TW201041805A - Method for preparing ceria powder and slurry composition having the same - Google Patents

Method for preparing ceria powder and slurry composition having the same Download PDF

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Publication number
TW201041805A
TW201041805A TW099116137A TW99116137A TW201041805A TW 201041805 A TW201041805 A TW 201041805A TW 099116137 A TW099116137 A TW 099116137A TW 99116137 A TW99116137 A TW 99116137A TW 201041805 A TW201041805 A TW 201041805A
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Taiwan
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cerium
cerium oxide
compound
temperature
particles
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TW099116137A
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Chinese (zh)
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Jong-Won Kim
Ho-Kyu Lee
Jong-Chul Shin
Hyun-Goo Kong
Jong-Dai Park
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Dongjin Semichem Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00Compounds of rare earth metals
    • C01F17/10Preparation or treatment, e.g. separation or purification
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • C09K3/1454Abrasive powders, suspensions and pastes for polishing
    • C09K3/1463Aqueous liquid suspensions
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00Compounds of rare earth metals
    • C01F17/20Compounds containing only rare earth metals as the metal element
    • C01F17/206Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
    • C01F17/224Oxides or hydroxides of lanthanides
    • C01F17/235Cerium oxides or hydroxides
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • C09K3/1409Abrasive particles per se
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/04Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/30Particle morphology extending in three dimensions

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)

Abstract

A method for preparing cerium oxide powder and a slurry composition having the same are disclosed. The slurry composition has a high polishing speed and a high polishing selectivity, and also reduces micro scratches in a chemical mechanical polishing process. The method for preparing cerium oxide powder includes the steps of: rapidly heating a cerium compound to the temperature of 700 to 1,000 DEG C; calcining the cerium compound at the temperature of 700 to 1,000 DEG C to form calcined cerium oxide; and rapidly cooling the calcined cerium oxide to the temperature of 15 to 30 DEG C. Preferably, the step of calcining the cerium compound is carried out for 10 minutes to 2 hours, in the rapid heating step, the cerium compound is heated with a heating speed of 20 to 900 DEG C/min, and, in the rapid cooling step, the calcined cerium oxide is cooled with a cooling speed of 20 to 400 DEG C/min.

Description

201041805 六、發明說明: 露之所有内谷在此併入本文作為參考 本申請案主張韓國專利申請 優先權,該案於2009年5月 案 10-2009-0043970 號之 20曰提出申請,該案所揭 【發明所屬之技術領域】 0 本發明係關於製備氧化鈽(_)粉末之方法,以及 -種具有該氧化鈽粉末的漿料組成物。本發明之聚料組 成物具有高研磨速度以及高研磨選擇性,且亦減少化學 機械研磨製程中的微刮痕。 【先前技術】 當半導體元件的整合度增加冑,為#得用於生產半導 Ο 體70件之高精確暴露製程的餘裕,須導入總體平整化製 程。化學機械研磨(CMP)製程大體上用於總體平整化 半導體元件,且其具冑CM”“里之平整度優於其他平整 化方法、及製程相對簡單等優點。 用於CMP製程的研磨漿料組成物大體上包括研磨粒 子、去離子水以及各種添加物。研磨粒子之代表性範例 包括膠狀二氧化矽粒子及燻矽粒子等。然而,由於習知 研磨粒子對氧化物層具低研磨速度以及在氧化物層與氮 化物層之間具低研磨選擇性,習知研磨粒子無法全然獲 201041805 得滿足,因此,靈盈 額外製程以獲得期f的結果。 為了解決此類缺陷,已w 已研發使用氧化鈽粒子的漿料組 成物。氧化鈽粒子大體上 5|, ^ s v 已用於處理玻璃產物。亦認知 到包括氧化鈽粒子之艰4立 ,, 之表枓組成物改善對氧化物層的研磨 速度以及氧化物層與氮化物層之缺 而,氧化飾粒子的密度相較於二氧切粒子而言高/6 至8倍’其劣化襞料組成物的分散敎性。再者,氧化 Ο 〇 飾粒子在CMP製程期間易 易;聚集’其會產生非期望的微 刮痕於研磨基材上。牯201041805 VI. INSTRUCTIONS: All of Neigu is hereby incorporated by reference. This application claims priority to Korean Patent Application, which is filed on May 20, 2009, No. 10-2009-0043970, 20 TECHNICAL FIELD OF THE INVENTION The present invention relates to a method for preparing a cerium oxide (-) powder, and a slurry composition having the cerium oxide powder. The polymeric composition of the present invention has high milling speeds and high milling selectivity and also reduces micro-scratches in the CMP process. [Prior Art] When the degree of integration of the semiconductor element is increased, the margin for the high-precision exposure process for producing 70 parts of the semiconductor body must be introduced into the overall planarization process. The chemical mechanical polishing (CMP) process is generally used for the overall planarization of semiconductor components, and its flatness in 胄"" is superior to other planarization methods, and the process is relatively simple. The abrasive slurry composition used in the CMP process generally includes abrasive particles, deionized water, and various additives. Representative examples of abrasive particles include colloidal ceria particles and smoked particles. However, since the conventional abrasive particles have a low polishing rate for the oxide layer and a low polishing selectivity between the oxide layer and the nitride layer, the conventional abrasive particles cannot be fully satisfied by 201041805, and therefore, the Lingying extra process is Obtain the result of period f. In order to solve such defects, a slurry composition using cerium oxide particles has been developed. The cerium oxide particles are substantially 5|, ^ s v have been used to treat glass products. It is also recognized that the composition of the cerium oxide particles is improved, and the surface composition improves the polishing rate of the oxide layer and the deficiency of the oxide layer and the nitride layer, and the density of the oxidized particles is smaller than that of the diced particles. In terms of high/6 to 8 times, it degrades the dispersion properties of the dip composition. Furthermore, the yttrium oxide particles are susceptible to CMP processes; they can cause undesirable micro scratches on the abrasive substrate.牯

