CN110382655A - 加工介质、加工组合物及加工方法 - Google Patents
加工介质、加工组合物及加工方法 Download PDFInfo
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- CN110382655A CN110382655A CN201880008771.1A CN201880008771A CN110382655A CN 110382655 A CN110382655 A CN 110382655A CN 201880008771 A CN201880008771 A CN 201880008771A CN 110382655 A CN110382655 A CN 110382655A
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- Prior art keywords
- machining medium
- acid
- carboxylic acid
- polybasic carboxylic
- processing
- Prior art date
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- KSCQDDRPFHTIRL-UHFFFAOYSA-N auramine O Chemical compound [H+].[Cl-].C1=CC(N(C)C)=CC=C1C(=N)C1=CC=C(N(C)C)C=C1 KSCQDDRPFHTIRL-UHFFFAOYSA-N 0.000 description 1
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- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 description 1
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- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 1
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- 230000001050 lubricating effect Effects 0.000 description 1
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- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- KWKAKUADMBZCLK-UHFFFAOYSA-N methyl heptene Natural products CCCCCCC=C KWKAKUADMBZCLK-UHFFFAOYSA-N 0.000 description 1
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- 239000000983 mordant dye Substances 0.000 description 1
- JILXUIANNUALRZ-UHFFFAOYSA-N n',n'-diethylbutane-1,4-diamine Chemical compound CCN(CC)CCCCN JILXUIANNUALRZ-UHFFFAOYSA-N 0.000 description 1
- SCZVXVGZMZRGRU-UHFFFAOYSA-N n'-ethylethane-1,2-diamine Chemical compound CCNCCN SCZVXVGZMZRGRU-UHFFFAOYSA-N 0.000 description 1
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- 229910052759 nickel Inorganic materials 0.000 description 1
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- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- PBMFSQRYOILNGV-UHFFFAOYSA-N pyridazine Chemical compound C1=CC=NN=C1 PBMFSQRYOILNGV-UHFFFAOYSA-N 0.000 description 1
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- ADRDEXBBJTUCND-UHFFFAOYSA-N pyrrolizidine Chemical compound C1CCN2CCCC21 ADRDEXBBJTUCND-UHFFFAOYSA-N 0.000 description 1
- 235000012950 rattan cane Nutrition 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
