TWI437087B - 研磨液及使用此研磨液的基板的研磨方法 - Google Patents
研磨液及使用此研磨液的基板的研磨方法 Download PDFInfo
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- TWI437087B TWI437087B TW100148169A TW100148169A TWI437087B TW I437087 B TWI437087 B TW I437087B TW 100148169 A TW100148169 A TW 100148169A TW 100148169 A TW100148169 A TW 100148169A TW I437087 B TWI437087 B TW I437087B
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- Prior art keywords
- acid
- polishing
- polishing liquid
- mass
- water
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- UAXOELSVPTZZQG-UHFFFAOYSA-N tiglic acid Natural products CC(C)=C(C)C(O)=O UAXOELSVPTZZQG-UHFFFAOYSA-N 0.000 description 1
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- HOGWBMWOBRRKCD-BUHFOSPRSA-N trans-2-pentadecenoic acid Chemical compound CCCCCCCCCCCC\C=C\C(O)=O HOGWBMWOBRRKCD-BUHFOSPRSA-N 0.000 description 1
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- YIYBQIKDCADOSF-ONEGZZNKSA-N trans-pent-2-enoic acid Chemical compound CC\C=C\C(O)=O YIYBQIKDCADOSF-ONEGZZNKSA-N 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- ILJSQTXMGCGYMG-UHFFFAOYSA-N triacetic acid Chemical compound CC(=O)CC(=O)CC(O)=O ILJSQTXMGCGYMG-UHFFFAOYSA-N 0.000 description 1
- GTSMGKYOGFOSAR-UHFFFAOYSA-N tridecane-1-sulfonic acid Chemical compound CCCCCCCCCCCCCS(O)(=O)=O GTSMGKYOGFOSAR-UHFFFAOYSA-N 0.000 description 1
- DXNCZXXFRKPEPY-UHFFFAOYSA-N tridecanedioic acid Chemical compound OC(=O)CCCCCCCCCCCC(O)=O DXNCZXXFRKPEPY-UHFFFAOYSA-N 0.000 description 1
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- SJEYEFOHSMBQIX-UHFFFAOYSA-N undecane-1-sulfonic acid Chemical compound CCCCCCCCCCCS(O)(=O)=O SJEYEFOHSMBQIX-UHFFFAOYSA-N 0.000 description 1
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- WKOLLVMJNQIZCI-UHFFFAOYSA-N vanillic acid Chemical compound COC1=CC(C(O)=O)=CC=C1O WKOLLVMJNQIZCI-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- 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
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3105—After-treatment
- H01L21/31051—Planarisation of the insulating layers
- H01L21/31053—Planarisation of the insulating layers involving a dielectric removal step
