TW200946619A - Polishing copper-containing patterned wafers - Google Patents
Polishing copper-containing patterned wafers Download PDFInfo
- Publication number
- TW200946619A TW200946619A TW098102429A TW98102429A TW200946619A TW 200946619 A TW200946619 A TW 200946619A TW 098102429 A TW098102429 A TW 098102429A TW 98102429 A TW98102429 A TW 98102429A TW 200946619 A TW200946619 A TW 200946619A
- Authority
- TW
- Taiwan
- Prior art keywords
- bta
- acid
- copper
- ions
- polishing
- Prior art date
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- 239000010949 copper Substances 0.000 title claims abstract description 51
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 41
- 238000005498 polishing Methods 0.000 title claims abstract description 31
- 235000012431 wafers Nutrition 0.000 title description 17
- 229910052751 metal Inorganic materials 0.000 claims abstract description 33
- 239000002184 metal Substances 0.000 claims abstract description 33
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims abstract description 26
- 150000001875 compounds Chemical class 0.000 claims abstract description 25
- 239000012964 benzotriazole Substances 0.000 claims abstract description 22
- 239000002244 precipitate Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 18
- 150000002500 ions Chemical class 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003112 inhibitor Substances 0.000 claims abstract description 10
- 230000001590 oxidative effect Effects 0.000 claims abstract description 5
- 239000007864 aqueous solution Substances 0.000 claims abstract 2
- 238000000227 grinding Methods 0.000 claims description 27
- 239000002002 slurry Substances 0.000 claims description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 229910052799 carbon Chemical group 0.000 claims description 7
- 239000008346 aqueous phase Substances 0.000 claims description 6
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 5
- -1 Cu+2 ions Chemical class 0.000 claims description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- 108010008488 Glycylglycine Proteins 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims 1
- YMAWOPBAYDPSLA-UHFFFAOYSA-N glycylglycine Chemical compound [NH3+]CC(=O)NCC([O-])=O YMAWOPBAYDPSLA-UHFFFAOYSA-N 0.000 claims 1
- 239000004065 semiconductor Substances 0.000 abstract description 6
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 abstract description 4
- 229910001431 copper ion Inorganic materials 0.000 abstract description 3
- 239000000243 solution Substances 0.000 abstract 3
- 230000000536 complexating effect Effects 0.000 abstract 2
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 45