制和士 特別疋在STI (淺溝道隔離)CMP 裝程中,溝道的深度是漤的 %的。因此,在STI CMP製程期 a >成的微刮痕會嚴重地劣 — 劣化+導體兀件的品質及生產 率。微到痕的形成如所知是 — 丨疋視研磨粒子的尺寸及形狀而 疋。 粒::用於製備氧化飾粒子之方法及一種包括該氧化筛 'CMP漿料組成物已揭露於韓國專利公開號 0087037 (國際申請案號為·· WO 2000/39843 ) 中。在該公開的專利中 肀揭露了用於STICMP漿料組成 :之研磨粒子的期望特性以及期望的添加物。同時,在 國專利公_,使漿料組成物老 化以減少形成微刮痕。在 1〇 良 在韓國專利公開號 02-0009619 (國際 φ 軎安 & 甲凊案诡為:WO 2000/73211 ), ^露―種根據加熱速度而製備氧化鈽粒子的方法。然 用於製傷氧化鈽粒子的弁& ,, 卞的先刖方法不能全然滿足減少 由氧化鈽敉子衍生的微刮痕之問題。 5 201041805 【發明内容】In the STI (Shallow Trench Isolation) CMP process, the depth of the channel is % of 漤. Therefore, the micro-scratches formed during the STI CMP process will be severely inferior—deterioration + quality and yield of the conductor components. The formation of micro-to-marks is known as - defying the size and shape of the abrasive particles. Granules: A method for preparing oxidized granules and a CMP composition comprising the oxidizing sifter is disclosed in Korean Patent Publication No. 0087037 (International Application No. WO 2000/39843). The disclosed patents disclose the desired properties of the abrasive particles for the STICMP paste composition as well as the desired additives. At the same time, in the national patent, the slurry composition is aged to reduce the formation of micro scratches. In 1 〇 良 In Korean Patent Publication No. 02-0009619 (International φ 軎安 & A 凊 诡: WO 2000/73211), 露-species method for preparing cerium oxide particles according to heating rate. However, the 弁&, 卞 method used to make cerium oxide particles does not fully satisfy the problem of reducing micro-scratches derived from oxidized scorpions. 5 201041805 [Summary content]

因此,本發明的宗旨為提供一種用於製備氧化鈽 (ceria)粉末的方法,以及以及-種具有該氧化鈽粉末 的’灸料組成物,其具有高研磨速度以及高研磨選擇性, 且亦減少化學機械研磨製程中的微到痕。本發明之另— 宗旨為提供-種用於製備氧化鈽粉末的方法,以及—種 Ο 具有該氧化飾粉末的聚料組成物,其特別適合用於STI (淺溝道隔離)CMP製程。 為了達成該等目標,本發明提供一種製備氧化鈽粉末 、方法包3以下步驟:快速加熱一鈽化合物達700 C至looot之溫度;於7〇〇u l〇〇〇t^溫度假燒該錦 口物以形成假燒氧化鈽;以及,快速冷卻該煆燒氧化 鈽至15 c至30 C之溫度。較佳地,煆燒該鈽化合物之步 驟執行達10分鐘至2小時’在快速加熱步驟中,飾化合 物以20°C/分至90(TC/分之加熱速度加熱,且在快速冷卻 步驟中,煆燒氧化鈽以2(rc/分至4〇(rc/分之冷卻速度冷 部。本發明亦提供一種具有氧化鈽的漿料組成物,其包 3 .基於該漿料組成物之總重量,重量百分比為〇 1%至 10%的氧化鈽粒子;以及基於該等氧化鈽粒子之重量, 重量百分比為2❶/。到20¼的分散劑;以及平衡量的水。 本發明中用於製備氧化鈽粉末的方法藉由在煆燒製程 期間快速加熱及快速冷卻,而產生微裂隙於氧化鈽粒子 6 201041805 (研磨粒…表面上。該所產生的 :表面以及低粒子密度,且易於受外部衝擊而破;:: 壓力Π明之研磨粒子在晶圓研磨製程期間容易因外部 壓力破裂’因而減少研磨表面上形成微刮痕 磨粒子也會發生在研磨晶圓中。因此, ^ 成物具有高研磨速度以及古研磨選㈣明之漿料組Accordingly, it is an object of the present invention to provide a method for preparing a ceria powder, and a 'hyperbum composition having the cerium oxide powder, which has high polishing speed and high polishing selectivity, and Reduce micro-marks in the chemical mechanical polishing process. Another object of the present invention is to provide a method for preparing cerium oxide powder, and a cerium composition having the oxidized powder, which is particularly suitable for use in an STI (Shallow Channel Isolation) CMP process. In order to achieve the above objectives, the present invention provides a method for preparing cerium oxide powder, and the method includes the following steps: rapidly heating a hydrazine compound to a temperature of 700 C to looot; and submerging the koji at a temperature of 7 〇〇ul〇〇〇t^ To form a pseudo-sintered yttrium oxide; and to rapidly cool the yttrium-doped yttrium oxide to a temperature of 15 c to 30 C. Preferably, the step of calcining the ruthenium compound is carried out for 10 minutes to 2 hours. In the rapid heating step, the decorative compound is heated at a heating rate of 20 ° C / min to 90 (TC / min, and in the rapid cooling step煆 钸 钸 钸 钸 2 2 2 2 2 2 2 rc rc rc rc rc rc rc rc rc rc rc rc rc rc rc rc rc rc rc rc rc rc rc rc rc rc rc rc rc rc rc rc rc rc rc rc The weight percentage is 〇1% to 10% of cerium oxide particles; and the weight percentage is 2 ❶/. to 201⁄4 based on the weight of the cerium oxide particles; and a balanced amount of water. The method of yttrium oxide powder is produced by rapid heating and rapid cooling during the sinter firing process to produce micro-cracks on the surface of cerium oxide particles 6 201041805 (abrasive grains... which are produced: surface and low particle density, and are susceptible to external Breaking and breaking;:: Pressure-sensitive abrasive particles are easily broken by external pressure during the wafer grinding process', thus reducing the formation of micro-scratches on the abrasive surface. The abrasive particles also occur in the polished wafer. Therefore, the product has a high research And (iv) selected from ancient polishing speed of the slurry is set out