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- 235000009165 saligot Nutrition 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
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- URLJMZWTXZTZRR-UHFFFAOYSA-N sodium myristyl sulfate Chemical compound CCCCCCCCCCCCCCOS(O)(=O)=O URLJMZWTXZTZRR-UHFFFAOYSA-N 0.000 description 1
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- 239000000758 substrate Substances 0.000 description 1
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- 235000020679 tap water Nutrition 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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- 229940086542 triethylamine Drugs 0.000 description 1
- 229960004418 trolamine Drugs 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M173/00—Lubricating compositions containing more than 10% water
- C10M173/02—Lubricating compositions containing more than 10% water not containing mineral or fatty oils
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M129/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
- C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
- C10M129/26—Carboxylic acids; Salts thereof
- C10M129/28—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M129/30—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having 7 or less carbon atoms
- C10M129/32—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having 7 or less carbon atoms monocarboxylic
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M129/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
- C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
- C10M129/26—Carboxylic acids; Salts thereof
- C10M129/48—Carboxylic acids; Salts thereof having carboxyl groups bound to a carbon atom of a six-membered aromatic ring
- C10M129/52—Carboxylic acids; Salts thereof having carboxyl groups bound to a carbon atom of a six-membered aromatic ring polycarboxylic
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M133/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen
- C10M133/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen having a carbon chain of less than 30 atoms
- C10M133/04—Amines, e.g. polyalkylene polyamines; Quaternary amines
