TW201742138A - Set of compositions for polishing, pre-polishing composition, and method of polishing silicon wafer - Google Patents

Set of compositions for polishing, pre-polishing composition, and method of polishing silicon wafer Download PDF

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TW201742138A
TW201742138A TW106107058A TW106107058A TW201742138A TW 201742138 A TW201742138 A TW 201742138A TW 106107058 A TW106107058 A TW 106107058A TW 106107058 A TW106107058 A TW 106107058A TW 201742138 A TW201742138 A TW 201742138A
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polishing
composition
finishing
polishing composition
wafer
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TW106107058A
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TWI724117B (en
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土屋公亮
浅田真希
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福吉米股份有限公司
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00—Lapping machines or devices; Accessories
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/14—Anti-slip materials; Abrasives
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting

Abstract

Provided is a set of compositions for polishing with which it is possible to achieve a high-quality polished surface by reducing haze. This set of compositions for polishing is provided with: a finish polishing composition to be used in a finish polishing step of finish polishing a silicon wafer; and a pre-polishing composition to be used in a pre-polishing step, which is a polishing step preformed one step prior to the finish polishing step. A hydrophilicity parameter P1 of the pre-polishing composition, obtained from a standard test 1, is less than 100; a finishing accuracy parameter P2 of the pre-polishing composition, obtained from a standard test 2, is at most equal to 1000; and a polishing processability parameter F1 of the finish polishing composition, obtained from a standard test 3, is at most equal to 80.

Description

研磨用組成物套組、前研磨用組成物及矽晶圓之研磨方法 Grinding composition kit, pre-polishing composition, and polishing method of tantalum wafer

本發明係有關研磨用組成物套組、前研磨用組成物及矽晶圓之研磨方法。 The present invention relates to a polishing composition set, a front polishing composition, and a polishing method for a tantalum wafer.

為了降低矽晶圓之表面之濁度，曾出現各種有關研磨用組成物及研磨方法之提案(例如參考專利文獻1、2)。但近年來逐步提升有關矽晶圓之表面品質之要求水準，因此要求進一步改良該等技術。 In order to reduce the turbidity of the surface of the tantalum wafer, various proposals have been made regarding the polishing composition and the polishing method (for example, refer to Patent Documents 1 and 2). However, in recent years, the level of requirements for the surface quality of germanium wafers has been gradually increased, and further improvements in such technologies are required.

[先前技術文獻] [Previous Technical Literature] [專利文獻] [Patent Literature]

專利文獻1：日本國專利公報第5204960號 Patent Document 1: Japanese Patent Laid-Open No. 5204960

專利文獻2：日本國專利公開公報2015年第185672號 Patent Document 2: Japanese Patent Publication No. 185672, 2015

為了解決上述般先前技術所具有之問題點，本發明之課題為，提供可降低濁度而實現高品質之被研磨面之研磨用組成物套組，及前研磨用組成物及矽晶圓之研磨方法。 In order to solve the problems of the prior art described above, an object of the present invention is to provide a polishing composition set for polishing a surface that can reduce turbidity and to achieve high quality, and a pre-polishing composition and a silicon wafer. Grinding method.

為了解決前述課題，本發明一態樣之研磨用組成物套組之要旨為，備有使用於使矽晶圓進行精加工研磨之精加工研磨步驟之精加工研磨用組成物，與使用於精加工研磨步驟之前一階段之研磨步驟的前研磨步驟之前研磨用組成物的研磨用組成物套組中，標準試驗1所求取之前研磨用組成物之親水性參數P1為未達100，標準試驗2所求取之前研磨用組成物之精加工精準度參數P2為1000以下，標準試驗3所求取之精加工研磨用組成物之研磨加工性參數F1為80以下。 In order to solve the above problems, the gravitational composition kit of one aspect of the present invention has a finishing polishing composition for use in a finishing polishing step for finishing a tantalum wafer, and is used for fine polishing. In the polishing composition set of the polishing composition before the pre-grinding step of the grinding step before the grinding step, the hydrophilicity parameter P1 of the polishing composition before the standard test 1 is less than 100, the standard test The finishing precision parameter P2 of the polishing composition before the determination is 2 or less, and the polishing processability parameter F1 of the finishing polishing composition obtained in the standard test 3 is 80 or less.

又，本發明其他態樣之前研磨用組成物之要旨為，使用於使矽晶圓進行精加工研磨之精加工研磨步驟之前一階段之研磨步驟的前研磨步驟之前研磨用組成物中，標準試驗1所求取之親水性參數P1為未達100，標準試驗2所求取之精加工精準度參數P2為1000以下。 Further, the other aspect of the composition for polishing of the present invention is to use a composition for polishing in a polishing composition before a pre-grinding step of a polishing step of a stage prior to the finishing polishing step of the enamel wafer. The hydrophilicity parameter P1 obtained by 1 is less than 100, and the precision precision parameter P2 obtained by the standard test 2 is 1000 or less.

另外本發明其他態樣之矽晶圓之研磨方法的要旨為，備有使矽晶圓進行精加工研磨之精加工研磨步驟，與精加工研磨步驟之前一階段之研磨步驟的前研磨步驟之矽晶圓之研磨方法中，使用上述一態樣之研磨用組成 物套組進行精加工研磨步驟及前研磨步驟，又使用有關上述其他態樣之前研磨用組成物進行前研磨步驟。 In addition, the gravitational method of the wafer of the other aspect of the present invention is characterized in that a finishing polishing step for finishing the silicon wafer and a pre-grinding step for the polishing step before the finishing polishing step are provided. In the polishing method of the wafer, the polishing composition using the above aspect is used. The kit is subjected to a finishing grinding step and a pre-grinding step, and a pre-grinding step is performed using the polishing composition before the other aspects described above.

藉由本發明可降低濁度而實現高品質之被研磨面。 By the present invention, it is possible to reduce the turbidity and realize a high-quality surface to be polished.

實施發明之形態 Form of implementing the invention

下面將詳細說明本發明一實施形態。本實施形態之研磨用組成物套組為備有，使用於使矽晶圓進行精加工研磨之精加工研磨步驟之精加工研磨用組成物，與使用於精加工研磨步驟之前一階段之研磨步驟的前研磨步驟之前研磨用組成物。其次標準試驗1所求取之前述研磨用組成物之親水性參數P1為未達100，標準試驗2所求取之前研磨用組成物之精加工精準度參數P2為1000以下，標準試驗3所求取之精加工研磨用組成物之研磨加工性參數F1為80以下。 An embodiment of the present invention will be described in detail below. The polishing composition kit of the present embodiment is provided with a finishing polishing composition for finishing polishing and polishing a tantalum wafer, and a polishing step for use in a stage before the finishing polishing step. The composition for polishing before the pre-grinding step. Next, the hydrophilicity parameter P1 of the polishing composition obtained in the standard test 1 is less than 100, and the precision of the finishing precision P2 of the polishing composition before the standard test 2 is 1000 or less, and the standard test 3 is required. The polishing processability parameter F1 of the composition for finishing polishing is 80 or less.

又，本實施形態之前研磨用組成物為，使用於使矽晶圓進行精加工研磨之精加工研磨步驟之前一階段的研磨步驟之前研磨步驟的研磨用組成物。又，標準試驗1所求取之親水性參數P1為未達100，標準試驗2所求取之精加工精準度參數P2為1000以下。 Further, the polishing composition before the present embodiment is a polishing composition used in the polishing step before the polishing step in the first step before the finishing polishing step of finishing the polishing of the tantalum wafer. Further, the hydrophilicity parameter P1 obtained in the standard test 1 is less than 100, and the precision precision parameter P2 obtained in the standard test 2 is 1000 or less.

