200813204 九、發明說明 【發明所屬之技術領域】 本發明係有關以氧化鈽做爲砥材使用之 物及其製造方法。 本申請係依2006年7月13日，日本 2006- 1 92899號爲基準優先權之主張，將其 【先前技術】 近年來，電腦相關技術的進步極爲醒目 年進展高積體化，磁碟之記憶容量亦鑽硏增 支撐此基本技術之一者如：以微細元件、配 對象之硏磨加工例。 如：LSI裝置之製造步驟中，以使伴隨 細化之微影步驟下之焦點深度問題的減輕化 導入以層間絕緣膜爲對象之硏磨技術，進行 爲形成微細配線之埋入金屬硏磨（波 damascene)，爲實現於狹窄面積由先行技多 區間砂氧化，Local Oxidation of Silicon) 淺切割分離法（Shallow Trench Isolation) LSI裝置之製造中不可或缺之重要技術者， 工技術之應用。 層間絕緣膜硏磨、淺切割分離法中，主 溶液中懸浮以氣相法取得之二氧化矽微粉末 硏磨材料組成 所申請之特願 內容應用於此 ，LSI裝置年 大一途。做爲 線構造爲硏磨 設計規則之微 爲主要目的， 實用化。又， 形花紋法， Ϊ 之 LOCOS ( 法分離元件之 等，做爲二代 被推薦硏磨加 要討論鹼性水 之漿料，於水 -5- 200813204 中懸浮氧化鈽粉末之漿料。另外，金屬硏磨中 水中懸浮以氣相法取得之二氧化矽粉末或氧化 加硝酸鐵、過氧化氫等氧化劑之漿料。 此LSI裝置領域中，當然被要求高精密度 而且硏磨加工中期待降低缺陷、高能率化、穩 ，爲於硏磨加工露出高精密度面，務必使硏磨 次微粒程度進行微細化\而硏磨材料粒子愈小 愈遲緩。亦即，面精密度與硏磨速度有著協調 不易兼倂。故於上述LSI裝置硏磨用之硏磨材 ，仍未能取得完全滿足缺陷小、面積密度、硏 磨速度之穩定性等之水準。 其中，最理想之實用化層間絕緣膜之硏磨 高度面精密度，而使用二氧化矽微粉末之鹼性 硏磨速度緩慢不盡理想。又，此層間絕緣膜之 換頂多1 # m，因此硏磨時間多半爲數分鐘之 硏磨速度由硏磨開始漸次增大，經過一定時間 分鐘以上）後’具有穩定化之傾向。因此，此 之硏磨中，開始之硏磨時間於不穩定領域下結 此於終點檢出明顯加重負擔。 對於此，氧化鈽漿料於層間絕緣膜硏磨、 法中意味著利於容易取得更高度硏磨速度與高 於淺切割分離法時，於做爲硏磨對象之二氧化 相較於此二氧化矽膜配合硏磨速度遲緩之氮化 ，氮化矽膜較可做爲抑制器功能。此時，以氮 仍主要討論 鋁粉末，添 之加工面， 定化等。惟 材料粒子以 其硏磨速度 關係，因此 料組成物中 磨速度、硏 中，爲取得 漿料，惟其 硏磨中，更 程度。一般 (通常爲數 層間絕緣膜 束硏磨，因 淺切割分離 精密度。更 矽膜之下， 矽膜，因此 化矽膜之硏 -6-BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a material which is used as a coffin and a method for producing the same. This application is based on the claim of July 13, 2006, Japan 2006- 1 92899 as the benchmark priority, and its [prior art] In recent years, the progress of computer-related technology has been remarkable and the progress has been high. The memory capacity is also one of the basic techniques for supporting such a basic technique: a honing processing example of a fine component and a matching object. For example, in the manufacturing process of the LSI device, the immersion technique for the interlayer insulating film is introduced to reduce the depth of focus problem in the lithography step with the refinement, and the buried metal honing for forming the fine wiring is performed ( Wave damascene), in order to achieve a narrow area by prior art sand oxidation, Local Oxidation of Silicon) Shallow Trench Isolation is an indispensable technology in the manufacture of LSI devices, the application of engineering technology. In the interlayer insulating film honing and shallow-cutting separation method, the composition of the cerium oxide micropowder honing material obtained by suspending the gas phase method in the main solution is applied to this, and the LSI device is one of the best in the year. As a line structure, the design rule is the main purpose and practical. In addition, the pattern method, LO LOCOS (method separation element, etc., as the second generation is recommended to honing plus to discuss the alkaline water slurry, suspending the cerium oxide powder slurry in water -5 - 200813204. A slurry of cerium oxide powder obtained by gas phase method in a metal honing water or an oxidizing agent such as iron nitrate or hydrogen peroxide. In the field of LSI devices, high precision is required, and honing processing is expected. Reduce the defects, high energy rate, and stability. In order to expose the high-precision surface in the honing process, it is necessary to make the honing of the secondary particles to be finer and the honing material particles are smaller and slower. That is, the surface precision and honing The speed is not easy to co-ordinate. Therefore, the honing material used for honing the above LSI device has not yet achieved the level of completely satisfying the defects, the area density, and the stability of the honing speed. Among them, the most practical practical layer The honing of the insulating film is highly precise, and the alkaline honing speed using the cerium oxide micropowder is not satisfactory. Moreover, the interlayer insulating film is more than 1 # m, so the honing time is mostly a few points. The mill speed begins WH WH progressively increase from the grinding, after a certain time or more minutes) after 'having a tendency of stabilization. Therefore, in this honing, the initial honing time is in the unstable field, and the end point detection obviously increases the burden. For this reason, the cerium oxide slurry is honed in the interlayer insulating film, and the method means that it is easy to obtain a higher honing speed than when the shallow cutting separation method is used, and the oxidizing phase which is the object of honing is compared with the oxidizing phase. The ruthenium film is combined with the nitriding speed of the honing, and the tantalum nitride film can be used as a suppressor function. At this time, the aluminum powder is still mainly discussed as the aluminum powder, the processing surface, the definition, and the like. However, the material particles are related to the honing speed, so the grinding speed and enthalpy in the material composition are obtained in order to obtain the slurry, but in the honing, to a greater extent. In general (usually a plurality of interlayer insulating film bundle honing, the precision is separated by shallow cutting. Under the ruthenium film, the ruthenium film, thus the ruthenium film -6-