- C10M133/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
- C10M133/08—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms containing hydroxy groups
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Physics & Mathematics (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Computer Hardware Design (AREA)
- Manufacturing & Machinery (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
本发明提供一种兼具防锈性能及防止金属污染性能的加工介质、加工组合物及加工方法。本发明的加工介质含有或在已中和的状态下含有碳数为2以上且7以下的多元羧酸、芳香族单羧酸及碱性物质。
Description
技术领域
本发明涉及一种加工介质、加工组合物及加工方法。
背景技术
在进行将锭(铸块)等被加工物切割成晶圆状的加工、或对被加工物的切割面进行研磨(研削)的加工、或进而将被加工物的切割面研磨成镜面的加工时,对于工具(例如线锯、带锯、内径刀片、研磨压盘等)与被加工物的接触部分供给加工介质(加工液、切削液、冷却剂)。加工介质用水等溶剂进行稀释后使用,或进而掺合研磨粒而以加工组合物(研削液、研磨液、浆料)的形式使用。加工介质具有如下作用,即,将在工具与被加工物之间所产生的热冷却的冷却作用;使工具与被加工物之间变得润滑的润滑作用;对加工时所产生的颗粒(切屑、研削屑、研磨屑)与工具或被加工物的熔接进行防护的熔接防护作用等。
源自因加工而产生的颗粒的金属氧化物的微粒子状污物容易附着(固着、再次附着)于被加工物的表面。若污物附着于被加工物的表面,则导致被加工物的金属污染。此外,在加工时因与工具、配管等金属的接触而溶出至加工介质中的金属离子容易附着(或渗透、扩散)于被加工物表面。金属离子于被加工物的表面容易移动,因金属离子的移动而有时会发生下述等问题:形成于被加工物(例如晶圆)的电晶体等元件的误动作、漏电流。因此,为了抑制污物或金属离子对被加工物的不良影响,而提出有各种加工介质、加工组合物。
例如在专利文献1中,揭示有一种含有伯烷醇胺、羧酸、二胺的水溶性切削油剂作为抑制防锈性降低的物质。此外,在专利文献2中,揭示有一种由四唑化合物及其水溶性盐构成的水溶性金属防蚀剂作为对各种金属具有优异的防锈能力的物质。
此外,在专利文献3中,揭示有一种含有螯合剂、碱性化合物、二氧化硅及水的研磨用组合物作为有效地抑制由金属杂质引起的晶圆污染的物质。此外,在专利文献4中,揭示有一种含有氧化硅、碱性物质、氨基聚膦酸及水的研磨组合物作为有效地防止镍、铬、铁、铜等的金属污染的物质。此外,在专利文献5中,揭示有一种含有氧化硅、碱性物质、氨基酸衍生物、其盐及水的研磨组合物作为能够防止金属污染尤其是铜污染的物质。此外,在专利文献6中,揭示有一种含有氧化硅、碱性物质、具有羟基的聚氨基聚羧酸化合物及水的研磨组合物作为能够防止金属污染尤其是铜污染的物质。此外,在专利文献7中,揭示有一种含有二氧化硅、碱性化合物及具有膦酸基的螯合剂的研磨用组合物作为有效地抑制由金属杂质引起的晶圆污染的物质。进而,在专利文献8中,揭示有一种含有单斜晶锆、羧酸及氢氧化季烷基铵的研磨浆料作为能够有效地防止铜污染的物质。
背景技术文献
专利文献
专利文献1:日本专利特开昭64-43598号公报
专利文献2:日本专利特开平7-145491号公报
专利文献3:国际公开第2004/042812号说明书
专利文献4:日本专利特开2005-347737号公报
专利文献5:国际公开第2006/046641号说明书
专利文献6:国际公开第2006/126432号说明书
专利文献7:日本专利特开2014-82509号公报
专利文献8:日本专利第5002175号公报。
发明内容
发明所欲解决的课题
然而,在现有的加工组合物等中并未发现兼具防锈性及防止金属污染的。
本发明的主要课题在于提供一种兼具防锈性能及防止金属污染性能的加工介质、加工组合物及加工方法。
解决课题的技术手段
本发明的加工介质含有或在已中和的状态下含有碳数为2以上且7以下的多元羧酸、芳香族单羧酸及碱性物质。
本发明的加工组合物含有上述加工介质与研磨粒。
本发明的加工方法将上述加工介质或上述加工组合物供给至工具与被加工物的接触部分而对上述被加工物进行加工。
发明的效果
根据本发明,可提供一种兼具防锈性能及防止金属污染性能的加工介质、加工组合物及加工方法。
附图说明
图1为表示硅晶圆的金属污染评价的判定方法的照片。
具体实施方式
以下,对实施方案进行说明。再者,在本申请中附有附图标记的情形时,其等主要用以帮助理解,并非意欲限定附图的方案。此外,下述实施方案仅为例示,并不限定本发明。
