TWI791585B - 研磨用組合物、研磨用組合物的製造方法、研磨方法及半導體基板的製造方法 - Google Patents
研磨用組合物、研磨用組合物的製造方法、研磨方法及半導體基板的製造方法 Download PDFInfo
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- TWI791585B TWI791585B TW107127584A TW107127584A TWI791585B TW I791585 B TWI791585 B TW I791585B TW 107127584 A TW107127584 A TW 107127584A TW 107127584 A TW107127584 A TW 107127584A TW I791585 B TWI791585 B TW I791585B
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Classifications
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- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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- 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
- B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
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- 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
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- C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
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- C—CHEMISTRY; METALLURGY
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
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- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
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- C—CHEMISTRY; METALLURGY
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01G—WEIGHING
- G01G1/00—Weighing apparatus involving the use of a counterweight or other counterbalancing mass
- G01G1/02—Pendulum-weight apparatus
- G01G1/04—Pendulum-weight apparatus the pendulum having a fixed pivot axis
- G01G1/06—Pendulum-weight apparatus the pendulum having a fixed pivot axis with a plurality of pendulums
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- G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
- G09G—ARRANGEMENTS OR CIRCUITS FOR CONTROL OF INDICATING DEVICES USING STATIC MEANS TO PRESENT VARIABLE INFORMATION
