TW201518490A - 研磨用組成物 - Google Patents
研磨用組成物 Download PDFInfo
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- TW201518490A TW201518490A TW103132069A TW103132069A TW201518490A TW 201518490 A TW201518490 A TW 201518490A TW 103132069 A TW103132069 A TW 103132069A TW 103132069 A TW103132069 A TW 103132069A TW 201518490 A TW201518490 A TW 201518490A
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- 150000003866 tertiary ammonium salts Chemical class 0.000 description 1
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- CBDKQYKMCICBOF-UHFFFAOYSA-N thiazoline Chemical compound C1CN=CS1 CBDKQYKMCICBOF-UHFFFAOYSA-N 0.000 description 1
- 150000003573 thiols Chemical class 0.000 description 1
- UAXOELSVPTZZQG-UHFFFAOYSA-N tiglic acid Natural products CC(C)=C(C)C(O)=O UAXOELSVPTZZQG-UHFFFAOYSA-N 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
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- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 229940005605 valeric acid Drugs 0.000 description 1
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- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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- 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
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Abstract
本發明提供一種保管安定性優異之研磨用組成物。
本發明係一種研磨用組成物,其包含研磨粒與含鹵原子之氧化劑,研磨用組成物中之前述研磨粒所具有之矽醇基數之總和(A)(單位:個)除以研磨用組成物中之前述氧化劑之濃度(B)(單位:質量%)之值(A/B)為8×1023以下。
Description
本發明係關於研磨用組成物。
近年來,隨著LSI之高積體化、高性能化,已開發新的微細加工技術。化學機械研磨(以下亦單簡稱為CMP)法亦為其一種,係於LSI製造步驟,尤其是多層配線形成步驟中之層間絕緣膜之平坦化、金屬插塞形成、埋入配線(金屬鑲嵌(damascene)配線)形成中頻繁被利用之技術。該技術已揭示於例如美國專利第4944836號說明書中。金屬鑲嵌配線技術可簡化配線步驟,或提高良率及信賴性,認為爾後會擴大其應用。
高速邏輯裝置(logic device)中,作為金屬鑲嵌配線目前由於為低電阻之故,因此主要使用銅作為配線金屬,銅被認為在今後以DRAM為代表之記憶體裝置中亦將被廣泛使用。金屬CMP之一般方法係將研磨墊貼附於圓形之研磨壓盤(platen)上,以研磨劑浸漬研磨墊表面,且壓抵向基板之形成有金屬膜之面,於自其背面施加特定壓力(以下亦有單簡稱為研磨壓力)之狀態下旋轉研磨壓
盤,藉由研磨劑與金屬膜之凸部之機械摩擦,而去除凸部之金屬膜者。
另一方面,於配線之銅或銅合金等之下層形成有鉭、鉭合金、或鉭化合物等,作為用於防止銅對層間絕緣膜中之擴散之障壁層。因此,埋入銅或銅合金之配線部分以外,有必要藉由CMP去除露出之障壁層。然而,障蔽層相較於銅或銅合金而言一般硬度較高,故使用銅或銅合金用之研磨材料之組合之CMP中,大多情況無法獲得足夠之CMP速度。
另一方面,作為障蔽層使用之鉭、鉭合金、或鉭化合物等難以化學安定地蝕刻,且由於硬度高故即使機械研磨亦不像銅或銅合金那般容易。此外,近年來,已探討釕、釕合金、釕化合物等貴金屬材料作為障蔽層用之材料。釕、釕合金、釕化合物等貴金屬材料之電阻率低於鉭、鉭合金、或鉭化合物,而可藉化學氣相成長法(CVD)成膜,就可對應於更細微寬度之配線方面而言較優異。然而,釕、釕合金、或釕化合物等貴金屬材料與鉭、鉭合金、或鉭化合物同樣,化學上安定且硬度高,故難以研磨。