实施方案的加工介质为在进行对硅、碳化硅、蓝宝石、氮化镓的锭等被加工物进行切割的加工、对晶圆等被加工物的切割表面进行研磨的加工、进而将切割表面研磨成镜面的加工等加工时,被供给至工具(例如线锯、带锯、内径刀片、研磨压盘(例如单面压盘、双面压盘、铸铁压盘、铜压盘等)等)与被加工物的接触部的介质(加工液、切削液、冷却剂等)。加工介质可用水进行稀释后使用。加工介质可进而任意地掺合研磨粒(例如金刚石、氧化锆、氧化铝、碳化硅、立方晶氮化硼等)而以加工组合物(例如研削液、研削组合物、研磨液、研磨组合物、浆料、悬浊液等)的形式使用。加工介质例如于切割装置(切片装置、切割机)、研削装置(精磨(ラッピング)装置)、研磨装置(抛光装置)等加工装置中使用。再者,在加工装置中,自加工介质的槽直至供给部的配管大多使用铜。
加工介质为在将铜浸渍在加工介质中时加工介质中的铜离子浓度,优选为70ppm以下,更优选为60ppm以下,尤其优选为50ppm以下。若变得大于70ppm,则变得容易发生形成于被加工物的电晶体等元件的误动作、漏电流等。
加工介质含有或在已中和的状态下含有多元羧酸、芳香族单羧酸、碱性物质及水。此处,所谓含有或在已中和的状态下,是指处于酸及碱未中和的状态、酸及碱为离子的状态、酸及碱已中和的状态中的任一状态或所有状态。
多元羧酸为碳数为2以上且7以下的多元羧酸。多元羧酸主要有抑制被加工物的金属污染的作用。作为多元羧酸,例如可使用:草酸、丙二酸、琥珀酸、延胡索酸、戊二酸、己二酸、庚二酸等二羧酸;乌头酸等三羧酸;苹果酸、柠檬酸等羟酸;草酰乙酸等。多元羧酸的碳数优选为2以上且6以下。若碳数变得大于7,则变得无法抑制被加工物的金属污染。上述多元羧酸中,草酸其防止通常被使用于工具的铁的溶出的效果优异。此外,柠檬酸其防止铜的溶出的效果优异。
芳香族单羧酸为具有至少1个芳香环与1个羧基的化合物。作为芳香族单羧酸,例如可使用:对叔丁基苯甲酸、邻叔丁基苯甲酸、间叔丁基苯甲酸、硝基苯甲酸、苯乙酸、萘羧酸等。其中,对叔丁基苯甲酸主要有抑制被使用于工具的金属材料的氧化(确保防锈性)的作用,故而优选。
此处,已知为了防止金属的腐蚀而使用对叔丁基苯甲酸及碱(例如参照专利文献2的[0002]),但并未揭示及暗示将碳数为2~7的分子量小的多元羧酸与对叔丁基苯甲酸组合而使用。
再者,在被加工物的加工中应注意如下情况,即被使用于工具或加工装置的配管等的铜发生离子化而吸附(或渗透、扩散)于被加工物从而产生污染。众所周知为了防止铜的腐蚀或溶出而使用苯并三唑类(例如参照专利文献2的[0002]),但在使用苯并三唑的情形时,若掺合量过多,则有时会无法抑制对铜以外的金属的被加工物的金属污染,故而苯并三唑优选将掺合量限制于微量,更优选为不使用。
关于多元羧酸及芳香族单羧酸的合计掺合量,在加工介质中优选为0.05wt%以上且15wt%以下,更优选为0.1wt%以上且4wt%以下,进而优选为0.2wt%以上且2wt%以下。若浓度低于0.05wt%,则难以抑制被加工物的金属污染,另一方面,若浓度高于15wt%,则需要较多用以中和其的碱,若碱性物质不足,则铜离子变得容易溶出。
多元羧酸及芳香族单羧酸的掺合比优选为1∶4以上且未达2∶1,更优选为1∶1.8以上且1.8∶1以下,进而优选为1∶1.5以上且1.5∶1以下。若变成未达1∶4,则铜离子的溶出量变多,另一方面,即便为2∶1以上,铜离子的溶出量亦变多。
碱性物质为钠化合物、钾化合物、铵化合物、胺化合物中的任意一种以上。碱性物质优选包含有钠化合物或钾化合物与胺化合物,进而优选包含有多种胺化合物。作为碱性物质,可使用其水溶液显示碱性(碱性;pH值大于7)的化合物,例如可使用:氢氧化钠、碳酸钠等钠化合物;氢氧化钾、碳酸钾等钾化合物;四甲基氢氧化铵、氢氧化铵等铵化合物;甲基胺、二甲胺、三甲胺、乙基胺、二乙胺、单乙醇胺、N-乙醇胺、二乙醇胺、三乙胺、三乙醇胺、单异丙醇胺、二异丙基乙基胺、二异丙醇胺、二亚乙基三胺、三亚乙基四胺、聚(丙二醇)二胺、三羟甲基丙烷聚(氧亚丙基)三胺、亚乙基二胺、四甲基亚乙基二胺、2-氨基-2-甲基丙醇、月桂基氨基丙基胺、乙基氨基乙基胺、油基氨基丙基胺、二乙基氨基丁基胺、乙基氨基己基胺、环己基氨基丙基胺、六亚甲基二胺、精三胺、苯胺、苯乙胺、甲苯胺、吡咯啶、哌啶、哒嗪、嘧啶、吡嗪、恶唑、噻唑、N,N-二甲基-4-氨基吡啶、醚胺、无水哌嗪、哌嗪六水合物、1-哌嗪、N-甲基哌嗪等胺化合物。
本发明的加工介质通过含有碱性物质,而使芳香族单羧酸可溶于水,故而可获得均匀且稳定的溶液。碱性物质的掺合量在加工介质中优选为0.1wt%以上且20wt%以下,更优选为0.2wt%以上且10wt%以下,进而优选为0.5wt%以上且5wt%以下。若浓度低于0.1wt%,则会对被加工物的金属污染带来不良影响,若碱性物质不足而pH值成为7以下,则失去防锈性。另一方面,在浓度高于20wt%的情形时,铜离子变得容易溶出。碱性物质设为中和多元羧酸及芳香族单羧酸的两者的分量以上,优选以加工介质的pH值变得大于7的方式进行掺合,可以成为更优选为8以上且12.5以下、进而优选为8.5以上且10以下的方式进行掺合。若考虑加工介质的处理性及成本,则优选设为pH值为12.5以下。
水为成为原液成分的多元羧酸、芳香族单羧酸及碱性物质的稀释介质。关于水的掺合量,只要能够用水将原液稀释成任意浓度,则并无特别限定,若考虑处理性及成本,则优选为50wt%以上且99.7wt%以下,更优选为80wt%以上且99.5wt%以下,进而优选为90wt%以上且98wt%以下。