- G09G1/00—Control arrangements or circuits, of interest only in connection with cathode-ray tube indicators; General aspects or details, e.g. selection emphasis on particular characters, dashed line or dotted line generation; Preprocessing of data
- G09G1/04—Deflection circuits ; Constructional details not otherwise provided for
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- 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
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
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- H01L21/3105—After-treatment
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- H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
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Abstract
本發明相關的研磨用組合物,包含:二氧化矽;陰離子性水溶性高分子;選自由含有膦酸基的化合物、含有磷酸基的化合物、及含有胺基的化合物所組成之群之至少1種化合物;及分散媒。
Description
本發明係關於研磨用組合物、研磨用組合物的製造方法、研磨方法及半導體基板的製造方法。
近年,隨著半導體基板表面的多層線路化,在製造裝置時,利用將半導體基板物理性地研磨而平坦化的所謂化學機械研磨(chemical mechanical polishing;CMP)技術。CMP是使用包含二氧化矽或氧化鋁、二氧化鈰等的研磨粒、防蝕劑、界面活性劑等的組合物(漿料),將半導體基板等的研磨對象物(被研磨物)的表面平坦化的方法,具體而言,其使用於淺溝隔離(STI)、層間絕緣膜(ILD膜)的平坦化、鎢插塞形成、由銅與低介電常數膜等所構成的多層線路的形成等的步驟。在如此的CMP,要求將絕緣膜(氮化矽等)與導電物質(氮化鈦等)以高研磨選擇比研磨去除(即,以比氮化鈦等的導電物質更高的研磨速率去除氮化矽等的絕緣膜)。
作為提升氮化矽與氮化鈦的研磨選擇比的手段,可考慮控制氮化鈦的研磨速率。例如,美國專利申請公開第2015/221521號說明書,揭示藉由使用含有研磨粒與界面活性劑的研磨用組合物,可抑制氮化鈦的研磨速率。
但是,本發明者,使用上述美國專利申請公開第2015/221521號說明書的研磨用組合物,研磨含有氮化矽及氮化鈦的研磨對象物時,發現特別是在強酸性(pH為2.5以下),依然無法得到氮化矽與氮化鈦的高研磨速率比。
本發明是有鑑於上述課題而完成,以提供即使在強酸性(pH為2.5以下),相對於氮化鈦的研磨速率,氮化矽的研磨速率為充分高(即,氮化矽/氮化鈦的選擇比高)的研磨用組合物為目標。
本發明者有鑑於上述課題,專心進行研究。結果發現,藉由使用包含:二氧化矽;陰離子性水溶性高分子;選自由含有膦酸基的化合物、含有磷酸基的化合物、及含有胺基的化合物所組成之群之至少1種化合物;及分散媒的研磨用組合物,可解決上述課題,而完成本發明。
[用於實施發明的形態]
以下說明本發明。再者,本發明並非限定於以下的實施形態。此外,若無特別提及,操作及物性等的測定是在室溫(20~25°C)/相對濕度40~50%RH的條件下測定。
再者,在本說明書,在化合物的具體名所記述的「(甲基)丙烯醯基」是表示「丙烯醯基」及「甲基丙烯醯基」,「(甲基)丙烯酸酯」是表示「丙烯酸酯」及「甲基丙烯酸酯」。
本發明相關的研磨用組合物,期待可對包含一般的絕緣膜及導電物質的研磨對象物有效。上述絕緣膜,可列舉,例如,氧化矽、氮化矽等。上述導電物質,可列舉,例如,鈦、氮化鈦、鉭、氮化鉭等。其中,由於對包含氮化矽(SiN)及氮化鈦(TiN)的研磨對象物有顯著的效果,因而較佳。作為包含氮化矽(SiN)及氮化鈦(TiN)的研磨對象物的具體例,可列舉具有在氮化矽膜上形成氮化鈦膜的構造的半導體基板,或是具有氮化矽膜與氮化鈦膜均露出的構造的半導體基板等。