又,貴金屬材料係使用作為於例如DRAM電容器構造之製造步驟中之電極材料。而且,為了去除由含有如釕單質體或氧化釕(RuOx)之貴金屬之材料所成之部分的一部分時,係利用使用了研磨用組成物的研磨而進行。然而,與前述障蔽層用之貴金屬材料同樣地,於去除含有化
學上安定之貴金屬之材料時一般較花費時間,故對於該種研磨用組成物之進一步改良以提高處理量之需求強烈。
CMP中所用之研磨劑一般包含氧化劑及研磨粒。由該CMP用研磨劑進行之CMP之基本機制可認為係首先,以氧化劑使金屬膜表面氧化,且以研磨粒削除所得金屬膜表面之氧化層者。凹部之金屬膜表面之氧化層不太碰觸到研磨墊,達不到利用研磨粒之削除效果,故在CMP之進行同時,一起去除凸部之金屬膜使基板表面平坦化。
CMP中,要求對配線金屬的高研磨速度、研磨速度之安定性及研磨表面之低缺陷密度。然而,含釕之膜由於相較於如銅、鎢之其他金屬鑲嵌配線金屬膜更為化學安定且為高硬度,故難以研磨。作為含如此貴金屬之膜,尤其是含釕之膜的研磨液,於例如日本特開2004-172326號公報中提案含有研磨粒、氧化劑及苯并三唑之研磨液。
且,作為降低電晶體之消耗電力或提高性能(動作特性)之技術之一,已進行提高載子之移動度之高移動度通道(channel)材料之探討。該等提高載子之輸送特性之通道由於提高導通之汲極電流,故一方面獲得充分之導通電流,一方面可降低電源電壓。該組合獲得在低電力下之更高MOSFET(金屬氧化物半導體場效電晶體(metal oxide semiconductor field-effect transistor))之性能。
高移動度通道材料期待應用僅由III-V族化合物、IV族化合物、Ge(鍺)、C(碳)所成之石墨烯等。目前,III-V族化合物通道之形成由於存在有尚未確立能提高通
道之結晶性、良好地進行形狀之控制.成長之技術的課題,故對於較III-V族化合物更易於導入之IV族化合物,尤其是SiGe與Ge等積極地進行探討。
使用高移動度材料之通道,可對具有IV族化合物通道、及/或Ge通道(以下亦稱為Ge材料部分)與含有矽材料之部分(以下亦稱為矽材料部分)之研磨對象物進行研磨而形成。此時,除了以高的研磨速度研磨Ge材料部分以外,亦要求在研磨對象物研磨後之表面不產生因蝕刻造成之階差。例如,日本特開2010-130009號公報(美國專利第8338302號說明書)及日本特表2010-519740號公報(美國專利申請公開第2011/117740號說明書)中揭示於研磨Ge基板之用途中使用之研磨用組成物。
然而,日本特開2010-130009號公報(美國專利第8338302號說明書)及日本特表2010-519740號公報(美國專利申請公開第2011/117740號說明書)中記載之研磨用組成物有保管安定性低之問題。
因此本發明之目的係提供一種保管安定性優異之研磨用組成物。
為解決上述課題,本發明者重複積極研究。結果,發現藉由使研磨用組成物中之研磨粒所具有之矽醇基數之總和除以研磨用組成物中之氧化劑之濃度之值為特定範圍內之研磨用組成物,可解決上述課題。因此,基於上述見
解,終於完成本發明。
亦即,本發明係一種研磨用組成物,其包含研磨粒與含鹵原子之氧化劑,且研磨用組成物中之前述研磨粒所具有之矽醇基數之總和(A)(單位:個)除以研磨用組成物中之前述氧化劑之濃度(B)(單位:質量%)之值(A/B)為8×1023以下。
本發明係一種研磨用組成物,其包含研磨粒與含鹵原子之氧化劑,且研磨用組成物中之前述研磨粒所具有之矽醇基數之總和(A)(單位:個)除以研磨用組成物中之前述氧化劑之濃度(B)(單位:質量%)之值(A/B)為8×1023以下。藉由成為如此構成,而提高研磨用組成物之保管安定性。
本發明之研磨用組成物之保管安定性會提高之詳細理由並不清楚,但認為保管安定性之降低係因研磨用組成物中所含之氧化劑分解所致。相對於此,本發明之研磨用組成物之研磨用組成物中之前述研磨粒所具有之矽醇基數之總和(A)(單位:個)除以研磨用組成物中之前述氧化劑之濃度(B)(單位:質量%)之值(A/B)為特定之範圍。該A/B意指對氧化劑濃度與氧化劑分解造成影響之矽醇基數之比率,認為藉由將該值控制在某特定值以下,可將氧化劑分解的比例抑制在容許範圍內,而提高研磨用組成物之保管安定性。
本發明人發現作為氧化劑之分解抑制之機制係鹵系之氧化劑與矽醇基相互作用,具體而言使鹵系之氧化劑作用於矽醇基,而使氧化劑本身分解且使濃度減少。與一定量之矽醇基數相互作用而分解之氧化劑之量為一定,而藉由增加氧化劑濃度,或減少研磨粒濃度,使因分解而減少之氧化劑相對於初期添加之氧化劑濃度之比率變小,結果,可認為使研磨性能安定,而提高研磨用組成物之保存安定性。
又,上述機制係經推測者,本發明並不受上述機制之任何限制。
本發明之研磨對象物並無特別限制,但可較佳地用於研磨具有含IV族材料之層之研磨對象物之用途。更詳細而言,係於研磨該研磨對象物而製造基板之用途中使用。研磨對象物亦可進一步具有矽材料部分。IV族材料之例列舉為Ge(鍺)、SiGe(矽鍺)等。此外,矽材料之例列舉為多晶矽、氧化矽、氮化矽等。
接著,針對本發明之研磨用組成物之構成加以詳細說明。
研磨用組成物中所含之研磨粒具有機械研磨研磨對象物之作用,且提高研磨用組成物對研磨對象物的研磨速
度。
本發明中使用之研磨粒只要具有矽醇基者即無特別限制。其具體例列舉為例如由二氧化矽、氧化鋁、氧化鋯、氧化鈦等金屬氧化物所成之粒子。該研磨粒可單獨使用或亦可混合2種以上使用。此外,該研磨粒可使用市售品亦可使用合成品。