- 239000002253 acid Substances 0.000 description 26
- 239000002245 particle Substances 0.000 description 16
- 150000003839 salts Chemical class 0.000 description 15
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 12
- 229920001577 copolymer Polymers 0.000 description 12
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- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 10
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 10
- 229920000388 Polyphosphate Polymers 0.000 description 10
- WDJHALXBUFZDSR-UHFFFAOYSA-N acetoacetic acid Chemical compound CC(=O)CC(O)=O WDJHALXBUFZDSR-UHFFFAOYSA-N 0.000 description 10
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- 229910052698 phosphorus Inorganic materials 0.000 description 10
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 9
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- 239000003082 abrasive agent Substances 0.000 description 7
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- NBZBKCUXIYYUSX-UHFFFAOYSA-N iminodiacetic acid Chemical compound OC(=O)CNCC(O)=O NBZBKCUXIYYUSX-UHFFFAOYSA-N 0.000 description 7
- 239000000463 material Substances 0.000 description 7
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- 239000004254 Ammonium phosphate Substances 0.000 description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 6
- 235000019289 ammonium phosphates Nutrition 0.000 description 6
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- 230000002209 hydrophobic effect Effects 0.000 description 4
- YSRVJVDFHZYRPA-UHFFFAOYSA-N melem Chemical compound NC1=NC(N23)=NC(N)=NC2=NC(N)=NC3=N1 YSRVJVDFHZYRPA-UHFFFAOYSA-N 0.000 description 4
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
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- OMSYGYSPFZQFFP-UHFFFAOYSA-J zinc pyrophosphate Chemical compound [Zn+2].[Zn+2].[O-]P([O-])(=O)OP([O-])([O-])=O OMSYGYSPFZQFFP-UHFFFAOYSA-J 0.000 description 1
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 description 1
- CZPRKINNVBONSF-UHFFFAOYSA-M zinc;dioxido(oxo)phosphanium Chemical compound [Zn+2].[O-][P+]([O-])=O CZPRKINNVBONSF-UHFFFAOYSA-M 0.000 description 1
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- H—ELECTRICITY
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- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
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- H01L21/321—After treatment
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- H01L21/3212—Planarisation by chemical mechanical polishing [CMP]
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- 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
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Description