該類本實施形態之研磨用組成物套組及前研磨用組成物適用於研磨單體矽、矽化合物、金屬、陶瓷等 各種之研磨對象物，可實現濁度較低之高品質被研磨面，又，亦可能實現微小缺陷較少之被研磨面，特別是使用本實施形態之研磨用組成物套組或前研磨用組成物研磨矽晶圓時，可製造具有濁度較低之高品質表面之矽單結晶晶圓等之矽晶圓。 The polishing composition kit and the pre-polishing composition of the present embodiment are suitable for polishing a monomer, a ruthenium compound, a metal, a ceramic, or the like. Various polishing objects can realize a high-quality surface to be polished having a low turbidity, and it is also possible to realize a surface to be polished having a small number of defects, in particular, the use of the polishing composition kit or the front polishing of the present embodiment. When the composition is polished to a silicon wafer, a germanium wafer such as a single crystal wafer having a high-quality surface having a low turbidity can be produced.

詳細而言為了實現濁度較低之高品質被研磨面，使用加工性較低可製作高精準度之被研磨面的精加工研磨用組成物進行矽晶圓之精加工研磨係重點。因此需使前研磨步驟結束後之被研磨面為具有適度表面保護性及良好品質(濁度較低)之表面。即，為了進行使前研磨步驟結束後之被研磨面為具有適度表面保護性及良好品質之表面般之前研磨，以形成表面保護性不會過高且具有某程度良好品質之表面，因此可使用減輕研磨加工步驟之負荷，加工性較低可製作高精準度之被研磨面之精加工研磨用組成物進行精加工研磨。藉此可實現濁度較低之高品質被研磨面。前研磨步驟結束後之被研磨面又以具有更高品質為佳。 In detail, in order to realize a high-quality polished surface having a low turbidity, it is important to use a finishing polishing composition which is capable of producing a high-precision polished surface with a high degree of workability. Therefore, it is necessary to make the surface to be polished after the end of the pre-polishing step a surface having moderate surface protection and good quality (low turbidity). In other words, in order to perform polishing before the surface to be polished after the completion of the pre-polishing step is a surface having appropriate surface protection and good quality, it is possible to form a surface having a surface protective property that is not excessively high and has a certain degree of good quality. The load on the polishing step is reduced, and the workability is low, and the finishing polishing composition for the polished surface with high precision can be produced for finishing polishing. Thereby, a high-quality surface to be polished having a low turbidity can be achieved. It is preferred that the surface to be polished after the end of the pre-grinding step has a higher quality.

為了上述理由因此要求前研磨用組成物具有可進行使前研磨步驟結束後之被研磨面為具有適度親水性及良好品質之表面般之研磨性能。前研磨步驟結束後之被研磨面之親水性係以親水性參數P1表示，該親水性參數P1可由標準試驗1求取。又，前研磨用組成物之研磨性能係以精加工精準度參數P2表示，該精加工精準度參數P2可由標準試驗2求取。 For the above reasons, the pre-polishing composition is required to have a polishing property such that the surface to be polished after the completion of the pre-polishing step is a surface having moderate hydrophilicity and good quality. The hydrophilicity of the surface to be polished after the end of the pre-grinding step is represented by the hydrophilicity parameter P1, which can be obtained by Standard Test 1. Further, the polishing performance of the pre-polishing composition is expressed by the finishing precision parameter P2, which can be obtained by the standard test 2.

又因要求加工研磨用組成物可高精準度加工被研磨面，故需將加工性抑制於較低。精加工研磨用組成物之研磨加工性係以研磨加工性參數F1表示，該研磨加工性參數F1可由標準試驗3求取。 Further, since it is required to process the polishing composition to process the surface to be polished with high precision, it is necessary to suppress the workability to be low. The polishing processability of the finishing polishing composition is represented by a polishing process parameter F1, which can be obtained by the standard test 3.

求取親水性參數P1、精加工精準度參數P2、研磨加工性參數F1之標準試驗1、2、3如後詳細。 The standard test 1, 2, and 3 for obtaining the hydrophilicity parameter P1, the finishing precision parameter P2, and the grinding processability parameter F1 are as follows.

又，本發明之前研磨步驟係指，矽晶圓之研磨方法所備有之複數研磨步驟中精加工研磨加工步驟之前一階段之研磨步驟。因此矽晶圓之研磨方法為，例如備有預備研磨步驟之第一次研磨步驟、第二次研磨步驟與精加工研磨步驟之三種研磨步驟時，前研磨步驟相當於第二次研磨步驟。又，矽晶圓之研磨方法為，例如備有預備研磨步驟之第一次研磨步驟與精加工研磨步驟之二種研磨步驟時，前研磨步驟相當於第一次研磨步驟。 Further, the pre-grinding step of the present invention refers to a grinding step of a stage before the finishing of the lapping step in the plurality of grinding steps of the rubbing method of the crucible wafer. Therefore, the polishing method of the silicon wafer is, for example, three polishing steps including a first polishing step, a second polishing step, and a finishing polishing step of the preliminary polishing step, and the front polishing step corresponds to the second polishing step. Further, the polishing method of the ruthenium wafer is, for example, the two polishing steps of the first polishing step and the finishing polishing step of the preliminary polishing step, and the front polishing step corresponds to the first polishing step.

下面將詳細說明本實施形態之前研磨用組成物、精加工研磨用組成物及研磨用組成物套組。又，以下所說明之各種操作及物性測定法無特別註明下，係指室溫(20℃以上25℃以下)，相對濕度40%以上50%以下之條件下進行之物。 The polishing composition, the finishing polishing composition, and the polishing composition before the present embodiment will be described in detail below. Further, the various operations and physical property measurement methods described below are carried out under the conditions of room temperature (20° C. or higher and 25° C. or lower) and relative humidity of 40% or more and 50% or less, unless otherwise specified.

1.有關前研磨用組成物 1. About the former polishing composition

矽晶圓之前研磨步驟所使用之前研磨用組成物為，標準試驗1所求取之親水性參數P1為未達100，標準試驗2所求取之精加工精準度參數P2為1000以下。下面將說明 標準試驗1及2。 The polishing composition before the polishing step is used. The hydrophilicity parameter P1 obtained in the standard test 1 is less than 100, and the precision precision parameter P2 obtained in the standard test 2 is 1000 or less. Will be explained below Standard Tests 1 and 2.

1-1 有關標準試驗1 1-1 Relevant standard test 1

親水性參數P1係由依序進行下述a1步驟、a2步驟、a3步驟及a4步驟之標準試驗1求取。 The hydrophilicity parameter P1 was determined by sequentially performing the standard test 1 of the following steps a1, a2, a3, and a4.

[標準試驗1] [Standard Test 1]

(a1)使用前研磨用組成物研磨與研磨對象物之矽晶圓同材質之矽試驗片。矽試驗片可使用圓形晶圓，或切成四角形之薄片。研磨該矽試驗片時例如可使用日本恩吉斯股份公司製之桌上研磨機EJ-380IN、富吉朋股份公司製之研磨台POLYPAS27NX。又，研磨矽試驗片之研磨條件例如可為，研磨荷重16kPa、底盤回轉速度30rpm、載體回轉速度30rpm、研磨時間2min、前研磨用組成物之供給速度30mL/min、前研磨用組成物之溫度20℃。 (a1) A test piece of the same material as the tantalum wafer of the object to be polished is polished by using the composition for polishing before use. The ruthenium test piece can be used as a round wafer or as a quadrangular sheet. When the ruthenium test piece is ground, for example, a table grinder EJ-380IN manufactured by Nippon Co., Ltd., and a polishing table POLYPAS27 NX manufactured by Fujie Pang Co., Ltd. can be used. Further, the polishing conditions of the polishing flaw test piece may be, for example, a polishing load of 16 kPa, a chassis rotation speed of 30 rpm, a carrier rotation speed of 30 rpm, a polishing time of 2 minutes, a supply rate of the pre-polishing composition of 30 mL/min, and a temperature of the pre-polishing composition. 20 ° C.

(a2)以純水洗淨矽試驗片被研磨後之表面，以清洗前研磨用組成物。 (a2) The surface of the ruthenium test piece to be polished was washed with pure water to clean the composition before polishing.

