wire saw of the above 1 or 2 is used for water-soluble processing of oil and gas, 1 '(6) di-oroxate is a salt of 8 to 20 bis of the miscible alcohol amine: 4. As in the above 1 to 3 ^ - The free abrasive grain line (4) The water-soluble processing agent, wherein the molecular weight of the alkylene oxide adduct of the (D) alkanediol is 5,000. ', ° ° 5. A kind of refining processing refining, which is a water-soluble processing oil agent and abrasive grain for the abrasive abrasive wire saw which contains the above-mentioned 丨 to 4 - item. The method for processing a brittle material is to cut off the inert material using the above-mentioned 5 refining material. 7. The method according to the above 6, wherein the brittle material is a stone brittle material. 8. A stone-like enamel material which is processed according to the processing method of the brittle material of the above 6 or 7. (Effects of the Invention) i The ratio of the amount of (B) diethylene glycol of the present invention to the amount of (A) propylene glycol, the specific ratio of water solubility plus H and the oil agent outside the range of the specific ratio described above In comparison, the dispersion stability of the abrasive grains of the refining pad, the adhesion to the abrasive grains of the cutting jigsaw (adhesiveness), the peeling property, and the cutting efficiency are high, and the cutting is added with one side. Excellent precision. 'In the washing step of removing the refining after the cutting process, it is also easy to wash with water without using the cold shoulder, and there is no need to worry about the ignitability, and even if the grinding is scattered, the deposit is deposited on the cutting machine. On the surface or floor, etc., 320544 8 200918662 can also be easily cleaned 'so it will not make - high productivity. Further, it is helpful to provide an embodiment. In the oil agent of the present invention, the amount of the preparation of the (A) propylene glycol-Ethylene glycol is 15 to 18 times. In the case of "B), when the partial wafer is dropped from the slicing table, the abrasive grain adhesion (adhesiveness) of the Yixian mine may be "two pairs of cuts of the oil agent of the present invention. (A) propylene glycol human Dan. [Quality is good. If it is less than 30% by mass, there is a tendency for gradual deterioration of 3 liters to 33 (stickiness). When the amount is more than 33, the oil of the present invention is preferably 59% by mass of the component (8). If it is less than 45 - it is known that the 3 1 is 45 to the natural tendency, and if it exceeds 59% by mass, the degree of "breaking" is likely to gradually deteriorate (adhesion). The abrasive grains of the wire-cut ore are attached to the components used in the present invention (when, the dispersion of the abrasive grains is facilitated, the redispersibility is made into a millability, etc.) The dicarboxylic acid particles used in the present invention are aligned. The number of attachments is 8 to 20 bis and the number of carbons is 2 to 12; ^ For example, carbon is preferably an aromatic dicarboxylic acid, specifically a salt of a dicarboxylic acid. Specific examples of the amine can be exemplified by an acid, an iso-, an ethylamine, a monoisopropanolamine, a diiso, an ethylamine, an ethanolic saddle, a monoethylethanolamine, etc. ~, a propanolamine, The solubility of the dicaprate used in the present invention for water is 2〇32 (200918662 °C, 1 is better than 5^_ water), and the wire is 5^ bay water, then a slow acid salt is easy. In the oil agent of the present invention, the content of the dicaprate is preferably 〇5 to 1% by mass, more preferably 〇5 to 5% by mass, and most preferably 〇5 to 2% by mass. If it is less than 5% by mass, the effect of improving the dispersibility of the abrasive grains in the grinding process may be insufficient, and even if it exceeds 10% by mass, the effect of improving the dispersibility is insufficient, and in the economical aspect No The epoxy burnt adduct of the alcohol of the component (8) used in the above (4) may, for example, be ethylene glycol and/or inferior __containing 哔夂/or propyl oxime oxirane and/or epoxy Propane adduct. The addition molar number is preferably from 5 to 100, more preferably from 10 to 8 Torr, and the molecular weight is preferably from 500 to 5,000, more preferably from 1 to 2 Torr. The epoxy burned adduct is preferably more than 5 g / 100 g of water for the solubility of water. 