在此,就發揮本發明的效果的觀點而言,本發明的一形態相關的研磨用組合物,較佳為用於研磨包含氮化矽與氮化鈦的研磨對象物的步驟。該研磨對象物,推測是藉由後述的作用機制,選自由陰離子性水溶性高分子,含有膦酸基的化合物、含有磷酸基的化合物、及含有胺基的化合物所組成之群之至少1種化合物的研磨抑制作用變得更強。
本發明者,推定藉由本發明解決上述課題的機制如下。惟,下述機制僅為推測,本發明的範圍並非限定於此。
本發明相關的研磨用組合物,研磨用組合物所含有的各成分與研磨對象物相互作用的結果,具有抑制氮化鈦的研磨速率的功能。本發明相關的研磨用組合物,包含:二氧化矽;陰離子性水溶性高分子;選自由含有膦酸基的化合物、含有磷酸基的化合物、及含有胺基的化合物所組成之群之至少1種化合物(以下亦簡稱為TiN抑制劑);及分散媒。pH為酸性時,由於氮化鈦膜的表面會帶正電,故陰離子性水溶性高分子吸附在氮化鈦膜,而在氮化鈦膜的表面形成保護膜,因而能夠抑制氮化鈦的研磨。惟,隨著pH變得更強酸性,陰離子性水溶性高分子對氮化鈦的吸附會變弱,而無法充分抑制氮化鈦的研磨速率。因此,本發明者專心進行研究,結果發現,藉由進一步添加TiN抑制劑,可抑制氮化鈦的研磨速率。其理由在於,TiN抑制劑會極化成具有正電荷的部分與具有負電荷的部分,即使在強酸性下,具有負電荷的部分仍可強固地吸附在氮化鈦膜的表面,但是分子量小而無法充分覆蓋氮化鈦的表面。然而,併用TiN抑制劑與陰離子性水溶性高分子時,陰離子性水溶性高分子會進一步電性吸附在TiN抑制劑之具有正電荷的部分。因此,藉由併用TiN抑制劑及陰離子性水溶性高分子,即使在強酸性下,亦能夠充分覆蓋氮化鈦膜的表面,能夠形成保護膜而抑制研磨速率。特別是在pH為2.5以下的強酸性下,可顯著地顯現如此的效果。由以上情況來看,本發明的研磨組合物,能夠以高速度研磨氮化矽,同時能夠抑制氮化鈦的研磨速率,因而被認為可實現氮化矽與氮化鈦的高研磨選擇比。因此,根據本發明,可提供即使在強酸性(pH為2.5以下),相對於氮化鈦的研磨速率,氮化矽的研磨速率為充分高(即,氮化矽/氮化鈦的選擇比高)的研磨用組合物。
(二氧化矽) 本發明相關的研磨用組合物,含有二氧化矽。包含在研磨用組合物中的二氧化矽,具有對研磨對象物進行機械性研磨的作用。二氧化矽的種類,並無特別限定,可列舉,例如,膠態二氧化矽、氣相二氧化矽(fumed silica)、溶膠凝膠法二氧化矽等。該等之中,就可有效地發揮與研磨對象物的固相反應的觀點而言,以膠態二氧化矽為佳。
膠態二氧化矽的製造方法,可列舉矽酸鈉法、溶膠凝膠法,以任一種製造方法所製造的膠態二氧化矽皆可。此外,作為膠態二氧化矽的市售品之例,可列舉,例如,日產化學工業株式會社製、日揮觸媒化成株式會社製、日本化學工業株式會社製、扶桑化學工業株式會社製、株式會社ADEKA製、Akzo Nobe1公司製、AZ Electronic Materials公司製、Nalco公司製、WRGrace公司製等的膠態二氧化矽。
二氧化矽的平均一次粒徑的下限,以6nm以上為佳,以8nm以上為更佳,以10nm以上為進一步更佳。在如此的範圍,能夠維持高研磨速率,因而可適合使用於粗研磨步驟等。此外,二氧化矽的平均一次粒徑的上限,以200nm以下為佳,以100nm以下為更佳,以50nm以下為進一步更佳,以30nm以下為特佳。在如此的範圍內,能夠更加抑制在研磨後的研磨對象物表面發生缺陷。再者,二氧化矽的平均一次粒徑,例如,可根據BET法所測定的二氧化矽的比表面積而計算。
二氧化矽的平均二次粒徑的下限,以15nm以上為佳,以20nm以上為更佳,以25nm以上為進一步更佳。在如此的範圍內,能夠維持高研磨速率,因而可適合使用在粗研磨步驟。此外,二氧化矽的平均二次粒徑的上限,以300nm以下為佳,以200以下為更佳,以100nm以下為進一步更佳,以50nm以下為特佳。在如此的範圍內,能夠更加抑制在研磨後的矽晶圓表面發生缺陷。二氧化矽的平均二次粒徑,例如,可藉由動態光散射法測定。
二氧化矽的含量,相對於研磨用組合物,以0.1質量%以上為佳,以0.5質量%以上為更佳,以1.0質量%以上為進一步更佳,以1.4質量%以上為特佳。在如此的範圍,能夠維持高研磨速率,因而可適合使用在粗研磨步驟等。此外,就防止刮痕等的觀點而言,二氧化矽的含量,通常為10質量%以下,以5質量%以下為佳,以4質量%以下為更佳,以3質量以下為特佳。減少二氧化矽的含量,就經濟性的觀點而言亦為較佳。