200813204 磨速度除以二氧化矽膜之硏磨進度後之値（稱爲 被要求爲高値者，而此點中對於二氧化矽膜而1 高度硏磨速度之氧化鈽漿料。 另外，使用氧化鈽漿料時，以刮傷爲始之I 成問題點（如：專利文獻1、2 )。爲迴避此.問是 文獻1中被揭示有於氧化鈽粒子中其二次粒徑I 上之粒子含率爲1 %以下之含氧化鈽，分散劑及 硏磨劑。其中二次粒徑係指CMP硏磨劑中之| 之粒徑之意，做爲該測定方法者如：光子相關名 ，光子相關法係可於極稀薄之粒子濃度中進行i 際之使用濃度完全背離之條件下測定之方法。 又，於專利文獻2中被揭示含有，使一次| 値爲 30〜2 50nm、粒徑中央値爲 150〜600nm，tl 7〜45m2/g之氧化鈽粒子分散於媒體之漿料其平 2OOnm以上40 0nm以下，使粒度分佈之半値寬 以下之氧化鈽粒子分散於媒體之漿料的氧化鈽 ，此專利文獻2中，雖記載半値寬度，卻未詳 義之說明。 〔專利文獻1〕特開2003-1 71 653號公報 〔專利文獻2〕特開200 1 -3 2925 1號公報 近年來，伴隨裝置之設計規則之微細化， CMP硏磨面之高度的平坦性、均勻性、或各種舍 曰益嚴格。特別有關缺陷面，伴隨檢出感度之| 烈要求稱爲抑制刮傷之無大損傷、微細刮傷、i 選擇比） 利於取得 :陷時常造 ί，於專利 ^ 3 ν m 以 水之 CMP ，化鈽粒子 :之例。惟 丨定，由實 【徑之中央 t表面積爲 均粒徑爲 [爲 3 0Onm f磨劑。惟 &包含其定 要求進行 陷的低減 昇，被強 面粒子、 200813204 埋沒粒子、無割裂、殘餘漿料、污染等各種缺陷之整體低 減。 惟，即使使用此先行技術之氧化鈽製造LSI裝置硏磨 用之硏磨材料組成物，仍無法取得可整體上減少各種缺陷 ，高精度且穩定之硏磨面。 【發明內容】 因此，本發明係鑑於上述情況，被提案者，以提供一 種可防止混入雜質，且於硏磨加工中以高效率取得無缺陷 之高精密度之硏磨材料組成物及其製造方法者爲目的。本 發明特別以提供一種於LSI裝置之製造步驟中，使二氧化 矽膜、氮化矽膜、有機膜等之絕緣膜進行硏磨加工時，可 兼具整體性缺陷少、面精密度與硏磨速度，同時達成高於 現況水準之硏磨速度之穩定化，另外，可以利於工業方法 實現之LSI裝置硏磨用之硏磨材料組成物及其製造方法爲 目的。 本發明者爲解決上述課題，進行精密硏討結果發現’ 提供以下之硏磨材料組成物及其製造方法後，可輕易進行 解決該課題。 (1 )至少含有水及氧化鈽粒子之硏磨材料組成物， 該氧化鈽之粒度分佈以其製品粒子濃度所測定之粒子體積 基準平均圓相當粒徑爲1 // m以下，且圓相當粒徑之低於 0.2 # m粒子之體積分率爲0.01〜10%範圍之硏磨材料組成 物0 -8 - 200813204 (2 )該氧化鈽之粒度分佈之該圓相當粒徑超出1 /z m 粒子之個數分率爲〇〜5 %範圍之上述（1 )所載之硏磨材料 組成物。 (3) 該氧化鈽二次粒子之圓形度爲0.8〜0.97之上述 (1 )或（2 )所載之硏磨材料組成物。 (4) 該氧化鈽濃度爲0.01〜10質量％之上述1〜3項中 任一項之硏磨材料組成物。 (5 )製品粒子濃度作爲硏磨材料組成物中之氧化鈽 濃度爲1質量％之上述（1 )或（2 )所載之硏磨材料組成 物。 (6)於LSI裝置製造步驟之絕緣膜硏磨中使用上述 (1 )〜（5 )中任一項之硏磨材料組成物之LSI裝置之製 造方法。 (7 )上述（1 )〜（5 )中任一項之硏磨材料組成物之 製造方法，其係使氧化鈽之粉體以粒子濃度於0.1〜10容 積％範圍下進行濕式分級之硏磨材料組成物之製造方法。 (8)該濕式分級之分級區域之溫度偏差爲0.01〜5°C 之上述（7 )所載之硏磨材料組成物之製造方法。 如此，本發明可藉由控制氧化鈽之粒度分佈於上述範 圍後，以高水準取得達成兼具面精密度與硏磨速度之高性 能硏磨材料組成物。因此，使用此氧化鈽粒子爲砥材時， 可防止混入雜質，同時硏磨加工中可以高效率取得無缺陷 之高精密度面。本發明特別於LSI裝置之製造步驟中，進 行二氧化矽膜、氮化矽膜、有機膜等絕緣膜之硏磨加工時 -9 - 200813204 ，整體缺陷少、兼具面精密度與硏磨速度，同時使硏磨速 度之穩定化優於現狀達高水準，且可以利於工業方法實現 【實施方式】 〔發明實施之最佳形態〕 以下，針對適用本發明之硏磨材料組成物及其製造方 法進行詳細說明。 本發明硏磨材料組成物之特徵爲至少含有水及氧化鈽 粒子之硏磨材料組成物，該氧化鈽之粒度分佈以其製品粒 子濃度所測定之粒子體積基準平均圓相當粒徑爲1 // m以 下，且圓相當粒徑之低於 0.2 μ m粒子之體積分率爲 0.0 1〜1 0 %之範圍。 具體而言，有關本發明所使用之氧化鈽係以更高純度 者宜，該純度以99質量％以上者宜，更佳者爲99.9質量％ 以上。此氧化鈽之純度太低，則即使進行硏磨後L SI裝置 之洗淨，仍不易由LSI裝置表面除去對於LSI裝置特性有 不良影響之雜質元素。因此，將增加不良品，導致收率不 良，而不理想。 氧化鈽係進行煅燒如··碳酸鹽、硝酸鹽、硫酸鹽、草 酸鹽等鈽化合物後，此經由氧化取得。有關鈽化合物之煅 燒，——般可使用煅燒法。煅燒溫度只要於可取得穩定之氧 化鈽之條件下即可，並未特別限定，一般爲500〜1 000°C者 宜。 -10- 200813204 又，煅燒取得之氧化鈽一次結晶尺寸（平 )通常以0·00 5〜0.5/zm者宜，更佳者爲0.02〃 即，未達0· 005 // m時，以二氧化矽膜、氮化 膜爲始之絕緣膜硏磨速度則明顯變小，反之’ 則易於硏磨表面出現傷痕，而不理想。 煅燒後之氧化鈽呈乾粉狀態，以此狀態下 現部份凝聚狀態，因此，以氧化鈽經粉碎後’ 定的粒徑。另外，煅燒後，未將氧化鈽粉碎 LSI裝置硏磨時，於硏磨面開始出現極多刮痕 ，故不易製造有價値製品之裝置。 又，進行上述氧化鈽之粉碎處理時，在不 置硏磨用之硏磨材料組成物特性之範圍下，亦 適當有機或無機系添加劑爲助劑。 使用上述氧化鈽粉體，進行本發明硏磨材 製造時，將此氧化鈽粉體分散於分散媒體中。 以水爲硏磨材料組成物之分散媒體之使用。此 溶媒，該水之硏磨促進作用較大。如：硏磨玻 水的存在，於玻璃表面形成水合層。此時，進 可以高度硏磨速度取得高度面精密度。實際上 媒爲分散媒體使用時，對於玻璃幾乎不具硏磨 硏磨金屬時，仍於水之存在下使金屬表面水解 氧化物層或氫氧化物層時，可以高硏磨速度耳3 密度。因此，以有機溶媒爲分散媒體使用時， 水時，其硏磨速度明顯變低。故無法以高水準 均一次粒徑 -0 · 2 μ m 〇 亦 矽膜、有機 超出0.5 // m 其相互粒呈 務必調整一 ，直接用於 ，產生缺陷 影響LSI裝 可預先添加 料組成物之 一般，多半 相較於有機 璃時，藉由 行硏磨時， ，以有機溶 力。另外， ，形成金屬 得高度面精 相較於使用 實現本發明 -11 - 200813204 目的之面精密度與硏磨速度。 本發明硏磨材料組成物可於水，較佳者於純水中分散 上述氧化鈽之粉體後取得。有關無機化合物之分散方法並 未特別限定，——般可使用常用攪拌器，如：勻漿器、渦輪 式混合器、媒體攪拌硏磨器等公知之分散機器。另外，此 時亦可添加適於水系漿料之如：聚羧酸鹽、萘磺酸鹽甲醛 縮合物等之分散劑。進一步爲去除粗凝聚粒子，亦可進行 沈澱分級、過濾等。又，本發明之硏磨材料組成物亦可混 合黏度調節制、pH調整劑、緩衝劑、螯合劑、界面活性 劑、有機酸及其鹽等，該領域下公知之各種添加劑。 本發明中，將上述氧化鈽之粉體分散於水後，爲滿足 後述硏磨材料製品粒子濃度中氧化鈽之粒度分佈爲所定條 件，而進行分級操作者宜。 其中，「分級」係指由具有所定粒度分佈之粒子群選 擇性採取目的之粒度域之粒子群的單位操作。又，分級時 有乾式與濕式，更且，乾式分級與濕式分級中，有使用離 心力之方法，使用慣性力之方法，使用重力之方法等。本 發明其中又以使用濕式分級（濕式分級機），可提高分級 精密度爲較理想者。 該濕式分級中之粒子濃度以0.1〜10容積％者宜，更佳 者爲1〜5容積％。當粒子濃度低於0.1容積％時，爲進行 分級務必極大型之裝置而極不實用，另外，若粒子濃度爲 超出1 0容積％則粒子間相互作用增大，導致分級精密度不 良而不理想。 -12- 200813204 又，濕式分級之分級區域中之溫度偏差以0.01〜5°c者 宜。當溫度偏差低於〇· 01 °c時，則溫度控制不易，反之’ 溫度偏差超出5°c，則降低分級精密度而不理想。 經由如上述之分級操作取得之硏磨材料組成物中之氧 化鈽粒度分佈只要可於硏磨材料之製品粒子濃度中測定即 可，不限定其機種，通常，於測定用護套液膜之間形成挾 住被測定漿料之流下液膜後，由一方照射頻閃發光之光， 於另一方配置受光元件後，直接拍攝粒子影像，以畫像解 析法求取粒度分佈之方式者宜。 其中，「硏磨材料之製品粒子濃度」係指硏磨材料之 製品不經由一般粒度測定時進行之水或分散液之稀釋，直 接進行測定之濃度之意。而，本發明之氧化鈽粒度分佈中 ，以此製品粒子濃度所測定粒子之體積基準平均圓相當粒 徑爲l#m以下者宜，較佳者爲0.3〜0.8//m之範圍，且圓 相當粒徑爲低於0.2 // m之粒子體積分率爲0.01〜10%之範 圍者，較佳者於0.1〜5%之範圍，爲極重要者。另外，「 圓相當粒徑」係具有相同於粒子投影面積之面積的圓之直 徑，「體積基準平均圓相當粒徑」係代表具與粒子相同之 圓相當粒徑之球形粒子之以體積基準之平均直徑。 亦即，以製品粒子濃度所測定之粒子體積基準平均圓 相當粒徑若超出1 // m時，則增大微刮傷而無法取得高精 密度之硏磨面。又，圓相當粒徑爲低於0.2 /z m之粒子體 積分率若爲低於0.0 1 %則將無法有效生產所定製品，反之 ，超出1 〇%則增力Π源於粒子之缺陷，亦無法取得高精密度 -13- 200813204 之硏磨面。 本發明之圓相當粒徑超出1 // m之粒子個數分率更以 0〜5 %之範圍者宜，較佳者爲〇 · 〇 1〜3 %之範圍。此個數分率 若超出5%則將增加抑制刮傷。 含於本發明硏磨材料組成物之氧化鈽二次粒子之圓形 度以0.8〜0.97者宜，更佳者爲〇·8 5〜0.95。其中，「二次 粒子」係煅燒鈽化合物後取得之氧化鈽粉碎後之粒子。 「二次粒子之圓形度」係定義爲（相同於粒子影像面 積之圓的周圍長度）+(實際粒子之周圍長度），代表氧 化鈽粉碎後之粒子形狀的圓形狀態。 又，該二次粒子之圓形度係針對統計學個數進行評定 後作爲適當指標。本發明中針對1 000個以上之二次粒子 算出該圓形度，以其平均値作爲「二次粒子之圓形度」。 當此値低於0 · 8時，則異形粒子比例增加，硏磨時以刮傷 爲始增加缺陷，反之此値超出0.9 7則硏磨速度下降，導 致硏磨效率不佳。 有關含於本發明硏磨材料組成物之氧化铈濃度依其硏 磨時之加工壓力等硏磨條件，所使用分散劑或添加劑之種 類、量、分散方法等而異，一般以0.0 1〜1 0質量％者宜， 較佳者爲〇·1〜5質量％，更佳者爲0.3〜3質量％之範圍。當 濃度未達〇·〇1質量％時，二氧化矽膜、氮化矽膜、有機膜 爲始其絕緣膜之硏磨速度將變小，反之，超出1 0質量％則 藉由增量後減少效果提昇，亦即，二氧化矽膜、氮化矽膜 、有機膜爲始之絕緣膜之硏磨速度之提昇減少，不利經濟 -14- 200813204 面爲不理想者。 如以上所製作之本發明硏磨材料組成物係可防止混入 雜質，同時可於硏磨加工中以高效率取得無缺陷之高精密 度面。本發明硏磨材料組成物特別可適用於LSI裝置之製 造步驟中之絕緣膜硏磨，於以二氧化矽膜、氮化矽膜、有 機膜爲始之絕緣膜之硏磨加工時，整體缺陷少、兼具面精 密度與硏磨速度，同時使硏磨速度之穩定化優於現狀達高 水準，且可以利於工業方法實現。 針對使用該本發明硏磨材料組成物之絕緣膜之硏磨進 行具體的說明。 作爲硏磨對象之二氧化矽膜等之絕緣膜係可於基板上 利用定壓CVD法、電漿CVD法等形成之。 其中，以定壓CVD法形成氧化矽膜時，係使用單矽 院（SiH4)爲Si源，使用氧（〇2)爲氧源，於350〜400。〇 之低溫下進行此SiH4-0系氧化反應後，可形成氧化矽膜 〇 另外，電漿CVD法通常於熱平衡下，具有於低溫下 進行務必爲高溫之化學反應之優點。針對電漿產生法有容 量結合型與衍生結合型之2例。又，反應氣體之例如：s i 源之單矽烷（SiH4 )、氧源之使用亞氧化氮（n2〇 )之 SiHd^O系氣體，使四乙氧基矽烷（TE〇s)用於si源之 TE0S-02系氣體（TEOS-電漿CVD法）等例。 又’上述二氧化矽膜中亦可摻雜如：磷、硼等之元素 -15· 200813204 又，有關作爲硏磨對象之基板，如：於半導體晶圓基 板上均勻形成始於二氧化矽膜之絕緣膜的基板，預先形成 電路圖案之基板等例。 本發明中使形成於此基板之絕緣膜以該本發明硏磨材 料組成物經由硏磨加工後，解除絕緣膜表面之段差，可沿 著半導體基板整體做成平滑面。 其中，針對硏磨裝置，具備保持半導體基板之托板與 貼附硏磨墊片之定盤，可使用可變更旋轉數之一般硏磨裝 置。有關硏磨墊片可使用一般的不織布，發泡聚胺基甲酸 乙酯等。 又，硏磨墊片中以進行同心圓狀或放射狀之溝加工者 宜。有關硏磨條件並未特別受限。托板與定盤之旋轉速度 以不飛出半導體基板者宜。加於半導體基板之壓力於硏磨 後以不出現刮傷之0.1 MPa以下爲宜。硏磨當中，以泵等 進行連續性供應漿料於硏磨墊片。此供應量並未特別限定 ，一般使硏磨墊片表面經常被漿料覆蓋者宜。 硏磨結束後之半導體基板於流水中充分洗淨後，利用 旋轉乾燥器等將附著於表面之水滴撥掉後，利用所定洗淨 液進行洗淨及乾燥者宜。 〔實施例〕 以下，列舉實施例，進行本發明更詳細的說明，惟本 發明未受限於此等實施例。 -16- 200813204 (實施例1 ) 實施例1中使用1 〇kg之市售高純度碳酸鈽（和光純 藥工業製）爲原料，此利用旋轉窯以設定溫度800°C進行 煅燒。