TWI593792B - 研磨用組成物及使用其之研磨方法及基板之製造方法 - Google Patents
研磨用組成物及使用其之研磨方法及基板之製造方法 Download PDFInfo
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- TWI593792B TWI593792B TW101144482A TW101144482A TWI593792B TW I593792 B TWI593792 B TW I593792B TW 101144482 A TW101144482 A TW 101144482A TW 101144482 A TW101144482 A TW 101144482A TW I593792 B TWI593792 B TW I593792B
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- Prior art keywords
- polishing
- polishing composition
- particles
- cerium oxide
- protrusions
- Prior art date
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Description
本發明係有關一種含有在表面上具複數個突起之砥粒的研磨用組成物。而且,本發明係有關使用該研磨用組成物之研磨方法及基板之製造方法。
使用非球形粒子作為研磨用組成物之砥粒,係有效地作為藉由研磨用組成物以提高研磨速度之手段。例如日本特開2007-153732號公報(專利文獻1)中揭示,於矽晶圓之鏡面研磨時使用在表面上具有多數小突起的膠體二氧化矽粒子。另外,於日本特開2009-149493號公報(專利文獻2)中揭示,使用含有在表面上具有短徑/長徑比為0.01~0.8範圍的複數個疣狀突起的二氧化矽粒子之二氧化矽溶膠作為砥粒之研磨用組成物。
[專利文獻1]日本特開2007-153732號公報
[專利文獻2]日本特開2009-149493號公報
本發明之發明人等重複進行實驗有關含有在表面上具有複數個突起之砥粒的研磨用組成物之結果,發現藉由該
研磨用組成物之親水性研磨對象物的研磨速度受到研磨用組成物中所含的有機鹼的影響很大。本發明係以本發明人之新穎見解為基準者,其目的係提供可以更高的研磨速度進行研磨親水性研磨對象物之研磨用組成物,以及提供使用該研磨用組成物之研磨方法及基板之製造方法。
為達成上述目的時,本發明之第1形態係提供一種研磨用組成物,其係為使親水性研磨對象物之表面進行研磨時之研磨用組成物,其特徵為含有在表面上具有複數個突起之砥粒,且前述砥粒中直徑較砥粒之體積基準平均粒子直徑更大的砥粒,藉由以表面上具有的突起之高度除以各相同突起的基部之寬度所得的值之平均值為0.170以上,前述砥粒中粒子直徑較砥粒之體積基準平均粒子直徑更大的砥粒在表面上具有的突起之平均高度為3.5nm以上,研磨用組成物中所含的有機鹼之量,以研磨用組成物中之前述砥粒1kg為基準時為100 mmol以下。
於上述形態中,研磨用組成物之pH值以在有機鹼之酸解離定數pKa之值±2的範圍內較佳。
於上述形態中,前述砥粒可為膠體二氧化矽。此時,該膠體二氧化矽中所含的金屬雜質之量為1質量ppm以下較佳。
本發明之第2形態係提供一種研磨方法,其特徵為使用上述第1形態之研磨用組成物,使具有40度以下之水接觸角的研磨對象物之表面(例如金屬氧化物膜)進行研磨。
本發明之第3形態係提供一種基板之製造方法,其特徵為使用上述第1形態之研磨用組成物,藉由研磨具有40度以下之水接觸角的研磨對象物之表面,製造基板。
藉由本發明,可提供一種可以高研磨速度進行研磨親水性研磨對象物之研磨用組成物,與使用該研磨用組成物之研磨方法及基板之製造方法。