曰 In the oil agent of the present invention, the alkylene oxide adduct of the alkylene glycol of the component (D) is 2 It is preferable to set it to 10%, preferably 3 to 1% by mass. If the content is less than 2% by mass, the effect of improving the adhesion of the abrasive grains to (4) is low, and even if it exceeds 10% by mass, the effect is It is saturated and uneconomical. Examples of the material to be processed which is suitable for the cutting process using the oil agent of the present invention include, for example, an inert material which is widely used in the field of the electronics industry, and specific examples thereof include: Semiconductors such as monoterpenes, polycrystals, and shattered; ceramics such as oxidized inscriptions, cerium oxides, etc.; broken glass in glass, glass, and other materials. In the case of lanthanum, the oil is preferably 5 to 9. In this case, it is better to use an organic substance than an inorganic substance in the case of an alkaline substance. In other words, it is mild to triethanolamine and triisopropyl. Alcoholic cavity and other tertiary alcohol amines 320544 10 200918662 are preferred. - Water used in the oil agent of the present invention can be used as ultrapure water 'steamed water, ion exchange water, tap water, city water, industrial water, etc. The content of water is preferably from 5 to 22.5 mass%. If the water content exceeds 22.5 mass%, the viscosity of the refining is too low, and the cutting processability is lowered. If it is less than 5% by mass, When the cutting process is performed, heat is generated to evaporate the water jet (moisture in the oil) in the refining, which causes the oil itself to be flammable and loses the characteristics of the water-soluble oil agent. f - The oil agent of the present invention can be easily produced by mixing and dissolving the components (^) to (E) under appropriate temperature conditions (e.g., about 40 to 70 C). In this case, if necessary, it may be appropriately added to contain a surfactant (anionic, nonionic), water-borne tackifier, preservative, mold inhibitor, non-ferrous metal rust inhibitor, pH buffer. Wait. The oil agent of the present invention usually has an oil agent and abrasive grains G such as Gc, green carbonized cerium abrasive grains in a mass ratio of oil: abrasive particles = 1. 〇: " to u: u (for example, 1.0.0. 9) After mixing, it is used as a cutting material for brittle materials. (Example) Hereinafter, the water-soluble oil agent of the present invention will be described in further detail by way of examples and comparative examples, but the present invention is not limited thereto. 1. Method for measuring properties of oil agent (a) pH measurement Each oil agent was diluted twice with ion-exchanged water, and then measured by a jis_z_88〇2 glass electrode method. 2. Test method for refining properties 320544 11 200918662 The refining of each oil agent (mass ratio: oil: Gc#i_abrasive 1.0: 0.9) was measured according to the following test conditions and test methods. (a) Abrasive dispersion stability test and placed at room temperature The slurry of each oil was placed in a measuring cylinder of 10 ml after 12 hours. The dispersion stability of the abrasive particles was visually observed. The evaluation is based on the following criteria. 〇: The oil content of the separated oil is less than 10ml X: The oil content of the separated oil is more than 10ml. (b) The adhesion test of the abrasive grains to the wire. The wire is immersed in the refining in the container for 5 seconds and then picked up and placed in a vertical state. After 10' seconds of placement, it was observed and evaluated by a microscope. The evaluation is based on the following criteria. 