(分散媒) 本發明相關的研磨用組合物,包含用於分散或溶解各成分的分散媒。作為分散媒,就阻礙清洗對象物的污染或其他的成分的作用的觀點而言,水,以盡可能以不含雜質的水為佳。作為如此的水,例如,較佳為過渡金屬離子的合計含量為100ppb以下的水。在此,例如,可使用離子交換樹脂去除雜質離子、藉由過濾器去除異物、藉由蒸餾等的操作而提升水的純度。具體而言,水,以使用,例如,去離子水(離子交換水)、純水、超純水、蒸餾水等為佳。
分散媒,為了分散或溶解各成分,亦可為水與有機溶劑的混合溶劑。此時,可使用的有機溶劑,可列舉可與水混合的有機溶劑的丙酮、乙腈、乙醇、甲醇、異丙醇、甘油、乙二醇、丙二醇等。此外,亦可將該等有機溶劑不與水混合使用,先將各成分分散或溶解之後,再與水混合。該等有機溶劑,可以單獨亦可組合2種以上使用。
(陰離子性水溶性高分子) 本發明相關的研磨用組合物,含有陰離子性水溶性高分子。在研磨上述的研磨對象物的用途使用研磨用組合物時,研磨用組合物中的陰離子性水溶性高分子,會吸附在氮化鈦的層的表面上。藉此,本發明相關的研磨用組合物能夠抑制氮化鈦的研磨速率。
作為陰離子性水溶性高分子的陰離子性基,羧酸基(羧基)、磺酸基、硫酸酯基、磷酸酯基、膦酸基等,就減低刮痕、粒子的觀點而言,以具有羧酸基之物為佳,以僅具有羧酸基之物為更佳。即,在本發明,上述陰離子性水溶性高分子,以聚羧酸(polycarboxylic acid)為佳。再者,該等陰離子性基亦可採取已中和的鹽的形態。
作為具有羧酸基的水溶性高分子,可列舉來自具有羧酸基的單體的構成單位的(共)聚合物或其鹽。作為具有羧酸基的單體,可列舉,例如,伊康酸、(甲基)丙烯酸、馬來酸或其鹽等。陰離子性水溶性高分子,亦可包含2種以上來自具有羧酸基的單體的構成單位。該等之中,作為陰離子性水溶性高分子,可列舉聚(甲基)丙烯酸、及(甲基)丙烯酸-馬來酸共聚物或其鹽。
上述陰離子性水溶性高分子,在發揮本發明的效果的範圍內,亦可含有來自含有陰離子性基的單體以外的單體的構成單位成分。
研磨用組合物中的陰離子性水溶性高分子的含量,以1質量ppm以上為佳,以10質量ppm以上為更佳,以100質量ppm以上為進一步更佳,以1000質量ppm以上為又進一步更佳,以2000質量ppm以上為特佳。隨著陰離子性水溶性高分子的含量變多,吸附在氮化鈦膜上的陰離子性水溶性高分子變多,能夠有效地抑制氮化鈦的研磨速率。
研磨用組合物中的陰離子性水溶性高分子的含量,以100000質量ppm以下為佳,以10000質量ppm以下為更佳,以8000質量ppm以下為進一步更佳,以6000質量ppm以下為又進一步更佳,以4000質量ppm以下為特佳。隨著水溶性聚合物的含量變少,研磨用組合物中的研磨粒會變得不容易團聚。因此,具有提升研磨用組合物的儲存穩定性之有利效果。
研磨用組合物中的陰離子性水溶性高分子的重量平均分子量(Mw),以1000以上為佳,以1500以上為更佳,以2000以上為進一步更佳,以3000以上為進一步更佳,以4000以上為進一步更佳,以4500以上為特佳。隨著陰離子性水溶性高分子的分子量變大,容易在氮化鈦層的表面吸附充分量的高分子,因而能夠抑制研磨用組合物對氮化鈦層的研磨速率。
研磨用組合物中的陰離子性水溶性高分子的重量平均分子量(Mw),以10000以下為佳,以6000以下為更佳,以5500以下為進一步更佳,以5400以下為又進一步更佳,以5300以下為特佳。隨著水溶性聚合物的分子量變小,研磨用組合物中的研磨粒會變得不容易團聚。因此,具有提升研磨用組合物的儲存穩定性之有利效果。高分子化合物的重量平均分子量,是使用以凝膠滲透層析儀(GPC)所測定的重量平均分子量(聚乙二醇換算)之值。重量平均分子量,是以下述裝置及條件測定。
GPC裝置︰株式會社島津製造所製 型式︰Prominence+ELSD檢測器(ELSD-LTII) 管柱︰VP-ODS(株式會社島津製造所製) 移動相A︰MeOH B:乙酸1%水溶液 流量︰1mL/分 檢測器︰ELSD ,temp.:40°C,Gain:8,N2
GAS:350kPa 烘箱溫度︰40°C 注入量︰40μL。
(TiN抑制劑)