於下述中,說明本發明之一實施形態。
本實施形態之研磨用組成物,係於研磨親水性研磨對象物表面之用途時使用。更具體而言,使用於研磨形成於矽晶圓或化合物半導體晶圓等之半導體晶圓上之金屬氧化物膜的用途,特別是研磨形成於矽晶圓上之氧化矽膜的用途。氧化矽膜係由矽之單一氧化物或複合氧化物所形成的膜,其具體例如TEOS(tetraethyl orthosilicate)膜、BPSG(borophosphosilicate glass)膜、PSG(phosphosilicate glass)膜、SOG(spin on glass)膜、熱氧化膜。惟金屬氧化物膜不受限於氧化矽膜,其他的金屬氧化物膜之例如鋁、鋯、鈦、錫、鋅、銻、銦、鎂、硼、鈮等金屬之單一氧化物或複合氧化物所形成的膜。另外,金屬氧化物膜可為由如以銻摻雜氧化錫(ATO)、氟摻雜氧化錫、磷摻雜氧化錫、錫摻雜氧化銦(ITO)、或氟摻雜氧化銦之摻雜
物修飾的金屬氧化物所形成者。研磨對象物之親水性的程度,可藉由水接觸角表示,本實施形態之研磨用組成物,特別是使用於研磨具有40度以下之水接觸角的研磨對象物的表面之用途,進一步而言使用於研磨該研磨對象物以製造基板的用途。水接觸角之測定,一般而言以θ/2法進行,例如可使用協和界面科學股份有限公司製之晶圓洗淨處理評估裝置“CA-X200”進行。
本實施形態之研磨用組成物,係至少含有在表面上具有複數個突起之砥粒。使用該異形砥粒與使用非異形(即球形)之砥粒相比時,可有利地藉由研磨用組成物來提高研磨速度。
研磨用組成物中之砥粒,例如由金屬氧化物、鑽石、碳化矽、氮化矽或氮化硼所形成的粒子,惟不受此等所限制。金屬氧化物粒子之具體例,如二氧化矽、氧化鋁、氧化鋯、氧化鈰、氧化鈦或氧化鎂所形成的粒子。其中,以二氧化矽粒子較佳,更佳者為膠體二氧化矽。
研磨用組成物中之砥粒在表面上具有的突起數,係以每一砥粒中平均為3個以上較佳,更佳者為5個以上。
此處所指的突起,與砥粒之粒子相比時,具有充分小值的高度及寬度。換言之,於第1圖中表示通過點A及點B之曲線AB的部分之長度,係不會超過砥粒之最大內接圓的圓周長(更正確而言,內接於投影砥粒之外形的輪廓之最大圓的圓周長)之1/4的突起。而且,突起之寬度係指突起之基部的寬度,於第1圖中以點A與點B間的距離
表示。另外,突起之高度係指突起之基部與自其基部最遠的突起之部位間的距離。於第1圖中以垂直於直線AB的線份CD之長度表示。
研磨用組成物之砥粒中直徑較砥粒之體積基準平均粒子直徑更大的砥粒,藉由以表面上具有的突起之高度除以各相同突起的基部之寬度所得的值之平均值必須為0.170以上,較佳者為0.245以上,更佳者為0.255以上。隨著該平均值變大,突起之形狀變得較為尖銳的理由,係因藉由研磨用組成物而提高研磨速度之故。而且,砥粒之各突起的高度及其基部之寬度,係使用一般的影像解析軟體,藉由掃描型電子顯微鏡解析砥粒的影像予以求取。
研磨用組成物之砥粒中直徑較砥粒之體積基準平均粒子直徑更大的砥粒,在表面上具有的突起之高度的平均值必須為3.5nm以上,較佳者為4.0nm以上。伴隨該突起之平均高度變大,提高藉由研磨用組成物之研磨速度。
研磨用組成物中砥粒之體積基準平均粒子直徑,以10~300nm較佳。砥粒之體積基準平均粒子直徑在上述範圍內時,除可提高研磨用組成物之沉澱安定性外,使用研磨用組成物進行研磨後之研磨對象物的表面粗糙度容易變小。砥粒之體積基準平均粒子直徑,與直至達到研磨用組成物中全部砥粒之累積體積的50%為止,自藉由動態光繞射法之粒子直徑的小砥粒順序累積砥粒之體積時,最後所累積的砥粒之粒子直徑相等。
研磨用組成物中砥粒之體積基準95%粒子直徑(D95
值),以500nm以下較佳,更佳者為400nm以下。伴隨砥粒之體積基準95%粒子直徑變小,除可提高研磨用組成物之沉澱安定性外,容易使使用研磨用組成物進行研磨後之研磨對象物的表面粗糙度變小。砥粒之體積基準95%粒子直徑,與直至達到研磨用組成物中全部砥粒之累積體積的95%為止,自藉由動態光繞射法之粒子直徑的小砥粒順序累積砥粒之體積時最後所累積的砥粒之粒子直徑相等。