- H01L21/31055—Planarisation of the insulating layers involving a dielectric removal step the removal being a chemical etching step, e.g. dry etching
-
- C—CHEMISTRY; METALLURGY
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- B24B37/00—Lapping machines or devices; Accessories
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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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Description
本發明是有關於一種研磨液及使用此研磨液的基板的研磨方法。更詳細而言,本發明是有關於使用於作為半導體元件製造技術的基板表面的平坦化步驟、特別是層間絕緣膜、BPSG膜(摻雜硼、磷的二氧化矽膜)的平坦化步驟、及淺溝槽隔離(STI,shallow trench isolation)的形成步驟等的研磨液及使用此研磨液的基板的研磨方法。
目前的超大型積體電路(ULSI,ultra large scale integration)半導體元件製造步驟中,正在研究開發用於半導體元件的高密度、微細化的加工技術。此加工技術之一的CMP(chemical mechanical polishing:化學機械研磨)技術,在半導體元件製造步驟中,在進行層間絕緣膜的平坦化、STI形成、插塞及嵌入金屬配線形成等時,成為必需的技術。
先前,在半導體元件製造步驟中,氧化矽膜等無機絕緣膜是藉由電漿CVD(chemical vapor deposition,化學氣相成長)、低壓-CVD(化學氣相成長)等方法而形成。普遍研究了使用燻矽系研磨液作為用以使此無機絕緣膜平坦化的化學機械研磨液。燻矽系研磨液是藉由以下方式而製造:對調配了利用熱分解等方法使四氯化矽酸進行粒成長而得的粒子的漿料的pH值進行調節。但此種燻矽系研磨液存在研磨速度低的技術問題。
並且,在設計規則0.25 μm以後的下一代中,在積體電路內的元件分離中使用STI。STI中,為了將基板上成膜的多餘的氧化矽膜去除而使用CMP技術。此時,為了使研磨停止在任意深度,而於氧化矽膜下形成研磨速度較低的終止膜。終止膜使用氮化矽膜等。為了將多餘的氧化矽膜有效地去除,並且充分地抑制其後的研磨的進行,較理想為氧化矽膜與終止膜的研磨速度之比較大。但是,先前的膠體氧化矽系研磨液中,氧化矽膜與終止膜的研磨速度比為3左右較小,作為STI用途,不具有耐用的特性。
另一方面,針對光罩或透鏡等玻璃表面的研磨液是使用包含氧化鈰粒子的氧化鈰研磨液。氧化鈰粒子與氧化矽粒子或氧化鋁粒子相比,硬度更低,且研磨時難以損傷研磨表面,因此對於拋光鏡面研磨較為有用。並且,氧化鈰研磨液與燻矽系或膠體氧化矽系等的氧化矽研磨液相比,具有研磨速度更快的優點。
作為氧化鈰研磨液,在下述專利文獻1中記載有使用高純度氧化鈰研磨粒的半導體用CMP研磨液。並且,下述專利文獻2中記載有為了控制氧化鈰研磨液的研磨速度,並提高全域的平坦性而加入添加劑的技術。
[先前技術文獻]
[專利文獻]
專利文獻1:日本專利特開平10-106994號公報
專利文獻2:日本專利3278532號公報
然而,隨著配線或STI的設計規則的微細化的進展,而對如上所述的氧化鈰研磨液要求平坦性進一步的提高(例如絕緣膜的凹陷量的降低)。並且,亦要求半導體裝置的生產的精度進一步提高,例如要求溝槽密度不同的部分的絕緣膜的殘膜厚差較小,或終止膜的過度研磨的量較少。而且,同時研磨製程的似然度較大對於精度較高的半導體裝置生產亦較為重要。
本發明是鑒於上述情況而完成,其目的是提供一種在對形成於基板表面的被研磨膜進行研磨的CMP技術中,可提高被研磨膜的研磨速度,而且提高研磨後的平坦性的研磨液及使用此研磨液的基板的研磨方法。
本發明提供一種研磨液,其是包含氧化鈰粒子、有機酸A、具有羧酸基或羧酸鹽基的高分子化合物B及水的CMP用研磨液,且有機酸A具有選自由-COOM基、-Ph-OM基、-SO3
M基及-PO3
M2
基(式中,M為選自H、NH4
、Na及K的任意一種,Ph表示可具有取代基的苯基)所組成群中的至少一種基,有機酸A的pKa小於9,有機酸A的含量相對於研磨液總質量為0.001質量%~1質量%,高分子化合物B的含量相對於研磨液總質量為0.01質量%~0.50質量%,pH值為4.0以上7.0以下。
本發明的研磨液中,在對形成於基板表面的被研磨膜(例如層間絕緣膜、BPSG膜、STI膜)進行研磨的CMP技術中,可提高被研磨膜的研磨速度,且提高研磨後的平坦性。
本發明的研磨液能以包括第1液以及第2液的二液式研磨液的方式保存,上述第1液包含上述氧化鈰粒子及上述水,上述第2液包含上述有機酸A、上述高分子化合物B及上述水。藉此,可更良好地保持氧化鈰粒子的分散穩定性直至要使用研磨液之前,並可獲得更有效果的研磨速度及平坦性。
另外,本發明的研磨液較佳為上述第1液還包含分散劑。藉此,可更加良好地保持氧化鈰粒子的分散穩定性。