200946619 六、發明說明: 【發明所屬之技術領域】 本發明係有關於一種半導體晶圓材料之 簡,且特別是有關於在具有電介質 磨 晶圓上研磨金屬内連線之CMP方法以及CMp障^^導體 【先前技術】 組合物。 得統上 ----卞守骽晶圓係具有介電層之矽晶圓,日* 電層中包括呈圖案化排狀多個溝槽以作為内連接電 用。此@賴財通常具有金聽嵌結構麵重 結構。阻障層係覆蓋圖案化介電層且金 : :電=::r_案化漠槽中填滿編: CMP流程通常包含多重研磨步驟。例如,第 2始高速率移除過量的内連線金屬,如銅。在第-步驟移 内連線金屬之後,第二步驟可研磨移除殘留在金 ❹ 、、-外面之阻障層上的金屬。後讀的研磨步驟可自丰 導體晶圓之下方介電層移除阻障層,藉以使得介電層與金 屬内連線具有平坦之研磨後表面。 位於半導體基材之溝槽或溝渠(through)中的金屬係 用來提供金屬線以形成金屬電路。其中之一個需要克服的 問題在於研錢作常會從每個溝槽或錢巾移除金屬,而 造成金屬產生凹陷。此種凹陷會造成金屬電路之臨界尺寸 -(critical dimension)產生改變,因此這種凹陷是不受歡 迎。為了減少凹陷,所以需要在較低的研磨壓力下進行研 3 94611 200946619 磨。然而,只降低研磨壓力,卻需要延長研磨一段時間。 — 但是,延長研磨一段時間之後,仍會產生凹陷,因此對於 效能之改善並無多大幫助。 美國專利案第7, 086, 935號(Wang)係揭示在圖案化晶 · 圓上使用不含研磨劑(abrasive-free)之銅配方,此配方包 含甲基纖維素(methyl cellulose)、丙烯酸/甲基丙烯酸共 聚物(acrylic acid/methacrylic acid copolymer)、苯并 三唑(benzotriazole ; BTA)與可溶混之溶劑。此配方能夠 移除與潔淨銅且具有少量凹陷之銅,但是在快速研磨中, ❹ 此配方卻會在研磨墊與晶圓上沉澱綠色Cu-BTA化合物。因 此,這些沉殿物需要對研磨塾進行研磨後潔淨以避免這些 膠狀沉殿物降低了研磨移除速率,並且它們需要對晶圓進 行研磨後潔淨步驟以避免產生缺陷。這些潔淨步驟需要大 量且Φ貴的潔淨溶液,並會使得晶圓處理速度變慢,而增 加整體成本。 因此’需要提供能夠使㈣淨後之銅具有低缺陷率、
低凹陷、低触且均不會產生Gu_BTA沉澱物之研磨組合 G 物。再者’需要提供具有上述研磨特性之低刮傷配方。 【發明内容】 本發月之目的在於提供一種以研磨塾研磨具有銅内連 線金屬之圖案化晶圓之方法,包括下列步驟:提供水相研 磨液,此研磨液包括苯并三唾⑽)抑軸以及具有下列化 學式之錯合物: 94611 4 200946619
OH R—N—CH2C=〇
I ch2c=o
I
OH 其中,R為氫或含碳化合物’此錯合物可錯合鋼離子 與+水;以水相研磨液與研磨墊研磨圖案化晶圓使銅溶解成 Cu離子,其中Cu+1離子與BTA抑制劑之濃度為當水相研磨 ❹液中不含錯合物時[BTA]*[Cu+i] > Cu_BTA沉殿物之W;以 及將至少部份之Cu+1離子氧化成Cu+2離子以避免Cu_BTA沉 澱物在研磨時沉澱在圖案化晶圓與研磨墊上。 【實施方式】 ❹ 人當以研磨組合物對半導體晶圓進行CMp處裡時,此细 合物與方法可提供良好的金屬移除速率且可潔淨金屬以及 =得金屬内連線具有低凹陷(low dishing),其中此研為 2物包括錯合物組合水溶性改性纖維素、非醣類水溶担 聚。物、氧化劑、抑制劑與餘量水。添加錯合物之額外好 處在於可降低Cu~BTA(Cu+1)沉殿物所造成之綠色污物。從 =經驗中可知,當Cu離子⑻與BTA之滚度乘積大於制 物〆研磨^度下之Ksp時,則會形成不可溶之Cu_bta沉滿 在本說明書中’ Cu-BTA沉澱物包括非液體,例如固體 :體j聚合物’且可包括Cu+2離子、尖晶石沉澱物、似尖 曰曰石=殿細切》;錢Ksp代表在其操作或研磨溫度 下之溶解度乘積(solubility product)。在研磨液中,係 94611 5 200946619 依據下列平衡式(1)而產生Cu-BTA沉澱物: (1) BTAH + Cu+ e(慢)(怏)-> Cu-BTA + H+ 雖然某些胺類能夠有效地從晶圓與研磨墊上溶解綠色 “黏泥狀,,沉澱物,然而特殊的錯合物則可降低或消除 Cu-BTA沉澱物之有害數量。尤其是具有下列之化學式之錯 合物:
OH
I R—N—CH2C=0
I ch2c=o
I
OH 其中,R為氫或含碳化合物。此錯合物能夠錯合單價 (+1)與雙價(+2)之銅離子。在研磨時,錯合劑係用來錯合 足量之銅離子以降低Cu-BTA沉澱物之生成並且控制下列 式(2)之Cu+2離子之形成速率。 (2) 2Cu+ Cu° + Cu+2 此流程以銅溶解成Cu+1離子,且Cu+1離子與BTA抑制 劑之濃度為當水相研磨液中不含錯合物時[BTA]*[Cu+1]> Cu-BTA沉源:物之Ksp之方式而有助於以水相研磨液與研磨 墊研磨圖案化晶圓。添加酸化合物使得研磨方法從會產生 Cu-BTA沉殿物轉變成能夠避免產生Cu_BTA沉澱物問題。 1流程將至少部份之Cu”離子氧减Cl^離子以避免研磨 ¥在圖案化晶®與研磨塾上沉殿Cu_BTA沉殿物。此流程亦 可在其他銅錯合劑存在的情況下進行。例如,第一酸錯合 6 94611 200946619 劑可與第二錯合劑’如有機酸,一同使用,以降低或消除 研磨液產生Cu-BTA沉澱物之傾向。薄度為〇. 〇5至20重量 百分比之錯合物可降低Cu-BTA沉;殿物之生成。例如,濃度 範圍為0.1至10重量百分比之錯合物可減少Cu-BTA沉殿 物。其優點在於,此配方中具有濃度至少為〇.4重量百分 比的酸化合物,奴0.4至5重量百分比之錯合物,藉以控 制Cu-BTA沉澱物之產生。當錯合物濃度大於約0 4重量百 分比時’增加錯合物之濃度可增加或加速銅的移除速率; ❹ 以及當錯合物濃度介於0至約0.4重量百分比時,增加錯 合物之濃度可減少銅的移除速率。尤其,亞胺二乙酸 (iminodiacetic acid, IDA 或 diglycine)與乙二胺四乙酸 (ethylenediaminetetraacetic acid ; EDTA)中的至少一者 提供有效地降低Cu-BTA沉澱物之手段。