研磨用組成物中之砥粒,以鈉、鉀、鈣、硼、鋁、鈦、鋯、錳、鐵、鈷、銅、鋅、銀、鉛等之金屬雜質的含量,以1質量ppm以下較佳。金屬雜質之含量,例如可藉由ICP質量分析裝置測定。
在表面上具有複數個突起之膠體二氧化矽砥粒,例如可以下述方法製造。換言之,首先藉由加入有作為觸媒之銨水的甲醇與水之混合溶液中連續添加烷氧基矽烷進行水解,製得含有膠體二氧化矽粒子之漿料。使所得的漿料加熱,餾去甲醇及銨。然後,藉由將作為觸媒之有機鹼加入漿料後,再度於70℃以上之溫度下連續添加烷氧基矽烷進行水解,在膠體二氧化矽粒子之表面上形成複數個突起。此處可使用的有機鹼之具體例,如三乙醇胺等之胺化合物、或氫氧化四甲銨等之四級銨化合物。藉由該方法,可容易製得金屬雜質之含量為1質量ppm以下的膠體二氧化矽砥粒。
而且,藉由烷氧基矽烷水解以製造膠體二氧化矽之一般方法,例如記載於作花濟夫所著的「溶膠-凝膠法之科
學」之第154~156頁。而且,於日本特開平11-60232號公報中揭示,藉由將矽酸甲酯或矽酸甲酯與甲醇之混合物滴入水、甲醇及銨或銨與銨鹽所形成的混合溶劑中,使矽酸甲酯與水反應所製造的繭型膠體二氧化矽。於日本特開2001-48520號公報中揭示,藉由使甲矽酸烷酯以酸觸媒予以水解後,加入鹼觸媒進行加熱,且進行矽酸之聚合予以粒子成長所製造的細長形狀膠體二氧化矽。於日本特開2007-153732號公報中記載,藉由使用特定量之特定種類的水解觸媒,可以易水解性有機基矽酸酯作為原料,製造具有多數小突起之膠體二氧化矽。於日本特開2002-338232號公報中記載,藉由在單分散的膠體二氧化矽中添加凝聚劑,予以二次凝聚成球狀。日本特開平07-118008號公報及國際公開第2007/018069號公報中揭示,為製得細長等異形的膠體二氧化矽時,在由矽酸鈉所得的活性矽酸中添加鈣鹽或鎂鹽。於日本特開2001-11433號公報中揭示,藉由在由矽酸鈉所得的活性矽酸中添加鈣鹽,製得數珠狀膠體二氧化矽。於日本特開2008-169102號公報中記載,藉由在種子粒子表面上生成微小粒子或予以成長,可製造如糖球之具有多數小突起的膠體二氧化矽。在表面上具有複數個突起之膠體二氧化矽砥粒,亦可藉由單獨使用此等文獻所記載的方法或組合予以製造。
本實施形態之研磨用組成物中,於製造砥粒時無法避免混入作為觸媒所使用的有機鹼。另外,亦可在研磨用組成物中添加有機鹼。然而,研磨用組成物中所含的有機鹼
之量,皆必須在每1kg研磨用組成物之砥粒中為100 mmol以下。其理由係因研磨用組成物會大為降低研磨速度。特別是具有pH值接近有機鹼之酸解離定數pKa值的研磨用組成物時,研磨速度顯著降低。此外,因有機鹼而引起研磨速度降低的理由,係推測在研磨用組成物中解離的有機鹼吸附於親水性研磨對象物之表面、更具體而言吸附於金屬氧化物膜的表面之故。如矽基板之疏水性研磨對象物時,推測不會有因有機鹼而降低研磨速度的情形。
另外,研磨用組成物中有機鹼的含量限制於上述範圍時,研磨用組成物之pH值接近有機鹼之pKa時、更具體而言具有pH值為有機鹼的pKa值±2的研磨用組成物時,可有效地抑制研磨速度降低情形。該推測以具有pH值接近有機鹼之酸解離定數pKa值之研磨用組成物時,親水性研磨對象物之研磨速度顯著降低的本發明人之新穎見解為基準所得者。例如,研磨用組成物中所含的有機鹼為三乙醇胺時,由於三乙醇胺的pKa值為7.6,故研磨用組成物之pH值為5.6~9.6之範圍時特別有效。而且,研磨用組成物中所含的有機鹼為氫氧化四甲銨時,由於氫氧化四甲銨的pKa值為9.8,故研磨用組成物之pH值為7.8~11.8之範圍時特別有效。
而且,研磨用組成物中有機鹼之含量,為使藉由研磨用組成物更為提高親水性研磨對象物之研磨速度,在每1kg研磨用組成物之砥粒中為50 mmol以下較佳。研磨用組成物中之有機鹼的含量,可以毛細管電泳法(CE)或毛