本發明還提供使用本發明的研磨液對形成於基板表面的被研磨膜進行研磨的基板的研磨方法。根據使用本發明的研磨液的研磨方法,可提高被研磨膜的研磨速度,而且可提高研磨後的平坦性。
[發明的效果]
根據本發明,可提供一種在對形成於基板表面的被研磨膜(例如STI膜)進行研磨的CMP技術中,可提高被研磨膜的研磨速度,而且可提高研磨後的表面平坦性的研磨液及使用此研磨液的基板的研磨方法。
以下,對本發明的實施形態進行詳細說明。
[研磨液]
本實施形態的研磨液是包含氧化鈰粒子、分散劑、有機酸A、高分子化合物B、及水的CMP用研磨液。以下,對本實施形態的研磨液所含的各成分進行詳細說明。
(氧化鈰粒子)
氧化鈰粒子並無特別限制,可使用公知的氧化鈰粒子。通常氧化鈰是藉由將碳酸鹽、硝酸鹽、硫酸鹽、草酸鹽等鈰化合物氧化而得。製作氧化鈰粒子的方法可列舉:煅燒、利用過氧化氫等的氧化法等。
以TEOS-CVD(四乙氧基矽烷-化學氣相成長)法等所形成的氧化矽膜的研磨中使用氧化鈰粒子時,氧化鈰粒子的微晶徑(微晶的直徑)越大、且結晶應變越少,即結晶性越佳,則越可高速研磨,但具有被研磨膜容易產生研磨損傷的傾向。就該些觀點而言,氧化鈰粒子較佳為包含2個以上的微晶,且具有結晶晶界的粒子,更佳為微晶徑為1 nm~300 nm的範圍內的粒子。
上述微晶徑可藉由利用掃描型電子顯微鏡(SEM,scanning electron microscope)的觀察而測定。具體而言,根據藉由掃描型電子顯微鏡(SEM)觀察而得的圖像,測定粒子的長徑與短徑,並將長徑與短徑之積的平方根設為粒徑。
氧化鈰粒子中的鹼金屬及鹵素類的含有率就可較佳地用於半導體元件製造的研磨中的方面而言,較佳為10 ppm以下。
氧化鈰粒子的平均粒徑較佳為10 nm~500 nm,更佳為20 nm~400 nm,尤佳為50 nm~300 nm。若氧化鈰粒子的平均粒徑為10 nm以上,則有可獲得良好的研磨速度的傾向,若氧化鈰粒子的平均粒徑為500 nm以下,則有難以對被研磨膜產生損傷的傾向。
此處,氧化鈰粒子的平均粒徑是藉由雷射繞射式粒度分布計(例如馬爾文(Malvern)公司製造、商品名:Master Sizer Microplus、折射率:1.93、光源:He-Ne雷射、吸收0)測定的D50的值(體積分布的中值粒徑、累積中央值)。平均粒徑的測定是使用將研磨液稀釋成適當濃度(例如針對He-Ne雷射的測定時透射率(H)為60%~70%的濃度)的樣品。另外,氧化鈰研磨液分成如後述般將氧化鈰粒子分散於水中而得的氧化鈰漿料、以及使添加劑溶解於水中而得的添加液而保存時,可將氧化鈰漿料稀釋成適當的濃度而測定。
氧化鈰粒子的含量就具有可獲得良好的研磨速度的傾向的觀點而言,以研磨液總質量基準計較佳為0.1質量%以上,更佳為0.5質量%以上。並且,氧化鈰粒子的含量就具有抑制粒子的凝聚而難以對被研磨膜產生損傷的傾向的觀點而言,較佳為20質量%以下,更佳為5質量%以下,尤佳為1.5質量%以下。
(有機酸A)
本實施形態的研磨液包含有機酸及/或其鹽作為有機酸A。藉此可提高研磨速度,且可提高研磨結束後的被研磨膜(例如氧化矽膜)的平坦性。更詳細而言,對具有凹凸的被研磨面進行研磨時,可縮短研磨時間,此外可抑制一部分過度研磨而產生如皿般下凹的現象即所謂的凹陷(Dishing)。此效果藉由併用有機酸及/或其鹽與氧化鈰粒子而可更有效地獲得。
有機酸及/或其鹽為具有選自由-COOM基、-Ph-OM基(酚性-OM基)、-SO3
M基及-PO3
M2
基(式中,M為選自由H、NH4
、Na及K所組成的族群中的任意一種,Ph表示可具有取代基的苯基)所組成的族群中的至少一種基的有機酸及/或其鹽,較佳為水溶性有機化含物。
有機酸A例如可列舉:甲酸、乙酸、丙酸、丁酸、戊酸、環己烷甲酸、苯基乙酸、苯甲酸、鄰甲苯甲酸、間甲苯甲酸、對甲苯甲酸、鄰甲氧基苯甲酸、間甲氧基苯甲酸、對甲氧基苯甲酸、丙烯酸、甲基丙烯酸、丁烯酸、戊烯酸、己烯酸、庚烯酸、辛烯酸、壬烯酸、癸烯酸、十一碳烯酸、十二碳烯酸、十三碳烯酸、十四碳烯酸、十五碳烯酸、十六碳烯酸、十七碳烯酸、異丁酸、異戊酸、肉桂酸、喹哪啶酸、菸鹼酸、1-萘甲酸、2-萘甲酸、吡啶甲酸、乙烯基乙酸、苯基乙酸、苯氧基乙酸、2-呋喃甲酸、巰基乙酸、乙醯丙酸、草酸、丙二酸、丁二酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸、1,9-壬二酸、1,10-癸二酸、1,11-十一碳二酸、1,12-十二碳二酸、1,13-十三碳二酸、1,14-十四碳二酸、1,15-十五碳二酸、1,16-十六碳二酸、順丁烯二酸、反丁烯二酸、衣康酸、檸康酸、中康酸、喹啉酸、奎寧酸、萘二甲酸、鄰苯二甲酸、間苯二甲酸、對苯二甲酸、乙醇酸、乳酸、3-羥基丙酸、2-羥基丁酸、3-羥基丁酸、4-羥基丁酸、3-羥基戊酸、5-羥基吉草酸、奎尼酸、犬尿喹酸、水楊酸、酒石酸、烏頭酸、抗壞血酸、乙醯基水楊酸、乙醯基蘋果酸、乙炔二酸、乙醯氧基丁二酸、乙醯乙酸、3-側氧基戊二酸、α-苯丙烯酸、2-苯乳酸、蒽醌甲酸、蒽甲酸、異己酸、異降莰三酸、異丁烯酸、2-乙基-2-羥基丁酸、乙基丙二酸、乙氧基乙酸、草醯乙酸、氧基二乙酸、2-氧基丁酸、降莰三酸、檸檬酸、乙醛酸、縮水甘油酸、甘油酸、葡萄糖二酸、葡萄糖酸