IDA似乎是能夠最 有效降低Cu-BTA沉澱物的錯合劑。 本發明之組合物係使用0. 001至15重量百分比之缓酸 ^ 官能基改性之水溶性纖維素與可溶混於水之有機溶劑,例 如醇與酮。此組合物較佳為包括〇· 005至5重量百分比之 水溶性纖維素。此組合物最佳為包括〇· 01至3重量百分比 之水溶性纖維素。改性纖維素的例子係陰離子膠(例如遭膠 (agar gum)、阿拉伯樹膠(3^13化运11111)、印度樹膠(21^1:·^ gum)、梧桐膠(karaya gum)、瓜耳膠(guar gum)、果膠 (pectin)、刺槐豆膠(locust bean gum)、西黃蓍膠 (tragacanth gum)、羅望子膠(tamarind gum)、鹿角菜膠 (carrageenan gum)與黃原膠(xanthan gum)之至少一者); 7 94611 200946619 改性殿粉;藻酸(alginic acid);甘露糖酸酸(mannuronic acid);古羅糖搭酸(guluronic acid)及其衍生物與共聚 物。較佳之水溶性纖維素(羧甲基纖維素(CMC))之取代度為 0. 1至3. 0且重量平均分子量為1K至1000K。在本說明書 中’分子量係指纖維素之重量平均分子量。更佳者為CMC 之取代度為0. 7至1· 2且重量平均分子量為40K至250K。 CMC之取代度係指在纖維素分子之每個葡萄糖殘基 (anhydroglucose unit)上之乙酸鹽醚化羥基(acetate etherified hydroxyl group)的平均數量。CMC 之取代度 ^ 可被視為CMC之羧基之“密度”之度量單位。 本發明之非醣類水溶性聚合物包括利用丙烯酸單體或 甲基丙烯酸單體合成之丙烯酸聚合物、曱基丙烯酸聚合物 與共聚物。在本發明中,非醣類水溶性聚合物亦包括各種 分子量之聚合物與低分子量之募聚物。共聚物包括由丙烯 酸與曱基丙烯酸組合而形成之共聚物,而且尤其是,由丙 烯酸與曱基丙烯酸之莫耳比範圍為丨:3〇至3〇 :丨,較佳 為1 : 9至9 : 1之範圍,最佳為約2 : 3所形成之共聚物。❹ 此共聚物之較佳重量平均分子量範圍為1K至1〇〇〇κ,更佳 之範圍為10Κ至500Κ 〇 另-種可作為替代之非醣類水溶性聚合物則為兩親聚 合物(amPhiphilicpolymer),如由丙烯酸或甲基丙烯酸形 成之共聚物。在本說明書中,兩親聚合物係指由疏水性鏈 段與親水性鏈段組成之嵌段共聚物。疏水性鍵段可為碳數 於2至250變化之聚合物鍵。在本說明書中,碳數代表在 94611 8 200946619 ,水性鏈段中碳原子之數量。較佳之魏為5至.且 最佳之碳數為5至5G。親水性鏈段_子性的。親水性鍵 段之單體單元之較佳數量範圍為i至1〇〇。較佳的組合物 包括0. 005至5重量百分比之非酷類水溶性聚合物。更佳 的組合物包括0.G1至3重量百分比之麵類水溶性聚合 物。最佳的組合物則包括請^重量百分比之非聽類水 溶性聚合物。 兩親聚合物之較佳數量平均分子量為50至5000 ’本 說明書提到兩親聚合物時是㈣數量平均分子量且明確來 說係指使用串聯之 TSK-GEL pn/08025 GMPWx與 TSK-GEL pn/ 08020 G2500PWX柱以及折射率偵測器(refractive detector)與磷酸鈉緩衝液沖提劑(eluent)之水性凝膠滲 透色譜法(aqueous gel permeation chromatography)測得 者。更佳之數量平均分子量為介於5〇至4000,且最佳之 數量平均分子量為介於1〇〇至3〇〇〇。離子性鏈段包括陽離 _子性' 陰離子性與兩性離子(聚兩性電解質與聚甜菜鹼)。 較佳之親水性鏈段為陰離子性的、例如聚丙烯酸或聚甲基 丙稀酸。親水性鏈段較佳包括聚丙烯酸、聚甲基丙烯酸或 丙烯酸與曱基丙烯酸之共聚物。將這些鏈段組合成共聚物 時會產生性質不同於其各自均聚物之分子,因此有助於進 行潔淨且不會造成金屬内連線產生過量之凹陷。聚合物之 疏水性端可包括礙氫鏈或燒基硫醇(alkylmercaptan)。最佳 地’疏水性鏈段與親水性鏈段組合成嵌段共聚物形式。 此溶液包括氧化劑。較佳之溶液為包括〇. 5至25重量 9 94611 200946619 百刀比之氧化劑。更佳為氧化劑之重量百分比範圍為1至 10在=pH範圍時,此氧化劑對於幫助溶液移除 =:劑可為多種氣化化合物之至少-者,例如= 乙酸與其他過:、過::鹽、過鄰苯,、過 鐵鹽、鈽鹽、Mn⑴n|S =、廣酸鹽、過破酸鹽、確酸鹽、 銅鹽、職、姑越、Γΐ (Ιν)鹽、瓣D鹽、娘鹽、 使用氧化劑化合二混:物= =合:〜 ,定之氧化劑如過氧化氫:疋=最:研磨裝包 疋在=當Γ1將氧化劑現入組: 情况 他移除機^控細靜態,# 時’可藉由在保護金屬二:除速率。調整抑制劑之濃户 之移除速率。較佳之溶液為刻,而調整内迷綠金; :制劑。最佳之溶液為包括01至丨:重量百分比之 劑。此抑制劑可由唑 至1.0重篁百分比 :三幼制劑對於如純混合物所級成。: 率實—試指出増加抑連線金屬特 速率。但是増加唑類 】之濃度可增加研磨時的: CU~BTA化合物之缺點。〜部有造成研磨液傾向^ 除了抑制劑之外 _ ’ & =,以用於_連㈣擇性地包㈣ 址合物包括0.01 i ’如銅,之移除速率。:, 15重1百分此之第二〜較= 200946619 之組合物包括0.1至1重量百分比之第二銅錯合劑。第二 銅錯合劑之例子包括乙酸(acetic acid)、檸檬酸(citric acid)、乙醯乙酸乙酯(ethyl acetoacetate)、乙醇酸 (glycolic acid)、乳酸(lactic acid)、蘋果酸(malic acid)、草酸(oxalic acid)、水楊酸(salicylic acid)、二 硫代胺甲酸二乙酯鈉(sodium diethyl dithiocarbamate)、 琥珀酸(succinic acid)、酒石酸(tartaric acid)、硫代 乙醇酸(thioglycolic acid)、甘胺酸(glycine)、丙胺酸 ❹(alanine)、天門冬胺酸(aspartic acid)、乙二胺(ethylene diamine)、三甲基二胺(trimethyl diamine)、丙二酸 (malonic acid)、戊二酸(glutaric acid)、3-經基丁酸 (3-hydroxybutyric acid)、丙酸(propionic acid)、鄰苯 二甲酸(phthalic acid)、間苯二曱酸(isophthalic acid)、 3-經基水楊酸(3-hydroxy salicylic acid)、3, 5-二經基水 揚酸(3, 5-dihydroxy salicylic acid)、沒食子酸(gallic ❹ acid)、匍萄糖酸(gluconic acid)、兒茶驗(pyrocatechol)、 五倍子iHpyrogallol)、單寧酸(tannicacid),包括其鹽 類及其混合物。