此外,在加工介质中可视需要而添加界面活性剂、消泡剂、防腐剂、香料、染料等。
界面活性剂可考虑研磨粒的分散性或液体的渗透性而进行掺合。作为界面活性剂,可使用非离子型界面活性剂、阳离子型界面活性剂、阴离子型界面活性剂、两性界面活性剂等,例如可使用:月桂酸甘油、单硬脂酸甘油等酯型非离子型界面活性剂、聚亚烷基二醇单丁醚、聚氧乙烯烷基醚等醚型非离子型界面活性剂;聚氧乙烯山梨醇酐脂肪酸酯、聚氧乙烯已糖醇酐(ヘキシタン)脂肪酸酯等酯醚型非离子型界面活性剂;月桂酸二乙醇酰胺、油酸二乙醇酰胺等烷醇酰胺型非离子型界面活性剂;辛基葡萄糖苷、癸基葡萄糖苷等烷基葡萄糖苷型非离子型界面活性剂;鲸蜡醇、硬脂醇等高级醇型非离子型界面活性剂;四甲基氯化铵、四甲基氢氧化铵等四级铵盐型阳离子型界面活性剂;单甲基胺盐酸盐、二甲胺盐酸盐等烷胺盐型阳离子型界面活性剂;氯化丁基吡啶鎓、氯化十二烷基吡啶等吡啶环型阳离子型界面活性剂;辛酸钠、癸酸钠等羧酸型阴离子型界面活性剂;1-己烷磺酸钠、1-辛烷磺酸钠等磺酸型阴离子型界面活性剂;月桂基硫酸钠、肉豆蔻基硫酸钠等硫酸酯型阴离子型界面活性剂;月桂基磷酸、月桂基磷酸钠等磷酸酯型阴离子型界面活性剂;月桂基二甲氨基乙酸甜菜碱、硬脂基二甲氨基乙酸甜菜碱等烷基甜菜碱型两性界面活性剂;椰子酰胺丙基甜菜碱、椰子酰胺丙基羟基磺基甜菜碱等脂肪酸酰胺丙基甜菜碱型两性界面活性剂;2-烷基-N-羧甲基-N-羟乙基咪唑啉鎓甜菜碱等烷基咪唑型两性界面活性剂;月桂酰麸胺酸钠、月桂酰麸胺酸钾等氨基酸型两性界面活性剂;月桂基二甲胺基N-氧化物、油基二甲胺基N-氧化物等胺氧化物型两性界面活性剂等。界面活性剂的掺合量可相对于加工介质100wt%,设为0.01wt%以上且5wt%以下,优选为0.02wt%以上且3wt%以下,更优选为0.05wt%以上且1wt%以下。
消泡剂可考虑加工介质自槽的溢出或再利用时的操作而进行掺合。作为消泡剂,例如可使用:硅酮油、改质硅酮、HLB(亲水亲油平衡)为7以上的非离子型界面活性剂;2-乙基己醇、二异辛基醚等有机极性化合物;山梨醇酐酯类、プルロニックL-61等低亲水性界面活性剂;添加有脂肪酸金属盐的矿物油等。消泡剂的掺合量可相对于加工介质100wt%,设为0.001wt%以上且1wt%以下,优选为0.002wt%以上且0.5wt%以下,更优选为0.005wt%以上且0.1wt%以下。
作为防腐剂,例如可使用:2-甲基-4-异噻唑啉-3-酮、5-氯-2-甲基-4-异噻唑啉-3-酮、对羟基苯甲酸酯类及苯氧基乙醇等。
作为香料,例如可使用:乳香油、洋芹油、大茴香油等天然香料;香旱芹酮、大茴香脑、水杨酸甲酯等合成香料;调合香料等。
作为染料,例如可使用:阿特拉斯红(アトラスレッド)R、偶氮蓝、偶氮紫(アゾモーブ)AM等直接染料、金胺G、金胺II、从而斯麦棕等碱性染料;杰纳斯蓝G、杰纳斯绿B、杰纳斯蓝R等碱性杰纳斯染料;苏木、黄栌色素(フスチック)、茜草、茜素等媒染染料;蒽醌、靛类等瓮染料等。
再者,关于上述多元羧酸、芳香族单羧酸及碱性物质,可使用多元羧酸及芳香族单羧酸与碱性物质已中和的状态的盐作为原料以代替所述混合物。
作为上述加工介质的制造方法,例如使碱性物质溶解于水中,进而加入多元羧酸及芳香族单羧酸并进行搅拌,由此可获得成为中和盐水溶液的加工介质。可视需要在加工介质中加入界面活性剂、防腐剂、消泡剂、香料、染料等,并加入水以调整浓度。于获得加工组合物的情形时,可在加工介质中任意地掺合研磨粒并进行搅拌。再者,加工介质及加工组合物的制造方法并不限于上述。以上述方式获得的加工介质或加工组合物被注入至加工装置的槽中,将加工介质或加工组合物供给至该加工装置的工具与被加工物的接触部,而对该被加工物进行加工。
根据本实施方案,可通过多元羧酸而防止(抑制)溶解至加工介质中的金属离子吸附(或渗透、扩散)于被加工物,故而可防止(抑制)被加工物的金属污染。此外,根据本实施方案,可通过芳香族单羧酸而防止(抑制)被使用于工具的金属材料的氧化,故而可防止(抑制)污物附着于被加工物。进而,根据本实施方案,可通过多元羧酸、芳香族单羧酸及碱性物质的组合而防止(抑制)被使用于工具或加工装置的工具等的的铜的离子化,故而可防止(抑制)被加工物的铜污染。
实施例
其次,对加工介质的实施例及比较例进行说明。
[试样的制作]
首先,以表1-表7中所示的掺合成分的组成制作实施例1-24及比较例1-11的加工介质(试样)。此处,使碱性物质溶解至水中,加入多元羧酸及作为芳香族单羧酸的对叔丁基苯甲酸并进行搅拌,视需要加入界面活性剂、1,2,3-苯并三唑,并加入水以调整浓度,由此获得加工介质。再者,此处,不含防腐剂、消泡剂、香料、染料等。
再者,表1-表7所记载的掺合成分的商品名、制造商名如下所述。
掺合成分:商品名,制造商名
·草酸:草酸二水合物,菱江化学(股)
·苹果酸:DL-Malic Acid,东京化成工业(股)
·延胡索酸:延胡索酸,扶桑化学工业(股)
·柠檬酸:柠檬酸(晶体)H,扶桑化学工业(股)
·辛酸:Lunac(注册商标)8-98,花王(股)
·癸二酸:癸二酸SR,伊藤制油(股)
·对叔丁基苯甲酸:4-叔丁基苯甲酸(PTBBA),扶桑化学工业(股)
·氢氧化钠:苛性钠(固体),鹤见曹达(股)
·单异丙醇胺:单异丙醇胺(MIPA),NANJING HBL ALKYLOL AMINES CO.,LTD.