該等研磨粒中以二氧化矽粒子較佳,特佳為膠體二氧化矽。
研磨粒亦可經表面修飾。通常之膠體二氧化矽由於在酸性條件下之仄他(Zeta)電位值接近於零,故在酸性條件下二氧化矽粒子彼此間不會電排斥而容易引起凝聚。相對於此,即使以在酸性條件下具有仄他電位較大之負值的方式經表面修飾之研磨粒,在酸性條件下相互間強烈排斥而良好分散之結果,提高了研磨用組成物之保存安定性。如此之表面修飾研磨粒可藉由例如使鋁、鈦或鋯等金屬或該等之氧化物與研磨粒混合而摻雜於研磨粒之表面而獲得。
其中,尤特佳為固定化有有機酸之膠體二氧化矽。有機酸對研磨用組成物中所含之膠體二氧化矽表面之固定化係藉由例如使有機酸之官能基化學鍵結於膠體二氧化矽表面而進行。僅單使膠體二氧化矽與有機酸共存,無法達成有機酸對膠體二氧化矽之固定化。若使有機酸之一種的磺酸固定化於膠體二氧化矽上,則可藉例如”Sulfonic acid-functionalized silica through quantitative oxidation of thiol
groups",Chem.Commun.246-247(2003)中所記載之方法進行。具體而言,使3-巰丙基三甲氧基矽烷等之具有硫醇基之矽烷偶合劑偶合於膠體二氧化矽上後,以過氧化氫使硫醇基氧化,藉此可獲得磺酸固定化於表面之膠體二氧化矽。或者,若使羧酸固定化於膠體二氧化矽上,則可藉例如”Novel Silane Coupling Agents Containing a Photolabile 2-Nitrobenzyl Ester for Introduction of a Carboxy Group on the Surface of Silica Gel”,Chemistry Letters,3,228-229(2000)中所記載之方法進行。具體而言,在將含有光反應性2-硝基苄酯之矽烷偶合劑偶合於膠體二氧化矽後,藉由光照射,可獲得使羧酸固定化於表面之膠體二氧化矽。
研磨粒之平均一次粒徑之下限較佳為5nm以上,更佳為7nm以上,又更佳為10nm以上。又,研磨粒之平均一次粒徑之上限較佳為500nm以下,更佳為300nm以下,又更佳為200nm以下。若為該範圍,則研磨用組成物對研磨對象物之研磨速度獲得提高,且,可進一步抑制使用研磨用組成物研磨後之研磨對象物表面產生凹陷(dising)。又,研磨粒之平均一次粒徑係採用基於例如以BET法測定之研磨粒之比表面積算出。
研磨用組成物中之研磨粒之含量(濃度)下限較佳為0.0002g/L以上,更佳為0.002g/L以上,又更佳為0.02g/L以上。另外,研磨用組成物中之研磨粒之含量(濃度)上限較佳為200g/L以下,更佳為100g/L以下,又更佳為
50g/L以下。若在該範圍,則一方面可抑制成本,一方面獲得高的研磨速度,且可有效率地進行加工。
本發明之研磨用組成物中,研磨用組成物所含之研磨粒具有之矽醇基數之總和(A)(單位:個)除以研磨用組成物中之氧化劑之濃度(B)(單位:質量%)之值(A/B)為8×1023以下之範圍。該A/B值意指對氧化劑濃度與氧化劑分解造成影響之矽醇基數之比率,可認為藉由控制該值,將氧化劑之分解比例抑制在容許之範圍內,提高研磨用組成物之保管安定性。
A/B超過8×1023時,因矽醇基使氧化劑之分解比率變高,而發生研磨性能大幅變化之缺點。A/B之上限值為8×1023以下,較佳為3×1023以下。
研磨用組成物中所含研磨粒所具有之矽醇基數之總和(A)可利用以下方法算出。
.研磨粒之一次粒徑[nm](實測值):以由BET法計算出之比表面積(SA)為基準,假設研磨粒為真球,使用SA=4πR2之公式算出研磨粒之直徑(一次粒徑)
.每1個研磨粒之體積(計算值):使用由比表面積(SA)算出之一次粒徑,由下式計算
每1個研磨粒之體積=4/3π×(研磨粒之一次粒徑/2)3
.每1個研磨粒之重量(計算值):使用以計算求出之每1個研磨粒之體積,由下式計算
每1個研磨粒之重量=每1個研磨粒之體積×研磨粒之比重(膠體二氧化矽時為2.2)
.每1個研磨粒之表面積(計算值):使用由比表面積(SA)算出之一次粒徑,由下式計算
每1個研磨粒之表面積=4π×(研磨粒之一次粒徑/2)2
.研磨用組成物中之研磨粒個數(計算值):研磨用組成物中之研磨粒濃度除以每1個研磨粒之重量而計算
.研磨用組成物中之研磨粒之總表面積[nm2](計算值):由每1個研磨粒之表面積與研磨用組成物中之研磨粒個數之乘積而算出。
.矽醇基數(實測值):算出以Sears法求出之每單位表面積之矽醇基數[矽醇數/nm2]
Sears法係參照G.W.Sears,Jr.,”Determination of Specific Surface Area of Colloidal Silica by Titration with Sodium Hydroxide”,Analytical Chemistry,28(12),1981(1956)實施。測定係使用二氧化矽水溶液(1wt%),滴加之NaOH之每一次滴加量為0.01ml,滴加間隔為30秒。
.研磨用組成物中之研磨粒所具有之矽醇基數之總和(個)(A)(計算值):以Sears法求出之矽醇基數(實測值)[個/nm]與使用BET比表面積與研磨用組成物中之研磨粒濃度所計算之研磨用組成物中之研磨粒之總表面積[nm2](計算值)之乘積而計算。