較佳之第二銅錯合劑係選自乙酸、檸檬酸、 乙醯乙酸乙酯、乙醇酸、乳酸、蘋果酸、草酸及其混合物 所組成之族群。最佳之第二鋼錯合劑係蘋果酸。蘋果酸所 提供之額外優點在於可改善平坦性。 組合物可選擇性地包括0至15含磷化合物(文中有稱 為=化合物的情形)。在本說明書中,“含填化合物,,係任 何3有磷原子之化合物。較佳之含磷化合物例如為磷酸鹽 11 94611 200946619 (phosphate)、焦填酸鹽(pyrophosphate)、聚碟酸鹽 (polyphosphate)、膦酸鹽(phosphonate),包括彼等之酸 類、鹽類、混合之酸式鹽類、酯類、部分酯類、混合之酯 ' 類及其混合物,例如碟酸。尤其,較佳之水相研磨組合物 之配製可使用,例如,下列之含磷化合物:磷酸鋅(zinc phosphate)、焦填酸鋅(zinc pyrophosphate)、聚填酸鋅 (zinc polyphosphate)、膦酸鋅(zinc phosphonate)、麟 酸敍(ammonium phosphate)、焦填酸錄(ammonium pyrophosphate)、聚鱗酸錄(ammonium polyphosphate)、 〇 膦酸錄(ammonium phosphonate)、填酸氫二銨(diammonium phosphate)、焦鱗酸氫二錄(diammonium pyrophosphate)、聚鱗酸氳二敍(diammonium polyphosphate)、膦酸氫二敍(diammonium phosphonate)、填酸脈(guanidine phosphate)、焦填酸胍 (guanidine pyrophosphate)、聚填酸胍(guanidine polyphosphate)、膦酸胍(guanidine phosphonate)、磷酸 鐵(iron phosphate)、焦鱗酸鐵(iron pyrophosphate)、 聚構酸鐵(iron polyphosphate)、膦酸鐵(iron phosphonate)、鱗酸錦(cerium phosphate)、焦鱗酸錦 (cerium pyrophosphate)、聚鱗酸錦(cerium polyphosphate)、膦酸鋪(cerium phosphonate)、乙二胺 礙酸鹽(ethylene-diamine phosphate)、派哄鱗酸鹽 (piperazine phosphate)、旅哄焦碟酸鹽(piperazine pyrophosphate)、e底哄膦酸鹽(piperazine phosphonate)、 12 94611 200946619 三聚氰胺磷酸鹽(melamine phosphate)、雙三聚氰胺鱗酸 鹽(dimelamine phosphate)、三聚氰胺焦磷酸鹽(melamine pyrophosphate)、三聚氰胺聚碌酸鹽(melamine polyphosphate)、三聚氰胺膦酸鹽(melamine phosphonate)、蜜白胺碟酸鹽(melam phosphate)、蜜白胺 焦填酸鹽(melam pyrophosphate)、蜜白胺聚碌酸鹽(melam polyphosphate)、蜜白胺膦酸鹽(melamphosphonate)、蜜 勒胺磷酸鹽(melem phosphate)、蜜勒胺焦填酸鹽(melem ❹ pyrophosphate)、蜜勒胺聚鱗酸鹽(meiem polyphosphate)、蜜勒胺膦酸鹽(melem ph〇Sph〇nate)、二 氰二胺鱗酸鹽(dicyanodiamide phosphate)、尿素填酸鹽 (urea phosphate),包括彼等之酸類、鹽類、混合之酸式 鹽類、酯類、部分酯類、混合酯類及其混合物❶同樣,亦 可使用麟氧化物(phosphine oxide)、膊硫化物(phosphine sulphide)與鱗雜環己烧(phosphorinane)及其膦酸鹽、亞 ❹碟酸鹽(phosphites)與次膦酸鹽(ph〇Sphinates),包括彼 等之酸類、鹽類、混合之酸式鹽類、酯類、部分酯類與混 合酯類。較佳之含磷化合物為碟酸銨。 其優點在於’本發明之研磨組合物中含有有效數量之 含磷化合物以增加於低的下壓力時的研磨速率。據信,即 使研磨組合物中僅有微量的含磷化合物亦能夠有效地研磨 銅。當研磨組合物中具有約〇. 〇5至約1〇重量百分比之含 磷化合物時,即可在可接受之研磨下壓力下獲得令人滿意 的研磨速率。含磷化合物之較佳範圍為佔研磨組合物之約 13 · 94611 200946619 0·1至約5重量百分比。含磷化合物之最佳範圍為佔研磨 組合物之約0· 3至約2重量百分比。 在含有餘量水的溶液中’此化合物之效力可及於很廣 之pH值範圍。此溶液之有用ΡΗ值範圍係從至少2延伸至 12。有利地,此溶液具有酸性PH值,如pH2至約7,如低 於7。此外’此/备液較佳為依賴去離子水作為餘量水以限 制偶而產生之雜質。本發明之研磨漿的較佳pH值為2至6 且更佳之pH值為2.5至5.5。在本發明中,用來調整組合 物之pH值之酸類例如為靖酸、硫酸、鹽酸與碟酸等。而用 來調整本發明組合物之pH值之驗的例子,則例如為氫氧化 銨(ammon i um hydrox i de)與氫氧化鉀(potass 士 um hydroxide) o 選擇性地出現在改性纖維素化合物之醇或酮係提供可 接受之金屬移除速率且潔淨銅時為少凹陷。此組合物可包 括非醣類水溶性聚合物且選擇性包括鱗化合物。