·二异丙醇胺:二异丙醇胺85%GT级,ダウ·ケミカル日本(股)
·三乙醇胺:TEA(三乙醇胺)99,ジャパンケムテック(股)
·三羟甲基丙烷聚(氧亚丙基)三胺:JEFFAMINE(注册商标)T-403,ハンツマン·ジャパン(股)
·聚亚烷基二醇单丁醚:ユニルーブ(注册商标)50MB-5,日油(股)
·1,2,3-苯并三唑:サンライト123.BTA、サンワ化成(股)
·水:自来水(铜离子溶解量为测定极限以下的水)
[加工组合物的制作]
对实施例及比较例的加工介质100wt%,加入研磨粒(氧化铝基底研磨材料:FO#1000,フジミインコーポレーテッド(股))30wt%并进行搅拌,而获得加工组合物(浆料)。
[研磨加工方法]
将实施例及比较例的加工组合物供给至铸铁压盘(工具)与硅晶圆(被加工物)的接触部,而对硅晶圆进行研磨加工。研磨加工条件如下所述。
[研磨加工条件]
研磨加工机:磨擦试验机GP1(マル卜ー股份有限公司)
压盘:铸铁制直径250mm
压盘槽形状:格子状(格子1边25mm×25mm)
压盘转速:100rpm
对试片的面压力:0.6g/mm2
试片:单晶硅晶圆直径125mm
加工组合物供给量:1L/min
[铸铁压盘防锈性评价]
由于加工组合物与铸铁压盘总是接触,故而假定因铸铁压盘生锈而硅晶圆受到污染,并以下述方式进行铸铁压盘的防锈性的评价。将使用实施例及比较例的加工组合物进行过硅晶圆的研磨加工的铸铁压盘(村料:FC200)的试片以浸渍在加工组合物中的状态于30℃静置10分钟,利用目视评价铸铁压盘表面有无生锈。于铸铁压盘(面积:70mm×50mm)中,将未生锈的情形评价为〇,将产生10个以下的个数的锈迹的情形评价为△,将产生大于10个的个数的锈迹的情形评价为×。
[硅晶圆的金属污染评价]
利用目视观察研磨加工后的硅晶圆,进行是否产生由沿着铸铁压盘的槽的颗粒引起的硅晶圆表面的金属污染(由污物形成的污垢)的试验。将硅晶圆1无金属污染物的情形评价为〇(图1的判定:参照〇的照片),将虽有金属污染物2但于干燥前用纸巾擦拭1次可去除金属污染物2(变色)的情形评价为△,将有金属污染物2且于干燥前即便用纸巾擦拭1次亦无法去除金属污染的情形评价为×(图1的判定:参照×的照片)。
[铜离子溶出量评价]
假定“铜离子自研磨加工机的配管类或在将硅晶圆切出前的步骤中所附着的铜或其合金溶出,硅晶圆表面因溶出的铜离子而受到污染”,测定使用铜试片的铜离子溶出量。在实施例及比较例的加工介质50g(不含研磨粒者)中以浸渍试片(长度约75mm,宽度约12.5mm,厚度1.5-3.0mm)的一半的方式浸渍JIS K 2513(石油制品-铜板腐蚀试验方法)用的铜板(材料:C1100P),于25℃静置18小时后取出加工介质,利用ICP(感应耦合等离子体;发射光谱分析法)装置测定加工介质中的铜离子溶出量。ICP装置的详细内容如下所述。
[ICP装置]
制造商:AMETEK(MATERIALS ANALYSIS DIVISION,材料分析部门)
装置名:SPECTRO ARCOS(注册商标)
型号:FHM22
类型:MV130(多视图)
测定条件:原液测定
测定方法:SOP(Side On Plasma)侧面方向(径向)
[pH值测定]
使用pH值测定器(堀场制作所制造,“玻璃电极式氢离子浓度计pH METER F-11”,“pH电极LAQUA(注册商标)6377”)而测定pH值。
[表1]
[表2]
[表3]
[表4]
[表5]
[表6]
[表7]
[多元羧酸与单羧酸的组合的评价]
关于不含有多元羧酸且含有对叔丁基苯甲酸的比较例1,由于缺少多元羧酸及对叔丁基苯甲酸的两者的作用,故而无铸铁压盘的防锈性而无法抑制硅晶圆的金属污染及铜离子的溶出量。但是,关于不含有多元羧酸且含有对叔丁基苯甲酸的比较例3,即便无多元羧酸及对叔丁基苯甲酸的两者的作用,亦通过成为铜溶出防止剂的1,2,3-苯并三唑的作用而具有铸铁压盘的防锈性,且铜离子的溶出量得到抑制,但是无法抑制硅晶圆的金属污染。因此,可知1,2,3-苯并三唑虽然具有铸铁压盘的防锈性,但是并无抑制硅晶圆的金属污染的作用。
关于含有柠檬酸(碳数6)作为多元羧酸且不含有对叔丁基苯甲酸的比较例2,由于缺少多元羧酸及对叔丁基苯甲酸的两者的作用,故而无铸铁压盘的防锈性,亦无法抑制硅晶圆的金属污染及铜离子的溶出量。