針對煅燒後之氧化鈽進行X線衍射之結果，未出現 氧化鈽以外之波峯。 接著使用2kg取得之氧化鈽粉，以市售球磨機（內容 積10L)經由乾式進行粉碎處理。 再將取得之氧化铈粉末投入脫離子水後，製造懸浮漿 料。又，此漿料中所含之氧化鈽濃度爲1 7質量％。 接著將此漿料導入靜止型分級容器，經過5小時及15 小時之沈澱操作後，取出粗與細爲分級之漿料。而將此漿 料進行離心沈澱，去除上澄液，加入脫離子水後，取得氧 化鈽濃度爲1 〇質量％之漿料。 再將此漿料進一步以脫離子水稀釋爲1 0倍，製成氧 化鈽濃度爲1質量％之製品漿料，依以下硏磨條件及評定 方法進行對於二氧化矽膜之硏磨試驗。 (硏磨條件）被硏磨材料·· 以熱氧化法於6inch中、厚度625 /zm之聚矽氧晶圓 上形成之二氧化矽膜（膜厚約1 # m ) 硏磨墊片：雙層型之LSI裝置硏磨用墊片（nitahas 製之 IC1000/Suba400) 硏磨機：LSI裝置硏磨用單面磨光機（Speedp製 之型號SH-24、定盤徑61〇mm) -17- 200813204 定盤旋轉速度：70rpm 力口 工壓力·· 3 00gf/cm2 ( 2.94N/cm2 ) 漿料供給速度：1 〇 〇 m 1 / m i η 硏磨時間：1 min (評定方法）硏磨速度：利用光干擾式膜厚測定裝置 ，以硏磨時間除以去除量後算出。 缺陷：利用光學式缺陷檢測裝置，進行計數〇 · 1 3 6从m 以上之缺陷總數。 上述硏磨試驗之結果顯示，實施例1中，其硏磨速度 爲6100Α/miii之高値。另外，缺陷總數爲每1片晶圓18 個，其中微刮傷爲7個之極良好的水準。 又，上述硏磨試驗之前，利用市售之粒子畫像攝影裝 置（cismex製之FPIA)，針對實施例1製品漿料，進行 拍攝漿料中之粒子影像後，進行1萬個粒子之粒度分佈解 析。其結果，體積基準平均圓相當粒徑爲0.52 // m、圓相 當粒徑爲低於0.2 a m之粒子體積分佈爲3%。超出1// m 粒子個數分率爲1 .1 %。另外，針對實施例1之製品漿料 ，利用相同於進行粒度分佈解析機械之裝置，求出漿料中 之1萬個二次粒子的圓形度。其結果，圓形度爲0.91。 (實施例2) 實施例2中，使用2kg相同於上述實施例1之煅燒後 之氧化鈽粉末，以市售球磨機（內容積1 〇L )經由乾式進 -18 - 200813204 行粉碎處理。 接著，於脫離子水中投入取得之氧化姉粉末後’製造 懸浮漿料。又，含於此漿料中之氧化鈽濃度爲16質量％。 再於靜止型分級容器中導入此漿料’經過6小時及13 小時之沈澱操作，取出粗與細兩者做成分級漿料。而此漿 料進行離心沈激，去除上澄液’加入脫離子水後’取得氧 化鈽濃度爲1 〇質量％之漿料。 接著，進一步以脫離子水進行稀釋此漿料爲10倍後 ，製作氧化鈽濃度爲1質量％之製品漿料，與實施例1同 法進行對於二氧化矽膜之硏磨試驗’其硏磨速度爲 640〇A/min。又，缺陷總數爲每1片晶圓15個’其中微刮 傷爲5個之極良好的水準。 又，於該硏磨試驗之前’利用市售之粒子畫像攝影裝 置（cismex製之FPIA)，針對實施例2之製品漿料，拍 攝漿料中之粒子影像後，進行1萬個粒子之粒度分佈解析 。其結果，體積基準平均圓相當粒徑爲0 · 5 5 // m、圓相當 粒徑爲低於〇·2μπι之粒子體積分率爲1·5%。更，超出1 /zm之粒子個數分率爲〇·9%。另外，針對實施例2之製品 漿料，利用相同於進行粒度分佈解析機械之裝置，求出漿 料中1萬個二次粒子之圓形度。其結果，圓形度爲0.92。 (比較例1 ) 比較例1中，利用2kg之相同於該實施例1之煅燒後 氧化鈽之粉末，以市售球磨機（內容積l〇L)經由乾式進 -19- 200813204 行粉碎處理。 再於脫離子水中投入取得之氧化鈽粉末，製造懸浮漿 料。又，含於此漿料中之氧化鈽濃度爲1 6質量％。 接著，於靜止型分級容器中導入此漿料，經過6小時 沈澱操作，取得去除粗粒之分級漿料。而，進行此漿料之 離心沈澱，除去上澄液，加入脫離子水後，取得氧化鈽濃 度爲10質量％之漿料。 進一步以脫離子水進行此漿料爲1 〇倍稀釋，製作氧 化鈽濃度爲1質量％之製品漿料，與實施例1同法進行對 於二氧化矽膜之硏磨試驗，其硏磨速度爲5900A/min。又 ，缺陷總數爲每1片晶圓47個，其中微刮傷爲1 2個之極 差水準。 又，於該硏磨試驗之前，針對比較例1之製品漿料， 利用市售粒子影像攝影裝置（cismex製之FPIA)，拍攝 漿料中之粒子影像後，進行1萬個粒子之粒度分佈解析。 其結果，體積基準平均圓相當粒徑爲〇. 5 2 // m，圓相當粒 徑爲低於0.2 // m之粒子體積分率爲12%。更，超出1 # m 之粒子個數分率爲4%。另外，針對比較例1之製品漿料 ’利用相同於進行粒度分佈解析之機械裝置，求出漿料中 1萬個二次粒子之圓形度。其結果，圓形度爲0.96。 (比較例2 ) 比較例2中，使用2kg之與該實施例1之煅燒後氧化 鈽粉末，以市售球磨機（內容積1 〇 L )，經由乾式進行粉 -20- 200813204 碎處理。 再於脫離子水中投入取得之氧化鈽粉末’製造懸浮漿 料。又，含於此漿料中之氧化鈽濃度爲16質量％。 接著，於靜止型分級容器中導入此漿料’經過4小時 之沈澱操作，取得取去粗粒之分級漿料。將此漿料進行離 心沈灑，去除上澄液’加入脫離子水後’取待化姉？辰度 爲10質量％之漿料。 進一步以脫離子水進行此漿料之10倍稀釋’製作氧 化鈽濃度爲1質量％之製品漿料，以相同於實施例1之方 法進行對於二氧化矽膜之硏磨試驗，其硏磨速度爲 5 400 A/min。又，缺陷總數爲每1片晶圓63個，其中微刮 傷爲1 8個之極差水準者。 於上述硏磨試驗前，針對比較例2之製品漿料，利用 市售之粒子畫像攝影裝置（Cismex製之FPIA)，拍攝漿 料中之粒子影像，進行1萬個粒子之粒度分佈解析。其結 果，體積基準平均圓相當粒徑爲0.49 /z m，圓相當粒徑爲 低於〇·2μπι之粒子體積分率爲17%。更，超出之粒 子個數分率爲7%。另外，針對比較例2之製品漿料，利 用相同於進行粒度分佈解析機械之裝置，求出漿料中1萬 個二次粒子之圓形度。其結果圓形度爲0.94。 〔產業上可利用性〕 本發明適用於使用氧化鈽爲砥材之硏磨材料組成物及 其製造方法。 -21 -200813204 The grinding speed is divided by the enthalpy of the cerium oxide film (referred to as the sputum slag which is required to be sorghum, and this is a high honing speed for the cerium oxide film. In addition, oxidation is used. When the slurry is smeared, the problem is caused by scratching (for example, Patent Documents 1 and 2). To avoid this, it is revealed in Document 1 that the secondary particle diameter I is in the cerium oxide particles. The cerium oxide containing cerium oxide, a dispersing agent and a honing agent are contained in a particle content of less than 1%, wherein the secondary particle diameter means the particle diameter of | in the CMP honing agent, and the method is as follows: photon correlation name The photon correlation method is a method in which the concentration of the extremely thin particles can be measured under the condition that the concentration is completely deviated. Further, it is disclosed in Patent Document 2 that the primary | 値 is 30 to 2 50 nm, and the particles are obtained. The diameter of the center of the crucible is 150 to 600 nm, and the cerium oxide particles of tl 7 to 45 m 2 /g are dispersed in the slurry of the medium, and the cerium oxide particles having a particle size distribution of less than half a width are dispersed in the slurry of the medium. Cerium oxide, although Patent Document 2 describes a half-width, but does not [Patent Document 1] JP-A-2003-1 71 653 (Patent Document 2) JP-A No. 200 1 - 3 2925 1 In recent years, the height of the CMP honing surface is accompanied by the miniaturization of the design rules of the device. Flatness, uniformity, or a variety of strict benefits. Especially related to the defect surface, accompanied by the detection of sensitivity | Strong demand for suppression of scratches without major damage, fine scratch, i selection ratio) Conducive to: trapped ί, in the patent ^ 3 ν m with water CMP, bismuth particles: an example. However, it is determined that the center of the diameter t surface area is the average particle size [for 3 0Onm f grinding agent. However, & includes its low requirement for depression, which is reduced by the overall defects of strong particles, 200813204 buried particles, no cracks, residual slurry, and pollution. However, even if the honing material composition for honing of the LSI device manufactured by this prior art is used, it is not possible to obtain a honing surface which can reduce various defects as a whole and is highly accurate and stable. SUMMARY OF THE INVENTION Therefore, the present invention has been made in view of the above circumstances, and it is proposed to provide a honing material composition capable of preventing impurities from being mixed and achieving high precision without defects in honing processing and manufacturing