(a3)該矽試驗片為圓形時使直徑沿著垂直方向般之姿勢，又該矽試驗片為四角形時以使一方對角線沿著垂直方向般之姿勢，靜置純水洗淨後之矽試驗片30秒後，測定直徑或一方對角線中矽試驗片之表面未被純水潤濕之領域的長度，再以該長度作為排水距離。 (a3) When the test piece is circular, the diameter is in the vertical direction, and when the test piece is square, the diagonal line is oriented in the vertical direction, and the pure water is left to be washed. After 30 seconds, the length of the field in which the surface of the ruthenium test piece in the diameter or one of the diagonals was not wetted by pure water was measured, and the length was used as the drainage distance.

(a4)由所測得之排水距離，基於下述式算出前研磨用組成物之親水性參數P1。 (a4) From the measured drainage distance, the hydrophilicity parameter P1 of the pre-polishing composition was calculated based on the following formula.

親水性參數P1={(矽試驗片之直徑或對角線之長度[mm])-(排水距離[mm])}/(矽試驗片之直徑或對角線之長度[mm])×100 Hydrophilic parameter P1={(the diameter of the test piece or the length of the diagonal line [mm]) - (drainage distance [mm])} / (the diameter of the test piece or the length of the diagonal line [mm]) × 100

1-2 有關標準試驗2 1-2 Relevant standard test 2

精加工精準度參數P2係由依序進行下述b1步驟，b2步驟及b3步驟之標準試驗2求取。 The finishing precision parameter P2 is obtained by sequentially performing the following b1 step, b2 step and b3 step standard test 2.

[標準試驗2] [Standard Test 2]

(b1)使用前研磨用組成物研磨與研磨對象物之矽晶圓同材質之矽晶圓試驗片(即測定參數用矽晶圓)。研磨該矽晶圓試驗片時例如可使用岡本工作機械製作所股份公司製之研磨機PNX-332B、富吉朋股份公司製之研磨台POLYPAS27NX。又，研磨矽晶圓試驗片之研磨條件例如可為，研磨荷重15kPa、平板回轉速度30rpm、載體回轉速度30rpm、研磨時間2min、前研磨用組成物之供給速度2L/min、前研磨用組成物之溫度20℃、平板冷卻水之溫度20℃。 (b1) A wafer test piece (that is, a wafer for measurement parameters) of the same material as the wafer of the object to be polished is polished before use. For the polishing of the ruthenium wafer test piece, for example, a grinder PNX-332B manufactured by Okamoto Machine Works Co., Ltd., and a polishing table POLYPAS27NX manufactured by Fujimoto Co., Ltd. can be used. Moreover, the polishing conditions of the polished silicon wafer test piece may be, for example, a polishing load of 15 kPa, a flat plate rotation speed of 30 rpm, a carrier rotation speed of 30 rpm, a polishing time of 2 minutes, a supply rate of the front polishing composition of 2 L/min, and a pre-polishing composition. The temperature is 20 ° C, and the temperature of the flat cooling water is 20 ° C.

(b2)使用標準研磨用組成物研磨與研磨對象物之矽晶圓同材質之矽晶圓試驗片。研磨該矽晶圓試驗片時例如可使用岡本工作機械製作所股份公司製之研磨機PNX-332B、富吉朋股份公司製之研磨台POLYPAS27NX。又，研磨矽晶圓試驗片之研磨條件例如可為，研磨荷重15kPa、平板回轉速度30rpm、載體回轉 速度30rpm、研磨時間2min、標準研磨用組成物之供給速度2L/min、標準研磨用組成物之溫度20℃、平板冷卻水之溫度20℃。 (b2) A silicon wafer test piece of the same material as the tantalum wafer of the object to be polished is polished using the standard polishing composition. For the polishing of the ruthenium wafer test piece, for example, a grinder PNX-332B manufactured by Okamoto Machine Works Co., Ltd., and a polishing table POLYPAS27NX manufactured by Fujimoto Co., Ltd. can be used. Further, the polishing conditions of the polished silicon wafer test piece may be, for example, a polishing load of 15 kPa, a flat plate rotation speed of 30 rpm, and a carrier rotation. The speed was 30 rpm, the polishing time was 2 min, the supply rate of the standard polishing composition was 2 L/min, the temperature of the standard polishing composition was 20 ° C, and the temperature of the flat cooling water was 20 °C.

標準研磨用組成物為，含有平均一次粒徑35nm之膠質二氧化矽0.46質量%、氨0.009質量%、重量平均分子量25萬之羥基乙基纖維素0.017質量%，及由聚環氧乙烷與聚環氧丙烷所形成之共聚物0.002質量%，且殘部為水。 The standard polishing composition is a hydroxyethyl cellulose having a mean primary particle diameter of 35 nm of 0.46 mass%, an ammonia content of 0.009% by mass, a weight average molecular weight of 250,000 hydroxyethylcellulose, and 0.017 mass%, and a polyethylene oxide and a polyethylene oxide. The copolymer formed of polypropylene oxide was 0.002% by mass, and the residue was water.

(b3)測定b1步驟研磨後之矽晶圓試驗片之濁度h2，與b2步驟研磨後之矽晶圓試驗片之濁度α，基於下述式算出前研磨用組成物之精加工精準度參數P2。 (b3) Measure the turbidity h2 of the ruthenium wafer test piece after the b1 step polishing, and the turbidity α of the ruthenium wafer test piece after the b2 step polishing, and calculate the finishing precision of the pre-polishing composition based on the following formula Parameter P2.

精加工精準度參數P2=h2/α×100 Finishing precision parameter P2=h2/α×100

2.有關精加工研磨用組成物 2. Composition for finishing grinding

矽晶圓之精加工研磨步驟所使用之精加工研磨用組成物為，標準試驗3所求取之研磨加工性參數F1為80以下、研磨加工性參數F1係由依序進行下述c1步驟、c2步驟及c3步驟之標準試驗3求取。 The finishing polishing composition used in the finishing polishing step of the wafer is such that the polishing processability parameter F1 obtained in the standard test 3 is 80 or less, and the polishing process parameter F1 is sequentially performed in the following c1 step, c2 The standard test 3 of the step and the c3 step is obtained.

[標準試驗3] [Standard Test 3]

(c1)用精加工研磨用組成物研磨與研磨對象物之矽晶圓同材質之矽晶圓試驗片，研磨該矽晶圓試驗片時例如可使用岡本工作機械製作所股份公司製之研磨機PNX-322、富吉朋股份公司製之研磨台POLYPAS27NX。又， 研磨矽晶圓試驗片之研磨條件例如可為，研磨荷重15kPa、平板回轉速度30rpm、載體回轉速度30rpm、研磨時間15min、精加工研磨用組成物之供給速度0.4L/min、精加工研磨用組成物之溫度20℃、平板冷卻水之溫度20℃。 (c1) The 试验 wafer test piece of the same material as the 矽 wafer of the object to be polished is polished by the finishing polishing composition, and the pulverizer PNX manufactured by Okamoto Machine Tool Co., Ltd. can be used, for example, when the ruthenium wafer test piece is polished. -322, grinding table POLYPAS27NX made by Fujikeng Co., Ltd. also, The polishing conditions of the polished silicon wafer test piece may be, for example, a polishing load of 15 kPa, a flat plate rotation speed of 30 rpm, a carrier rotation speed of 30 rpm, a polishing time of 15 minutes, a supply speed of a finishing polishing composition of 0.4 L/min, and a finishing polishing composition. The temperature of the object was 20 ° C, and the temperature of the plate cooling water was 20 ° C.