疋又乂及问研磨選擇性,且特別適合STI (淺溝道隔離)CMP製程。 【實施方式】 藉由參考隨後詳細的說明書内容可更妥善瞭解本發明 之更完整的價值以及其許多值得注意的優點。 本發明之-種製備氧化飾粉末的方法,其包含以下步 驟:快速加熱一筛化合物S 7〇〇U 1〇〇(rc之溫度(較 佳為750°c至95(rc);於700°c至100(TC之溫度(較佳 為750 C至950°c )煆燒該鈽化合物以形成煆燒氧化鈽; 〇 卩及,快速冷卻該煆燒氧化鋅i 15U 30。(:之溫度,較 佳為1 8 c至28 c ’更佳為室溫(25)。該詞彙「假燒」 意指一種熱處理製程,其於高溫加熱一材料以全然或部 份移除材料中可揮發之成份。在本發明中,鈽化合物藉 由煆燒而轉化成氧化鈽(研磨顆粒)。例如,藉由煆燒, 一氧化碳(C〇2)和水(H20)從碳酸鈽(Ce2(c〇3)3. 6H2〇) 中移除以生產氧化鈽(2Ce〇2 )。 在本發明中,煆燒溫度可根據鈽化合物的種類而改 7 201041805 變’且其為約700°C至約100(TC,於杜达 較佳為約750。(:至約 950°C。較佳地,煆燒鈽化合物之步 乂驟執仃長達10分鐘 至2小時,較佳為15至90分鐘(嘏 V版魔時間)。倘若煆燒 時間少於Π)分鐘’則鈽化合物的概燒會不完整且氧化飾 會以不當的方式形成。倘若煆燒時間超過2小時,所生 產的氧化鈽之固結度會過度增加,固 长 0 77 固體乳化鈽會在研磨 表面(諸如晶圓)上形成刮痕,且立泛π、# R 且其為經濟效益上不受 期望的。倘若假燒溫度不在上述範圍内,鈽化合物之锻 燒會執行得不完整或過度’而氧化鈽不會具有期望的性 質。倘若快速冷卻溫度不在上述範圍内,微裂隙會不適 當地形成於氧化飾粒子的表面上。It also asks for grinding selectivity and is especially suitable for STI (Shallow Trench Isolation) CMP processes. [Embodiment] The more complete value of the present invention and its many notable advantages can be better understood by referring to the following detailed description. The method for preparing an oxidized decorative powder of the present invention comprises the steps of: rapidly heating a sieve compound S 7 〇〇 U 1 〇〇 (temperature of rc (preferably 750 ° C to 95 (rc); at 700 ° C to 100 (the temperature of TC (preferably 750 C to 950 ° C) sinters the bismuth compound to form bismuth oxide ruthenium; and rapidly cools the bismuth-fired zinc oxide i 15U 30. (: temperature, Preferably, it is preferably from 18 c to 28 c', preferably room temperature (25). The term "fake-burning" means a heat treatment process in which a material is heated at a high temperature to completely or partially remove volatile components of the material. In the present invention, the ruthenium compound is converted into ruthenium oxide (abrasive particles) by calcination. For example, by calcination, carbon monoxide (C〇2) and water (H20) from cesium carbonate (Ce2(c〇3) 3. 6H2〇) is removed to produce cerium oxide (2Ce 〇 2 ). In the present invention, the sinter temperature can be changed according to the type of the cerium compound 7 201041805 ' and it is about 700 ° C to about 100 (TC Preferably, it is about 750 in Duda. (: to about 950 ° C. Preferably, the step of calcining the compound is carried out for a period of from 10 minutes to 2 hours, preferably 15 minutes. 90 minutes (嘏V version magic time). If the simmering time is less than Π) minutes, the sinter compound will be incomplete and the oxidized decoration will be formed in an improper way. If the simmering time exceeds 2 hours, the produced The degree of consolidation of yttrium oxide will increase excessively, and a solid length of 0 77 solid emulsified enamel will form scratches on the abrasive surface (such as wafers), and will be π, # R and it is economically undesired. If the calcination temperature is not within the above range, the calcination of the antimony compound may be performed incompletely or excessively, and the antimony oxide will not have the desired properties. If the rapid cooling temperature is not within the above range, the microcracks may be improperly formed in the oxide decoration. On the surface of the particle.

較佳地,在快速加熱步驟中,鈽化合物以2(rc/分至 _t/分、較佳為50t/分至5〇〇。。/分之加熱速度從15 C至30 C、較佳為18 C至28°C、更佳為室溫(25°C ) 加熱。在快速冷卻步驟中,該煆燒氧化鈽以2〇<>c/分至 400°C/分、較佳為2〇ΐ/分至1〇(rc/分之冷卻速度冷卻。 倘若決速加熱速度不在上述範圍内,氧化鈽會不完整地 形成,或者微裂隙會不充分地形成於氧化鈽粒子表面 上。倘若快速冷卻速度不在上述範圍内,微裂隙會不充 分地形成於氧化鈽粒子表面上。 在本發明中’該快速加熱步驟、煆燒步驟以及快速冷 卻步驟執行至少1次,較佳為重複執行超過丨次,特別 為2或3久。藉由重複執行該快速加熱步驟,煆燒步驟 及快速冷卻步驟,氧化鈽粒子的表面變得更不規則,而 201041805 氧化鈽粒子的粒子密度更減少,且氧化鈽粒子可更容易 被外部衝擊摧毀。用於生產氧化鈽的習知鈽化合物可用 做本發明之鈽化合物。鈽化合物的較佳範例可選自由碳 酸鈽、氫氧化鈽、硫酸鈽、草酸鈽及其混合物所構成之 群組。更佳之鈽化合物為碳酸鈽。Preferably, in the rapid heating step, the cerium compound is heated at a rate of from 2 Cc to 30 cc, preferably from 50 t/min to 5%, preferably from 50 t/min to 5 Torr. It is heated at 18 C to 28 ° C, more preferably at room temperature (25 ° C.) In the rapid cooling step, the cerium oxide is enthalpy of 2 〇 <> c / min to 400 ° C / min, preferably It is cooled at a cooling rate of 2 〇ΐ / min to 1 〇 (rc / min.) If the deceleration heating rate is not within the above range, yttrium oxide may be formed incompletely, or micro-cracks may be insufficiently formed on the surface of the cerium oxide particles. If the rapid cooling rate is not within the above range, microcracks may be insufficiently formed on the surface of the cerium oxide particles. In the present invention, the rapid heating step, the calcining step, and the rapid cooling step are performed at least once, preferably repeating. Execute more than one time, especially 2 or 3. For the repeated heating step, the calcining step and the rapid cooling step, the surface of the cerium oxide particles becomes more irregular, and the particle density of the 201041805 cerium oxide particles is further reduced. And cerium oxide particles can be more easily destroyed by external impact. A conventional cerium compound which produces cerium oxide can be used as the cerium compound of the present invention. A preferred example of the cerium compound may be selected from the group consisting of cerium carbonate, cerium hydroxide, cerium sulfate, cerium oxalate, and mixtures thereof. It is barium carbonate.