本發明相關的研磨用組合物,包含:含有膦酸基的化合物、含有磷酸基的化合物、及含有胺基的化合物所組成之群之至少1種化合物作為TiN抑制劑。此外,如上所述,藉由添加陰離子性水溶性高分子,亦可抑制氮化鈦的研磨速率,惟,藉由添加TiN抑制劑,可更進一步抑制氮化鈦的研磨速率。
隨著研磨用組合物的pH變得更強酸性,僅使用陰離子性水溶性高分子,氮化鈦的研磨速率的抑制仍會變得不充分。因此,藉由併用TiN抑制劑與陰離子性水溶性高分子,即使在強酸性下仍可充分覆蓋氮化鈦膜的表面,能夠形成保護膜而抑制研磨速率。再者,TiN抑制劑,可使用1種亦可併用複數種。
可使用於作為TiN抑制劑的含有膦酸基的化合物,較佳的可列舉具有1~6個膦酸基的化合物。具體而言,包含1個膦酸基的化合物,可列舉膦酸、甲基膦酸、苯基膦酸、及1-萘基甲基膦酸等。此外,包含2個以上的膦酸基的化合物,可列舉亞甲基二膦酸(methylene diphosphonic acid, MDPNA)、伸乙基二膦酸(ethylenediphosphonic acid EDPNA)、1-羥基乙烷-1,1-二膦酸(etidronic acid, 艾提壯酸;1-hydroxyethane-1,1-diphosphonic acid , HEDP)、氮基三(亞甲基膦酸)(nitrilotris (methylenephosphonic acid), NTMP)、乙二胺四膦酸(ethylenediamine tetraphosphonic acid)、乙二胺四亞甲基膦酸(ethylenediamine tetramethylenephosphonic acid, EDTMP)及二伸乙三胺五(亞甲基膦酸)(diethylenetriaminepenta (methylenephosphonic acid, DTPMP)等。上述含有膦酸基的化合物之中,較佳為在1分子中具有2個以上膦酸基,以3~5個膦酸基的化合物為佳。例如,上述含有膦酸基的化合物,以氮基三(亞甲基膦酸)(NTMP)、乙二胺四亞甲基膦酸(EDTMP)及二伸乙三胺五(亞甲基膦酸)(DTPMP)為特佳。
可使用於作為TiN抑制劑的含有磷酸基的化合物,可列舉無機磷酸化合物及有機磷酸化合物。作為無機磷酸化合物,具體可列舉磷酸(正磷酸)、亞磷酸、次磷酸等的單磷酸類、焦磷酸、焦亞膦酸、三磷酸、四磷酸、六磷酸、環磷酸、偏磷酸(metaphosphoric acid)、六偏磷酸(hexametaphosphoric acid)等的多磷酸類、及該等的鹽。作為有機磷酸化合物,具體可列舉十四烷基磷酸、十六烷基磷酸、十八烷基磷酸、二癸基磷酸、10-甲基丙烯醯氧癸基二氫磷酸酯、12-丙烯醯氧十二烷基二氫磷酸酯、12-甲基丙烯醯氧十二烷基二氫磷酸酯、16-丙烯醯氧十六烷基二氫磷酸酯、16-甲基丙烯醯氧十六烷基二氫磷酸酯、20-丙烯醯氧二十烷基二氫磷酸酯、20-甲基丙烯醯氧二十烷基二氫磷酸酯、雙[8-丙烯醯氧辛基]氫磷酸酯、雙[8-甲基丙烯醯氧辛基]氫磷酸酯、雙[9-丙烯醯氧壬基]氫磷酸酯、雙[9-甲基丙烯醯氧壬基]氫磷酸酯、雙[10-丙烯醯氧癸基]氫磷酸酯、雙[10-甲基丙烯醯氧癸基]氫磷酸酯等的烷基磷酸酯類;雙辛基焦磷酸酯、雙[8-丙烯醯氧辛基]焦磷酸酯、雙[8-甲基丙烯醯氧辛基]焦磷酸酯、雙[10-丙烯醯氧癸基]焦磷酸酯、雙[10-甲基丙烯醯氧癸基]焦磷酸酯等的焦磷酸酯類。
研磨用組合物中的含有膦酸基的化合物或含有磷酸基的化合物的含量(包含二種以上時,為其合計量),以50質量ppm以上為佳,以100質量ppm以上為更佳,以120質量ppm以上為進一步更佳,以150質量ppm以上為進一步更佳,以220質量ppm以上為進一步更佳,以240質量ppm以上為進一步更佳,以260質量ppm以上為進一步更佳,以270質量ppm以上為特佳。隨著含有膦酸基的化合物或含有磷酸基的化合物的含量變多,吸附在氮化鈦膜上的TiN抑制劑變多,能夠有效地抑制氮化鈦的研磨速率。
研磨用組合物中的含有膦酸基的化合物或含有磷酸基的化合物的含量(包含二種以上時,為其合計量),以10000質量ppm以下為佳,以1000質量ppm以下為更佳,以800質量ppm以下為進一步更佳,以600質量ppm以下為進一步更佳,以500質量ppm以下為進一步更佳,以450質量ppm以下為進一步更佳,以400質量ppm以下為特佳。隨著含有膦酸基的化合物或含有磷酸基的化合物的含量變少,不容易降低研磨對象物,特別是包含在研磨對象物中的氮化矽的研磨速率。