、巴豆酸、環丁烷甲酸、環己烷二甲酸、二苯基乙酸、二-O-苯甲醯基酒石酸、二甲基丁二酸、二甲氧基鄰苯二甲酸、羥基丙二酸、鞣酸、噻吩甲酸、順芷酸、乙二醇三甲酸、四羥基丁二酸、四甲基丁二酸、特窗酸、去氫乙酸、芸香酸、托品酸、香草酸、副分解烏頭酸、羥基間苯二甲酸、羥基肉桂酸、羥基萘甲酸、鄰羥基苯基乙酸、間羥基苯基乙酸、對羥基苯基乙酸、3-羥基-3-苯基丙酸、三甲基乙酸、吡啶二甲酸、吡啶三甲酸、丙酮酸、α-苯基肉桂酸、苯基縮水甘油酸、苯基丁二酸、苯基乙酸、苯基乳酸、丙炔酸、己二烯酸、2,4-己二烯二酸、2-亞苄基丙酸、3-亞苄基丙酸、亞苄基丙二酸、二苯乙醇酸、苯三甲酸、1,2-苯二乙酸、苯甲醯氧基乙酸、苯甲醯氧基丙酸、苯甲醯基甲酸、苯甲醯基乙酸、O-苯甲醯基乳酸、3-苯甲醯基丙酸、沒食子酸、中草酸、5-甲基間苯二甲酸、2-甲基丁烯酸、α-甲基肉桂酸、甲基丁二酸、甲基丙二酸、2-甲基丁酸、鄰甲氧基肉桂酸、對甲氧基肉桂酸、巰基丁二酸、巰基乙酸、O-乳醯乳酸、蘋果酸、白酮酸、白羥酸、玫棕酸、玫紅酸、α-酮戊二酸、L-抗壞血酸、艾杜糖醛酸、半乳糖醛酸、葡糖醛酸、焦麩胺酸、乙二胺四乙酸、氰化三乙酸、天冬醯胺酸、麩胺酸、N'-羥基乙基N,N,N'-三乙酸及氮基三乙酸等羧酸;甲磺酸、乙磺酸、丙磺酸、丁磺酸、戊磺酸、己磺酸、庚磺酸、辛磺酸、壬磺酸、癸磺酸、十一烷磺酸、十二烷磺酸、十三烷磺酸、十四烷磺酸、十五烷磺酸、十六烷磺酸、十七烷磺酸、十八烷磺酸、苯磺酸、萘磺酸、甲苯磺酸、羥基乙磺酸、羥基苯酚磺酸及蒽磺酸等磺酸;癸基膦酸及苯基膦酸等膦酸等。而且,對於上述羧酸、磺酸及膦酸,可為將該些主鏈的質子藉由1個或2個以上的F、Cl、Br、I、OH、CN及NO2
等原子或原子團取代而得的衍生物。該些成分可單獨使用1種或將2種以上加以組合而使用。
有機酸A(有機酸及/或其鹽)的含量以研磨液總質量基準計為0.001質量%~1質量%。若有機酸及/或其鹽的含量為0.001質量%以上,則有可提高研磨結束後的被研磨膜(例如氧化矽膜)的平坦性的傾向,就此觀點而言,有機酸及/或其鹽的含量較佳為0.005質量%以上,更佳為0.01質量%以上。另一方面,若含量為1質量%以下,則有充分提高被研磨膜的研磨速度的傾向,並且有抑制氧化鈰粒子凝聚的傾向,就此觀點而言,有機酸及/或其鹽的含量較佳為0.1質量%以下,更佳為0.05質量%以下。
有機酸A在室溫(25℃)下的酸解離常數pKa(在pKa存在2個以上時是最低的第一階段的pKa1
)小於9,pKa較佳為小於8,更佳為小於7,尤佳為小於6,最佳為小於5。若有機酸A的pKa小於9,則研磨液中至少其一部分以上成為有機酸離子而釋放氫離子,而可將pH值保持在所需要的pH值區域。
(高分子化合物B)
本實施形態的研磨液包含具有羧酸基或羧酸鹽基的高分子化合物B。此處,羧酸基是以-COOH表示的官能基,羧酸鹽基是以-COOX表示的官能基(X為源自鹼的陽離子,例如可列舉銨離子、鈉離子及鉀離子)。特別較佳為包含具有羧酸基或羧酸鹽基的水溶性有機高分子及/或其鹽作為高分子化合物B。藉此,可提高研磨結束後的被研磨膜(例如氧化矽膜)的平坦性。更詳細而言,在對具有凹凸的被研磨面進行研磨時,可抑制一部分過度研磨而產生如皿般下凹的現象即所謂的凹陷。此效果藉由併用具有羧酸基或羧酸鹽基的水溶性有機高分子及/或其鹽、與有機酸及/或其鹽、以及氧化鈰粒子,而可更有效地獲得。
高分子化合物B(具有羧酸基或羧酸鹽基的水溶性有機高分子)的具體例可列舉:聚天冬醯胺酸、聚麩胺酸、聚離胺酸、聚蘋果酸、聚醯胺酸、聚醯胺酸銨鹽、聚醯胺酸鈉鹽及聚乙醛酸等聚羧酸及其鹽;丙烯酸、甲基丙烯酸、順丁烯二酸等具有羧酸基的單體的均聚物及此聚合物的羧酸基的部分為銨鹽等的均聚物等。
並且可列舉,具有羧酸鹽基的單體、與羧酸的烷基酯等衍生物的共聚物。其具體例可列舉:聚(甲基)丙烯酸、或聚(甲基)丙烯酸的羧酸基的一部分被取代成羧酸銨鹽基的聚合物(以下稱為聚(甲基)丙烯酸銨)等。此處所謂聚(甲基)丙烯酸,表示聚丙烯酸與聚甲基丙烯酸的至少一種。
高分子化合物B在上述中較佳為丙烯酸、甲基丙烯酸、順丁烯二酸等具有羧酸基的單體的均聚物及此聚合物的羧酸基的部分為銨鹽等的均聚物,更佳為(甲基)丙烯酸的均聚物(聚(甲基)丙烯酸)及其銨鹽,尤佳為聚丙烯酸及其銨鹽。
高分子化合物B的含量就具有可提高研磨結束後的被研磨膜(例如氧化矽膜)的平坦性的傾向的觀點而言,以研磨液總質量基準計宜為0.01質量%以上,就同樣的觀點而言,較佳為0.02質量%以上,更佳為0.05質量%以上。並且,若含量為0.50質量%以下,則有充分提高被研磨膜的研磨速度的傾向,並且具有抑制氧化鈰粒子凝聚的傾向,就上述觀點而言,高分子化合物B的含量以研磨液總質量基準計為0.50質量%以下,較佳為0.40質量%以下,更佳為0.30質量%以下,尤佳為0.20質量%以下。
高分子化合物B的重量平均分子量並無特別限制,就具有充分獲得被研磨膜的研磨速度的傾向,並且具有容易抑制氧化鈰粒子的凝聚的傾向的觀點而言,較佳為100000以下,更佳為10000以下。並且,就具有容易獲得平坦性提高效果的傾向的觀點而言,高分子化合物B的重量平均分子量較佳為1000以上。另外,重量平均分子量是藉由GPC(Gel Permeation Chromatography:凝膠滲透層析法)進行測定,並進行標準聚氧乙烯換算而得的值。