藉由本發明t方法製備的氧化鈽m繞射圖中顯示 -主峰,其2Θ值為27。至30。;以及一次峰,其2❹值為 3〇至35。’主峰及次峰的強度比(面積比即主峰/次 峰)為等於或超過3.0。氧化鈽粉末(粒子)的平均粒子 尺寸為2〇nm至50nm,較佳為25_至45細。欲計算 氧化鈽粉末的粒子(晶體)尺寸,可藉由⑽⑽方程 式結合利用由氧化鈽粉末之χ光繞射分析所決定的主峰 之半高寬(FWHM)值。偏若氧化鈽粉末的粒子尺寸少 ; m則CMP製程中研磨速度及研磨選擇性會劣 化。倘若氧化鈽粉末的粒子尺寸超過5〇職,在cMp製 程中微到痕會形成於研磨表面上。 本發明的衆料組成物包括氧化飾粒子,且特別適合用 於微刮痕會嚴會次彳卜京道Μ -., I嚴更名化牛導體凡件品質及生產率的The ruthenium oxide m diffraction pattern prepared by the t method of the present invention shows a - main peak having a Θ value of 27. To 30. And a peak with a value of 3〇 to 35. The intensity ratio (area ratio, main peak/secondary peak) of the main peak and the secondary peak is equal to or more than 3.0. The cerium oxide powder (particles) has an average particle size of from 2 Å to 50 nm, preferably from 25 to 45 Å. To calculate the particle (crystal) size of the cerium oxide powder, the full width at half maximum (FWHM) value of the main peak determined by the dioptric diffraction analysis of the cerium oxide powder can be combined by the equation (10)(10). The particle size of the cerium oxide powder is small; m is the deterioration of the polishing rate and the polishing selectivity in the CMP process. If the particle size of the cerium oxide powder exceeds 5 ,, a slight trace will be formed on the polished surface in the cMp process. The mass composition of the present invention comprises oxidized particles, and is particularly suitable for use in micro-scratches, which will be strictly controlled by the second-instance, and the quality and productivity of the beef conductors.

Mp製程中。本發明之漿料組成物包括:基於該衆料組 成物之總重量,重量百分比為請至iq%(較佳為〇 5% 至5%\的氧化鋅粒以及基於該等氧化鈽粒子之重量 (即該等氧化鈽粒子之重量&⑽%),重量百分比為 到:的分散劑,其較佳為重量百分比3%至15% ;以及 平衡買的水’較佳為去離子水或純水。倘若氧化飾粒子 201041805 的量少於重量百分比〇 J 0/〇 私2 ή 則乳化鈽粒子不足以如研磨 粒子般運作,其會劣化 唧熠逮度及研磨選擇性。倘若氣 化鈽粒子的量超過重量百分 倘右氧 隹… 里亶白刀比10°/。,則氧化鈽粒子會聚 票、形成晶團或沉殿,其會續遙將 /、f礴導漿枓組成物相分離,且 會進—步促使CMP製程中形成微到痕。 Ο ο 本發明之襞料組成物中,添加分散劑以均勾地分散漿 料組成物中的研磨粒子。做為本發明之分散劑,可使用 習知用於CMP漿料組成物的分散劑。用於本發明之分散 劑之例子可包括碳酸或其鹽類。較佳的分散劑為多:‘ 或其鹽類,最佳的分散劑為$丙烯酸或其鹽类員,諸如聚 丙烯酸的銨鹽。碳酸之特定實施例包括:戊二酸、葡萄 糖酸、乙醇酸、月桂酸、乳酸、頻果酸、丙二酸、戍酸、 檸檬酸、硬脂酸、丁二酸、乙酸、草酸、己二酸、癸酸、 己酸、辛酸、甲酸、丁烯二酸、苯二甲酸、丙酸、丙嗣 酸、酒石酸、聚丙烯酸、其鹽類及其混合物等。碳酸鹽 類包括習知鹽類,諸如鈉鹽、銨鹽及鉀鹽等。做為分散 劑,可使用至少一種碳酸或其鹽類。當分散劑為多羧酸 時’分散劑的重量平均分子量為5000至20000,較佳為 10000至15000。倘若分散劑的重量平均分子量少於5〇〇〇 或超過20000 ’漿料組成物的分散會不充分。倘若分散 劑的量少於重量百分比2% (基於該等氧化鈽粒子之重 量)’氧化鈽在漿料組成物中會分散得不充分,且會$ 集、形成晶團或沉澱。倘若分散劑的量超過重量百分比 20% (基於氧化鈽粒子之重量),過量的分散劑會成為雜 10 201041805 質’且其不具任何額外優點。 ❹ 藉由將氧化姉粒子及分散劑添加水中可製備氧化飾裝 料組成物》當分散氧化飾粒子於水中時,分散設備可用 於防止漿料組成物中氧化鈽粒子聚集。可使用習知的攪 拌器或分散裝置做為分散設備。分散設備的特定範例包 括:振動器、均質機、塗料振動器、超音波均質機、珠 磨機、輥磨機、頂磨機(apexmill)、振動球磨機、其組 合。在使用珠磨機的實例中,習知珠狀物(諸如氧化鍅 珠狀物、氧化鋁珠狀物及玻璃珠狀物等)可用做分散^ 質。 此後,提供較佳的範例及比較性的範例以利瞭解本發 明。然而’本發明不限於隨後的範例。 [範例1]氧化鈽之製備 將在室溫(251)下於翻碗中的3() g的碳酸鈽粉末緩 〇 慢地推入7〇rc (煆燒溫度)的管狀爐中。當推動銘碗 時,控制碗的移動速度以致碳酸鈽粉末的加熱速度為ι〇〇 c /分。當碳酸鈽粉末的溫度增加至煆燒溫度() 夺碳飾私末煆燒達!小時。然後,翻碗移動進入乾 燥器’且將假燒的氧化鈽冷卻至室S (冷卻速度:500c / 刀)以獲传贯色粉末。冷卻速度可藉由控制環繞乾燥器 的冷卻水溫度而調整。藉由x光繞射分析,可確認黃色 伞刀末為氧化鈽。X光繞射圖中的氧化飾粉末主峰之半高 寬(FWHM)值及Scherrer方程式用於喊定氧化飾粒子 201041805 '=粒子尺寸,其為約28 nm (表1 )。範例j中所生 產的氧化鈽粉末TEM (穿透式電子顯微鏡)圖顯示 1圖。 、示 [聋已例2至4]氧化鈽之製備 。除了將煆燒溫度從70(rc改變至8〇〇r (範例2)、9〇〇 C :範例3)及1〇〇(rc (範例4)之外,黃色粉末為根In the Mp process. The slurry composition of the present invention comprises: based on the total weight of the mass composition, the weight percentage is up to iq% (preferably 〇5% to 5%\ of zinc oxide particles and based on the weight of the cerium oxide particles) (i.e., the weight of the cerium oxide particles & (10)%), the weight percentage of the dispersant to: preferably 3% to 15% by weight; and the balance of purchased water 'preferably deionized water or pure If the amount of oxidized particles 201041805 is less than the weight percentage 〇J 0/〇私 2 ή, the emulsified cerium particles are not enough to work like abrasive particles, which will deteriorate the enthalpy and grinding selectivity. If the amount exceeds the weight percentage, if the right oxime is 10°/, the cerium oxide particles will accumulate votes, form a crystal cluster or sink the temple, which will continue to separate the composition phase of the / 礴 礴 礴Separation, and further progress to promote the formation of microscopic marks in the CMP process. ο ο In the composition of the present invention, a dispersing agent is added to uniformly disperse the abrasive particles in the slurry composition. For the agent, a dispersing agent conventionally used for the CMP slurry composition can be used. Examples of the dispersing agent of the present invention may include carbonic acid or a salt thereof. Preferred dispersing agents are many: 'or a salt thereof, and the most preferred dispersing agent is acrylic acid or a salt thereof, such as an ammonium salt of polyacrylic acid. Specific examples of carbonic acid include: glutaric acid, gluconic acid, glycolic acid, lauric acid, lactic acid, frequency acid, malonic acid, citric acid, citric acid, stearic acid, succinic acid, acetic acid, oxalic acid, hexane Acid, citric acid, caproic acid, octanoic acid, formic acid, butenedioic acid, phthalic acid, propionic acid, propionic acid, tartaric acid, polyacrylic acid, salts thereof, mixtures thereof, etc. Carbonates include conventional salts, For example, a sodium salt, an ammonium salt, a potassium salt, etc. As the dispersing agent, at least one carbonic acid or a salt thereof can be used. When the dispersing agent is a polycarboxylic acid, the weight average molecular weight of the dispersing agent is from 5,000 to 20,000, preferably 10,000. To 15000. If the weight average molecular weight of the dispersant is less than 5 〇〇〇 or more than 20,000', the dispersion of the slurry composition may be insufficient. If the amount of the dispersant is less than 2% by weight (based on the weight of the cerium oxide particles) )' cerium oxide in the slurry composition Dispersion is insufficient, and it will collect, form crystal clusters or precipitate. If the amount of dispersant exceeds 20% by weight (based on the weight of cerium oxide particles), the excess dispersant will become miscellaneous 10 201041805 and it does not have any Additional advantages ❹ An oxidized decorative composition can be prepared by adding cerium oxide particles and a dispersing agent to water. When the dispersed oxidized particles are in water, the dispersing device can be used to prevent aggregation of cerium oxide particles in the slurry composition. Conventional agitators or dispersing devices are used as dispersing devices. Specific examples of dispersing devices include: vibrators, homogenizers, paint shakers, ultrasonic homogenizers, bead mills, roll mills, top mills (apexmill), Vibratory ball mills, combinations thereof. In the case of using a bead mill, conventional beads such as cerium oxide beads, alumina beads, glass beads, and the like can be used as the dispersion. Hereinafter, preferred examples and comparative examples are provided to facilitate the understanding of the present invention. However, the invention is not limited to the following examples. [Example 1] Preparation of cerium oxide 3 () g of cerium carbonate powder in a tumbling bowl at room temperature (251) was slowly pushed into a tubular furnace of 7 〇 rc (steaming temperature). When the bowl is pushed, the movement speed of the bowl is controlled so that the heating rate of the strontium carbonate powder is ι 〇〇 c / min. When the temperature of the barium carbonate powder is increased to the temperature of the calcination () hour. Then, the bowl was moved into the dryer ' and the sintered yttria was cooled to the chamber S (cooling rate: 500 c / knife) to obtain a color-transparent powder. The cooling rate can be adjusted by controlling the temperature of the cooling water surrounding the dryer. By x-ray diffraction analysis, it was confirmed that the yellow umbrella blade was yttrium oxide. The half-height width (FWHM) of the main peak of the oxidized powder in the X-ray diffraction pattern and the Scherrer equation are used to smear the oxidized particles 201041805 '=particle size, which is about 28 nm (Table 1). The TEM (transmissive electron microscope) image of the cerium oxide powder produced in Example j shows 1 image. , [聋 聋 Example 2 to 4] Preparation of cerium oxide. In addition to changing the calcination temperature from 70 (rc to 8〇〇r (example 2), 9〇〇 C: example 3) and 1〇〇 (rc (example 4), the yellow powder is root