(c2)使用標準試驗2之標準研磨用組成物研磨與研磨對象物之矽晶圓同材質之矽晶圓試驗片。研磨該矽晶圓試驗片時例如可使用岡本工作機械製作所股份公司製之研磨機PNX-322、富吉朋股份公司製之研磨台POLYPAS27NX。又，研磨矽晶圓試驗片之研磨條件例如可為，研磨荷重15kPa、平板回轉速度30rpm、載體回轉速度30rpm、研磨時間15min、標準研磨用組成物之供給速度0.4L/min、標準研磨用組成物之溫度20℃、平板冷卻水之溫度20℃。 (c2) A silicon wafer test piece of the same material as the tantalum wafer of the object to be polished was polished using the standard polishing composition of Standard Test 2. For the polishing of the tantalum wafer test piece, for example, a grinder PNX-322 manufactured by Okamoto Machine Works Co., Ltd., and a polishing table POLYPAS27NX manufactured by Fujie Pang Co., Ltd. can be used. Further, the polishing conditions of the polished silicon wafer test piece may be, for example, a polishing load of 15 kPa, a flat plate rotation speed of 30 rpm, a carrier rotation speed of 30 rpm, a polishing time of 15 minutes, a supply rate of a standard polishing composition of 0.4 L/min, and a standard polishing composition. The temperature of the object was 20 ° C, and the temperature of the plate cooling water was 20 ° C.

(c3)由c1步驟之研磨前後之矽晶圓試驗片的質量差算出c1步驟研磨時之研磨速度R，同時由c2步驟之研磨前後之矽晶圓試驗片的質量差算出c2步驟研磨時之研磨速度β。其次基於下述式算出精加工研磨用組成物之研磨加工性參數F1。 (c3) Calculating the polishing rate R during the polishing in the c1 step from the difference in the mass of the wafer test piece before and after the polishing in the step c1, and calculating the mass difference of the wafer test piece before and after the polishing in the c2 step. Grinding speed β. Next, the polishing processability parameter F1 of the finishing polishing composition is calculated based on the following formula.

研磨加工性參數F1=R/β×100 Grinding processability parameter F1=R/β×100

3.有關研磨用組成物套組 3. About the composition of the polishing composition

本實施形態之研磨用組成物套組因具有前研磨用組成物與精加工研磨用組成物，故可使用備有二種以上研磨步 驟之矽晶圓之研磨方法，例如可使用備有預備研磨步驟的第一次研磨步驟與精加工研磨步驟之二種研磨步驟的矽晶圓之研磨方法，又可使用備有預備研磨步驟的第一次研磨步驟、第二次研磨步驟與精加工研磨步驟之三種研磨步驟的矽晶圓之研磨方法。 Since the polishing composition kit of the present embodiment has a pre-polishing composition and a finishing polishing composition, two or more polishing steps can be used. For the polishing method of the wafer, for example, a method of polishing a tantalum wafer provided with a first grinding step of a preliminary grinding step and a finishing step of a finishing grinding step, or a preliminary grinding step may be used. A method of grinding a tantalum wafer of three grinding steps of a first grinding step, a second grinding step, and a finishing grinding step.

備有三種以上之研磨步驟的矽晶圓之研磨方法係使用本實施形態之研磨用組成物套組時，精加工研磨步驟可使用本實施形態之精加工研磨用組成物，精加工研磨步驟之前一階段之研磨步驟的前研磨步驟可使用本實施形態之前研磨用組成物，除此之外之各研磨步驟可各自適當選擇適用於該研磨步驟之研磨用組成物。 When the polishing method for the tantalum wafer having three or more kinds of polishing steps is the use of the polishing composition kit of the present embodiment, the finishing polishing step can use the finishing polishing composition of the present embodiment, before the finishing polishing step In the pre-polishing step of the one-step polishing step, the polishing composition before the present embodiment can be used, and the polishing composition suitable for the polishing step can be appropriately selected for each of the polishing steps.

其次將說明構成本實施形態之精加工研磨用組成物及前研磨用組成物之成分。本實施形態之精加工研磨用組成物及前研磨用組成物均為，含有磨粒、鹼性化合物、水溶性高分子及水之組成物。又可依所希望含有各種添加劑。 Next, the components constituting the finishing polishing composition and the pre-polishing composition of the present embodiment will be described. The finishing polishing composition and the pre-polishing composition of the present embodiment each contain a composition of abrasive grains, a basic compound, a water-soluble polymer, and water. It can also contain various additives as desired.

4.有關磨粒 4. About abrasive particles

磨粒為，具有物理性研磨矽晶圓表面之作用。磨粒之種類無特別限定，例如二氧化矽粒子、氧化鋁粒子、氧化鈰粒子、氧化鉻粒子、二氧化鈦粒子、氧化鋯粒子、氧化鎂粒子、二氧化錳粒子、氧化鋅粒子、氧化鐵紅粒子等之氧化物粒子，或氮化矽粒子、氮化硼粒子等之氮化物粒子、或碳化矽粒子、碳化硼粒子等之碳化物粒子、或碳酸 鈣、碳酸鉭等之碳酸鹽，或金剛石粒子等。 The abrasive particles have the function of physically grinding the surface of the wafer. The type of the abrasive grains is not particularly limited, and examples thereof include cerium oxide particles, alumina particles, cerium oxide particles, chromium oxide particles, titanium oxide particles, zirconia particles, magnesium oxide particles, manganese dioxide particles, zinc oxide particles, and iron oxide red particles. Oxide particles, or nitride particles such as tantalum nitride particles or boron nitride particles, or carbide particles such as niobium carbide particles or boron carbide particles, or carbonic acid Carbonate such as calcium or barium carbonate, or diamond particles.

該等具體例中較佳為二氧化矽。二氧化矽之具體例如，由膠質二氧化矽、煙化二氧化矽及溶膠凝膠法二氧化矽中所選出之二氧化矽粒子。該等二氧化矽粒子中就減少矽晶圓之被研磨面發生刮傷之觀點，較佳由膠質二氧化矽及煙化二氧化矽中所選出之二氧化矽粒子，特佳為使用膠質二氧化矽。磨粒可單獨使用其中一種，或二種以上組合使用。 Among these specific examples, cerium oxide is preferred. Specific examples of the cerium oxide include cerium oxide particles selected from colloidal cerium oxide, fumed cerium oxide, and sol-gel cerium oxide. The cerium oxide particles reduce the scratching of the polished surface of the germanium wafer, preferably the cerium oxide particles selected from the colloidal cerium oxide and the fumed cerium oxide, and particularly preferably the colloidal smear. Yttrium oxide. The abrasive grains may be used alone or in combination of two or more.

前研磨用組成物所使用之磨粒之平均一次粒徑較佳為5nm以上，又以10nm以上為佳，更佳為15nm以上，特佳為20nm以上。藉由增加磨粒之平均一次粒徑，可提升矽晶圓之研磨速度。又，前研磨用組成物所使用之磨粒之平均一次粒徑較佳為100nm以下，又以60nm以下為佳，更佳為50nm以下。藉由減低磨粒之平均一次粒徑，可提升被研磨面之平滑性。 The average primary particle diameter of the abrasive grains used in the pre-polishing composition is preferably 5 nm or more, more preferably 10 nm or more, still more preferably 15 nm or more, and particularly preferably 20 nm or more. By increasing the average primary particle size of the abrasive particles, the polishing speed of the tantalum wafer can be increased. Further, the average primary particle diameter of the abrasive grains used in the pre-polishing composition is preferably 100 nm or less, more preferably 60 nm or less, still more preferably 50 nm or less. By reducing the average primary particle size of the abrasive particles, the smoothness of the surface to be polished can be improved.

精加工研磨用組成物所使用之磨粒之平均一次粒徑較佳為5nm以上，更佳為10nm以上。藉由增加磨粒之平均一次粒徑，可提升矽晶圓之研磨速度。又，精加工研磨用組成物所使用之磨粒之平均一次粒徑較佳為100nm以下，又以60nm以下為佳，更佳為50nm以下，特佳為40nm以下。藉由減低磨粒之平均一次粒徑，可提升被研磨面之平滑性。 The average primary particle diameter of the abrasive grains used for the finishing polishing composition is preferably 5 nm or more, and more preferably 10 nm or more. By increasing the average primary particle size of the abrasive particles, the polishing speed of the tantalum wafer can be increased. Further, the average primary particle diameter of the abrasive grains used for the finishing polishing composition is preferably 100 nm or less, more preferably 60 nm or less, still more preferably 50 nm or less, and particularly preferably 40 nm or less. By reducing the average primary particle size of the abrasive particles, the smoothness of the surface to be polished can be improved.