(水)
水並無特別限制,較佳為去離子水、離子交換水及超純水等。水的含量可為上述各含有成分的含量的殘留部份,只要於研磨液中含有,則並無特別限定。另外,研磨液根據需要還可含有水以外的溶劑例如乙醇、丙酮等極性溶劑等。
(分散劑)
本實施形態的研磨液可含有用以使氧化鈰粒子分散的分散劑。分散劑可列舉:水溶性陰離子性分散劑、水溶性非離子性分散劑、水溶性陽離子性分散劑及水溶性兩性分散劑等,其中較佳為水溶性陰離子性分散劑。該些分散劑可單獨使用一種或將二種以上加以組合而使用。另外,亦可使用作為高分子化合物B而例示的上述化合物(例如聚丙烯酸銨)作為分散劑。
水溶性陰離子性分散劑較佳為含有丙烯酸作為共聚合成分的高分子及其鹽,更佳為此高分子的鹽。含有丙烯酸作為共聚合成分的高分子及其鹽例如可列舉:聚丙烯酸及其銨鹽、丙烯酸與甲基丙烯酸的共聚物及其銨鹽、以及丙烯酸醯胺與丙烯酸的共聚物及其銨鹽。
其他水溶性陰離子性分散劑例如可列舉:月桂基硫酸三乙醇胺、月桂基硫酸銨、聚氧乙烯烷基醚硫酸三乙醇胺及特殊聚羧酸型高分子分散劑。
並且,水溶性非離子性分散劑例如可列舉:聚乙二醇單月桂酸酯、聚乙二醇單硬脂酸酯、聚乙二醇二硬脂酸酯、聚乙二醇單油酸酯、聚氧乙烯烷基胺、聚氧乙烯硬化蓖麻油、甲基丙烯酸2-羥基乙酯及烷基烷醇醯胺。
水溶性陽離子性分散劑例如可列舉:聚乙烯吡咯啶酮、可可胺乙酸酯及硬脂基胺乙酸酯。
水溶性兩性分散劑例如可列舉:月桂基甜菜鹼、硬脂基甜菜鹼、月桂基二甲基氧化胺及2-烷基-N-羧基甲基-N-羥基乙基咪唑啉鎓甜菜鹼。
分散劑的含量就提高氧化鈰粒子的分散性而抑制沈澱,並進一步減少被研磨膜的研磨損傷的觀點而言,以研磨液總質量基準計較佳為0.001質量%~10質量%的範圍。
分散劑的重量平均分子量並無特別限制,較佳為100~150000,更佳為1000~20000。若分散劑的分子量為100以上,則在對氧化矽膜或氮化矽膜等被研磨膜進行研磨時,有容易獲得良好的研磨速度的傾向。若分散劑的分子量為150000以下,則有研磨液的保存穩定性難以降低的傾向。另外,重量平均分子量是藉由GPC進行測定,並進行標準聚氧乙烯換算而得的值。
[其他添加劑]
本實施形態的研磨液中,可使用水溶性高分子作為與有機酸及/或其鹽、以及具有羧酸基或羧酸鹽基的水溶性有機高分子及/或其鹽不同的添加劑。此種水溶性高分子例如可列舉:海藻酸、果膠酸、羧基甲基纖維素、瓊脂、卡德蘭多糖及普魯蘭多糖等多糖類;聚乙烯醇、聚乙烯吡咯啶酮及聚丙烯醛等乙烯系聚合物等。
該些水溶性高分子的重量平均分子量較佳為500以上。另外,重量平均分子量是藉由GPC進行測定,並進行標準聚氧乙烯換算而得的值。並且,該些水溶性高分子的含量以研磨液總質量基準計較佳為0.01質量%~5質量%。
[研磨液的製備、保存方法]
本實施形態的研磨液例如藉由在調配氧化鈰粒子、水及分散劑而使氧化鈰粒子分散後,再添加有機酸A及高分子化合物B而獲得。另外,本實施形態的研磨液能以包含氧化鈰粒子、分散劑、有機酸A、高分子化合物B、水及任意的水溶性高分子的一液式研磨液的形態保存,亦能以由包含氧化鈰粒子、分散劑及水的氧化鈰漿料(第1液)、與包含有機酸A、高分子化合物B、水及任意的水溶性高分子的添加液(第2液)構成的二液式研磨液的形態保存。
另外,在二液式研磨液時,有機酸A及高分子化合物B以外的添加劑可包含在氧化鈰漿料與添加液的任一種中,就對氧化鈰粒子的分散穩定性無影響的方面而言,較佳為包含於添加液中。
以分成氧化鈰漿料與添加液的二液式研磨液的形態保存時,可藉由任意改變該些二液的調配來調整平坦化特性與研磨速度。在使用二液式研磨液進行研磨時,可使用以下方法:將氧化鈰漿料及添加液分別以不同的配管送液,使該些配管在供給配管出口的正前方合流而將兩液混合供給至研磨墊上的方法;或者在將要研磨前將氧化鈰漿料與添加液混合的方法。
本實施形態的研磨液及漿料就可抑制儲存、搬運、保管等的成本的觀點而言,能以在使用時藉由水等液狀介質稀釋成例如2倍以上而使用的研磨液用儲存液或漿料用儲存液的形態保管。上述各儲存液在將要研磨前可藉由液狀介質稀釋,亦可在研磨墊上供給儲存液與液狀介質而於研磨墊上進行稀釋。
上述儲存液的稀釋倍率是倍率越高則儲存、搬運、保管等的成本的抑制效果越高,因此,較佳為2倍以上,更佳為3倍以上。並且,上限並無特別限制,倍率越高則儲存液中所含的成分的量越多(濃度越高),而有保管中的穩定性降低的傾向,因此通常較佳為10倍以下,更佳為7倍以下,尤佳為5倍以下。另外,可將構成成分分成三液以上,對於此種情況而言亦相同。
本實施形態的研磨液是調節成所需要的pH值而供於研磨。pH值調節劑並無特別限制,例如可列舉:硝酸、硫酸、鹽酸、磷酸、硼酸及乙酸等酸,以及氫氧化鈉、氨水、氫氧化鉀及氫氧化鈣等鹼。在將研磨液用於半導體研磨時,可較佳地使用氨水、酸成分。pH調節劑可使用預先藉由氨進行部分中和而得的水溶性高分子的銨鹽。