細管電泳-質量分析法(CE-MS)進行測定。
藉由本實施形態,可得下述之作用效果。
本實施形態之研磨用組成物中所含的砥粒中直徑較砥粒之體積基準平均粒子直徑更大的砥粒,藉由以表面上具有的突起之高度除以各相同突起的基部之寬度所得的值之平均值為0.170以上。而且,研磨用組成物之砥粒中直徑較砥粒之體積基準平均粒子直徑更大的砥粒,在表面上具有的突起之高度為3.5nm以上。總之,研磨用組成物之砥粒中機械研磨作用特高的大粒子直徑之砥粒,具有較長且尖銳的形狀之突起。因此,本實施形態之研磨用組成物,可以高研磨速度研磨研磨對象物。
此外,本實施形態之研磨用組成物中所含的有機鹼之量,係每1kg研磨用組成物之砥粒中為100 mmol%。有機鹼吸附於親水性研磨對象物之表面時,因研磨用組成物而阻害研磨對象物之研磨,故藉由限制該研磨用組成物中之有機鹼的含量,可有效地抑制降低有機鹼之研磨速度的原因。
而且,本實施形態之研磨用組成物可使用於研磨親水性研磨對象物之表面的用途,更具體而言可使用於研磨金屬氧化物膜之用途。
前述實施形態亦可作下述之變更。
.前述實施形態之研磨用組成物,視其所需亦可進一步含有周知的添加劑。例如,可含有(a)鹼金屬之氫氧化物、鹼金屬鹽、銨、銨鹽等之無機鹼,(b)鹽酸、磷
酸、硫酸、膦酸、硝酸、次膦酸、硼酸等之無機酸、或醋酸、衣康酸、琥珀酸、酒石酸、檸檬酸、馬來酸、乙二醇酸、丙二酸、甲烷磺酸、甲酸、蘋果酸、三甲基乙酸、甘胺酸、谷胺酸、乳酸、氫氧亞乙基二磷酸(hydroxyethylidene diphosphonic acid(HEDP))、次胺基[亞甲基膦酸](nitrilotris[methylene phosphonic acid](NTMP))、膦醯基丁烷三羧酸(phosphonobutane tricarboxylic acid(PBTC))等之有機酸,(c)非離子性、陰離子性、陽離子性或兩性界面活性劑,(d)水溶性纖維素、乙烯基系聚合物、聚氧化亞烷基等之水溶性聚合物,(e)聚胺、聚膦酸、聚胺基羧酸、聚胺基膦酸等之螯合劑,(f)過氧化氫、過氧化物、過氧酸、酸性金屬鹽化合物等之氧化劑,(g)防黴劑、殺菌劑、殺生物劑等之其他添加劑中之任何一種。
.前述實施形態之研磨用組成物,亦可藉由以水稀釋研磨用組成物之原液予以調製。
.前述實施形態之研磨用組成物,亦可使用於除研磨親水性研磨對象物以外之用途。
其次,說明本發明之實施例及比較例。
藉由混合膠體二氧化矽砥粒與純水,調製膠體二氧化矽砥粒之含量為10.0質量%之研磨用組成物。所使用的膠體二氧化矽砥粒係如第2(a)圖所示以掃描型電子顯微鏡照片可見的在表面上具有複數個突起。膠體二氧化矽砥粒中粒子直徑較砥粒體積基準平均粒子直徑更大的膠體二氧化矽砥粒,在表面上具有的突起之高度平均值為4.25nm。膠體二氧化矽砥粒中粒子直徑較砥粒之體積基準平均粒子直徑更大的膠體二氧化矽砥粒,藉由以表面上具有的突起之高度除以各相同突起的基部之寬度所得的值之平均值為0.310以上。膠體二氧化矽砥粒之體積基準平均粒子直徑為85nm。膠體二氧化矽砥粒之體積基準95%粒子直徑為116nm。膠體二氧化矽砥粒中之金屬雜質的含量未達1ppm。測定所得的研磨用組成物之pH值時,其值為7.0。另外,研磨用組成物中,無法避免混入有製造膠體二氧化矽砥粒時作為觸媒所使用的三乙醇胺,測定其含量時,在每1kg研磨用組成物中之膠體二氧化矽砥粒中為5 mmol。
在實施例1之研磨用組成物中添加三乙醇胺,使研磨用組成物中所含的有機鹼之量在每1kg研磨用組成物中之膠體二氧化矽砥粒中增加至50 mmol。添加三乙醇胺後,測定研磨用組成物之pH值,其值為8.5。