範例1之方法製備。藉由χ光繞射分析,可確認黃色 ^末為氧化鈽。根據範例1的方法確定氧化鈽粒子的平 ^粒子尺寸,其於表1中提出。範例2至4中所生產的 #飾奋末ΤΕΜ (穿透式電子顯微鏡)圖顯示於第 至第4圖。 [範例5至8]氧化鈽之製備 除了將煆燒溫度從70(rc改變至9〇(rc及將加熱速度 〇 從100 C /分改變至2〇°C /分(範例5)、50°c /分(範例6)、 〇 C /刀(範例7 )及9〇(rc /分(範例8 )之外,黃色粉 2根據範例1之方法製備。藉由X光繞射分析,可確 ^只色粉末為氧化鈽。根據範例i的方法確定氧化鈽粒 的平均粒子尺寸,其於表1中提出。範例5至8中所 生產的氧化鈽粉末TEM (穿透式電子顯微鏡)圖顯示於 第5圖至第8圓。 [範例9至U]氧化鈽之製備 12 201041805 除了將煆燒溫度從70(TC改變至900°C、將加熱速度從 l〇〇°C/分改變至45(TC/分、及將冷卻速度從5(rc/分改變 至20°C/分(範例9)、100艺/分(範例1〇)及200t/分 (範例11 )之外,黃色粉末為根據範例1之方法製備。 藉由X光繞射分析,可確認黃色粉末為氧化鈽。根據範 例1的方法確定氧化鈽粒子的平均粒子尺寸,其於表i 中長:出範例9至11中所生產的氧化飾粉末TEM (穿 透式電子顯微鏡)圖顯示於第9圖至第u圖。 [範例12]氧化鈽之製備 除了將煆燒溫度從7G(rc改變至9⑽。c、將加熱速度從 l〇〇C/分改變至45(rc/分、將假燒時間從!小時改變成 3:分鐘且進一步再-次執行加熱步驟、假燒步驟及冷卻Prepared by the method of Example 1. By calender diffraction analysis, it can be confirmed that the yellow color is yttrium oxide. The flat particle size of the cerium oxide particles was determined according to the method of Example 1, which is presented in Table 1. The #饰奋ΤΕΜ (transmission electron microscope) images produced in Examples 2 to 4 are shown in the first to fourth figures. [Examples 5 to 8] Preparation of cerium oxide except for changing the calcination temperature from 70 (rc to 9 〇 (rc and changing the heating rate 100 from 100 C / min to 2 〇 ° C / min (example 5), 50 °) In addition to c / min (example 6), 〇 C / knife (example 7) and 9 〇 (rc / min (example 8), yellow powder 2 was prepared according to the method of Example 1. By X-ray diffraction analysis, it was confirmed ^Color-only powder is cerium oxide. The average particle size of cerium oxide particles was determined according to the method of Example i, which is presented in Table 1. The TEM (transmissive electron microscope) image of cerium oxide powder produced in Examples 5 to 8 shows 5 to 8 circles. [Example 9 to U] Preparation of yttrium oxide 12 201041805 In addition to changing the temperature of simmering from 70 (TC to 900 ° C, the heating rate is changed from l 〇〇 ° C / min to 45 (TC/min, and the cooling rate from 5 (rc/min to 20 °C/min (example 9), 100 y/min (example 1 〇) and 200 t/min (example 11), the yellow powder is Prepared according to the method of Example 1. It was confirmed by X-ray diffraction analysis that the yellow powder was cerium oxide. The average particle size of the cerium oxide particles was determined according to the method of Example 1, which is long in Table i: Example 9 to 1 The TEM (transmission electron microscope) image of the oxidized powder produced in 1 is shown in Fig. 9 to Fig. u. [Example 12] The preparation of yttrium oxide was changed from 7 G (rc to 9 (10). Change the heating rate from l〇〇C/min to 45 (rc/min, change the simmering time from ! hours to 3: minutes and further perform the heating step, the smoldering step and the cooling again