典型來 說,這種可溶混於水之有機溶劑為醇或酮,例如為曱醇 (methanol)、乙醇(ethanol)、1-丙醇(Ι-propanol)、2-丙醇(2-propanol)、乙二醇(ethylene glycol)、1,2-丙二 醇(1,2-propanediol)、丙三醇(glycerol)、丙酮(acetone) 與甲基乙基_(methyl ethyl ketone)之至少一者。其優點 在於,組合物包括0.005至10重量百分比之這些有機溶 劑,在本說明書中所提到的所有成份範圍均為重量百分 比。較佳的組合物為包括0. 01至7. 5重量百分比之這些有 機溶劑。最佳的組合物為包括〇. 02至5重量百分比之這些 14 94611 200946619 有機溶劑。 3 ’研:組合物可選擇性包括研磨劑, 量百为比之研磨劑’以幫助移除 3重 磨劑之數量須少於或等於】番县 θ 範圍中,研 物不含研磨劑。、量百分比。最佳之研磨組合 研磨劑之平均粒子 避免產生過多的金屬凹陷為雷:或等於_奈米㈤以 性。在本說明書中,粒子尺寸^質腐姓並藉以改善平坦 ❹較佳係使用平均粒子尺寸;研磨劑之平均粒子尺寸。 j v於或等於1〇〇 劑?外,當縣二氧切之平均粒子尺寸少於或等;T〇 :研磨劑可包括添加物,如分散劑、表面活性劑= 與抗微生物劑,藉以 =^研磨劑係取自法)普托市(Pute嶋)之克 P a司(Clariant S. A.)之膠狀二氧化石夕。同樣地也可 ❿使用其他的研磨劑,包括使用氣相式(Wd)、經過沉澱與 凝聚等之研磨劑。 研磨組合物可包括機械性移除金屬内連線層之研磨 劑。這些研磨劑之例子包括麵氧化物、錢氫氧化物、 無機氫氧化氧化物、金屬慨物、金屬碳化物、金屬氣化 物、聚合物粒子與包括至少上述之—者之混合物。適合之 無機氧化物包括例如,二氡切(SiQ2)、氧化銘(Ah〇3)、 氧化鍅(Zr〇2)、氧化鈽(ce〇2)、氧化錳(Mn〇2)、氧化鈇(Ti〇2) 或包括至少上述氧化物之一者之組合。適合之無機氫氧化 15 94611 200946619 氧化物’例如’包括水鋁土(Boehmite)。這些無機氧化物 之改性形式例如為塗覆有機聚合物之無機氧化物粒子,且 假使有需要的話也可以使用經無機塗覆之粒子。適合之金 屬碳化物、金屬硼化物與金屬氮化物包括例如,破化碎 (silicon carbide)、氮化矽(silicon nitride)、碳氮化 矽(silicon carbonitride ; SiCN)、碳化蝴(b〇ron carbide)、碳化鎢(tungsten carbide)、碳化锆(zirc〇nium carbide)、硼化鋁(aluminum boride)、碳化鈕(tantalum carbide)、碳化鈦(titanium carbide)或包括上述之金屬 碳化物、金屬蝴化物與金屬氮化物之至少一者的組合。假 使有需要的話,鑽石也可以作為研磨劑。其他可作為替代 之研磨劑同樣包括聚合物粒子、有塗覆之聚合物粒子與經 表面活性劑穩定之粒子。在使用時’較佳之研磨劑為二氧 化矽。 本發明之組合物係適用於任何包括如純銅或銅合金之 銅内連線金屬之半導體晶圓。在本說明書中,介電質這個 名詞係指具介電常數k之半導體材料,包括低k值與超低 k值之介電材料。此組合物與方法可非常有效地避免多重 晶圓構件之腐蝕,此晶圓構件例如為多孔性與非多孔性低 k電介質、有機與無機低k電介質、有機矽酸鹽玻璃(〇SG)、 氟矽酸鹽玻璃(FSG)、掺雜碳之氧化物(CD0)、四乙基正石夕 Sjl鹽(TE0S)與TE0S之二氧化碎衍生物。本發明之組合物可 同樣被用於電化學機械研磨(electrochemical mechanical polishing ; ECMP)。 16 94611 200946619 4 範例 在此範例中,所有之組合物包括0.32重量百分比之羧 甲基纖維素(CMC)、0. 1重量百分比之丙烯酸/曱基丙烯酸 共聚物(比例為2 : 3,分子量為23K)以及9. 00重量百分比 之過氧化氫,並且以硝酸調整pH值,與餘量蒸餾水。 應用材料公司(Applied Material,Inc.)之 Mirra 200 毫米(mm)研磨機配備有ISRM偵測系統並使用IC1010TM聚胺 酯研磨墊(羅門哈斯電子材料CMP公司;Rohm and Hass ❹ Electronic Materials CMP Inc.),其中下壓力條件為約 1.5磅每平方吋(psi)(10.3千帕(kPa))、研磨液流逮為2〇〇 立方厘米(cc)/分(min)、平台轉速為93 RPM以及平坦化 Cu晶圓之载體轉速為87RPM。使用Kinik鑽石研磨盤修整 研磨墊。在範例1至範例6中所測試之特定研磨漿與溶液 包含如下之基本配方: 0. 5 wt%笨并三唑(BTA) ❹ 〇. 22 wt%蘋果酸 〇·32 wt%羧甲基纖維素(分子量為2〇〇κ) 〇*1 wt%丙烯酸/曱基丙烯酸共聚物(比例為2 : 3,分子 量為23K) 9 wt% H2〇2 (研磨時加入) 以瑞酸調整至ρΗ3·5 (加入_前) 餘量去離子水 注意事項 在這些範例中 代表比較例。 ,數字代表本發明之例子且字母 94611 17 200946619 範例1 此範例篩選用以降低與在大量BTA存在下以高速銅研 磨相關之潛力銅錯合劑。 表一 樣品 添加至基本配方之添加物 (0· 5 wt%) Cu移除速率 (埃/分) 出現污物 (?) A 無(控制組) 4472 是 B 天門冬氨酸 7345 是 C 檸檬酸 2338 否 D 戊二酸 6899 是 E 乳酸 7194 是 F 馬來酸 6612 是. G 丙二酸 8327 是 Η 氮基三乙酸 3196 否 I 琥珀酸 6429 是 J 酒石酸 8901 是 1 K2EDTA 3791 否 2 亞胺二乙酸 4083 否 檸檬酸、EDTA、氮基三乙酸與亞胺二乙酸均可消除研 磨墊上之污物。但僅有亞胺二乙酸與EDTA可同時避免產生 污物並提供足夠之銅移除速率。 範例2 此範例係說明在基本配方具有0.44重量百分比之磷 18 94611 200946619 與綠色污物形成 酸鹽的情況下,亞胺二乙酸對於移除 之影響。 ' 表二 ❹