.氧化劑濃度(B)(實測值):使用氧化劑濃度為已知之藥劑時,由添加之量計算出。或者以氧化還原滴定進行定量。例如,NaClO時,係使用平成15年9月29日
日本厚生勞動省公告第318號之方法以滴定進行定量。
.氧化劑每1質量%之研磨粒之矽醇基數(計算值):研磨用組成物中之研磨粒所具有之矽醇基數之總和(個)(A)(計算值)除以氧化劑濃度(B)而算出。
研磨用組成物所含之研磨粒所具有之矽醇基數之總和(A)可藉由研磨粒濃度之增減、研磨粒之每單位面積之矽醇基數之增減加以控制。此外,研磨用組成物所含之研磨粒所具有之矽醇基數之總和(A)(單位:個)除以研磨用組成物中之氧化劑之濃度(B)(單位:質量%)之值(A/B),除了可藉由研磨粒濃度之增減、研磨粒之每單位面積之矽醇基數之增減而控制以外,亦可藉由增減氧化劑之添加量而控制。
本發明中使用之氧化劑含有鹵原子。該種氧化劑之具體例列舉為例如鹵酸及其鹽、亞氯酸(HClO2)、亞溴酸(HBrO2)、亞碘酸(HIO2)、亞氯酸鈉(NaClO2)、亞氯酸鉀(KClO2)、亞溴酸鈉(NaBrO2)、亞溴酸鉀(KBrO2)等之亞鹵酸或其鹽;氯酸鈉(NaClO3)、氯酸鉀(KClO3)、氯酸銀(AgClO3)、氯酸鋇(Ba(ClO3)2)、溴酸鈉(NaBrO3)、溴酸鉀(KBrO3)、碘酸鈉(NaIO3)等鹵酸或其鹽;過氯酸(HClO4)、過溴酸(HBrO4)、過碘酸(HIO4)、過碘酸鈉(NaIO4)、過碘酸鉀(KIO4)、過碘酸四丁基銨((C4H9)4NIO4)等
之過鹵酸或其鹽;次氟酸(HFO)、次氯酸(HClO)、次溴酸(HBrO)、次碘酸(HIO)等次鹵酸;次氟酸鋰(LiFO)、次氟酸鈉(NaFO)、次氟酸鉀(KFO)、次氟酸鎂(Mg(FO)2)、次氟酸鈣(Ca(FO)2)、次氟酸鋇(Ba(FO)2)等次氟酸之鹽;次氯酸鋰(LiClO)、次氯酸鈉(NaClO)、次氯酸鉀(KClO)、次氯酸鎂(Mg(ClO)2)、次氯酸鈣(Ca(ClO)2)、次氯酸鋇(Ba(ClO)2)、次氯酸第三丁酯(t-BuClO)、次氯酸銨(NH4ClO)、次氯酸三乙醇胺((CH2CH2OH)3N.ClO)等之次氯酸之鹽;次溴酸鋰(LiBrO)、次溴酸鈉(NaBrO)、次溴酸鉀(KBrO)、次溴酸鎂(Mg(BrO)2)、次溴酸鈣(Ca(BrO)2)、次溴酸鋇(Ba(BrO)2)、次溴酸銨(NH4BrO)、次溴酸三乙醇胺((CH2CH2OH)3N.BrO)等之次溴酸之鹽;次碘酸鋰(LiIO)、次碘酸鈉(NaIO)、次碘酸鉀(KIO)、次碘酸鎂(Mg(IO)2)、次碘酸鈣(Ca(IO)2)、次碘酸鋇(Ba(IO)2)、次碘酸銨(NH4IO)、次碘酸三乙醇胺((CH2CH2OH)3N.IO)等之次碘酸之鹽等。該等含鹵原子之氧化劑可單獨使用或亦可混合2種以上使用。
該等含有鹵原子之氧化劑中,尤以亞氯酸、次氯酸、氯酸、過氯酸及該等之鹽較佳。至於鹽可選擇銨鹽、鈉鹽、鉀鹽等。
本發明之研磨用組成物中之氧化劑濃度(B)之下限較佳為0.0001質量%以上,更佳為0.001質量%以上,又
更佳為0.005質量%以上。此外,本發明之研磨用組成物中之氧化劑濃度(B)之上限較佳未達0.5質量%,更佳為0.4質量%以下,又更佳為0.3質量%以下。若為該範圍,則可抑制含IV族材料之層之過度溶解,並且獲得高的研磨速度,可有效率地進行加工。
本發明之研磨用組成物較佳為進一步含有安定性提升劑。藉由含有安定性提升劑,而進一步提升本發明之研磨用組成物之保管安定性。
此種安定性提升劑之例子可舉例具有醯胺鍵之化合物。進一步之具體例可舉例具有以通式(1)或通式(2)表示之構造之化合物。
惟,上述通式(1)中,R1表示氫原子、羥基、醛基、羰基、羧基、胺基、亞胺基、偶氮基、硝基、亞硝基、硫醇基、磺酸基、磷酸基、鹵基、烷基(直鏈、分支、環狀之烷基,包含雙環烷基、活性次甲基(methine))、芳基或醯基。該等官能基可未取代亦可
經取代。通式(1)中,R2表示具有2個以上碳原子之雜環式構造。該等官能基為未取代或經取代均可。
取代基並無特別限制,列舉為例如以下者。
鹵原子(氟原子、氯原子、溴原子或碘原子)、烷基(直鏈、分支或環狀烷基,包含雙環烷基、活性次甲基)、烯基、炔基、芳基、雜環基(不管取代位置)、醯基、烷氧基羰基、芳基氧基羰基、雜環氧基羰基、胺甲醯基、N-羥基胺甲醯基、N-醯基胺甲醯基、N-磺醯基胺甲醯基、N-胺甲醯基胺甲醯基、硫胺甲醯基、N-胺磺醯基胺甲醯基、咔唑基、羧基或其鹽、草醯基、草醯胺醯基(oxamoyl)、氰基、碳二醯亞胺基、甲醯基、羥基、烷氧基(包含重複含有伸乙基氧基或伸丙基氧基單位之基)、芳氧基、雜環氧基、醯氧基、(烷氧基或芳氧基)羰基氧基、胺甲醯氧基、磺醯氧基、胺基、(烷基、芳基或雜環)胺基、醯基胺基、磺醯胺基、脲基、硫脲基、N-羥基脲基、醯亞胺基、(烷氧基或芳氧基)羰基胺基、胺磺醯基胺基、胺基脲(semicarbazide)基、硫胺基脲基、聯胺基、銨基(ammonio)、草醯胺醯基胺基、N-(烷基或芳基)磺醯基脲基、N-醯基脲基、N-醯基胺磺醯基胺基、羥基胺基、硝基、含4級化氮原子之雜環基(例如吡啶鎓基、咪唑鎓基、喹啉鎓基、異喹啉鎓基)、異氰基(isocyano)、亞胺基、巰基、(烷基、芳基或雜環)硫基、(烷基、芳基或雜環)二硫基、(烷基、或芳基)磺醯基、(烷基、或芳基)亞磺醯基、磺基或其鹽、胺磺醯