〇: The abrasive grains adhered well to the line X: a small amount of abrasive grains adhered to the wire and hardly adhered (C) Peeling test: Silicon Wafer (diameter: 3 inches 厚度 'thickness: 〇 8 _) was immersed in each oil After the agent was refining, it was placed vertically for 15 minutes. Next, the overlapping positions of the two wafers were slightly shifted to make them horizontal and the codes were placed, and then overlapped each other for 16 hours. After 16 hours, the two wafers which overlap each other were vertically suspended by the long tail clip, and the load was superimposed on each wafer at each stage of the wafer, and the load at the time of peeling of the overlapped wafer was recorded. The knife evaluation is based on the following criteria. 〇: Peel load is below 1 〇g (not easy to break) X: Peel load is above 2 〇g (easy to break) 320544 12 200918662 ' (d) Cut-off test is cut with a wire saw with a 3 inch ingot cut Broken. Cutting device: Multi-wire saw MS-34 (manufactured by Takatori Co., Ltd.) 1 Cutting material: single crystal 矽 casting rotation • Material size: Φ3 inch X6〇mmL Wire diameter: 0. 14mm Line speed • 200nun/min New Line supply: 8m/min Bending coefficient evaluation is used to measure the bending of the machined surface (Warp; that is, the undulation). The smaller one indicates that the machining accuracy is good. Evaluation of 7//m or less: Qualified (〇) More than 7/zm: Unqualified (x) Comprehensive evaluation qualified (〇): All cases are 【 [Failed (X): If there is X, the results are shown in Table 1 and 2 is shown. 320544 13 200918662 [Table l]

※工:烷二醇之環氧烷加成物A:乙二醇之環氧乙烷加成物(勿子里woo) ※之:烷二醇之環氧烷加成物b:丙二醇之環氧乙烷加成物(分子量2〇〇〇) 醇之環氧烧加成物C:乙二醇之環氧乙烧·環氧丙燒加成物(分 異駄酸三乙醇胺鹽係異歃酸與三乙醇胺之莫耳比為1:2之鹽 320544 14 200918662 [表2]※Work: Alkylene oxide adduct of alkanediol A: Ethylene oxide adduct of ethylene glycol (Wuzili woo) ※: Alkylene oxide alkylene oxide adduct b: Propylene glycol ring Oxyethane adduct (molecular weight 2 〇〇〇) Epoxy burnt adduct of alcohol C: Ethylene bromide/epoxy propylene bromide adduct of ethylene glycol (different citrate triethanolamine salt isomer The molar ratio of acid to triethanolamine is 1:2 salt 320544 14 200918662 [Table 2]

比較例 1 2 3 .4 5 6 7 (A) 丙二醇 81 35 .26 0 31 (B) 二乙二醇 0 46 55 81 52 (B)/(A) 0 1. 31 2. 12 〇〇 1. 68 (C) 異酞酸三乙醇胺鹽 1 1 1 1 1 ⑼ 烷二醇之環氧烷加 成物 3 3 3 3 — (E) 離子交換水 15 15 15 15 16 油劑 pH 7. 4 7. 3 7. 2 7.1 7. 5 8. 2 8. 5 磨漿 磨粒分散安定性 〇 〇 X X X X X @1^對線之附著性 〇 〇 X X X X X 剝離性 X X 〇 〇 Ό X X 切斷性 彎曲(#111)50片之 平均 6. 1 6. 3 13. 6 15. 2 12. 0 17. 6 21. 1 評估 〇 〇 X X X X X 綜合評估 X X X X X X X 比較例6及7係市售之水溶性切斷加工油劑。 相對於(A)丙二醇之調配量,(B)二乙二醇之調配量在 (丨· 50至1.80倍之範圍内之本發明之實施例1至5之磨漿, 分散安定性、磨粒附著性、剝離性及切斷性皆優良。 相對於(A)丙二醇之調配量,(B)二乙二醇之調配量未 達1. 5〇倍之比較例1及2之磨漿,分散安定性、磨粒附著 性及切斷性皆優良,但剝離性不良。 、相對於(A)丙二醇之調配量,(B)二乙二醇之調配量超 a . 8 〇倍之比較例3及4之磨漿,剝離性雖優良,但分散 $ &性、磨粒附著性及切斷性皆不良。 不含(D)烷二醇之環氧烷加成物之比較例5之磨漿,剝 320544 15 200918662 • 離性雖優良,但分散安定性、磨粒附著性及切斷性皆不良。 ,使用市售之油劑之磨漿,分散安定性、磨粒附著性、 剝離性及切斷性皆不良。 【圖式簡單說明】 •無。 【主要元件符號說明】 無。 16 320544Comparative Example 1 2 3 .4 5 6 7 (A) Propylene glycol 81 35 .26 0 31 (B) Diethylene glycol 0 46 55 81 52 (B)/(A) 0 1. 31 2. 12 〇〇1. 68 (C) Isodecanoic acid triethanolamine salt 1 1 1 1 1 (9) Alkylene oxide alkylene oxide adduct 3 3 3 3 — (E) Ion exchange water 15 15 15 15 16 Oil pH 7. 4 7. 3 7. 2 7.1 7. 5 8. 2 8. 5 Grinding abrasive dispersion stability 〇〇XXXXX @1^Adhesion to the wire 〇〇XXXXX Peelability XX 〇〇Ό XX Cut-off bending (#111) Average of 50 tablets 6. 1 6. 3 13. 6 15. 2 12. 0 17. 6 21. 