另外,室溫(25℃)的研磨液的pH值為4.0以上7.0以下。藉由pH值為4.0以上而具有研磨液的保存穩定性提高的傾向,並具有被研磨膜的損傷的產生數減少的傾向,就相同的觀點而言,上述pH值較佳為4.5以上,更佳為4.8以上。並且,藉由pH值為7.0以下,而可充分發揮出平坦性的提高效果,就相同的觀點而言,上述pH值較佳為6.5以下,更佳為6.0以下,尤佳為5.5以下。研磨液的pH值可藉由pH計(例如橫河電機股份有限公司製造的Model PH81(商品名))進行測定。例如可藉由使用標準緩衝液(鄰苯二甲酸鹽pH緩衝液pH值:4.21(25℃)、中性磷酸鹽pH緩衝液pH值6.86(25℃))進行2點校正後,將電極投入研磨液,測定於25℃經過2分鐘以上而穩定後的值,而測定研磨液的pH值。
接著,對本實施形態的研磨液在形成於基板表面的被研磨膜的研磨中的應用(Use)進行說明。
[研磨方法]
本實施形態的基板的研磨方法是使用上述研磨液對形成於基板表面的被研磨膜進行研磨。更詳細而言,例如在將形成於基板表面的被研磨膜按壓於研磨台的研磨墊的狀態下,一邊將上述研磨液供給至被研磨膜與研磨墊之間,一邊使基板與研磨台相對運動而對被研磨膜進行研磨。
基板可列舉:形成有電路元件及配線圖案的階段的半導體基板、或在形成有電路元件的階段的半導體基板等半導體基板上形成無機絕緣膜的基板等半導體元件製造的基板等。
上述被研磨膜例如可列舉:氧化矽膜、氮化矽膜、氧化矽膜的複合膜等無機絕緣膜等。藉由本實施形態的研磨液對上述基板上所形成的無機絕緣膜進行研磨,而可消除無機絕緣膜表面的凹凸,並使基板整面形成平滑的面。並且,本實施形態的研磨液亦可用於淺溝槽隔離。
以下,列舉形成有無機絕緣膜的半導體基板的情形作為例子,對基板的研磨方法進行更詳細地說明。
研磨裝置可使用具有固持器及研磨台的一般的研磨裝置,上述固持器將具有被研磨膜的半導體基板等基板加以保持,上述研磨台安裝有可改變轉速的馬達等,且可貼附研磨墊(研磨布)。研磨裝置例如可使用荏原製作所股份有限公司製造的研磨裝置:型號EPO-111、AMAT製造的MIRRA、Reflexion等。
研磨墊可無特別限制地使用一般的不織布、發泡聚胺基甲酸酯及多孔質氟樹脂等。並且,較佳為對研磨墊實施如滯留研磨液的槽加工。
研磨條件並無限制,但是研磨台的旋轉速度為了不使半導體基板飛出較佳為200轉/分鐘以下的低旋轉,施加於半導體基板的壓力(加工負荷)為了研磨後不產生損傷較佳為100 kPa以下。研磨期間,藉由泵等將研磨液連續地供給至研磨墊。此供給量並無限制,但是較佳為研磨墊的表面始終被研磨液覆蓋。
較佳為,研磨結束後的半導體基板在流水中充分清洗後,使用旋轉乾燥器等將附著於半導體基板上的水滴拂落而乾燥。
如此藉由研磨液對作為被研磨膜的無機絕緣膜進行研磨,而可消除表面的凹凸,並獲得半導體基板整面平滑的面。形成經平坦化的淺溝槽後,於無機絕緣膜上形成鋁配線,於此配線間及配線上再次形成無機絕緣膜後,使用研磨液對此無機絕緣膜進行研磨而獲得平滑的面。藉由將此步驟重複進行特定次數,而可製造具有所需要的層數的半導體基板。
藉由本實施形態的研磨液而研磨的無機絕緣膜例如可列舉氧化矽膜及氮化矽膜。氧化矽膜可摻雜磷及硼等元素。無機絕緣膜的製作方法可列舉:低壓CVD法、電漿CVD法等。
藉由低壓CVD法的氧化矽膜形成是使用單矽烷:SiH4
作為Si源,使用氧:O2
作為氧源。藉由在400℃以下的低溫下進行此SiH4
-O2
系氧化反應而獲得氧化矽膜。根據情況,藉由CVD而得的氧化矽膜可藉由1000℃或1000℃以下的溫度進行熱處理。為了實現藉由高溫回焊的表面平坦化,於氧化矽膜中摻雜磷:P時,較佳為使用SiH4
-O2
-PH3
系反應氣體。
電漿CVD法具有使在通常的熱平衡下需要高溫的化學反應可在低溫下進行的優點。電漿產生法可列舉:電容耦合型與電感耦合型2個類型。反應氣體可列舉:使用SiH4
作為Si源、使用N2
O作為氧源的SiH4
-N2
O系氣體,以及將四乙氧基矽烷(TEOS)使用於Si源的TEOS-O系氣體(TEOS-電漿CVD法)。基板溫度較佳為250℃~400℃,反應壓力較佳為67 Pa~400 Pa。
藉由低壓CVD法的氮化矽膜形成是使用二氯矽烷:SiH2
Cl2
作為Si源、使用氨:NH3
作為氮源。將此SiH2
Cl2
-NH3
系氧化反應於900℃的高溫下進行而獲得氮化矽膜。藉由電漿CVD法的氮化矽膜形成中反應氣體可列舉:使用SiH4
作為Si源、使用NH3
作為氮源的SiH4
-NH3
系氣體。基板溫度較佳為300℃~400℃。
本實施形態的研磨液及基板的研磨方法不僅可應用於形成於半導體基板的無機絕緣膜,而且亦可應用於各種半導體裝置的製造製程等。本實施形態的研磨液及基板的研磨方法例如亦可應用於研磨:形成於具有特定配線的配線板的氧化矽膜、玻璃及氮化矽等無機絕緣膜,多晶矽,主要含有Al、Cu、Ti、TiN、W、Ta及TaN等的膜,光罩、透鏡、稜鏡等光學玻璃,ITO等無機導電膜,包含玻璃及結晶質材料的光積體電路、光開關元件、光波導,光纖的端面,閃爍體等光學用單結晶,固體雷射單結晶,藍色雷射LED用藍寶石基板,SiC、GaP及GaAs等半導體單結晶,磁碟用玻璃基板、以及磁頭等。
實例
以下,藉由實例對本發明進行說明,但本發明並不限定於該些實例。
(氧化鈰粒子的製作)
將市售的碳酸鈰水合物40 kg投入至氧化鋁製容器,於830℃、空氣中煅燒2小時,而獲得黃白色粉末20 kg。藉由X射線繞射法對此粉末進行相鑑定,結果確認為氧化鈰。將所得的氧化鈰粉末20 kg使用噴射磨機進行乾式粉碎,而獲得粉末狀(粒子狀)氧化鈰。將所得的粉末狀氧化鈰藉由掃描型電子顯微鏡(SEM)進行觀察,結果包含微晶尺寸的粒子、與具有由2個以上微晶構成的結晶晶界的粒子。根據所得的SEM圖像任意選擇50個微晶,分別對50個微晶根據長徑與短徑之積的平方根求出粒徑,結果微晶徑均包含在1 nm~300 nm的範圍內。