thereof. The method is for the purpose. In the manufacturing process of the LSI device, the present invention provides a method of honing an insulating film such as a hafnium oxide film, a tantalum nitride film, or an organic film, and has both integral defects and surface precision. The grinding speed and the stabilization of the honing speed higher than the current level are achieved, and the honing material composition for honing of the LSI device and the manufacturing method thereof can be advantageously used in an industrial method. In order to solve the above problems, the inventors of the present invention have found that the following honing material composition and the method for producing the same can be easily solved. (1) A honing material composition containing at least water and cerium oxide particles, the particle size distribution of the cerium oxide being measured by the particle concentration of the product, and the average particle diameter of the particle is 1 // m or less, and the particle size is equal to The honing material composition having a volume fraction of less than 0.2 #m particles in the range of 0.01 to 10% is 0 -8 - 200813204 (2) The particle size distribution of the cerium oxide is equivalent to a particle size exceeding 1 /zm particle The number of the honing materials contained in the above (1) is in the range of 〇 5% to 5%. (3) The honing material composition of the above-mentioned (1) or (2) having a circularity of the cerium oxide secondary particles of 0.8 to 0.97. (4) The honing material composition according to any one of the above items 1 to 3, wherein the cerium oxide concentration is from 0.01 to 10% by mass. (5) The product particle concentration is a honing material composition as described in the above (1) or (2) in which the cerium oxide concentration in the honing material composition is 1% by mass. (6) A method of manufacturing an LSI device using the honing material composition according to any one of the above (1) to (5) in the insulating film honing of the LSI device manufacturing step. (7) The method for producing a honing material composition according to any one of the above (1) to (5), wherein the cerium oxide powder is subjected to wet classification in a particle concentration of 0.1 to 10% by volume. A method of manufacturing a grinding material composition. (8) A method for producing a honing material composition according to the above (7), wherein the temperature deviation of the wet classification step region is 0.01 to 5 °C. Thus, the present invention can achieve a high-performance honing material composition which achieves both surface precision and honing speed at a high level by controlling the particle size distribution of cerium oxide in the above range. Therefore, when the cerium oxide particles are used as the cerium material, it is possible to prevent the impurities from being mixed, and at the same time, the high-precision surface without defects can be efficiently obtained in the honing process. In the manufacturing process of the LSI device, the present invention performs honing processing of an insulating film such as a hafnium oxide film, a tantalum nitride film, or an organic film, -9 - 200813204, and has a small overall defect, and has both surface precision and honing speed. At the same time, the stabilization of the honing speed is superior to the current level, and can be achieved by an industrial method. [Embodiment] [Best Mode for Carrying Out the Invention] Hereinafter, the honing material composition to which the present invention is applied and a method for producing the same Detailed instructions are given. The honing material composition of the present invention is characterized by a honing material composition containing at least water and cerium oxide particles, and the particle size distribution of the cerium oxide is determined by the particle concentration of the product particles. Below m, the volume fraction of particles having a particle diameter of less than 0.2 μm is in the range of 0.01 to 10%. Specifically, the cerium oxide used in the present invention is preferably of higher purity, and the purity is preferably 99% by mass or more, and more preferably 99.9% by mass or more. When the purity of the cerium oxide is too low, even if the L SI device is washed after honing, it is difficult to remove the impurity element which adversely affects the characteristics of the LSI device from the surface of the LSI device. Therefore, defective products will be added, resulting in poor yield and unsatisfactory. The cerium oxide is obtained by calcining a hydrazine compound such as a carbonate, a nitrate, a sulfate or an oxalate. Regarding the calcination of the ruthenium compound, the calcination method can be generally used. The calcination temperature is not particularly limited as long as it can obtain stable cerium oxide, and is usually 500 to 1 000 °C. -10- 200813204 In addition, the primary crystal size (flat) of cerium oxide obtained by calcination is usually 0.00 5~0.5/zm, and more preferably 0.02〃, ie, less than 0·005 // m, When the yttrium oxide film or the nitride film is used, the honing speed of the insulating film is remarkably small. On the contrary, it is easy to honed the surface, and it is not desirable. After calcination, the cerium oxide is in a dry powder state, and in this state, a part of the condensed state is formed, and therefore, the cerium oxide is pulverized and