1 Evaluation 〇〇 XXXXXX Comprehensive evaluation XXXXXXX Comparative Examples 6 and 7 are commercially available water-soluble cutting processing oils. With respect to the blending amount of (A) propylene glycol, the blending amount of (B) diethylene glycol in the range of 丨·50 to 1.80 times of the refining of Examples 1 to 5 of the present invention, dispersion stability, abrasive grains The refining, dispersing of the comparative examples 1 and 2 is less than 1.5 times the amount of the blending of the (A) propylene glycol. Stability, abrasive adhesion and cuttability are all excellent, but the peelability is poor. Compared with (A) the amount of propylene glycol, (B) the amount of diethylene glycol is more than a. 8 times the comparison example 3 And the refining of 4, although the peeling property is excellent, but the dispersion of & the property, the abrasive adhesion and the cutting property are bad. The grinding of the comparative example 5 which does not contain the (D) alkylene oxide alkylene oxide adduct. Pulp, stripping 320544 15 200918662 • Although the separation is excellent, the dispersion stability, abrasive adhesion and cutting properties are all poor. Use of commercially available oil refining, dispersion stability, abrasive adhesion, peelability And the cutting property is bad. [Simple description of the diagram] • No. [Description of main component symbols] None. 16 320544

Claims (1)

200918662 十、申請專利範圍: 1 · 一種游離磨粒線鋸用水溶性加工油劑,係含有(A)丙二 ^ 醇 (B) 一乙一醇、(C)二羧酸鹽、(d)院二醇之環氧燒 • 加成物以及(E)水者,在該游離磨粒線鋸用水溶性加工 •油劑中, 相對於(A)丙二醇之調配量,(B)二乙二醇之調配量 為1. 50至1. 8〇倍。 2.如申請專利範圍第丨項之游離磨粒線鋸用水溶性加工 油劑,其中,含有(A)丙二醇30至33質量%、(B)二乙 一醇“至59質量%、(〇二羧酸鹽〇_ 5至1〇質量%、(D) 烷二醇之環氧烷加成物2至1〇質量%、(£)水5至22 5 質量%。 ' 3. 如申請專利範圍第!項或第2項之游離磨粒線鑛用水岛 性加工油劑,其中,(c)二羧酸鹽係碳數8至2〇之二奚 酸與烷醇胺之鹽。 — 4. 如申請專利範圍第1項 弟項中任一項之游離磨粒秦 1 鑛用水洛性加工油劑,i中 _ 你々八、干(D)烷一醇之環氧烷加居 物之刀子1係500至5000者。 5. —種切斷加工用磨漿,係含 浐 〒明寻利靶圍第1項至第 中任一項之游離磨粒線鋸 ^ ^ ^ ^ ^ 粒者。 丨王加工油劑及磨 6. 一種脆性材料之加工方法 τ5 — 系使用申5月專利筋圖當5 項之磨漿切斷脆性材料者。 』靶圍第5 7. 如申請專利範圍第6項之方法,苴 〃甲脆性材料係矽系 320544 17 200918662 < 脆性材料。 • 8. —種矽系脆性材料,係依申請專利範圍第6項或第7 項之脆性材料之加工方法加工而成。 18 320544 200918662 七、指定代表圖:本案無圖式。 • (一)本案指定代表圖為:第()圖。 (二)本代表圖之元件符號簡單說明: 八、本案若有化學式時,請揭示最能顯示發明特徵的化學式: 本案無化學式。 5 320544200918662 X. Patent application scope: 1 · A water-soluble processing oil agent for free abrasive wire saws containing (A) propylene glycol (B) monoethyl alcohol, (C) dicarboxylate, (d) Alcohol-based epoxidation • Addition and (E) water, in the water-soluble processing and oiling agent of the free abrasive wire saw, compared with (A) propylene glycol, (B) diethylene glycol blending The amount is 1.50 to 1.8 times. 2. The water-soluble processing oil for free abrasive wire saw according to the invention of claim 2, wherein (A) propylene glycol is 30 to 33% by mass, (B) diethyl diol is "to 59% by mass, (yttrium dicarboxylate) 〇 〇 5 to 1 〇 mass%, (D) alkylene oxide adduct of alkanediol 2 to 1% by mass, (£) water 5 to 22 5 mass%. ' 3. As claimed in the patent scope Or the second aspect of the free abrasive granule water-using island processing oil, wherein (c) the dicarboxylic acid salt is a salt of a dicarboxylic acid having 8 to 2 carbon atoms and an alkanolamine. The free abrasive grain Qin 1 mine water treatment oil agent of any one of the first paragraphs of the patent application scope, i _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ It is a product of 500 to 5000. 5. A kind of refining processing, which is a free abrasive wire saw ^ ^ ^ ^ ^ grain containing the first to the first of the target. Wang processing oil agent and grinding 6. A method for processing brittle materials τ5 — is to use the patented rib diagram of May to cut the brittle material when refining 5 items. 』 Target circumference 5 5. If the scope of patent application is 6 Square , bristle brittle material system 544 system 320544 17 200918662 < brittle material. 8. 8. 矽 脆 brittle material, processed according to the processing method of brittle material according to the scope of claim 6 or 7. 18 320544 200918662 VII. Designation of representative figure: There is no drawing in this case. • (1) The representative drawing of the case is: (). (2) The symbolic symbol of the representative figure is simple: 8. If there is a chemical formula in this case, please reveal The chemical formula that best shows the characteristics of the invention: There is no chemical formula in this case. 5 320544
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