(實例1-1)
將上述所製作的氧化鈰粒子200.0 g、與去離子水795.0 g混合,添加作為分散劑的聚丙烯酸銨水溶液(重量平均分子量:8000、40質量%)5 g,一邊攪拌一邊進行超音波分散,而獲得氧化鈰分散液。超音波分散是於超音波頻率400 kHz、分散時間20分鐘下進行。
然後,在1升容器(高度:170 mm)中投入1 kg氧化鈰分散液並靜置,進行沈澱分層。在分層時間15小時後,用泵將距水面的深度13 cm之上的上清液取出。將所得的上清液的氧化鈰分散液接著以氧化鈰粒子的含量為5質量%的方式使用去離子水稀釋而獲得氧化鈰漿料。
為了測定氧化鈰漿料中的氧化鈰粒子的平均粒徑(D50),以針對He-Ne雷射的測定時透射率(H)為60%~70%的方式稀釋上述漿料而製成測定樣品。使用雷射繞射式粒度分布計Master Sizer Microplus(馬爾文公司製造、商品名),以折射率:1.93、吸收:0的方式測定此測定樣品,結果D50的值為150 nm。
將作為有機酸A的對甲苯磺酸一水合物(pKa(25℃)=-2.8)0.1 g、與去離子水800 g混合,並添加作為高分子化含物B的聚丙烯酸水溶液(重量平均分子量:4000、40質量%)2.5 g後,添加氨水(25質量%)調節pH值為4.5(25℃)。再添加去離子水,使總體量為850 g而製成有機酸添加液。
於其中,添加上述氧化鈰漿料134 g,添加氨水(25質量%),並調節pH值為5.0(25℃),再添加去離子水,使總量為1000 g,而製作氧化鈰研磨液(氧化鈰粒子含量:0.67質量%)。
並且,以與上述相同的方式製備測定樣品,藉由雷射繞射式粒度分布計測定研磨液中的粒子的平均粒徑,結果D50的值為150 nm。
(絕緣膜的研磨)
使用SEMATECH公司製造的商品名「Pattern Wafer 764」(直徑:300 mm)作為研磨試驗晶圓。使用圖1(a)~圖1(c)對此研磨試驗晶圓及使用此研磨試驗晶圓的研磨特性的評價方法進行說明。
圖1(a)是研磨試驗晶圓的一部分的放大的示意剖面圖。晶圓1的表面形成有多個槽,於晶圓1的凸部表面形成厚度150 nm(1500)的氮化矽膜2。槽的深度(自凸部的表面至凹部的底面為止的階差)為500 nm(5000)。以下,將凸部稱為主動部、將凹部稱為溝槽部。另外,圖1(a)~圖1(c)中雖未明示,但晶圓1中形成有溝槽部/主動部的剖面寬度為100 μm/100 μm、20 μm/80 μm及80 μm/20 μm的3個區域。
圖1(b)是研磨試驗晶圓的一部分的放大的示意剖面圖。研磨試驗晶圓以自主動部的表面開始氧化矽膜3的厚度為600 nm(6000)的方式藉由電漿TEOS法而於主動部及溝槽部形成氧化矽膜3。研磨試驗中,對研磨試驗晶圓的氧化矽膜3進行研磨而使其平坦化。
圖1(c)是將氧化矽膜3研磨後的研磨試驗晶圓的一部分放大的示意剖面圖。在主動部的氮化矽膜2表面結束研磨,將此時的研磨所需要的時間設為研磨時間,將從溝槽部的深度4減去溝槽部內的氧化矽膜3的厚度5而得的值設為凹陷量6。另外,研磨時間較短為佳,凹陷量6較小為佳。
此種研磨試驗晶圓的研磨是使用研磨裝置(AMAT公司製造的Reflexion)。將研磨試驗晶圓設置於貼附了基板安裝用吸著墊的固持器上。在研磨裝置的直徑600 mm的研磨台上,貼附多孔質胺基甲酸酯樹脂製研磨墊(槽形狀=穿孔型:羅門哈斯(Rohm and Haas)公司製造、型號IC1010)。接著,使作為被研磨膜的絕緣膜(氧化矽被膜)面朝下將上述固持器載置於研磨台上,將加工負荷設定為210 gf/cm2
(20.6 kPa)。
一邊以250毫升/分鐘的速度將上述氧化鈰研磨液滴加至上述研磨墊上,一邊使研磨台與研磨試驗晶圓分別以130轉/分鐘動作,而將研磨試驗晶圓研磨。將100 μm/100 μm區域的主動部的氮化矽膜露出於表面時的研磨時間設為研磨結束時間。其中,平坦性的評價是對研磨結束的時刻起追加進行20%的過研磨(例如將研磨結束時間設為100秒,則自此時刻多追加20秒的時間進行研磨)的晶圓來進行。原因是,藉由過度研磨,而評價的項目的值容易出現差異,而容易評價,並且即便過度研磨數字亦較佳(特性佳),該些情況致使自研磨製程方面來看亦有製程的似然度(likelihood),而較為有利,因此亦可進行此證明。研磨後的研磨試驗晶圓藉由純水進行充分清洗後進行乾燥。
平坦性的評價項目是對以下的3個項目進行評價。
項目1:100 μm/100 μm區域的溝槽部的凹陷(Dishing)量:使用觸針式階差計(型號P16 KLA-tencor製造)進行測定。
項目2:100 μm/100 μm區域的主動部的SiN損失:使用耐諾(Nanometrics)公司製造的干擾式膜厚測定裝置Nanospec/AFT5100(商品名),測定藉由研磨而除去的氮化矽膜(SiN膜)的厚度。
項目3:20 μm/80 μm區域及80 μm/20 μm區域的溝槽部的SiO2
殘膜厚差(SiO2