又，前研磨用組成物及精加工研磨用組成物所使用之磨粒之平均一次粒徑值可基於BET法測得之磨 粒之比表面積算出。磨粒之比表面積例如可使用麥固洛公司製之型式「Flow Sorbll 2300」測定。 Further, the average primary particle diameter of the abrasive grains used in the pre-polishing composition and the finishing polishing composition can be measured by the BET method. The specific surface area of the particles was calculated. The specific surface area of the abrasive grains can be measured, for example, using the type "Flow Sorbll 2300" manufactured by McGraw.

前研磨用組成物所使用之磨粒之平均二次粒徑較佳為10nm以上，又以20nm以上為佳，更佳為30nm以上，特佳為40nm以上。藉由增加磨粒之平均二次粒徑，可提升矽晶圓之研磨速度。又，前研磨用組成物所使用之磨粒之平均二次粒徑較佳為150nm以下，又以100nm以下為佳，更佳為80nm以下，特佳為70nm以下。藉由減低磨粒之平均二次粒徑，可提升被研磨面之平滑性。 The average secondary particle diameter of the abrasive grains used in the pre-polishing composition is preferably 10 nm or more, more preferably 20 nm or more, still more preferably 30 nm or more, and particularly preferably 40 nm or more. By increasing the average secondary particle size of the abrasive particles, the polishing speed of the silicon wafer can be increased. Further, the average secondary particle diameter of the abrasive grains used in the pre-polishing composition is preferably 150 nm or less, more preferably 100 nm or less, still more preferably 80 nm or less, and particularly preferably 70 nm or less. By reducing the average secondary particle size of the abrasive particles, the smoothness of the surface to be polished can be improved.

精加工研磨用組成物所使用之磨粒之平均二次粒徑較佳為10nm以上，更佳為20nm以上。藉由增加磨粒之平均二次粒徑，可提升矽晶圓之研磨速度。又，精加工研磨用組成物所使用之磨粒之平均二次粒徑較佳為100nm以下，又以80nm以下為佳，更佳為70nm以下，特佳為60nm以下。藉由減低磨粒之平均二次粒徑，可提升被研磨面之平滑性。 The average secondary particle diameter of the abrasive grains used for the finishing polishing composition is preferably 10 nm or more, and more preferably 20 nm or more. By increasing the average secondary particle size of the abrasive particles, the polishing speed of the silicon wafer can be increased. Further, the average secondary particle diameter of the abrasive grains used for the finishing polishing composition is preferably 100 nm or less, more preferably 80 nm or less, still more preferably 70 nm or less, and particularly preferably 60 nm or less. By reducing the average secondary particle size of the abrasive particles, the smoothness of the surface to be polished can be improved.

又，前研磨用組成物及精加工研磨用組成物所使用之磨粒之平均二次粒徑值，例如可藉由使用日機裝股份公司製之UPA-UT151之動態光散射法測定。 In addition, the average secondary particle diameter value of the abrasive grains used for the pre-polishing composition and the finishing polishing composition can be measured, for example, by a dynamic light scattering method using UPA-UT151 manufactured by Nikkiso Co., Ltd.

前研磨用組成物中磨粒之含量較佳為0.01質量%以上，又以0.05質量%以上為佳，更佳為0.10質量%以上。磨粒之含量為上述範圍內時，可使矽晶圓具有優良研磨速度。 The content of the abrasive grains in the pre-polishing composition is preferably 0.01% by mass or more, more preferably 0.05% by mass or more, still more preferably 0.10% by mass or more. When the content of the abrasive grains is within the above range, the ruthenium wafer can have an excellent polishing rate.

前研磨用組成物中磨粒之含量較佳為3質量%以下， 又以1質量%以下為佳，更佳為0.5質量%以下。磨粒之含量為上述範圍內時，可提升前研磨用組成物之分散安定性。 The content of the abrasive grains in the pre-polishing composition is preferably 3% by mass or less. Further, it is preferably 1% by mass or less, more preferably 0.5% by mass or less. When the content of the abrasive grains is within the above range, the dispersion stability of the composition for pre-polishing can be improved.

精加工研磨用組成物中磨粒之含量較佳為0.01質量%以上，又以0.05質量%以上為佳，更佳為0.10質量%以上。磨粒之含量為上述範圍內時，可使矽晶圓具有優良研磨速度。 The content of the abrasive grains in the composition for finishing polishing is preferably 0.01% by mass or more, more preferably 0.05% by mass or more, still more preferably 0.10% by mass or more. When the content of the abrasive grains is within the above range, the ruthenium wafer can have an excellent polishing rate.

精加工研磨用組成物中磨粒之含量較佳為3質量%以下，又以1質量%以下為佳，更佳為0.5質量%以下，特佳為0.3質量%以下。磨粒之含量為上述範圍內時，可提升精加工研磨用組成物之分散安定性。 The content of the abrasive grains in the composition for finishing polishing is preferably 3% by mass or less, more preferably 1% by mass or less, still more preferably 0.5% by mass or less, and particularly preferably 0.3% by mass or less. When the content of the abrasive grains is within the above range, the dispersion stability of the composition for finishing polishing can be improved.

5.有關鹼性化合物 5. About basic compounds

精加工研磨用組成物及前研磨用組成物為，含有鹼性化合物。鹼性化合物相對於矽晶圓之被研磨面可賦予化學性作用而進行化學性研磨(化學蝕刻)。藉此易提升研磨矽晶圓時之研磨速度。 The composition for polishing and the composition for pre-polishing contain a basic compound. The alkaline compound can be chemically polished (chemically etched) by imparting a chemical action to the surface to be polished of the tantalum wafer. This makes it easy to increase the polishing speed when polishing the silicon wafer.

鹼性化合物之具體例如，無機之鹼性化合物、鹼金屬或鹼土類金屬之氫氧化物或鹽、氫氧化四級銨或其鹽、氨、胺等。鹼金屬之具體例如，鉀、鈉等。鹽之具體例如，碳酸鹽、碳酸氫鹽、硫酸鹽、乙酸鹽等。四級銨之具體例如，四甲基銨、四乙基銨、四丁基胺等。鹼金屬之氫氧化物或鹽之具體例如，氫氧化鉀、碳酸鉀、碳酸氫鉀、硫酸鉀、乙酸鉀、氯化鉀等。 Specific examples of the basic compound include inorganic basic compounds, hydroxides or salts of alkali metal or alkaline earth metals, quaternary ammonium hydroxide or salts thereof, ammonia, amines and the like. Specific examples of the alkali metal include potassium, sodium, and the like. Specific examples of the salt include carbonate, hydrogencarbonate, sulfate, acetate, and the like. Specific examples of the quaternary ammonium are, for example, tetramethylammonium, tetraethylammonium, tetrabutylamine and the like. Specific examples of the hydroxide or salt of the alkali metal include potassium hydroxide, potassium carbonate, potassium hydrogencarbonate, potassium sulfate, potassium acetate, potassium chloride and the like.

氫氧化四級銨或其鹽之具體例如，氫氧化四甲基銨、氫氧化四乙基銨、氫氧化四丁基銨等。胺之具體例如，甲基胺、二甲基胺、三甲基胺、乙基胺、二乙基胺、三乙基胺、伸乙基二胺、單乙醇胺、N-(β-胺基乙基)乙醇胺、六伸甲基二胺、二伸乙基三胺、三伸乙基四胺、哌嗪酐、哌嗪六水合物、1-(2-胺基乙基)哌嗪、N-甲基哌嗪、脈、咪唑或***等之唑類等。該等鹼性化合物可單獨使用一種，或二種以上組合使用。 Specific examples of the quaternary ammonium hydroxide or a salt thereof include tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrabutylammonium hydroxide and the like. Specific examples of the amine are, for example, methylamine, dimethylamine, trimethylamine, ethylamine, diethylamine, triethylamine, ethylidene diamine, monoethanolamine, N-(β-amino group B Ethylamine, hexamethylenediamine, di-ethyltriamine, tri-ethyltetramine, piperazine anhydride, piperazine hexahydrate, 1-(2-aminoethyl)piperazine, N- An azole such as methyl piperazine, vein, imidazole or triazole. These basic compounds may be used alone or in combination of two or more.