研磨用組合物中的含有膦酸基的化合物或含有磷酸基的化合物的分子量,就SiN的研磨速率的觀點而言,以未滿1000為佳,以未滿600為更佳。分子量小的含有膦酸基的化合物或含有磷酸基的化合物,不容易使SiN的研磨速率下降。
可使用於研磨組合物的含有胺基的化合物,可列舉,例如,胺基酸、含有胺基的聚烷二醇(polyalkylene glycol)、一級脂肪族胺等。該等之中,以胺基酸為特佳。上述胺基酸,是指具有胺基與羧基的雙方的官能基的有機化合物。作為胺基酸的具體例,可列舉甘胺酸、α-丙胺酸、β-丙胺酸、N-甲基甘胺酸、N,N-二甲基甘胺酸(N,N-dimethylglycine)、2-胺基丁酸、正纈胺酸(norvaline)、纈胺酸(valine)、白胺酸(leucine)、正白胺酸(norleucine)、異白胺酸(isoleucine)、苯基丙胺酸、脯胺酸(proline)、肌胺酸(sarcosine)、鳥胺酸(ornithine)、離胺酸(lysine)、牛磺酸(taurine)、絲胺酸(serine)、蘇胺酸(threonine)、高絲胺酸(homoserine)、酪胺酸(tyrosine)、羥乙甘胺酸(bicine)、三(羥甲基)甲基甘胺酸(tricine)、3,5-二碘酪胺酸(3,5-diiodo-tyrosine)、β-(3,4-二羥苯基)丙胺酸、甲狀腺素(thyroxine)、4-羥基脯胺酸、半胱胺酸(cysteine)、甲硫胺酸(methionine)、乙硫胺酸、羊毛硫胺酸(lanthionine)、胱硫醚(cystathionine)、胱胺酸(cystine)、氧化半胱胺酸(cysteic acid)、天冬胺酸(aspartic acid)、麩胺酸(glutamic acid)、S-(羧甲基)- 半胱胺酸、4-胺基丁酸、天冬醯胺酸(asparagine)、麩醯胺酸(glutamine)、氮絲胺酸(azaserine)、精胺酸(arginine)、刀豆胺酸(canavanine)、瓜胺酸(citrulline)、δ-羥基-離胺酸(δ-hydroxy-lysine)、肌酸(creatine)、組胺酸(histidine)、1-甲基組胺酸、3-甲基組胺酸及色胺酸(tryptophan)。其中,就SiN的研磨速率的觀點而言,以鹼性胺基酸為更佳,具體而言,以精胺酸、離胺酸、色胺酸、組胺酸及瓜胺酸為特佳。本發明的研磨用組合物的pH,由於比鹼性胺基酸的等電點(iso-electrostatic point)低,故鹼性胺基酸會帶正電,或不帶電,含有膦酸基的化合物或含有磷酸基的化合物會使SiN的研磨速率不容易下降。
研磨用組合物中的含有胺基的化合物的含量(包含二種以上時,為其合計量),以100質量ppm以上為佳,以1000質量ppm以上為更佳,以5000質量ppm以上為進一步更佳。在如此的範圍,能夠以高研磨速率研磨SiN。研磨用組合物中的含有胺基的化合物的含量,以100000質量ppm以下為佳,以50000質量ppm以下為更佳,以20000質量ppm以下為進一步更佳,10000質量ppm以下為特佳。在如此的範圍,能夠減少用於調整為目標pH的pH調整劑的量,可得到漿料穩定性的效果。
(pH及pH調整劑) 根據本發明的實施形態,研磨用組合物的pH,並無特別限制,下限以1.0以上為佳,以1.5以上為更佳,以1.7以上為進一步更佳,以2.0以上為特佳。另一方面,上限以7.0以下為佳,以5.0以下為更佳,以3.0以下為進一步更佳,以2.5以下為特佳。因此,根據本發明的一實施形態,研磨用組合物的pH為1.0~7.0。從本發明的機制來看,藉由該實施形態,提高研磨時的選擇比的效果特別顯著。
作為pH調整劑,可使用習知的酸、鹼,或該等的鹽。
可使用於作為pH調整劑的酸的具體例,可列舉,例如,鹽酸、硫酸、硝酸、氫氟酸、硼酸、碳酸、次磷酸、亞磷酸、及磷酸等的無機酸、或甲酸、乙酸、丙酸、丁酸、戊酸、2-甲基丁酸、正己酸、3,3-二甲基丁酸、2-乙基丁酸、4-甲基戊酸、正庚酸、2-甲基己酸、正辛酸、2-乙基己酸、安息香酸、乙醇酸(glycolic acid)、水楊酸、甘油酸、草酸、丙二酸、琥珀酸、戊二酸、己二酸、庚二酸、馬來酸、鄰苯二甲酸、蘋果酸、葡萄糖酸(gluconic acid)、伊康酸、酒石酸、檸檬酸、乳酸、縮二羥乙酸(diglycolic acid)、2-呋喃甲酸(2-furancarboxylic acid)、2,5-呋喃二甲酸(2,5-furandicarboxylic acid)、3-呋喃甲酸(3-furancarboxylic acid)、2-四氫呋喃甲酸(2-tetrahydrofuran carboxylic acid)、甲氧基乙酸(methoxyacetic acid,)、甲氧基苯乙酸(methoxyphenylacetic acid)、及苯氧乙酸(phenoxyacetic acid)等的有機酸。使用無機酸作為pH調整劑時,就提升研磨速率的觀點而言,以硫酸、硝酸、磷酸等為特佳,使用有機酸作為pH調整劑時,以乙醇酸、琥珀酸、馬來酸、檸檬酸、酒石酸、蘋果酸、葡萄糖酸、及伊康酸等為佳。