基、N-醯基胺磺醯基、N-磺醯基胺磺醯基或其鹽、膦基、氧膦基(phosphinyl)、氧膦基氧基、氧膦基胺基、矽烷基等。
又其中,所謂活性次甲基意指以2個拉電子基取代之次甲基,此處所謂拉電子基意指醯基、烷氧基羰基、芳氧基羰基、胺甲醯基、烷基磺醯基、芳基磺醯基、胺磺醯基、三氟甲基、氰基、硝基、碳醯亞胺基。此處2個拉電子基亦可相互鍵結成為環構造。此外,所謂鹽意指鹼金屬、鹼土類金屬、重金屬等陽離子、或銨離子、鏻離子等之有機陽離子。
該等取代基亦可經與上述相同之取代基進一步取代。
以上述通式(1)表示之化合物之具體例列舉為例如2-吡咯啶酮、1-甲基-2-吡咯啶酮、1-乙基-2-吡咯啶酮、5-甲基-2-吡咯啶酮、1-(2-羥基甲基)-2-吡咯啶酮、1-(2-羥基乙基)-2-吡咯啶酮、1-(氯甲基)-2-吡咯啶酮、1-乙醯基-2-吡咯啶酮、5-硫代吡咯啶-2-酮、焦麩胺酸(pyroglutamic acid)、焦麩胺酸甲酯、焦麩胺酸乙酯、琥珀醯亞胺、N-溴琥珀醯亞胺、N-氯琥珀醯亞胺、N-碘琥珀醯亞胺、N-羥基琥珀醯亞胺、N-甲基琥珀醯亞胺、N-苯基琥珀醯亞胺、N-甲基-2-苯基琥珀醯亞胺、2-乙基-2-甲基琥珀醯亞胺、六氫鄰苯二甲醯亞胺、連苯四酸二醯亞胺、六氫鄰苯二甲醯亞胺、2-氧代吡咯啶-1-乙醯胺、1-甲基-5-氧代-2-吡咯啶乙酸、2-(2-氧代吡咯啶-1-基)丁烷醯胺、5-甲氧基吡咯啶-2-酮、2-(3-甲基-2,5-二氧代吡咯
啶-1-基)丙-1-烯酸甲酯(Versimide)、4-羥基-2-氧代-1-吡咯啶乙醯胺、4-羥基-2-吡咯啶酮、1-羥基-3-胺基-2-吡咯啶酮、1-(2-羥基乙基)-2-吡咯啶酮、2-吡咯啶酮-5-羧酸、1,2-二氫-3H-吡咯嗪(pyrrolizine)-3-酮等。
其中,上述通式(2)中,R3及R4各自獨立表示氫原子、羥基、醛基、羰基、羧基、胺基、亞胺基、偶氮基、硝基、亞硝基、硫醇基、磺酸基、磷酸基、鹵基、烷基(直鏈、分支、環狀之烷基,包含雙環烷基、活性次甲基)、芳基或醯基。該等官能基可未取代亦可經取代。n表示重複單位之數。
以通式(2)表示之化合物之具體例列舉為聚-N-乙烯基乙醯胺等。
該等安定性提升劑可單獨使用或亦可混合2種以上使用。
本發明之研磨用組成物中之安定性提升劑之含量下限較佳為0.001質量%以上,更佳為0.01質量%以上,又更佳為0.1質量%以上。又,本發明之研磨用組成物中之安定性提升劑含量之上限較佳為20質量%以下,更佳為10
質量%以下,又更佳為5質量%以下。若為該範圍,則可抑制成本,並且進一步提高本發明之研磨用組成物之保管安定性。
本發明之研磨用組成物之pH較佳為5以上,更佳為7以上。又,本發明之研磨用組成物之pH較佳為12以下,更佳為10以下。若為該範圍,則可抑制研磨對象物之過度溶解並且有效率地實施研磨。
前述pH可藉由適量添加pH調節劑加以調整。為了將研磨用組成物之pH調整至期望之值而視需要使用之pH調整劑可為酸或鹼之任一種,又,亦可為無機化合物及有機化合物之任一種。酸之具體例列舉為例如硫酸、硝酸、硼酸、碳酸、次磷酸、亞磷酸及磷酸等無機酸;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、苯甲酸、乙醇酸、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、酒石酸、檸檬酸及乳酸等之羧酸,以及甲烷磺酸、乙烷磺酸及羥乙磺酸等有機硫酸等之有機酸等。鹼之具體例列舉為氫氧化鉀等鹼金屬之氫氧化物、氨、乙二胺及哌啶等之胺,以及四甲基銨及四乙基銨等之4級銨鹽。該等pH調節劑可單獨使用或亦可混合2種以上使用。
本發明之研磨用組成物較佳含有水作為用以使各成分分散或溶解之分散介質或溶劑。就抑制阻礙其他成分之作用之觀點而言,較佳為儘可能不含雜質之水,具體而言較佳為以離子交換樹脂去除雜質離子後,通過過濾器去除異物之純水或超純水、或蒸餾水。
本發明之研磨用組成物亦可視需要進一步含有金屬防腐蝕劑、防腐劑、防黴劑、水溶性高分子、用以使難溶性之有機物溶解之有機溶劑等其他成分。以下針對較佳之其他成分之金屬防腐蝕劑、防腐劑、及防黴劑加以說明。
藉由於研磨用組成物中添加金屬防腐蝕劑,可進一步抑制因使用研磨用組成物研磨而在配線之側邊產生凹陷。另外,可進一步抑制使用研磨用組成物研磨後在研磨對象物之表面產生凹陷。
可使用之金屬防腐蝕劑並無特別限制,但較佳為雜環式化合物或界面活性劑。雜環式化合物中之雜環之員數並無特別限制。且,雜環式化合物可為單環化合物,亦可為具有縮合環之多環化合物。該金屬防腐蝕劑可單獨使用或混合2種以上使用。另外,該金屬防腐蝕劑可使用市售
品,亦可使用合成品。
可作為金屬防腐蝕劑使用之雜環化合物之具體例列舉為例如吡咯化合物、吡唑化合物、咪唑化合物、三唑化合物、四唑化合物、吡啶化合物、吡嗪化合物、嗒嗪化合物、4-氮茚化合物、吲哚嗪(indolizine)化合物、吲哚化合物、異吲哚化合物、吲唑化合物、嘌呤化合物、喹嗪(quinolizine)化合物、喹啉化合物、異喹啉化合物、萘啶化合物、酞嗪化合物、喹噁啉化合物、喹唑啉化合物、噌啉化合物、喋啶化合物、噻唑化合物、異噻唑化合物、噁唑化合物、異噁唑化合物、呋呫(furazane)咱化合物等含氮雜環化合物。