出現綠色Cu-BTA污物(?) ❹ 二例3 ^ 1G均與銅錯合以降低μ 成。然而,研磨液6至1η π π 綠色污物纽合。最狀__率與消畴 3 ^ 5 PH^i 破會產生綠色沉澱物轉變成不會產4 綠色銅-BTA沉澱物。 範例3 此祀例係說明鱗酸錢與pH值對於銅凹陷與移除速_ 效能之影響。 19 94611 200946619 表三 IDA百分比 (wt%) 磷酸銨百分比 (Wt%) pH 銅移除速率 (人/分) 凹陷 100X100 特徵(A) 墊上有泠物 A 0(控制組) 0.44 3.5 4664 349 是〆 11 0.44 1.5 3.7 4345 391 否 / 12 0.44 1.5 3.9 3882 383 否 > 13 0.44 2 4.1 3538 324 否 > 14 0.4 1.5 4.1 3330 332 是 15 0.35 1.5 4.1 3282 270 是__ 16 0.3 1.5 4.1 3094 270 是 _ 17 0.25 1.5 4.1 2873 258 增加磷酸銨濃度會增加銅移除速率。此外,增加pH值 會減少銅凹陷,但也減少銅移除速率。 範例4 此衆液評估基本配方經修改而包括研磨劑粒子與〇. 44 重量百分比之磷酸銨後之數據。 表四 樣品 粒子形式 粒子量之百分比 (wt%) 銅移除速率 (A/分) 步驟餘留之 ΙΟΟΠΟΟ 特徵(A) A — 一 18 — 無 0 ] 5320 1247 50咖 Si〇2 1 1 6357 1092 19 — 一 20 球狀Al2〇3 0.1 5576 1245 ΓίΪΑΐ2〇3 Π 0.1 5828 1047 污物 一職/⑺ ^5^7 是 飞Γϋν否 ~〇Γ44%/^ 此範例說明此配方係適用於納入研磨劑粒子。尤其, 二氧化矽與氧化鋁粒子均可增加銅移除速率。 範例5 此範例係說明蘋果酸對於具有或不含亞胺二乙酸之基 本配方之影響。 20 94611. 200946619 表五 樣品 蘋果酸之濃度,以重 量百分比計 亞胺二乙酸之濃度,以 重量百分比計 銅移除速率 (埃/分) 出現污物 (?> A 0.22 (控制組) 0 4472 是 21 1 0 3594 是 22 1.6 0 3880 23 2.2 0 4132 是 24 2.8 0 4335 25 0 0. 44 2782 否 26 0.22 0.44 3412 否 27 0 0.6 3025 否 28 0 1 3541 否 此範例係說明蘋果酸、亞胺二乙酸以及蘋果酸與亞胺 二乙酸之組合,可增加銅移除速率。此外,進一步之測試 說明蘋果酸可改善研磨液之平坦化能力。 範例6 下列之測試係組合1. 5重量百分比之磷酸銨下變化亞 胺二乙酸之濃度。 表六 IDA百分比 磷酸銨百 分比 pH 銅移除速率 (A/分) 凹陷 100X100 特徵(A) 墊上有污物 (?) A 0(控制組) 0. 44 3.5 4127 353 29 0.5 1.5 4.1 2731 248 否 30 0.6 1.5 4.1 3272 354 否 31 0.7 1.5 4.1 3630 305 否 32 0.8 1.5 4.1 3841 291 否 33 0.9 1.5 4.1 4240 344 否 34 1 1.5 4.1 4231 282 否 表六係說明當pH值為4. 1時,在很廣之亞胺二乙酸之 濃度範圍中,研磨液可提供有效的污物控制與低凹陷。 21 94611 200946619 範例7 此範例係說明流程參數所能產生的進一步好處。 表八 樣品 BTA 顏果酸 CMC 共聚物 IDA NH4H2PO4 H2O2 pH 35 0.50 0.22 0.32 0.10 0. 44 2.00 9.00 4. 10 36 0.3 0.22 0. 32 0.1 1 1.5 9 4.1 表七 樣品 修整器(cond i t i oner) 研磨墊 晶圓數目 污物 (?) 35 Kinik AD3CG181060/異位(ex situ) IC1010 124 是* 36 Kinik AD3CG181060/部份原位(in situ) IC1010 127 否 36 Kinik AD3CG181060/異位 IC1010 127 否 *減少,發生於數片晶圓之後。 〇 這些數據係說明原位修整可進一步減少研磨墊留下有 害之銅-BTA沉澱物之能力。這些流程參數可降低亞胺二乙 酸有效控制銅-BTA沉澱物之所需含量。一個有效配方的具 體例子係如下所示:0. 3wt%BTA、0. 22wt%蘋果酸、 0. 32wt%CMC、0. lwt%丙烯酸/曱基丙烯酸共聚物(比例為2 : 3,分子量為23K)、lwt%亞胺二乙酸、1. 5wt%磷酸二氫銨 (NH4H2P〇4)以及9wt%H2〇2(研磨前立即加入),其中在加入H202 之前,量測到的pH值為4. 1。 【圖式簡單說明】 22 94611 200946619 無 【主要元件符號說明】 無
23 94611
Claims (1)
- 200946619 七、申請專利範圍: 1. 一種以研磨墊研磨具有銅内連線金屬之圖案化晶圓之 方法,包括下列步驟: a.提供水相研磨液,該研磨液含苯并三唑(BTA)抑制劑 以及下列化學式之錯合物: R—N—CH^C^O I ' ch2c=o I OH ❹ 其中’ R為氫或含碳化合物,該錯合物可錯合鋼離 子與水; b. 以該水相研磨液與該研磨墊研磨該圖案化晶圓使銅 溶解成Cu+1離子,其中該Cu+1離子與該BTA抑制劑之 濃度為當該水相研磨液中不含該錯合物時 [BTA]*[Cu+1 ] > Cu-BTA 沉澱物之 Ksp ;以及 c. 將至少部份之該Cu+l離子氧化成Cu+2離子以避免該 〇 Cu-BTA沉澱物在研磨時沉澱在該圖案化晶圓與該研 磨塾上。 2. 如申請專利範圍第1項所述之方法,其中該錯合物至少 包含乙二胺四乙酸(ethylenediaminetetraacetic acid)與亞胺二乙酸(diglycine)其中之一者。 3. 如申請專利範圍第1項所述之方法,更包括以純化水溶 液潔淨該研磨墊之步驟。 24 94611 200946619 4. 如申請專利範圍第1項所述之方法,其中該研磨液不含 研磨劑。 5. 如申請專利範圍第1項所述之方法,其中增加該錯合物 I 之濃度會加速銅移除速率。25 94611 200946619 四、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: OHCH2C=0 五、本案若有化學式時,請揭示最能顯示發明特徵的化學式: OH 94611