可使用於作為pH調整劑的鹼的具體例,可列舉,例如,脂肪族胺、芳香族胺等的胺、氫氧化四級銨等的有機鹼、氫氧化鉀等的鹼金屬的氫氧化合物、鹼土金屬的氫氧化合物、氫氧化四甲基銨、及氨等。該等之中,就取得容易性而言,以氫氧化鉀或氨為佳。
pH調整劑的添加量,並無特別限制,只要將研磨用組合物適宜調整為所期望的pH即可。
(研磨用組合物的製造方法) 本發明相關的研磨用組合物的製造方法,並無特別限制。例如,可將二氧化矽、陰離子性水溶性高分子、TiN抑制劑及視需要的其他的添加劑,在分散媒中攪拌混合而得。在一實施形態提供一種研磨用組合物的製造方法,其包含:將二氧化矽、陰離子性水溶性高分子、選自由含有膦酸基的化合物、含有磷酸基的化合物、及含有胺基的化合物所組成之群之至少1種化合物、及分散媒混合。
(研磨方法) 在一實施形態提供一種研磨方法,其包含:使本發明相關的研磨用組合物對研磨對象物進行研磨的步驟。
例如,準備包含本發明相關的研磨用組合物的工作漿料(working slurry)。接著,將該研磨用組合物供給到研磨對象物,藉由常法研磨。例如,將研磨對象物安裝在一般的研磨裝置,將研磨用組合物通過該研磨裝置的研磨墊供給到該研磨對象物表面(研磨對象面)。典型的做法是連續供給上述研磨用組合物,同時將研磨墊向研磨對象物的表面按押,而使兩者相對移動(例如,旋轉移動)。經由該研磨步驟完成研磨對象物的研磨。
在上述研磨步驟所使用的研磨墊,並無特別限制。可使用,例如,發泡聚胺酯型、不織布型、搖擺型、包含研磨粒之物、不含研磨粒之物等的任一者。此外,上述研磨裝置,可使用同時對研磨對象物的兩面進行研磨的兩面研磨裝置,亦可使用僅對研磨對象物的一面進行研磨的單面研磨裝置。
上述研磨用組合物,以一旦用於研磨即丟的一次性的態樣(所謂「流放」)使用亦可,循環重複使用亦可。作為循環使用研磨用組合物的方法的一例,可列舉將從研磨裝置所排出的已使用的研磨用組合物回收到桶槽內,將回收的研磨用組合物再度供給到研磨裝置的方法。與以流放使用的情形相比,循環使用研磨用組合物時,可減少作為廢液處理的已使用的研磨用組合物的量,而可降低環境負荷。此外,藉由減少研磨用組合物的使用量可抑制成本。
在此,在一實施形態,上述研磨對象物以包含氮化矽與氮化鈦為佳。
(半導體基板的製造方法) 在一實施形態,提供一種半導體基板的製造方法,其包含:藉由上述研磨方法對研磨對象物進行研磨的步驟。 上文詳細地說明了本發明相關的實施形態,惟此僅為說明且例示而並非限定,本發明的範圍應以附件的專利申請範圍所解釋。 本發明包含下述態樣及形態。
1. 一種研磨用組合物,包含: 二氧化矽; 陰離子性水溶性高分子; 選自由含有膦酸基的化合物、含有磷酸基的化合物、及含有胺基的化合物所組成之群之至少1種化合物;及 分散媒。
2. 如上述1所述之研磨用組合物,其中pH為1.0~7.0。
3. 如上述1或2所述之研磨用組合物,其中上述陰離子性水溶性高分子為聚羧酸。
4. 如上述1至3之任何一項所述之研磨用組合物,其中上述含有膦酸基的化合物具有1~6個膦酸基。
5. 如上述1至4之任何一項所述之研磨用組合物,其中上述含有膦酸的化合物是選自由氮基三(亞甲基膦酸)、乙二胺四亞甲基膦酸、及二伸乙三胺五(亞甲基膦酸)所組成之群之至少1種。
6. 如上述1至5之任何一項所述之研磨用組合物,其中上述含有磷酸基的化合物是選自由無機磷酸化合物及有機磷酸化合物所組成之群之至少1種。
7. 如上述1至6之任何一項所述之研磨用組合物,其中上述含有胺基的化合物為胺基酸。
8. 如上述1至7之任何一項所述之研磨用組合物,其用於研磨含有氮化矽與氮化鈦的研磨對象物的步驟。
9.一種製造方法,其係上述1至8之任何一項所述之研磨用組合物的製造方法,包含:將上述二氧化矽、上述陰離子性水溶性高分子、上述選自由含有膦酸基的化合物、含有磷酸基的化合物、及含有胺基的化合物所組成之群之至少1種化合物、及上述分散媒混合。