关于不含有多元羧酸且含有对叔丁基苯甲酸的比较例4,虽然通过其他单羧酸(辛酸)的作用而有铸铁压盘的防锈性,但是由于缺少多元羧酸及对叔丁基苯甲酸的两者的作用,故而亦无法抑制硅晶圆的金属污染及铜离子的溶出量。
关于含有癸二酸(碳数10)作为多元羧酸且含有对叔丁基苯甲酸的比较例5,其中多元羧酸中的碳数过多,而无基于碳数7以下的多元羧酸及对叔丁基苯甲酸的两者的存在的作用,无铸铁压盘的防锈性,而无法抑制硅晶圆的金属污染、铜离子溶出量。
关于含有柠檬酸及癸二酸(碳数6及10)作为多元羧酸且不含有对叔丁基苯甲酸的比较例6,虽然通过多元羧酸的作用而有铸铁压盘的防锈性,但是缺少多元羧酸及对叔丁基苯甲酸的两者的作用,故而亦无法抑制硅晶圆的金属污染及铜离子的溶出量。
关于含有柠檬酸(碳数6)作为多元羧酸且不含有对叔丁基苯甲酸的比较例7,虽然通过单羧酸(辛酸)的作用而有铸铁压盘的防锈性,但是缺少多元羧酸及对叔丁基苯甲酸的两者的作用,故而亦无法抑制硅晶圆的金属污染及铜离子的溶出量。
关于含有间苯二甲酸(碳数8)作为多元羧酸且含有对叔丁基苯甲酸的比较例8,由于具有铸铁压盘的防锈性,可抑制硅晶圆的金属污染,故而具有与基于碳数7以下的多元羧酸及对叔丁基苯甲酸的两者存在的作用相同的作用,但是关于铜离子溶出量,尽管发现抑制的倾向但未达到合格基准。
另一方面,关于实施例1-9,通过对叔丁基苯甲酸的作用而具有铸铁压盘的防锈性,通过碳数2~7的多元羧酸的作用而可抑制硅晶圆的金属污染,通过多元羧酸及对叔丁基苯甲酸的两者的作用的存在而亦可抑制铜离子的溶出量(参照表1)。再者,如实施例6般,若多元羧酸及对叔丁基苯甲酸的合计掺合量减少,则铸铁压盘的防锈性变小。
[多元羧酸及对叔丁基苯甲酸的掺合比的评价]
关于多元羧酸(柠檬酸:碳数6)及对叔丁基苯甲酸的掺合比,参照表3,1∶4以上且未达2∶1的实施例10-12具有铸铁压盘的防锈性,亦可抑制硅晶圆的金属污染及铜离子的溶出量。此外,关于多元羧酸(草酸:碳数2)及对叔丁基苯甲酸的掺合比,参照表5,未达2∶1的实施例19-21具有铸铁压盘的防锈性,可抑制硅晶圆的金属污染及铜离子的溶出量。
[多元羧酸及对叔丁基苯甲酸的合计掺合量的评价]
关于多元羧酸(柠檬酸:碳数6)及对叔丁基苯甲酸的合计掺合量,参照表4,处于0.05wt%以上且15wt%以下的范围内的实施例13-17具有铸铁压盘的防锈性,亦可抑制硅晶圆的金属污染及铜离子的溶出量。随着接近0.05wt%或15wt%,而有铸铁压盘的防锈性变小,硅晶圆的金属污染变大的倾向。此外,关于多元羧酸(草酸:碳数2)及对叔丁基苯甲酸的合计掺合量,参照表6,处于0.05wt%以上且15wt%以下的范围内的实施例22-24具有铸铁压盘的防锈性,可抑制硅晶圆的金属污染。
[碱性物质的评价]
参照表7,在不含有碱性物质的比较例11中,对叔丁基苯甲酸未溶于水中,而无法获得稳定的加工介质。
(附记)
在本发明中,能够实现上述加工介质的形态。
在上述加工介质中,上述多元羧酸的碳数优选为2以上且6以下、3以上且7以下,更优选为3以上且6以下。
在上述加工介质中,上述碱性物质为钠化合物、钾化合物、铵化合物及胺化合物中的任意一种以上。
在上述加工介质中,上述碱性物质包含有钠化合物及胺化合物。
在上述加工介质中,上述碱性物质包含有多种胺化合物。
在上述加工介质中,进而含有水。
在上述加工介质中,上述多元羧酸及上述芳香族单羧酸的合计为0.05wt%以上且15wt%以下,上述碱性物质为0.1wt%以上且20wt%以下,上述水为50wt%以上且99.7wt%以下。多元羧酸及芳香族单羧酸的合计掺合量更优选为0.1wt%以上且4wt%以下,进而优选为0.2wt%以上且2wt%以下。上述碱性物质的掺合量更优选为0.2wt%以上且10wt%以下,进而优选为0.5wt%以上且5wt%以下。水的掺合量更优选为80wt%以上且99.5wt%以下,进而优选为90wt%以上且98wt%以下。
在上述加工介质中,上述多元羧酸及上述芳香族单羧酸的掺合比为1∶4以上且未达2∶1。上述多元羧酸及芳香族单羧酸的掺合比更优选为1∶1.8以上且1.8∶1以下,进而优选为1∶1.5以上且1.5∶1以下。
在上述加工介质中,pH值大于7。上述pH值更优选为8以上且12.5以下,进而优选为8以上且10以下。
在上述加工介质中,含有界面活性剂、消泡剂、防腐剂、香料及染料的至少一种。