藉由混合膠體二氧化矽砥粒與純水,調製膠體二氧化矽砥粒之含量為10.0質量%之研磨用組成物。所使用的膠體二氧化矽砥粒係如第2(b)圖所示以掃描型電子顯微鏡照片可見在表面上不具突起。膠體二氧化矽砥粒之體積基準平均粒子直徑為131nm。膠體二氧化矽砥粒之體積基準95%粒子直徑為212nm。膠體二氧化矽砥粒中之金屬雜質的含量未達1ppm。測定所得的研磨用組成物之pH值時,其值為7.5。另外,該研磨用組成物中不含可檢測水平的有機鹼。
在實施例1之研磨用組成物中添加三乙醇胺,使研磨用組成物中所含的有機鹼之量在每1kg研磨用組成物中之膠體二氧化矽砥粒中增加至140 mmol。添加三乙醇胺後,測定研磨用組成物之pH值,其值為8.9。
在實施例1之研磨用組成物中添加氫氧化四甲銨,使研磨用組成物中所含的有機鹼之量在每1kg研磨用組成物中之膠體二氧化矽砥粒中增加至140 mmol。添加三乙醇胺後,測定研磨用組成物之pH值,其值為9.7。
藉由添加乳酸或氫氧化鉀以調整pH值,自實施例1,2及比較例1~3之各研磨用組成物調製pH值3.0、pH值
7.0及pH值11.0之研磨用組成物。各使用所得的研磨用組成物,以表1記載的條件研磨在表面上具有氧化矽膜之矽晶圓,具體而言直徑50.8mm之PE-TEOS(plasma-enhanced tetraethyl orthosilicate)包覆層晶圓之表面。此時,以下述計算式為基準所求得的研磨速度之值如表2及第3(a)、(b)圖所示。
研磨速度[Å/min]=研磨前後之晶圓重量差[g]/研磨時間[分]/晶圓表面之面積[cm2](20.26cm2)/TEOS膜之真密度[g/cm3](=2.2g/cm3)×108
如表2及第3(a)圖所示,使用實施例1,2之研磨用組成物時,與使用在砥粒表面上沒有突起的比較例1之研磨用組成物相比時,與pH值無關,可得高研磨速度。而且,與使用在每1kg膠體二氧化矽砥粒中三乙醇胺之含量超過100 mmol之比較例2的研磨用組成物相比時,與pH值無關,可得高研磨速度。
另外,如表2及第3(b)圖所示,使用實施例1,2之研磨用組成物,與使用在每1kg膠體二氧化矽砥粒中氫氧化四甲銨之含量超過100 mmol之比較例3的研磨用組成物相比時,至少pH值為11.0時,可得高研磨速度。
[第1圖]係表示使本發明一實施形態之研磨用組成物中所含的砥粒之外形投影的輪廓圖。
[第2圖](a)係表示實施例1,2及比較例2,3之研磨用組成物中使用的膠體二氧化矽砥粒之掃描型電子顯微鏡照片,(b)係表示比較例1之研磨用組成物中使用的膠體二氧化矽砥粒之掃描型電子顯微鏡照片。
[第3圖](a)及(b)係表示使用實施例1,2及比較例1~3之研磨用組成物,使氧化矽膜進行研磨時之研磨速度與pH值的關係圖。
Claims (5)
- 一種研磨用組成物,其係為使親水性研磨對象物之表面進行研磨時之研磨用組成物,其特徵為含有在表面上具有複數個突起之砥粒,且前述砥粒中直徑較砥粒體積基準平均粒子直徑更大的砥粒,藉由以表面上具有的突起之高度除以各相同突起的基部之寬度所得的值之平均值為0.170以上,前述砥粒中粒子直徑較砥粒之體積基準平均粒子直徑更大的砥粒在表面上具有的突起之平均高度為3.5nm以上,研磨用組成物中所含的有機鹼之量,以研磨用組成物中之前述砥粒1kg為基準時為100mmol以下,研磨用組成物之pH值在前述有機鹼之酸解離定數pKa之值±2的範圍內。
- 如申請專利範圍第1項之研磨用組成物,其中前述砥粒為膠體二氧化矽,該膠體二氧化矽中所含的金屬雜質之量為1質量ppm以下。
- 一種研磨方法,其特徵為使用如申請專利範圍第1或2項之研磨用組成物,使具有40度以下之水接觸角的研磨對象物之表面進行研磨。
- 如申請專利範圍第3項之研磨方法,其中前述研磨對象物為金屬氧化物膜。
- 一種基板之製造方法,其特徵為使用如申請專利範圍第1或2項之研磨用組成物,藉由研磨具有40度以下 之水接觸角的研磨對象物之表面,製造基板。
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