鹼性化合物中較佳為，由氨、銨鹽、鹼金屬氫氧化物、鹼金屬鹽及四級銨氫氧化物中所選出之至少一種。鹼性化合物中又以由氨、氫氧化鉀、氫氧化鈉、氫氧化四甲基銨、氫氧化四乙基銨、碳酸氫銨、碳酸銨、碳酸氫鉀、碳酸鉀、碳酸氫鈉及碳酸鈉中所選出之至少一種為佳。鹼性化合物中更佳為氨、氫氧化鉀、氫氧化鈉、氫氧化四甲基銨及氫氧化四乙基銨中所選出之至少一種，特佳為氨及氫氧化四甲基銨中至少一方，最佳為氨。 The basic compound is preferably at least one selected from the group consisting of ammonia, an ammonium salt, an alkali metal hydroxide, an alkali metal salt, and a quaternary ammonium hydroxide. The basic compound is further composed of ammonia, potassium hydroxide, sodium hydroxide, tetramethylammonium hydroxide, tetraethylammonium hydroxide, ammonium hydrogencarbonate, ammonium carbonate, potassium hydrogencarbonate, potassium carbonate, sodium hydrogencarbonate and carbonic acid. At least one selected from the sodium is preferred. More preferably, the basic compound is at least one selected from the group consisting of ammonia, potassium hydroxide, sodium hydroxide, tetramethylammonium hydroxide and tetraethylammonium hydroxide, and particularly preferably at least ammonia and tetramethylammonium hydroxide. One side, the best is ammonia.

前研磨用組成物中鹼性化合物之含量較佳為0.0001質量%以上，又以0.001質量%以上為佳，更佳為0.005質量%以上，特佳為0.01質量%以上。藉由增加前研磨用組成物中鹼性化合物之含量，傾向提升矽晶圓之研磨速度。 The content of the basic compound in the pre-polishing composition is preferably 0.0001% by mass or more, more preferably 0.001% by mass or more, still more preferably 0.005% by mass or more, and particularly preferably 0.01% by mass or more. By increasing the content of the basic compound in the pre-polishing composition, it tends to increase the polishing rate of the tantalum wafer.

前研磨用組成物中鹼性化合物之含量較佳為0.5質量%以下，又以0.1質量%以下為佳，更佳為0.05質量%以下。藉由減少前研磨用組成物中鹼性化合物之含 量，傾向提升研磨後矽晶圓表面之平滑性。 The content of the basic compound in the pre-polishing composition is preferably 0.5% by mass or less, more preferably 0.1% by mass or less, still more preferably 0.05% by mass or less. By reducing the inclusion of basic compounds in the pre-grinding composition The amount tends to improve the smoothness of the surface of the wafer after polishing.

精加工研磨用組成物中鹼性化合物之含量較佳為0.0001質量%以上，又以0.0005質量%以上為佳，更佳為0.001質量%以上。藉由增加精加工研磨用組成物中鹼性化合物之含量，傾向提升矽晶圓之研磨速度。 The content of the basic compound in the composition for polishing and polishing is preferably 0.0001% by mass or more, more preferably 0.0005 mass% or more, still more preferably 0.001% by mass or more. By increasing the content of the basic compound in the finishing polishing composition, it tends to increase the polishing rate of the silicon wafer.

精加工研磨用組成物中鹼性化合物之含量較佳為0.5質量%以下，又以0.1質量%以下為佳，更佳為0.05質量%以下，特佳為0.02質量%以下。藉由減少精加工研磨用組成物中鹼性化合物之含量，傾向提升研磨後矽晶圓表面之平滑性。 The content of the basic compound in the composition for finishing polishing is preferably 0.5% by mass or less, more preferably 0.1% by mass or less, still more preferably 0.05% by mass or less, and particularly preferably 0.02% by mass or less. By reducing the content of the basic compound in the finishing polishing composition, it tends to improve the smoothness of the surface of the wafer after polishing.

6.有關水溶性高分子 6. About water soluble polymers

水溶性高分子於研磨時或清洗處理時等矽晶圓實施表面處理時，可提高矽晶圓之被研磨面之潤濕性。精加工研磨用組成物及前研磨用組成物為，含有作為水溶性高分子用之調製精加工研磨用組成物及前矽磨用組成物時以固體或固體形態投入水中之固體原料的水溶性高分子。 When the water-soluble polymer is subjected to surface treatment such as polishing or cleaning, the wettability of the polished surface of the tantalum wafer can be improved. The composition for polishing and the composition for pre-polishing is a water-soluble material which is solid or solid-formed into a solid raw material when it is used as a composition for polishing a water-soluble polymer and a composition for a pre-honing composition. Polymer.

固體原料係指溶解於水之前，原料之狀態為溫度23℃、相對濕度50%及1氣壓之環境下以目視係固體或固體形態之物。又，水溶性高分子可為，於水或水與醇、酮等之水系有機溶劑之混合溶劑中由單體合成之物，又包含直接為該溶液形態的水系液形態之物，或餾去揮發性溶劑後之水溶液形態之物。又，以下將「固體原料之水溶性高分子」、「水系形態之水溶性高分子」、「水溶液 形態之水溶性高分子」單稱為「水溶性高分子」。 The solid raw material means a substance which is visually solid or solid in an environment of a temperature of 23 ° C, a relative humidity of 50% and a pressure of 1 ° before being dissolved in water. Further, the water-soluble polymer may be a product synthesized from a monomer in water, a mixed solvent of water and an aqueous organic solvent such as an alcohol or a ketone, or a form of an aqueous liquid directly in the form of the solution, or may be distilled off. The form of the aqueous solution after the volatile solvent. In addition, the following are "water-soluble polymers of solid raw materials", "water-soluble polymers in water form", and "aqueous solutions". The water-soluble polymer of the form is simply referred to as "water-soluble polymer".

水溶性高分子為，分子中具有由陽離子基、陰離子基及非離子基中所選出之至少一種官能基之物，具體上也可使用分子中含有羥基、羧基、醯氧基、磺基、醯胺基、脒基、亞胺基、醯亞胺基、四級氮結構、含有前述官能基單位之雜環結構、乙烯基結構、聚環氧烷結構等之物中任何一種。 The water-soluble polymer is one having at least one functional group selected from the group consisting of a cationic group, an anionic group and a nonionic group in the molecule, and specifically, a molecule having a hydroxyl group, a carboxyl group, a decyloxy group, a sulfo group or a fluorene group may also be used. Any one of an amine group, a mercapto group, an imido group, a quinone imine group, a quaternary nitrogen structure, a heterocyclic structure containing the aforementioned functional unit, a vinyl structure, a polyalkylene oxide structure or the like.