10.一種研磨方法,包含:使用上述1至8之任何一項所述之研磨用組合物對研磨對象物進行研磨的步驟。
11.如上述10所述之研磨方法,其中上述研磨對象物含有氮化矽與氮化鈦。
12.一種半導體基板的製造方法,包含:藉由上述10或11所述的研磨方法,對研磨對象物進行研磨的步驟。
〔實施例〕
使用以下的實施例及比較例更詳細地說明本發明。惟,本發明的技術範圍並非限定於以下的實施例。再者,若無特別提及,「ppm」、「%」及「份」分別是指「質量百萬分率」、「質量%」及「質量份」。
(研磨用組合物的調製)
實施例1的研磨用組合物的調製
以下列方式分別加入:相對於最終研磨用組合物為2質量%的膠態二氧化矽(平均一次粒徑:12nm;平均二次粒徑:30nm);相對於最終研磨組合物為3200ppm的聚丙烯酸(Mw=5000)、及相對於最終研磨用組合物為50ppm的二伸乙三胺五(亞甲基膦酸)(DTPMP),以使研磨用組合物的pH成為2.2之方式加入硝酸水溶液及水(超純水),而調製實施例1的研磨用組合物。實施例1的研磨用組合物(液溫:25℃)的pH值,是藉由pH計(株式會社堀場製造所製,型號:LAQUA(註冊商標))確認。
實施例2~23及比較例1~4的研磨用組合物的調製 如下述表1所示而變更各成分的種類及/或含量,除此之外,與實施例1的研磨用組合物的調製同樣地操作,而調製各實施例及比較例的研磨用組合物。再者,表中的「-」是表示並未使用該成分。
(CMP步驟) 針對半導體基板的氮化矽基板及氮化鈦基板,分別使用實施例1~23及比較例1~4的研磨用組合物,以如下條件進行研磨。在此,氮化矽基板及氮化鈦基板,是使用300mm晶圓。
(研磨裝置及研磨條件) 研磨裝置︰株式會社荏原製造所製,FREX(註冊商標)300E 研磨墊︰Dow IC1400 研磨壓力︰2.0psi (1psi=6894.76Pa,以下相同) 研磨定盤轉數︰60rpm 研磨頭轉數︰61rpm 研磨用組合物的供給︰放流 研磨用組合物供給量︰300ml/分 研磨時間︰30秒。
(研磨速率評價) 針對上述研磨後的各研磨對象物,使用如下式1求出研磨速率。將評價結果一併顯示於表1。
此外,在實施例,是分別使用氮化矽基板及氮化鈦基板進行評價,惟,推測使用含有氮化矽及氮化鈦的基板等的情形,亦可得到與上述相同的結果。
由表1的結果可知,使用本發明的研磨用組合物的實施例1~23,氮化矽的研磨速率對氮化鈦的研磨速率(SiN/TiN選擇比)為充分高。另一方面,不具有陰離子性水溶性高分子及TiN抑制劑的至少一方的比較例1~4,SiN/TiN選擇比低。此外,可知實施例中,使用DTPMP的實施例8的結果非常優良。 本發明是基於申請日為西元2017年9月26日的日本專利申請編號第2017-185460號案,且其揭示內容的全部以參照的方式納入本說明書。
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Claims (8)
- 一種研磨用組合物,包含:0.1~10質量%二氧化矽;1~100000質量ppm之聚羧酸;150~500質量ppm之選自由含有膦酸基的化合物、及含有磷酸基的化合物所組成之群之至少1種化合物;及分散媒,其中,上述含有膦酸基的化合物是選自由氮基三(亞甲基膦酸)(NTMP)、乙二胺四亞甲基膦酸(EDTMP)、及二伸乙三胺五(亞甲基膦酸)(DTPMP)所組成之群之至少1種。
- 如申請專利範圍第1項所述之研磨用組合物,其中pH為1.0~7.0。
- 如申請專利範圍第1或2項所述之研磨用組合物,其中上述含有磷酸基的化合物是選自由無機磷酸化合物及有機磷酸化合物所組成之群之至少1種。
- 如申請專利範圍第1或2項所述之研磨用組合物,其用於研磨含有氮化矽與氮化鈦的研磨對象物的步驟。
- 一種製造方法,其係如申請專利範圍第1~4項中任一項所述之研磨用組合物的製造方法,包含:將上述二氧化矽、上述聚羧酸、上述選自由含有膦酸基的化合物、及含有磷酸基的化合物所組成之群之至少1種化合物、及上述分散媒混合。
- 一種研磨方法,包含:使用如申請專利範圍第1~4項中任一項所述之研磨用組合物對研磨對象物進行研磨的步驟。
- 如申請專利範圍第6項所述之研磨方法,其中上述研磨對象物含有氮化矽與氮化鈦。
- 一種半導體基板的製造方法,包含:藉由如申請專利範圍第6或7項所述之研磨方法,對研磨對象物進行研磨的步驟。
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