若進一步列舉具體例,則吡唑化合物之例列舉為例如1H-吡唑、4-硝基-3-吡唑羧酸、3,5-吡唑羧酸、3-胺基-5-苯基吡唑、5-胺基-3-苯基吡唑、3,4,5-三溴吡唑、3-胺基吡唑、3,5-二甲基吡唑、3,5-二甲基-1-羥基甲基吡唑、3-甲基吡唑、1-甲基吡唑、3-胺基-5-甲基吡唑、4-胺基-吡唑并[3,4-d]嘧啶、異嘌呤醇(allopurinol)、4-氯-1H-吡唑并[3,4-D]嘧啶、3,4-二羥基-6-甲基吡唑并(3,4-B)吡啶、6-甲基-1H-吡唑并[3,4-b]吡啶-3-胺等。
咪唑化合物之具體例列舉為例如咪唑、1-甲基咪唑、2-甲基咪唑、4-甲基咪唑、1,2-二甲基咪唑、2-乙基-4-甲基咪唑、2-異丙基咪唑、苯并咪唑、5,6-二甲基苯并咪唑、2-胺基苯并咪唑、2-氯苯并咪唑、2-甲基苯并咪唑、2-(1-羥基乙基)苯并咪唑、2-羥基苯并咪唑、2-苯基苯
并咪唑、2,5-二甲基苯并咪唑、5-甲基苯并咪唑、5-硝基苯并咪唑、1H-嘌呤等。
三唑化合物之例列舉為例如1,2,3-三唑、1,2,4-三唑、1-甲基-1,2,4-三唑、甲基-1H-1,2,4-三唑-3-羧酸酯、1,2,4-三唑-3-羧酸、1,2,4-三唑-3-羧酸甲酯、1H-1,2,4-三唑-3-硫醇、3,5-二胺基-1H-1,2,4-三唑、3-胺基-1,2,4-三唑-5-硫醇、3-胺基-1H-1,2,4-三唑、3-胺基-5-苄基-4H-1,2,4-三唑、3-胺基-5-甲基-4H-1,2,4-三唑、3-硝基-1,2,4-三唑、3-溴-5-硝基-1,2,4-三唑、4-(1,2,4-三唑-1-基)苯酚、4-胺基-1,2,4-三唑、4-胺基-3,5-二丙基-4H-1,2,4-三唑、4-胺基-3,5-二甲基-4H-1,2,4-三唑、4-胺基-3,5-二庚基-4H-1,2,4-三唑、5-甲基-1,2,4-三唑-3,4-二胺、1H-苯并三唑、1-羥基苯并三唑、1-胺基苯并三唑、1-羧基苯并三唑、5-氯-1H-苯并三唑、5-硝基-1H-苯并三唑、5-羧基-1H-苯并三唑、5-甲基-1H-苯并三唑、5,6-二甲基-1H-苯并三唑、1-(1’,2’-二羧基乙基)苯并三唑、1-[N,N-雙(羥基乙基)胺基甲基]苯并三唑、1-[N,N-雙(羥基乙基)胺基甲基]-5-甲基苯并三唑、1-[N,N-雙(羥基乙基)胺基甲基]-4-甲基苯并三唑等。
四唑化合物之例列舉為例如1H-四唑、5-甲基四唑、5-胺基四唑、及5-苯基四唑等。
吲唑化合物之例列舉為例如1H-吲唑、5-胺基-1H-吲唑、5-硝基-1H-吲唑、5-羥基-1H-吲唑、6-胺基-1H-吲唑、6-硝基-1H-吲唑、6-羥基-1H-吲唑、3-羧基-5-甲基-
1H-吲唑等。
吲哚化合物之具體例列舉為1H-吲哚、1-甲基-1H-吲哚、2-甲基-1H-吲哚、3-甲基-1H-吲哚、4-甲基-1H-吲哚、5-甲基-1H-吲哚、6-甲基-1H-吲哚、7-甲基-1H-吲哚、4-胺基-1H-吲哚、5-胺基-1H-吲哚、6-胺基-1H-吲哚、7-胺基-1H-吲哚、4-羥基-1H-吲哚、5-羥基-1H-吲哚、6-羥基-1H-吲哚、7-羥基-1H-吲哚、4-甲氧基-1H-吲哚、5-甲氧基-1H-吲哚、6-甲氧基-1H-吲哚、7-甲氧基-1H-吲哚、4-氯-1H-吲哚、5-氯-1H-吲哚、6-氯-1H-吲哚、7-氯-1H-吲哚、4-羧基-1H-吲哚、5-羧基-1H-吲哚、6-羧基-1H-吲哚、7-羧基-1H-吲哚、4-硝基-1H-吲哚、5-硝基-1H-吲哚、6-硝基-1H-吲哚、7-硝基-1H-吲哚、4-腈基-1H-吲哚、5-腈基-1H-吲哚、6-腈基-1H-吲哚、7-腈基-1H-吲哚、2,5-二甲基-1H-吲哚、1,2-二甲基-1H-吲哚、1,3-二甲基-1H-吲哚、2,3-二甲基-1H-吲哚、5-胺基-2,3-二甲基-1H-吲哚、7-乙基-1H-吲哚、5-(胺基甲基)吲哚、2-甲基-5-胺基-1H-吲哚、3-羥基甲基-1H-吲哚、6-異丙基-1H-吲哚、5-氯-2-甲基-1H-吲哚等。
該等中較佳之雜環化合物為三唑化合物,特佳為1H-苯并三唑、5-甲基-1H-苯并三唑、5,6-二甲基-1H-苯并三唑、1-[N,N-雙(羥基乙基)胺基甲基]-5-甲基苯并三唑、1-[N,N-雙(羥基乙基)胺基甲基]-4-甲基苯并三唑、1,2,3-三唑、及1,2,4-三唑。該等雜環化合物由於對研磨對象物表面之化學或物理之吸附力高,故可在研磨對象物
之表面形成更堅固之保護膜。此在使用本發明之研磨用組成物研磨後對於提高研磨對象物之表面平坦性有利。
且,使用作為金屬防腐蝕劑之界面活性劑列舉為陰離子性界面活性劑、陽離子性界面活性劑、兩性界面活性劑及非離子性界面活性劑之任一種。
陰離子性界面活性劑之例列舉為聚氧乙烯烷基醚乙酸、聚氧乙烯烷基硫酸酯、烷基硫酸酯、聚氧乙烯烷基醚硫酸、烷基醚硫酸、烷基苯磺酸、烷基磷酸酯、聚氧乙烯烷基磷酸酯、聚氧乙烯磺基琥珀酸、烷基磺基琥珀酸、烷基萘磺酸、烷基二苯基醚二磺酸、及該等之鹽等。
陽離子性界面活性劑之例列舉為例如烷基三甲基銨鹽、烷基二甲基銨鹽、烷基苄基二甲基銨鹽、及烷基胺鹽等。
兩性界面活性劑之例列舉為例如烷基甜菜鹼及烷基氧化胺等。