has a predetermined particle diameter. Further, after calcination, when the yttrium oxide pulverization LSI device is not honed, a large number of scratches appear on the honing surface, so that it is difficult to manufacture a device having a valuable enamel product. Further, when the pulverization treatment of the cerium oxide is carried out, an organic or inorganic additive is also an auxiliary agent in the range in which the properties of the honing material composition for honing are not provided. When the cerium oxide powder of the present invention is produced by using the above cerium oxide powder, the cerium oxide powder is dispersed in a dispersion medium. The use of water as a dispersing medium for honing material composition. In this solvent, the honing effect of the water is large. For example, the presence of water in the honing water forms a hydrated layer on the surface of the glass. At this time, the height can be obtained at a high honing speed. In fact, when the medium is used as a dispersing medium, the glass is hardly honed. When the metal is honed, the metal surface is hydrolyzed with an oxide layer or a hydroxide layer in the presence of water, and the ear 3 density can be honed at a high speed. Therefore, when the organic solvent is used as a dispersion medium, the honing speed is remarkably low in water. Therefore, it is impossible to achieve a high level of primary particle size of -0 2 μm, and the organic film exceeds 0.5 // m. The mutual particle size must be adjusted one by one, and it is directly used to cause defects to affect the LSI package. In general, when compared with organic glass, when it is honed, it is organically soluble. Further, the surface finish precision and the honing speed for forming the metal are higher than those for using the object of the present invention -11 - 200813204. The honing material composition of the present invention can be obtained by dispersing the above cerium oxide powder in water, preferably in pure water. The dispersion method of the inorganic compound is not particularly limited, and a commonly used disperser such as a homogenizer, a turbo mixer, a media agitating honing machine or the like can be used. Further, at this time, a dispersing agent suitable for an aqueous slurry such as a polycarboxylate or a naphthalenesulfonate formaldehyde condensate may be added. Further, in order to remove coarsely aggregated particles, precipitation classification, filtration, and the like may be performed. Further, the honing material composition of the present invention may be mixed with a viscosity adjusting system, a pH adjusting agent, a buffering agent, a chelating agent, a surfactant, an organic acid and a salt thereof, and various additives known in the art. In the present invention, after dispersing the powder of cerium oxide in water, it is preferable to perform a classification operation in order to satisfy the particle size distribution of cerium oxide in the particle concentration of the honing material product described later. Here, "grading" means a unit operation of a particle group of a particle size domain which is selected by a particle group having a predetermined particle size distribution. Further, in the classification, there are dry and wet types, and in the dry classification and the wet classification, there are a method of using a centrifugal force, a method using an inertial force, and a method using gravity. In the present invention, it is preferable to use a wet classification (wet classifier) to improve the classification precision. The concentration of the particles in the wet classification is preferably from 0.1 to 10% by volume, more preferably from 1 to 5% by volume. When the particle concentration is less than 0.1% by volume, it is extremely impractical for the device to be classified as a very large type, and if the particle concentration exceeds 10% by volume, the interaction between particles increases, resulting in poor classification precision. . -12- 200813204 Further, the temperature deviation in the classification range of the wet classification is preferably 0.01 to 5 °C. When the temperature deviation is lower than 〇· 01 °c, the temperature control is not easy. On the contrary, if the temperature deviation exceeds 5 °c, the classification precision is lowered. The cerium oxide particle size distribution in the honing material composition obtained by the grading operation as described above may be measured as long as it can be measured in the product particle concentration of the honing material, and is not limited to the model, and is usually between the coating liquid films for measurement. After forming a liquid film that has been immersed in the slurry to be measured, one side is irradiated with stroboscopic light, and the light-receiving element is placed on the other side, and then the particle image is directly captured, and the particle size distribution is determined by image analysis. Here, the "particle concentration of the product of the honing material" means the concentration of the water or the dispersion which is obtained when the product of the honing material is not subjected to the measurement of the general particle size, and the concentration is directly measured. Further, in the particle size distribution of cerium oxide according to the present invention, the volume-based average circle-equivalent particle diameter of the particles measured by the particle