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US20140030897A1 (en) * | 2011-02-03 | 2014-01-30 | Sumco Corporation | Polishing composition and polishing method using the same |
US8435896B2 (en) | 2011-03-03 | 2013-05-07 | Rohm And Haas Electronic Materials Cmp Holdings, Inc. | Stable, concentratable chemical mechanical polishing composition and methods relating thereto |
US8440097B2 (en) | 2011-03-03 | 2013-05-14 | Rohm And Haas Electronic Materials Cmp Holdings, Inc. | Stable, concentratable, water soluble cellulose free chemical mechanical polishing composition |
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US4642221A (en) * | 1983-07-05 | 1987-02-10 | Atlantic Richfield Company | Method and composition for inhibiting corrosion in aqueous heat transfer systems |
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US6234875B1 (en) * | 1999-06-09 | 2001-05-22 | 3M Innovative Properties Company | Method of modifying a surface |
ATE292167T1 (de) * | 1999-08-13 | 2005-04-15 | Cabot Microelectronics Corp | Poliersystem mit stopmittel und verfahren zu seiner verwendung |
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US20020025762A1 (en) * | 2000-02-16 | 2002-02-28 | Qiuliang Luo | Biocides for polishing slurries |
US6451697B1 (en) * | 2000-04-06 | 2002-09-17 | Applied Materials, Inc. | Method for abrasive-free metal CMP in passivation domain |
US6409781B1 (en) * | 2000-05-01 | 2002-06-25 | Advanced Technology Materials, Inc. | Polishing slurries for copper and associated materials |
US20020068454A1 (en) * | 2000-12-01 | 2002-06-06 | Applied Materials, Inc. | Method and composition for the removal of residual materials during substrate planarization |
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JP2005142516A (ja) * | 2003-06-11 | 2005-06-02 | Toshiro Doi | 化学機械研磨用スラリー組成物及び化学機械研磨方法 |
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US7384871B2 (en) * | 2004-07-01 | 2008-06-10 | Rohm And Haas Electronic Materials Cmp Holdings, Inc. | Chemical mechanical polishing compositions and methods relating thereto |
US7435356B2 (en) * | 2004-11-24 | 2008-10-14 | Rohm And Haas Electronic Materials Cmp Holdings, Inc. | Abrasive-free chemical mechanical polishing compositions and methods relating thereto |
US7086935B2 (en) * | 2004-11-24 | 2006-08-08 | Rohm And Haas Electronic Materials Cmp Holdings, Inc. | Cellulose-containing polishing compositions and methods relating thereto |
JP2009503910A (ja) * | 2005-08-05 | 2009-01-29 | アドバンスド テクノロジー マテリアルズ,インコーポレイテッド | 金属フィルム平坦化用高スループット化学機械研磨組成物 |
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