非離子性界面活性劑列舉為例如聚氧乙烯烷基醚、聚氧伸烷基烷基醚、山梨糖醇酐脂肪酸酯、甘油脂肪酸酯、聚氧乙烯脂肪酸酯、聚氧乙烯烷基胺、及烷基烷醇醯胺等。
該等中較佳之界面活性劑為聚氧乙烯烷基醚乙酸鹽、聚氧乙烯烷基醚硫酸鹽、烷基醚硫酸鹽、烷基苯磺酸鹽、及聚氧乙烯烷基醚。該等界面活性劑由於對於研磨對象物表面之化學或物理性吸附力高,故可在研磨對象物表面形成更堅固之保護膜。此對於提高使用本發明之研磨用組成
物研磨後提高研磨對象物之表面之平坦性有利。
本發明中使用之防腐劑及防黴劑列舉為例如2-甲基-4-異噻唑啉-3-酮或5-氯-2-甲基-4-異噻唑啉-3-酮等之異噻唑啉系防腐劑,對羥基苯甲酸酯類、及苯氧基乙醇等。該等防腐劑及防黴劑可單獨使用或亦可混合2種以上使用。
本發明之研磨用組成物之製造方法並未特別限制,可藉由例如在水中攪拌混合研磨粒及含鹵原子之氧化劑、及視需要之其他成分而得。
混合各成分時之溫度並無特別限制,較佳為10~40℃,亦可加熱以提高溶解速度。又,混合時間亦無特別限制。
如上述,本發明之研磨用組成物係特別適合使用於具有含IV族材料之層之研磨對象物之研磨。因此,本發明提供以本發明之研磨用組成物研磨具有含IV族材料之層之研磨對象物之研磨方法。另外,本發明提供包含以前述研磨方法研磨具有含IV族材料之層之研磨對象物之步驟之基板製造方法。
研磨裝置可使用安裝有保持具有研磨對象物之基板等
之載具(holder)與可改變轉數之馬達等,且具有可貼附研磨墊(研磨布)之研磨壓盤之一般研磨裝置。
前述研磨墊可無特別限制地使用一般之不織布、聚胺基甲酸酯及多孔質氟樹脂等。研磨墊較佳施以可使研磨液積存之溝槽加工。
研磨條件亦無特別限制,例如研磨壓盤之轉數較佳為10~500rpm,對具有研磨對象物之基板施加之壓力(研磨壓力)較佳為0.5~10psi。將研磨用組成物供給於研磨墊之方法亦無特別限制,例如可採用泵等連續供給之方法。其供給量並無限制,但較佳隨時以本發明之研磨用組成物覆蓋研磨墊表面。
研磨結束後,在水流中洗淨基板,以旋轉乾燥機等甩掉附著於基板上之水滴予以乾燥,而獲得具有含IV族材料之層之基板。
使用以下實施例及比較例更詳細說明本發明。但,本發明之技術範圍並非僅限制於以下實施例。
在水中攪拌混合(混合溫度:約25℃,混合時間:約10分鐘)如表2所示之研磨粒、及次氯酸鈉水溶液(濃度:5.9質量%),調製實施例1~48及比較例1~7之研磨用組成物。研磨用組成物之pH係添加氫氧化鉀
(KOH)而調整,且以pH計確認為9.5。
又,表2所示研磨粒之種類係如下述表1,全部為以溶膠凝膠法合成者。
表2中之「NaClO(5.9質量%)添加量」之欄係表示研磨用組成物之製造時添加多少的NaClO(5.9質量%)水溶液者,「氧化劑濃度(B)」之欄係表示製作之研磨用組成物中含有多少氧化劑(NaClO)者。
實施例31係相對於組成物之總質量進而添加0.13質量%之2-吡咯啶酮,實施例32係相對於組成物之總質量進而添加0.39質量%之2-吡咯啶酮,實施例33係相對於組成物之總質量進而添加0.65質量%之2-吡咯啶酮。
實施例16、比較例2及比較例5之研磨粒係使用於
表面固定化有磺酸之膠體二氧化矽。
研磨用組成物中之研磨粒所具有之矽醇基數之總和(A)係利用以下之測定方法或計算方法,測定或算出各參數後,以下述方法算出。
.研磨粒之一次粒徑[nm](實測值):以由BET法計算出之比表面積(SA)為基準,假設研磨粒為真球,使用SA=4πR2之公式算出研磨粒之直徑(一次粒徑)
.每1個研磨粒之體積(計算值):使用由比表面積(SA)算出之一次粒徑,由下式計算
每1個研磨粒之體積=4/3π×(研磨粒之一次粒徑/2)3
.每1個研磨粒之重量(計算值):使用以計算求出之每1個研磨粒之體積,由下式計算
每1個研磨粒之重量=每1個研磨粒之體積×研磨粒之比重(膠體二氧化矽時為2.2)
.每1個研磨粒之表面積(計算值):使用由比表面積(SA)算出之一次粒徑,由下式計算
每1個研磨粒之表面積=4π×(研磨粒之一次粒徑/2)2
.研磨用組成物中之研磨粒之個數(計算值):研磨用組成物中之研磨粒濃度除以每1個研磨粒之重量而計算
.研磨用組成物中之研磨粒之總表面積[nm2](計算值):藉由每1個研磨粒之表面積與研磨用組成物中之研磨粒個數之乘積算出
.矽醇基數(實測值):算出以Sears法求出之每單位表面積之矽醇基數[矽醇基數/nm2]
Sears法係參照G.W.Sears,Jr.,”Determination of Specific Surface Area of colloidal Silica by Titration with Sodium Hydroxide”,Analytical Chemistry,28(12),1981(1956)進行。測定係使用二氧化矽水溶液(1wt%),滴加之NaOH之每一次滴加量為0.01ml,滴加間隔為30秒。
.研磨用組成物中之研磨粒具有之矽醇基數之總和(個)(A)(計算值):藉由Sears法求出之矽醇基數(實測值)[個/nm]與使用BET比表面積與研磨用組成物中之研磨粒濃度所計算之研磨用組成物中之研磨粒之總表面積[nm2](計算值)之乘積而計算。
.氧化劑濃度(B)(實測值):使用氧化劑濃度已知之藥劑時,係由添加之量計算。或者以氧化還原滴定進行定量。例如,NaClO之情況,係使用平成15年9月29日日本厚生勞動省公告第318號之方法以滴定進行定量。