concentration of the product is preferably 1 or less, preferably 0.3 to 0.8//m, and is round. A particle size fraction of a particle diameter of less than 0.2 // m is preferably in the range of 0.01 to 10%, preferably in the range of 0.1 to 5%, which is extremely important. In addition, the "circle-equivalent particle diameter" is a diameter of a circle having the same area as the area projected by the particle, and the "volume-based average circle-equivalent particle diameter" means a volume-based basis of spherical particles having the same particle diameter as the particle. The average diameter. That is, the particle volume reference average circle measured by the particle concentration of the product is larger than the particle diameter of 1 / m, and the micro-scratch is increased to obtain a high-density honing surface. Moreover, if the volume fraction of a particle having a particle diameter of less than 0.2 /zm is less than 0.01%, the product will not be efficiently produced. Conversely, if it exceeds 1%, the force will not be due to defects of the particle. Obtain a high-precision 13-200813204 honing surface. The particle size fraction of the particle having a diameter larger than 1 // m in the present invention is preferably in the range of 0 to 5 %, preferably in the range of 〇 · 〇 1 to 3%. If the number exceeds 5%, it will increase the suppression of scratches. The circularity of the cerium oxide secondary particles contained in the honing material composition of the present invention is preferably 0.8 to 0.97, more preferably 〇·8 5 to 0.95. Here, the "secondary particle" is a particle obtained by pulverizing the cerium oxide obtained after calcining the cerium compound. The "circularity of secondary particles" is defined as (the same length around the circle of the particle image area) + (the length around the actual particle), and represents the circular state of the particle shape after pulverization of the cerium oxide. Further, the circularity of the secondary particles is evaluated as a suitable index based on the statistical number. In the present invention, the circularity is calculated for 1 000 or more secondary particles, and the average enthalpy is referred to as "circularity of secondary particles". When the enthalpy is lower than 0 · 8 , the proportion of the irregular shaped particles increases, and the defect is increased by scratching during honing, and if the 値 exceeds 0.9 7 , the honing speed is lowered, resulting in poor honing efficiency. The concentration of cerium oxide contained in the honing material composition of the present invention varies depending on the honing conditions such as the processing pressure at the time of honing, the type, amount, dispersion method, etc. of the dispersing agent or additive used, and is generally 0.01 to 1 It is preferably 0% by mass, more preferably 〇1 to 5% by mass, and even more preferably 0.3 to 3% by mass. When the concentration is less than 质量·〇1% by mass, the honing speed of the ruthenium dioxide film, the ruthenium nitride film, and the organic film will be small, and if it exceeds 10% by mass, the increase will be made. The effect of the reduction is improved, that is, the increase in the honing speed of the insulating film of the ruthenium dioxide film, the tantalum nitride film, and the organic film is reduced, which is unfavorable for the economical-14-200813204 surface. The honing material composition of the present invention produced as described above can prevent the incorporation of impurities, and at the same time, can obtain a high-precision surface without defects in high efficiency in honing processing. The honing material composition of the present invention is particularly applicable to the honing of the insulating film in the manufacturing step of the LSI device, and the overall defect in the honing process of the insulating film starting from the cerium oxide film, the cerium nitride film, and the organic film. Less, both surface precision and honing speed, while stabilizing the honing speed is better than the current level, and can be achieved by industrial methods. The honing of the insulating film using the honing material composition of the present invention will be specifically described. An insulating film such as a cerium oxide film to be honed may be formed on a substrate by a constant pressure CVD method, a plasma CVD method, or the like. Among them, when a ruthenium oxide film is formed by a constant pressure CVD method, a single sputum (SiH4) is used as a Si source, and oxygen (〇2) is used as an oxygen source at 350 to 400. The SiH4-0 oxidation reaction can be carried out at a low temperature to form a ruthenium oxide film. In addition, the plasma CVD method generally has the advantage of performing a high-temperature chemical reaction at a low temperature under thermal equilibrium. There are 2 cases of capacitive binding method and derivative binding type for plasma generation method. Further, the reaction gas is, for example, a mono-decane (SiH4) derived from a source of Si, and a SiHd^O-based gas using a nitrogen oxide (n2〇) as an oxygen source, and tetraethoxy decane (TE〇s) is used for the source of Si. Examples of TE0S-02-based gas (TEOS-plasma CVD method). Further, the above-mentioned cerium oxide film may be doped with elements such as phosphorus and boron. -15. 