具體例如，纖維系衍生物、聚乙烯醇、聚(甲基)丙烯酸、聚(甲基)丙烯醯胺烷基磺酸、聚異戊二烯磺酸、聚乙烯基磺酸、聚烯丙基磺酸、聚異戊烯磺酸、聚苯乙烯磺酸鹽、聚(甲基)丙烯醯胺、聚烷基胺基烷基(甲基)丙烯醯胺、聚乙烯吡喀烷酮、部分結構含有聚乙烯基吡咯烷酮之共聚物、聚乙烯基己內醯胺、部分結構含有聚乙烯基己內醯胺之共聚物、聚烷氧基烷基(甲基)丙烯醯胺、聚羥基烷基(甲基)丙烯醯胺、聚(甲基)丙烯醯基嗎啉、聚脒、聚伸乙基亞胺、親水性聚醯亞胺、各種聚胺基酸、聚(N-醯基伸烷基亞胺)等之亞胺衍生物、聚乙烯醇之羥基部的一部份被四級氮結構取代之聚乙烯醇衍生物、聚環氧乙烷、具有聚氧基烯烴結構之聚合物、具有該等之二嵌段型、三嵌段型、無規型或交互型之複數種結構之聚合物等。又，聚(甲基)丙烯酸係指丙烯酸及/或甲基丙烯酸，其他化合物也相同。 Specifically, for example, a fiber-based derivative, polyvinyl alcohol, poly(meth)acrylic acid, poly(meth)acrylamide-alkylsulfonic acid, polyisoprenesulfonic acid, polyvinylsulfonic acid, polyallyl Sulfonic acid, polyisoprene sulfonic acid, polystyrene sulfonate, poly(meth) acrylamide, polyalkylaminoalkyl (meth) acrylamide, polyvinyl pyrrolidone, partial structure a copolymer containing polyvinylpyrrolidone, polyvinyl caprolactam, a copolymer having a partial structure containing polyvinyl caprolactam, a polyalkoxyalkyl (meth) acrylamide, a polyhydroxyalkyl group ( Methyl) acrylamide, poly(meth)propenyl morpholine, polyfluorene, polyethylenimine, hydrophilic polyimine, various polyamino acids, poly(N-fluorenylalkylene) An imine derivative such as an amine, a polyvinyl alcohol derivative in which a part of a hydroxyl group of the polyvinyl alcohol is substituted with a four-stage nitrogen structure, a polyethylene oxide, a polymer having a polyoxyalkylene structure, and the like Diblock, triblock, random or interactive polymers of a plurality of structures. Further, poly(meth)acrylic acid means acrylic acid and/or methacrylic acid, and other compounds are also the same.

水溶性高分子中就提升矽晶圓之被研磨面之潤濕性、抑制附著微片，及降低表面粗糙度等之觀點，較 佳為纖維素衍生物、聚乙烯醇、聚乙烯基吡咯烷酮、聚羥基烷基(甲基)丙烯醯胺、聚(甲基)丙烯醯基嗎啉，或具有聚氧基烯烴結構之聚合物。纖維素衍生物之具體例如，羥基乙基纖維素、羥基丙基纖維素、羥基乙基甲基纖維素、羥基丙基甲基纖維素、甲基纖維素、乙基纖維素、乙基羥基乙基纖維素、羧基甲基纖維素等。 In the water-soluble polymer, the wettability of the polished surface of the germanium wafer is improved, the adhesion of the microchip is suppressed, and the surface roughness is lowered. Preferred are cellulose derivatives, polyvinyl alcohol, polyvinyl pyrrolidone, polyhydroxyalkyl (meth) acrylamide, poly(meth) propylene decyl morpholine, or a polymer having a polyoxy olefin structure. Specific examples of the cellulose derivative are, for example, hydroxyethylcellulose, hydroxypropylcellulose, hydroxyethylmethylcellulose, hydroxypropylmethylcellulose, methylcellulose, ethylcellulose, ethylhydroxyl Cellulose, carboxymethylcellulose, and the like.

纖維素衍生物中就提高賦予矽晶圓之被研磨面之潤濕性能力，具有良好洗淨性之觀點，特佳為羥基乙基纖維素。又，水溶性高分子可單獨使用一種，或二種以上組合使用。 Among the cellulose derivatives, the ability to impart wettability to the surface to be polished of the wafer is improved, and from the viewpoint of good detergency, hydroxyethyl cellulose is particularly preferable. Further, the water-soluble polymers may be used alone or in combination of two or more.

前研磨用組成物所使用之水溶性高分子之重量平均分子量較佳為10000以上，又以20000以上為佳，更佳為30000以上。藉由水溶性高分子之重量平均分子量，傾向提升矽晶圓之研磨速度。 The weight average molecular weight of the water-soluble polymer used in the pre-polishing composition is preferably 10,000 or more, more preferably 20,000 or more, still more preferably 30,000 or more. The weight average molecular weight of the water-soluble polymer tends to increase the polishing rate of the silicon wafer.

前研磨用組成物所使用之水溶性高分子之重量平均分子量較佳為200萬以下，又以150萬以下為佳，更佳為120萬以下，又以100萬以下更佳，特佳為70萬以下。藉由減少水溶性高分子之重量平均分子量，傾向進一步保有前研磨用組成物之安定性。又，傾向降低矽晶圓之被研磨面之濁度。 The weight average molecular weight of the water-soluble polymer used in the pre-polishing composition is preferably 2,000,000 or less, more preferably 1.5 million or less, more preferably 1.2 million or less, still more preferably 1,000,000 or less, and particularly preferably 70. Less than 10,000. By reducing the weight average molecular weight of the water-soluble polymer, it tends to further maintain the stability of the pre-polishing composition. Further, it tends to lower the turbidity of the surface to be polished of the germanium wafer.

精加工研磨用組成物所使用之水溶性高分子之重量平均分子量較佳為10000以上，又以20000以上為佳，更佳為30000以上。藉由增加水溶性高分子之重量平均分子量，傾向提升矽晶圓之研磨速度。 The water-soluble polymer used for the finishing polishing composition preferably has a weight average molecular weight of 10,000 or more, more preferably 20,000 or more, still more preferably 30,000 or more. By increasing the weight average molecular weight of the water-soluble polymer, it tends to increase the polishing rate of the silicon wafer.

精加工研磨用組成物所使用之水溶性高分子之重量平均分子量較佳為200萬以下，又以150萬以下為佳，更佳為120萬以下為佳，又以100萬以下更佳，特佳為80萬以下，又以60萬以下特佳，最佳為30萬以下。藉由減少水溶性高分子之重量平均分子量，傾向進一步保有精加工研磨用組成物之安定性。又，傾向降低矽晶圓之被研磨面之濁度。 The weight average molecular weight of the water-soluble polymer used for the finishing polishing composition is preferably 2,000,000 or less, more preferably 1.5 million or less, more preferably 1.2 million or less, and even more preferably 1,000,000 or less. The best is less than 800,000, and the best is less than 600,000, and the best is less than 300,000. By reducing the weight average molecular weight of the water-soluble polymer, it is preferable to further maintain the stability of the composition for finishing polishing. Further, it tends to lower the turbidity of the surface to be polished of the germanium wafer.

前研磨用組成物中水溶性高分子之含量較佳為0.0001質量%以上，又以0.0005質量%以上為佳，更佳為0.001質量%以上。藉由增加前研磨用組成物中水溶性高分子之含量，傾向進一步提升矽晶圓之被研磨面之潤濕性。 The content of the water-soluble polymer in the pre-polishing composition is preferably 0.0001% by mass or more, more preferably 0.0005 mass% or more, still more preferably 0.001% by mass or more. By increasing the content of the water-soluble polymer in the pre-polishing composition, it tends to further improve the wettability of the surface to be polished of the tantalum wafer.

前研磨用組成物中水溶性高分子之含量較佳為0.5質量%以下，又以0.1質量%以下為佳，更佳為0.05質量%以下，又以0.01質量%以下更佳，特佳為0.005質量%以下。藉由減少前研磨用組成物中水溶性高分子之含量，傾向進一步保有前研磨用組成物之安定性。 The content of the water-soluble polymer in the pre-polishing composition is preferably 0.5% by mass or less, more preferably 0.1% by mass or less, still more preferably 0.05% by mass or less, still more preferably 0.01% by mass or less, and particularly preferably 0.005%. Below mass%. By reducing the content of the water-soluble polymer in the pre-polishing composition, it is preferable to further maintain the stability of the pre-polishing composition.

精加工研磨用組成物中水溶性高分子之含量較佳為0.0001質量%以上，又以0.0005質量%以上為佳，更佳為0.001質量%以上，特佳為0.005質量%以上。藉由增加精加工研磨用組成物中水溶性高分子之含量，傾向進一步提升矽晶圓之被研磨面之潤濕性。 The content of the water-soluble polymer in the finishing polishing composition is preferably 0.0001% by mass or more, more preferably 0.0005 mass% or more, still more preferably 0.001% by mass or more, and particularly preferably 0.005% by mass or more. By increasing the content of the water-soluble polymer in the composition for finishing polishing, it tends to further improve the wettability of the surface to be polished of the tantalum wafer.