.氧化劑每1質量%之研磨粒之矽醇基數(計算值):研磨用組成物中之研磨粒所具有之矽醇基數之總和(個)(A)(計算值)除以氧化劑濃度(B)而算出。
殘留之氧化劑之比例為保管前之研磨用組成物、與在25℃下保管7天後之研磨用組成物,使用平成15年9月29日日本厚生勞動省公告第318號之方法分別測定氧化劑之含量,且以下述式算出。
殘留之氧化劑之比例(%)=(保管後之研磨用組成物中之氧化劑之量)/(保管前之研磨用組成物中之氧化劑之量)×100
針對實施例39~48所得之研磨用組成物,以浸漬條件:在43℃下浸漬3cm×3cm之Ge基板5分鐘(邊使攪拌子以300rpm旋轉),由隨後之重量變化算出溶解量,且將其溶解量除以浸漬時間,測定Ge基板之蝕刻速度。
實施例及比較例之研磨用組成物之組成,以及研磨用組成物之保管安定性及Ge蝕刻速度之測定結果示於下述表2。
如表2所示可知,(A)/(B)落於特定範圍之實施例1~48之本發明之研磨用組成物相較於比較例之研磨用組成物,保管安定性較優異。此外,可知添加安定性提升劑時,可進一步提高保管安定性。
又,本申請案係基於2013年9月30日提出申請之日本專利申請案第2013-204170號,其揭示內容藉由參考以全體引用。
Claims (5)
- 一種研磨用組成物,其包含研磨粒與含鹵原子之氧化劑,研磨用組成物中之前述研磨粒所具有之矽醇基數之總和(A)(單位:個)除以研磨用組成物中之前述氧化劑之濃度(B)(單位:質量%)之值(A/B)為8×1023以下。
- 如請求項1之研磨用組成物,其係使用於研磨具有含IV族材料之層的研磨對象物之用途。
- 如請求項1或2之研磨用組成物,其中前述氧化劑之濃度為0.0001質量%以上且未達0.5質量%。
- 一種研磨方法,其係以如請求項1~3中任一項之研磨用組成物研磨具有含IV族材料之層的研磨對象物。
- 一種基板之製造方法,其包含以如請求項4之研磨方法研磨具有含IV族材料之層的研磨對象物之步驟。
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CN108117839B (zh) * | 2016-11-29 | 2021-09-17 | 安集微电子科技(上海)股份有限公司 | 一种具有高氮化硅选择性的化学机械抛光液 |
JP6811089B2 (ja) * | 2016-12-26 | 2021-01-13 | 花王株式会社 | シリコンウェーハ用研磨液組成物 |
EP3775076A4 (en) * | 2018-03-28 | 2021-12-22 | FUJIFILM Electronic Materials U.S.A, Inc. | CHEMICAL-MECHANICAL POLISHING SUSPENSION WITH RUTHENIUM BARRIER |
US10995238B2 (en) * | 2018-07-03 | 2021-05-04 | Rohm And Haas Electronic Materials Cmp Holdings | Neutral to alkaline chemical mechanical polishing compositions and methods for tungsten |
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US6290736B1 (en) * | 1999-02-09 | 2001-09-18 | Sharp Laboratories Of America, Inc. | Chemically active slurry for the polishing of noble metals and method for same |
US6299795B1 (en) * | 2000-01-18 | 2001-10-09 | Praxair S.T. Technology, Inc. | Polishing slurry |
US6332831B1 (en) * | 2000-04-06 | 2001-12-25 | Fujimi America Inc. | Polishing composition and method for producing a memory hard disk |
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US20070037892A1 (en) * | 2004-09-08 | 2007-02-15 | Irina Belov | Aqueous slurry containing metallate-modified silica particles |
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JP2015067752A (ja) | 2015-04-13 |
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US20160215170A1 (en) | 2016-07-28 |
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