200813204 Further, the substrate to be honed is, for example, uniformly formed on a semiconductor wafer substrate starting from a cerium oxide film. Examples of the substrate of the insulating film, a substrate on which a circuit pattern is formed in advance, and the like. In the present invention, the insulating film formed on the substrate is subjected to honing processing by the honing material composition of the present invention, and the step of the surface of the insulating film is released to form a smooth surface along the entire semiconductor substrate. Among them, the honing device is provided with a holder for holding a semiconductor substrate and a fixing plate to which a honing pad is attached, and a general honing device capable of changing the number of rotations can be used. For the honing pad, a general non-woven fabric, a foamed polyurethane, or the like can be used. Also, it is advisable to honing the gasket to perform a process of concentric or radial grooves. The conditions for honing are not particularly limited. The rotation speed of the pallet and the fixed plate is preferably not required to fly out of the semiconductor substrate. The pressure applied to the semiconductor substrate is preferably 0.1 MPa or less after scratching without scratching. In the honing process, the slurry is continuously supplied to the honing pad by a pump or the like. This supply amount is not particularly limited, and it is generally preferred that the surface of the honing pad is often covered by the slurry. After the semiconductor substrate after the honing is sufficiently washed in the running water, the water droplets adhering to the surface are removed by a spin dryer or the like, and then washed and dried by the predetermined cleaning liquid. [Examples] Hereinafter, the present invention will be described in more detail by way of examples, but the invention is not limited thereto. -16-200813204 (Example 1) In Example 1, commercially available high-purity cesium carbonate (manufactured by Wako Pure Chemical Industries, Ltd.) of 1 〇kg was used as a raw material, and this was calcined at a set temperature of 800 °C by a rotary kiln. As a result of X-ray diffraction of the cerium oxide after calcination, no peak other than cerium oxide appeared. Next, using 2 kg of the obtained cerium oxide powder, a pulverization treatment was carried out by a dry type in a commercially available ball mill (content volume: 10 L). Further, the obtained cerium oxide powder was placed in deionized water to prepare a suspended slurry. Further, the concentration of cerium oxide contained in the slurry was 17% by mass. The slurry was then introduced into a static classification vessel, and after a 5 hour and 15 hour precipitation operation, the coarse and finely classified slurry was taken out. The slurry was subjected to centrifugal precipitation to remove the supernatant liquid, and after the deionized water was added, a slurry having a cerium oxide concentration of 1 〇 mass% was obtained. Further, this slurry was further diluted to 10 times with deionized water to prepare a product slurry having a cerium oxide concentration of 1% by mass, and a honing test for the cerium oxide film was carried out in accordance with the following honing conditions and evaluation methods. (honing condition) honed material · · cerium oxide film formed by thermal oxidation on a hexagonal 625 /zm polysilicon wafer (film thickness about 1 # m) honing pad: double Multilayer LSI device honing pad (IC1000/Suba400 made by nitahas) Honing machine: LSI device honing single-side sander (Model SH-24 with Speedp, fixed diameter 61〇mm) -17 - 200813204 Plate rotation speed: 70 rpm Force pressure · · 3 00gf/cm2 ( 2.94N/cm2 ) Slurry supply speed: 1 〇〇m 1 / mi η Honing time: 1 min (assessment method) honing speed : Calculated by dividing the honing time by the amount of removal by the light interference type film thickness measuring device. Defect: The total number of defects 〇 · 1 3 6 from m or more is counted using an optical defect detecting device. The results of the above honing test showed that in Example 1, the honing speed was 6100 Α/miii. In addition, the total number of defects is 18 per wafer, and the micro-scratch is a very good level of 7. In addition, before the honing test, a particle image of the sample slurry of the first embodiment was imaged by using a commercially available particle image capturing apparatus (FPIA manufactured by Cismex), and then the particle size distribution analysis of 10,000 particles was performed. . As a result, the volume-based average circle-equivalent particle diameter was 0.52 // m, and the particle phase distribution of the particle diameter of less than 0.2 a m was 3%. The number of particles exceeding 1// m is 1.1%. Further, with respect to the product slurry of Example 1, the circularity of 10,000 secondary particles in the slurry was determined by the same apparatus as that of the particle size distribution analysis machine. As a result, the circularity was 0.91. (Example 2) In Example 2, 2 kg of the cerium oxide powder which was the same as that of the above-mentioned Example 1 was used, and was pulverized by a commercially available ball mill (internal volume 1 〇L) via dry type -18 - 200813204. Next, the obtained cerium oxide powder was placed in the deionized water to produce a suspension slurry. Further, the concentration of cerium oxide contained in the slurry was 16% by mass. Further, the slurry was introduced into a static classification vessel. After 6 hours and 13 hours