*驟之外’頁色粉末為根據範例1之方法製備。藉由X 〇 m析’可確認黃色粉末為氧化飾。根據範例!的 、、確定軋化鈽粒子的平均粒子尺 所生產的氧化鈽粉末^ 顯微鏡)圖顯示於第12圖。 [範例13]氧化鈽之製備 除了將煆燒時間從3〇分 办 刀鐘改變成2〇分鐘且進一步比 範例1再多2次執行加熱 進 AL ^ . 振·燒步驟及冷卻步驟之 分析:=為:二1“"2之方法製備。藉由X光繞射 ° w h末為氧㈣。根據範例1的方法蜂 13 201041805 定氧化鄉粒子的平均粒子尺寸,其於表1中提出。範例 13中所生產的氧化鈽粉末ΤΕΜ(穿透式電子顯微鏡)圖 顯示於第13圖。 [範例I4]氧化鈽之製備 除了將煆燒時間從30分鐘改變成15分鐘且進一步比 範例1再乡3二欠執行加熱步驟、料步驟及冷卻步驟之 外’黃色粉末為根據範例12之方法製備。藉由X光繞射 分析,可確認黃色粉末為氧化鈽。根據範例丨的方法確 定氧化鈽粒子的平均粒子尺寸,其於表丨中提出。範例 14中所生產的氧化鈽粉末TEM(穿透式電子顯微鏡)圖 顯示於第1 4圖。 [比較性範例1 ]氧化鈽之製備 將在室溫(251 )下於鉑碗中的30 g碳酸鈽粉末緩慢 〇 地推入900°c (煆燒溫度)的管狀爐中。當推動鉑碗時, 控制碗的移動速度以致碳酸鈽粉末的加熱速度為1(rc / 分。當碳酸鈽粉末的溫度增加至煆燒溫度(9〇〇〇c )時, 碳酸鈽粉末在90(TC煆燒達1小時。然後,在管狀爐中 將煆燒的氧化鈽冷卻至室溫(冷卻速度:i 〇 〇C /分)以獲 得黃色粉末。藉由X光繞射分析,可確認黃色粉末為氧 化铈。根據範例1的方法確定氧化鈽粒子的平均粒子尺 寸,其於表1中提出。比較性範例i中所生產的氧化鈽 粉末TEM (穿透式電子顯微鏡)圖顯示於第15圖。 201041805* The smear powder was prepared according to the method of Example 1. It was confirmed by X 〇 m 'the yellow powder was an oxidized decoration. According to the example! The yttrium oxide powder produced by the average particle size of the rolled ruthenium particles is shown in Fig. 12. [Example 13] The preparation of cerium oxide was carried out except that the calcination time was changed from 3 Torr to 2 〇 minutes and further heated to AL ^ 2 times more than Example 1. The analysis of the vibration and burning steps and the cooling step: = is: 2 1 "2 method preparation. By X-ray diffraction ° wh is oxygen (4). According to the method of Example 1, bee 13 201041805 determines the average particle size of the oxidized town particles, which is presented in Table 1. The yttrium oxide powder yttrium (transmissive electron microscope) pattern produced in Example 13 is shown in Fig. 13. [Example I4] Preparation of cerium oxide except that the smoldering time was changed from 30 minutes to 15 minutes and further than Example 1 In addition to the heating step, the material step and the cooling step, the yellow powder was prepared according to the method of Example 12. It was confirmed by X-ray diffraction analysis that the yellow powder was cerium oxide. The cerium oxide was determined according to the method of the example 丨. The average particle size of the particles is presented in the table. The TEM (transmissive electron microscope) image of the cerium oxide powder produced in Example 14 is shown in Figure 14. [Comparative Example 1] Preparation of cerium oxide will be Platinum at room temperature (251) The 30 g of strontium carbonate powder was slowly pushed into a tubular furnace at 900 ° C (baked temperature). When the platinum bowl was pushed, the movement speed of the bowl was controlled so that the heating rate of the strontium carbonate powder was 1 (rc / min. When the temperature of the barium carbonate powder is increased to the calcination temperature (9 ° C ), the barium carbonate powder is calcined at 90 °C for 1 hour. Then, the calcined barium oxide is cooled to room temperature in a tubular furnace ( Cooling rate: i 〇〇C / min) to obtain a yellow powder. It was confirmed by X-ray diffraction analysis that the yellow powder was cerium oxide. The average particle size of cerium oxide particles was determined according to the method of Example 1, which is shown in Table 1. The TEM (transmission electron microscope) image of the cerium oxide powder produced in Comparative Example i is shown in Fig. 15. 201041805