密度差):使用耐諾公司製造的干涉式膜厚測定裝置Nanospec/AFT5100(商品名),測定各區域的氧化矽膜(SiO2
膜)的殘膜厚,並求出其差值。
(實例1-2-~實例6-9及比較例1-1~比較例6-9)
以表1~表19所示的方式變更研磨液的pH值、有機酸A的種類及使用量、或高分子化合物B的使用量,除此以外,以與實例1-1相同的方式製作氧化鈰研磨液,並進行絕緣膜的研磨。將結果示於同一表中。根據表1~表19可明白:利用藉由本發明而提供的研磨液會提高研磨速度及平坦性,並達成凹陷的降低。
1...晶圓
2...氮化矽膜
3...藉由電漿TEOS法而形成的氧化矽膜
4...溝槽部的深度
5...研磨後的溝槽部的氧化矽膜厚
6...凹陷量
圖1(a)~圖1(c)表示研磨特性的評價基板的示意剖面圖。
1...晶圓
2...氮化矽膜
3...藉由電漿TEOS法而形成的氧化矽膜
4...溝槽部的深度
5...研磨後的溝槽部的氧化矽膜厚
6...凹陷量
Claims (9)
- 一種研磨液,其為包含氧化鈰粒子、對甲苯磺酸、具有羧酸基或羧酸鹽基的水溶性有機高分子及水的CMP用研磨液,上述對甲苯磺酸的含量相對於研磨液總質量為0.001質量%~1質量%,上述水溶性有機高分子的含量相對於研磨液總質量為0.01質量%~0.50質量%,且pH值為4.0以上7.0以下。
- 如申請專利範圍第1項所述之研磨液,其以包括第1液以及第2液的二液式研磨液的方式保存,上述第1液包含上述氧化鈰粒子及上述水,上述第2液包含上述對甲苯磺酸、上述水溶性有機高分子及上述水。
- 如申請專利範圍第2項所述之研磨液,其中上述第1液更包含分散劑。
- 如申請專利範圍第1項至第3項中任一項所述之研磨液,其中上述對甲苯磺酸的含量相對於研磨液總質量為0.005質量%~0.1質量%。
- 如申請專利範圍第1項至第3項中任一項所述之研磨液,其中上述水溶性有機高分子選自由聚天冬醯胺酸、聚麩胺酸、聚離胺酸、聚蘋果酸、聚醯胺酸、聚醯胺酸銨鹽、聚醯胺酸鈉鹽及聚乙醛酸;選自由丙烯酸、甲基丙烯酸及順丁烯二酸所構成的群組的具有羧酸基的單體的均聚物;上述均聚物的上述羧酸基的部份為銨鹽的均聚物;具 有羧酸鹽基的單體與羧酸的烷基酯的共聚物;以及聚(甲基)丙烯酸的羧酸基的一部分被取代成羧酸銨鹽基的聚合物所構成的群組。
- 如申請專利範圍第1項至第3項中任一項所述之研磨液,其中上述水溶性有機高分子的含量相對於研磨液總質量為0.02質量%~0.40質量%。
- 如申請專利範圍第1項至第3項中任一項所述之研磨液,其pH值為4.0以上6.0以下。
- 如申請專利範圍第7項所述之研磨液,其pH值為4.0以上5.5以下。
- 一種基板的研磨方法,其使用如申請專利範圍第1項至第8項中任一項所述之研磨液對形成於基板表面的被研磨膜進行研磨。
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JP2012146974A (ja) | 2012-08-02 |
CN103155112B (zh) | 2016-10-12 |
KR20140041388A (ko) | 2014-04-04 |
KR101886464B1 (ko) | 2018-08-07 |
JP5510575B2 (ja) | 2014-06-04 |
US20170133237A1 (en) | 2017-05-11 |
JP2012146971A (ja) | 2012-08-02 |
JP2012146972A (ja) | 2012-08-02 |
US9564337B2 (en) | 2017-02-07 |
CN106433480A (zh) | 2017-02-22 |
JP6269733B2 (ja) | 2018-01-31 |
SG190765A1 (en) | 2013-07-31 |
JP2012146976A (ja) | 2012-08-02 |
JP2013149988A (ja) | 2013-08-01 |
WO2012086781A1 (ja) | 2012-06-28 |
JP2012146973A (ja) | 2012-08-02 |
JP2012146975A (ja) | 2012-08-02 |
JP2016183346A (ja) | 2016-10-20 |
KR101389235B1 (ko) | 2014-04-24 |
KR20140039143A (ko) | 2014-04-01 |
TW201229222A (en) | 2012-07-16 |
JP2013149987A (ja) | 2013-08-01 |
TW201350567A (zh) | 2013-12-16 |
CN103155112A (zh) | 2013-06-12 |
JP2012146970A (ja) | 2012-08-02 |
JP5510574B2 (ja) | 2014-06-04 |
JP5333571B2 (ja) | 2013-11-06 |
US20130260558A1 (en) | 2013-10-03 |
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