在上述加工介质中,相对于根据权利要求5至7中任一项所述的加工介质100wt%,掺合有界面活性剂0.01wt%以上且5wt%以下。上述界面活性剂的掺合量优选为0.02wt%以上且3wt%以下,更优选为0.05wt%以上且1wt%以下。
在上述加工介质中,相对于根据权利要求5至7中任一项所述的加工介质100wt%,掺合有消泡剂0.001wt%以上且1wt%以下。上述消泡剂的掺合量优选为0.002wt%以上且0.5wt%以下,更优选为0.005wt%以上且0.1wt%以下。
在上述加工介质中,不含苯并三唑。
在上述加工介质中,在将铜浸渍在上述加工介质中时,上述加工介质中的铜离子为70ppm以下。在将铜浸渍在上述加工介质中时,上述加工介质中的铜离子优选为60ppm以下,更优选为50ppm以下。
在本发明中,能够实现上述加工组合物的形态。
在上述加工组合物中,在将上述加工组合物供给至铸铁压盘与硅晶圆的接触部而对上述硅晶圆进行研磨加工时,上述硅晶圆表面无金属污染物。或者,存在于上述硅晶圆表面的金属污染物于干燥前可被擦拭去除。
在上述加工组合物中,将使用上述加工组合物进行过硅晶圆的研磨加工的铸铁压盘以浸渍于上述加工组合物中的状态于30℃静置了10分钟时,上述铸铁压盘的表面未生锈,或者于70mm×50mm的面积中锈迹的产生数为10个以下。
在本发明中,能够实现上述加工方法的形态。
再者,通过引用将上述专利文献的揭示内容编入至本说明书中。在本发明的所有揭示(包含权利要求书及附图)的范围内,可进而基于其基本技术思想而进行实施方案或实施例的变更、调整。此外,在本发明的所有揭示的范围内,可对各种揭示要素(包含各权利要求书的各要素、各实施方案或实施例的各要素、各附图的各要素等)进行多种组合或选择(视需要不选择)。即,本发明当然包括本领域技术人员根据包含权利要求书及附图在内的所有揭示、技术思想所能实现的各种变形、修正。此外,关于本申请所记载的数值及数值范围,即便无说明,也视为记载了其任意的中间值、下位数值及小范围。
符号说明
1:硅晶圆
2:金属污染物
Claims (9)
1.一种加工介质,其含有或在已中和的状态下含有碳数为2以上且7以下的多元羧酸、芳香族单羧酸及碱性物质。
2.根据权利要求1所述的加工介质,其中,该碱性物质为钠化合物、钾化合物、铵化合物及胺化合物中的任意一种以上。
3.根据权利要求1或2所述的加工介质,其中,该碱性物质包含有多种胺化合物。
4.根据权利要求1至3中任一项所述的加工介质,其进而含有水。
5.根据权利要求4所述的加工介质,其中,该多元羧酸及该芳香族单羧酸的合计为0.05wt%以上且15wt%以下,
该碱性物质为0.1wt%以上且20wt%以下,
该水为50wt%以上且99.7wt%以下。
6.根据权利要求5所述的加工介质,其中,该多元羧酸及该芳香族单羧酸的掺合比为1∶4以上且未达2∶1。
7.根据权利要求4至6中任一项所述的加工介质,其pH值大于7。
8.一种加工组合物,其含有权利要求1至7中任一项所述的加工介质与研磨粒。
9.一种加工方法,其将权利要求1至7中任一项所述的加工介质或权利要求8所述的加工组合物供给至工具与被加工物的接触部分而对该被加工物进行加工。
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JPH1022241A (ja) * | 1996-07-08 | 1998-01-23 | Tokyo Fine Chem Kk | シリコンウェハ用ラップ液およびラップ剤 |
JP2005285944A (ja) * | 2004-03-29 | 2005-10-13 | Hitachi Chem Co Ltd | 金属用研磨液及び研磨方法 |
CN103555410A (zh) * | 2013-11-21 | 2014-02-05 | 李荣福 | 一种汽车连杆用水基防锈磨削冷却液及其制备方法和用途 |
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JP6661175B2 (ja) | 2020-03-11 |
KR20190112278A (ko) | 2019-10-04 |
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