表1 製備氧化鈽的條件 加熱速度 (〇C/分) 煆燒溫度 (°c) 煆燒時 間 (分) 冷卻速度 (〇C/分) 額外加熱 /冷卻 平均粒子 尺寸 (nm) 範例1 100 700 60 50 28 範例2 800 30 範例3 900 36 範例4 1000 42 範例5 20 900 36 範例6 50 35 範例7 450 31 範例8 900 29 範例9 450 20 31 範例10 100 38 範例11 200 39 範例12 30 50 1次 35 範例13 20 2次 34 範例14 15 3次 33 比較性 範例1 10 60 10 44 [範例1 5至28及比較性範例2]氧化鈽漿料組成物之 製備與評估 於預混合容器中緩慢添加1.5 kg的去離子水以及1.05 g的聚丙烯酸之銨鹽,並將之混合。然後,將15 g的於 範例1至14及比較性範例1中製備的氧化鈽粉末個別添 加至混合物中。該混合物以使用氧化錘珠狀物的珠磨機 分散30分鐘以生產氧化鈽漿料組成物(範例1 5至28及 15 201041805 比較性範例2 )。 漿料組成物評估 具有一氧化矽層(厚度:丨〇 μπι)的完整矽晶圓(直 徑8英吋)以及具有氮化矽層的完整矽晶圓(直徑8英 吋)以範例1 5至2 8及比較性範例2中的每一漿料組成 物及以美國Entrepix,Inc的IPEC AVANTI 472研磨裝置 〇 研磨。二氧化矽層以TEOS (石夕酸乙酯)_電漿CVD (化 學氣相沉積)法製備,而氮化矽層以低壓CVD方法製 備。以4psi之向下的研磨頭壓力、6〇rpm之機台速度、 50rPm的研磨頭速度及15〇cc/分的毅料流速執行研=! 分鐘。研磨後,晶圓以去離子水清洗並且乾燥。以光學 干涉儀測量殘留在晶圓上的二氧化矽層及氮化矽層的2 度,而確定二氧化矽層及氮化矽層的研磨速度,如表2 所示。亦測量到尺寸在0.3㈣至2 5 _之間的微到痕 〇 數’其亦於表2中提出。 評估 ~~~ 氧化物層的研磨速 氮化物層的研磨 --—....... 度(A/min) 速度(A /min) 微刮痕數 範例15 ~~-...... —· 2845 57 —~~__ 54 範例16 3194 72 Γ ^ 61 16 201041805Table 1 Conditions for preparing yttrium oxide Heating rate (〇C/min) Sintering temperature (°c) Sintering time (minutes) Cooling rate (〇C/min) Additional heating/cooling average particle size (nm) Example 1 100 700 60 50 28 Example 2 800 30 Example 3 900 36 Example 4 1000 42 Example 5 20 900 36 Example 6 50 35 Example 7 450 31 Example 8 900 29 Example 9 450 20 31 Example 10 100 38 Example 11 200 39 Example 12 30 50 1 Example 35 Example 13 20 2 times 34 Example 14 15 3 times 33 Comparative Example 1 10 60 10 44 [Examples 1 5 to 28 and Comparative Example 2] Preparation and evaluation of cerium oxide slurry composition in a premixed container Add 1.5 kg of deionized water and 1.05 g of ammonium polyacrylate and mix. Then, 15 g of the cerium oxide powders prepared in Examples 1 to 14 and Comparative Example 1 were individually added to the mixture. The mixture was dispersed in a bead mill using oxidized hammer beads for 30 minutes to produce a cerium oxide slurry composition (Examples 15 to 28 and 15 201041805 Comparative Example 2). The slurry composition was evaluated as a complete tantalum wafer (8 inches in diameter) having a tantalum oxide layer (thickness: 丨〇μπι) and a complete tantalum wafer (8 inches in diameter) having a tantalum nitride layer as an example 15 to 2 8 and each of the slurry compositions of Comparative Example 2 were ground with an IPEC AVANTI 472 grinding apparatus of Entrepix, Inc., USA. The ruthenium dioxide layer was prepared by TEOS (electrodesulfide)-plasma CVD (chemical vapor deposition) method, and the tantalum nitride layer was prepared by a low pressure CVD method. The grind head pressure of 4 psi, the machine speed of 6 rpm, the head speed of 50 rPm, and the flow rate of 15 〇 cc/min were performed for the test =! minutes. After grinding, the wafer was rinsed with deionized water and dried. The optical interferometer was used to measure the cerium oxide layer and the tantalum nitride layer remaining on the wafer at 2 degrees to determine the polishing rate of the cerium oxide layer and the cerium nitride layer, as shown in Table 2. A micro-to-mark ’ number between 0.3 (4) and 2 5 _ was also measured, which is also presented in Table 2. Evaluation ~~~ Grinding of the oxide layer of the oxide layer --.......degree (A/min) speed (A / min) Example of micro-scratch number 15 ~~-.... .. —· 2845 57 —~~__ 54 Example 16 3194 72 Γ ^ 61 16 201041805