of precipitation operation, both coarse and fine were taken out to prepare a classified slurry. The slurry was subjected to centrifugal swelling, and the slurry was removed after the addition of the deionized water was carried out to obtain a slurry having a cerium oxide concentration of 1 〇 mass%. Then, the slurry was further diluted 10 times with deionized water, and then a product slurry having a cerium oxide concentration of 1% by mass was prepared, and the honing test for the cerium oxide film was performed in the same manner as in Example 1 The speed is 640 〇A/min. Further, the total number of defects is 15 per wafer, and the number of micro-scratches is 5, which is a very good level. In addition, before the honing test, a particle image of 10,000 particles was obtained by photographing the particle image in the slurry of the product slurry of Example 2 using a commercially available particle image capturing device (FPIA manufactured by Cismex). Analysis. As a result, the volume-based average circle-equivalent particle diameter was 0 · 5 5 // m, and the circle-equivalent particle diameter was less than 〇·2 μm, and the particle volume fraction was 1.5%. Furthermore, the number of particles exceeding 1 /zm is 〇·9%. Further, with respect to the product slurry of Example 2, the circularity of 10,000 secondary particles in the slurry was determined by the same apparatus as that of the particle size distribution analysis machine. As a result, the circularity was 0.92. (Comparative Example 1) In Comparative Example 1, 2 kg of the powder of the calcined cerium oxide of the same manner as in Example 1 was used, and a commercially available ball mill (internal volume 〇L) was pulverized by dry-type -19-200813204. Further, the obtained cerium oxide powder was placed in the deionized water to prepare a suspended slurry. Further, the concentration of cerium oxide contained in the slurry was 16% by mass. Next, this slurry was introduced into a static classification vessel, and after 6 hours of precipitation operation, a classified slurry from which coarse particles were removed was obtained. Then, the slurry was centrifuged to remove the supernatant, and deionized water was added to obtain a slurry having a cerium oxide concentration of 10% by mass. Further, the slurry was diluted with 1 deuterium water to prepare a product slurry having a cerium oxide concentration of 1% by mass, and the honing test for the cerium oxide film was carried out in the same manner as in Example 1, and the honing speed was 5900A/min. Also, the total number of defects is 47 per wafer, and the micro-scratch is 12 to the extreme level. Further, before the honing test, the product slurry of Comparative Example 1 was imaged by using a commercially available particle image capturing apparatus (FPIA manufactured by Cismex) to image the particle image in the slurry, and then the particle size distribution analysis of 10,000 particles was performed. . As a result, the volume-based average circle has a particle diameter of 〇. 5 2 // m, and the volume of the particles having a diameter of less than 0.2 // m is 12%. Moreover, the number of particles exceeding 1 # m is 4%. Further, the product slurry of Comparative Example 1 was used to determine the circularity of 10,000 secondary particles in the slurry by the same mechanical device for performing particle size distribution analysis. As a result, the circularity was 0.96. (Comparative Example 2) In Comparative Example 2, 2 kg of the calcined cerium oxide powder of Example 1 was used, and a powder mill -20-200813204 was pulverized by a commercially available ball mill (internal volume 1 〇 L ). Further, the obtained cerium oxide powder was put into the deionized water to produce a suspended slurry. Further, the concentration of cerium oxide contained in the slurry was 16% by mass. Next, the slurry was introduced into a static classification vessel, and a precipitation operation was carried out for 4 hours to obtain a classified slurry from which coarse particles were taken. The slurry is subjected to centrifugation, and the supernatant is removed. The aging is 10% by mass of the slurry. Further, a 10-fold dilution of the slurry was carried out with deionized water to prepare a product slurry having a cerium oxide concentration of 1% by mass, and a honing test for the cerium oxide film was carried out in the same manner as in Example 1, and the honing speed was performed. It is 5 400 A/min. Further, the total number of defects is 63 per wafer, and the number of micro-scratches is 18. Before the honing test, the product slurry of Comparative Example 2 was imaged by using a commercially available particle image photographing apparatus (FPIA manufactured by Cismex) to analyze the particle size distribution of the 10,000 particles. As a result, the volume-based average circle has a specific particle diameter of 0.49 / z m, and the volume-equivalent particle size is less than 〇·2 μm. Moreover, the number of particles exceeded is 7%. Further, with respect to the product slurry of Comparative Example 2, the circularity of 10,000 secondary particles in the slurry was determined using the same apparatus as that of the particle size distribution analysis machine. The result was a circularity of 0.94. [Industrial Applicability] The present invention is applicable to a honing material composition using cerium oxide as a cerium material and a method for producing the same. -twenty one -