範例17 3318 81 63 範例18 3452 102 72 範例19 3128 74 65 範例20 3217 65 67 範例21 3026 57 48 範例22 2766 51 71 範例23 3157 81 66 範例24 3311 48 52 範例25 2631 50 75 範例26 3411 55 45 範例27 3215 53 37 範例28 3029 49 36 比較性範例 2 2455 107 176 如表2所示,與具有習知氧化鈽粒子(比較性範例1 ) 之漿料組成物相較,具有本發明之氧化飾粒子(範例1 至14 )之漿料組成物具有高的氧化物層研磨速度以及相 對低的氮化物層研磨速度,且乃至於具有氧化物層與氮 化物層間高的研磨選擇性。此外,如第1至14圖所示, 本發明之氧化鈽粒子具有多方向、不規則及黯淡的晶格 17 201041805 樣式。此不規則的晶格樣式是由氧化鈽粒子表面上微裂 隙所形成,該為裂隙是由控制加熱速度及冷卻速度所生 成。本發明之氧化鈽研磨粒子在研磨製程中易於受外部 壓力而破裂,其減少研磨層上的微刮痕生成。破裂的研 磨粒子亦發生在晶圓的研磨中。因此,本發明之漿料具 有高研磨速度及高研磨選擇性,且特別適合用於STI(淺 溝道隔離)CMP製程。 從範例2 1 (範例7 )及範例26至28 (範例12至14 ), 藉由進一步超過1次執行加熱步驟及冷卻步驟,漿料組 成物對氧化物層的研磨速度增加,而對氮化物層的研磨 速度減少,且微刮痕數減少。當比較第7圖及第12至 14圖,第12圖至第14圖中的研磨粒子之晶格樣式較第 7圖中的研磨粒子之晶格樣式更不規則。此差異是由於 藉由製備氧化鈽研磨粒子時重複快速加熱步驟及快速冷 步驟造成研磨粒子上形成的微裂隙增加之故。 【圖式簡單說明】 第1圖至第14圖是個別由本發明之範例1至範例i 4 所生產的氧化鈽粒子的TEM照片。 第15圖是比較性範例1所生產的氧化鈽粒子之tem 照片。 【主要元件符號說明】 201041805Example 17 3318 81 63 Example 18 3452 102 72 Example 19 3128 74 65 Example 20 3217 65 67 Example 21 3026 57 48 Example 22 2766 51 71 Example 23 3157 81 66 Example 24 3311 48 52 Example 25 2631 50 75 Example 26 3411 55 45 Example 27 3215 53 37 Example 28 3029 49 36 Comparative Example 2 2455 107 176 As shown in Table 2, the oxide composition of the present invention is compared with the slurry composition having the conventional cerium oxide particles (Comparative Example 1) The slurry composition of the particles (Examples 1 to 14) has a high oxide layer polishing rate and a relatively low nitride layer polishing rate, and has a high polishing selectivity between the oxide layer and the nitride layer. Further, as shown in Figs. 1 to 14, the cerium oxide particles of the present invention have a multi-directional, irregular and dimmed lattice 17 201041805 pattern. This irregular lattice pattern is formed by microcracks on the surface of the cerium oxide particles, which are generated by controlling the heating rate and the cooling rate. The cerium oxide abrasive particles of the present invention are susceptible to cracking by external pressure during the grinding process, which reduces the generation of micro scratches on the abrasive layer. Cracked abrasive particles also occur in the grinding of the wafer. Therefore, the slurry of the present invention has a high polishing rate and high polishing selectivity, and is particularly suitable for use in an STI (Shallow Trench Isolation) CMP process. From Example 2 1 (Example 7) and Examples 26 to 28 (Examples 12 to 14), by further performing the heating step and the cooling step more than once, the polishing rate of the slurry composition on the oxide layer is increased, and the nitride is added. The polishing rate of the layer is reduced and the number of micro scratches is reduced. When comparing Fig. 7 and Figs. 12 to 14, the lattice pattern of the abrasive particles in Figs. 12 to 14 is more irregular than the lattice pattern of the abrasive particles in Fig. 7. This difference is due to the fact that the micro-cracks formed on the abrasive particles are increased by repeating the rapid heating step and the rapid cooling step by preparing the cerium oxide abrasive particles. BRIEF DESCRIPTION OF THE DRAWINGS FIGS. 1 to 14 are TEM photographs of cerium oxide particles individually produced by Examples 1 to 4 of the present invention. Fig. 15 is a photograph of a tem of cerium oxide particles produced in Comparative Example 1. [Main component symbol description] 201041805

Claims (1)

201041805 七、申請專利範圍: 1. 一種用於製備氧化鈽粉末的方法,其包含以下步驟: 快速加熱一鈽化合物達7 0 0 °C至1 〇 〇 〇 之溫度; 於700 C至1000 C之溫度煆燒該鈽化合物以形成假燒氧 化鈽;以及, 快速冷卻該煆燒氧化鈽至15t至3 0°C之溫度。 2·如請求項第1項所述之用於製備氧化鈽粉末之方法, ® 其中該煆燒該鈽化合物之步驟執行達1〇分鐘至2小時, 在該快速加熱步驟中,該鈽化合物以2(rc /分至9〇〇它/ 分之一加熱速度加熱,且在該快速冷卻步驟中,該瑕燒 氧化鈽以20。〇/分至4〇〇°C/分之一冷卻速度冷卻。 3. 如請求項第丨項所述之用於製備氧化鈽粉末之方法, 其中該快速加熱步驟、該煆燒步驟及該快速冷卻步驟執 ^ 行超過1次。 4. 如請求項第1項所述之用於製備氧化铈粉末之方法, 其中該鈽化合物選自由以下物質所構成之群組:碳酸 鈽、氫氧化鈽、硫酸鈽、草酸鈽及其混合物。 5. —種具有氧化鈽的漿料組成物’其包含: 基於該漿料組成物之總重量,重直百分比為0.1 %至1 〇 〇/〇 20 201041805 的氧化鈽粒子; 基於該等氧化鈽粒子之重量,重量百分比為2%到20%的 分散劑;以及 平衡量的水, 其中’氧化鈽粒子是由包含以下步驟之方法所製備:快 速加熱一鈽化合物達700°C至1〇〇〇。(:之溫度;於700。(: 至1000。(:之溫度煆燒該鈽化合物以形成煆燒氧化鈽;以 及,快速冷卻該煆燒氧化鈽至丨5 °c至3 0 之溫度。201041805 VII. Patent Application Range: 1. A method for preparing cerium oxide powder, comprising the steps of: rapidly heating a compound to a temperature of 700 ° C to 1 ;; at 700 C to 1000 C The ruthenium compound is calcined to form a pseudo-fired ruthenium oxide; and the bismuth oxide ruthenium is rapidly cooled to a temperature of from 15 t to 30 °C. 2. The method for preparing a cerium oxide powder according to claim 1, wherein the step of calcining the cerium compound is performed for 1 minute to 2 hours, and in the rapid heating step, the cerium compound is 2 (rc / min to 9 〇〇 it / heating at a heating rate, and in the rapid cooling step, the bismuth oxide enthalpy is cooled at a cooling rate of 20 〇 / min to 4 〇〇 ° C / min 3. The method for preparing a cerium oxide powder according to the above item, wherein the rapid heating step, the calcining step, and the rapid cooling step are performed more than once. 4. If the claim is the first item The method for preparing a cerium oxide powder, wherein the cerium compound is selected from the group consisting of cerium carbonate, cerium hydroxide, cerium sulfate, cerium oxalate, and mixtures thereof. Slurry composition 'comprising: cerium oxide particles having a percentage by weight of 0.1% to 1 〇〇 / 〇 20 201041805 based on the total weight of the slurry composition; based on the weight of the cerium oxide particles, the weight percentage is 2% to 20% of the dispersant; Measured water, where 'the cerium oxide particles are prepared by a method comprising the steps of: rapidly heating a compound up to 700 ° C to 1 〇〇〇. (: temperature; at 700. (: to 1000. (: The ruthenium compound is calcined to form a bismuth oxide ruthenium; and the bismuth oxide ruthenium is rapidly cooled to a temperature of from 5 ° C to 30 °. 21twenty one
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