精加工研磨用組成物中水溶性高分子之含量較佳為0.5質量%以下，又以0.1質量%以下為佳，更佳為 0.05質量%以下，又以0.01質量%以下更佳。藉由減少精加工研磨用組成物中水溶性高分子之含量，傾向進一步保有精加工研磨用組成物之安定性。 The content of the water-soluble polymer in the composition for finishing polishing is preferably 0.5% by mass or less, more preferably 0.1% by mass or less, more preferably It is more preferably 0.05% by mass or less and further preferably 0.01% by mass or less. By reducing the content of the water-soluble polymer in the composition for finishing polishing, it is preferable to further maintain the stability of the composition for finishing polishing.

精加工研磨用組成物及前研磨用組成物中磨粒、水溶性高分子及鹼性化合物之含量之質量比可為50~99：0.5~20：0.5~30。藉由使含量之質量比為該範圍內，可提升精加工研磨用組成物及前研磨用組成物之分散安定性，且提升洗淨後矽晶圓之乾淨性。 The mass ratio of the abrasive grains, the water-soluble polymer, and the basic compound in the composition for polishing and the pre-polishing composition may be 50 to 99: 0.5 to 20: 0.5 to 30. When the mass ratio of the content is within this range, the dispersion stability of the composition for polishing and the composition for pre-polishing can be improved, and the cleanness of the wafer after washing can be improved.

7.有關精加工研磨用組成物及前研磨用組成物之pH 7. The pH of the finishing polishing composition and the pre-polishing composition

前研磨用組成物之pH無特別限定，較佳為9.0以上，又以9.5以上為佳，更佳為10.0以上。藉由提高pH，傾向提升矽晶圓之研磨速度。 The pH of the pre-polishing composition is not particularly limited, but is preferably 9.0 or more, more preferably 9.5 or more, still more preferably 10.0 or more. By increasing the pH, it tends to increase the polishing speed of the wafer.

前研磨用組成物之pH較佳為11.5以下，又以11.0以下為佳，更佳為10.8以下，藉由降低pH，傾向提升矽晶圓之面精準度。 The pH of the pre-polishing composition is preferably 11.5 or less, more preferably 11.0 or less, still more preferably 10.8 or less, and the pH is lowered to increase the surface accuracy of the wafer.

精加工研磨用組成物之pH無特別限定，較佳為9.0以上，又以9.5以上為佳，更佳為9.8以上。藉由提高pH，傾向提升矽晶圓之研磨速度。 The pH of the finishing polishing composition is not particularly limited, but is preferably 9.0 or more, more preferably 9.5 or more, still more preferably 9.8 or more. By increasing the pH, it tends to increase the polishing speed of the wafer.

精加工研磨用組成物之pH較佳為11.5以下，又以11.0以下為佳，更佳為10.5以下。藉由降低pH，傾向提升矽晶圓之面精準度。精加工研磨用組成物及前研磨用組成物之pH可藉由，例如添加後述之pH調整劑而調整。 The pH of the finishing polishing composition is preferably 11.5 or less, more preferably 11.0 or less, still more preferably 10.5 or less. By lowering the pH, it tends to increase the accuracy of the wafer surface. The pH of the composition for polishing and the composition for pre-polishing can be adjusted by, for example, adding a pH adjuster described later.

8.有關水 8. About water

水係作為磨粒、鹼性化合物、水溶性高分子等之其他成分之分散劑或溶劑。為了極力回避阻礙精加工研磨用組成物及前研磨用組成物所含有之其他成分之作用，水較佳為例如使過渡金屬離子之合計含量為100ppb以下。例如可使用離子交換樹脂去除不純物離子、藉由濾器去除粒子、藉由蒸餾等操作以提高水之純度。具體上又以使用離子交換水、純水、超純水、蒸餾水等為佳。 The water system is used as a dispersing agent or solvent for other components such as abrasive grains, basic compounds, and water-soluble polymers. In order to prevent the action of the finishing polishing composition and the other components contained in the pre-polishing composition as much as possible, the water preferably has a total content of the transition metal ions of, for example, 100 ppb or less. For example, an ion exchange resin can be used to remove impurities ions, particles are removed by a filter, and distillation or the like can be used to increase the purity of water. Specifically, ion-exchanged water, pure water, ultrapure water, distilled water or the like is preferably used.

9.有關添加劑 9. Related additives

本實施形態之精加工研磨用組成物及前研磨用組成物為了提升其性能，必要時可添加pH調整劑、表面活性劑、螯合劑、防黴劑等各種添加劑。但以實質不含氧化劑為佳。 In order to improve the performance, the finishing polishing composition and the pre-polishing composition of the present embodiment may be added with various additives such as a pH adjuster, a surfactant, a chelating agent, and a mold inhibitor. However, it is preferred that the oxidant is substantially absent.

9-1 有關pH調整劑 9-1 About pH adjuster

本實施形態之精加工研磨用組成物及前研磨用組成物之pH值可藉由添加pH調整劑而調整。藉由調整精加工研磨用組成物及前研磨用組成物之pH，可控制研磨對象物之研磨速度及磨粒之分散性等。pH調整劑之添加量無特別限定，可依精加工研磨用組成物及前研磨用組成物所希望之pH適當調整。 The pH of the finishing polishing composition and the pre-polishing composition of the present embodiment can be adjusted by adding a pH adjusting agent. By adjusting the pH of the finishing polishing composition and the pre-polishing composition, the polishing rate of the object to be polished, the dispersibility of the abrasive grains, and the like can be controlled. The amount of the pH adjuster to be added is not particularly limited, and can be appropriately adjusted depending on the desired pH of the finishing polishing composition and the pre-polishing composition.

pH調整劑之具體例如無機酸或羧酸、有機硫酸等之有機酸。無機酸之具體例如，鹽酸、硫酸、硝酸、 氟酸、硼酸、碳酸、次亞磷酸、亞磷酸、磷酸等。又，羧酸之具體例如，甲酸、乙酸、丙酸、丁酸、戊酸、2-甲基丁酸、n-己酸、3,3-二甲基丁酸、2-乙基丁酸、4-甲基戊酸、n-庚酸、2-甲基己酸、n-辛酸、2-乙基己酸、苯甲酸、乙醇酸、水楊酸、甘油酸、草酸、丙二酸、琥珀酸、戊二酸、己二酸、庚二酸、馬來酸、酞酸、蘋果酸、酒石酸、檸檬酸、乳酸、二甘醇酸、2-呋喃羧酸、2,5-呋喃二羧酸、3-呋喃羧酸、2-四氫呋喃羧酸、甲氧基乙酸、甲氧基苯基乙酸、苯氧基乙酸等。另外有機硫酸之具體例如，甲烷磺酸、乙烷磺酸、羥乙磺酸等。該等之酸可單獨使用一種，或二種以上組合使用。 Specific examples of the pH adjuster include inorganic acids or organic acids such as carboxylic acids and organic sulfuric acids. Specific examples of inorganic acids, for example, hydrochloric acid, sulfuric acid, nitric acid, Fluoric acid, boric acid, carbonic acid, hypophosphorous acid, phosphorous acid, phosphoric acid, and the like. Further, specific examples of the carboxylic acid are formic acid, acetic acid, propionic acid, butyric acid, valeric acid, 2-methylbutyric acid, n-hexanoic acid, 3,3-dimethylbutyric acid, 2-ethylbutyric acid, 4-methylpentanoic acid, n-heptanoic acid, 2-methylhexanoic acid, n-octanoic acid, 2-ethylhexanoic acid, benzoic acid, glycolic acid, salicylic acid, glyceric acid, oxalic acid, malonic acid, amber Acid, glutaric acid, adipic acid, pimelic acid, maleic acid, citric acid, malic acid, tartaric acid, citric acid, lactic acid, diglycolic acid, 2-furancarboxylic acid, 2,5-furandicarboxylic acid , 3-furancarboxylic acid, 2-tetrahydrofurancarboxylic acid, methoxyacetic acid, methoxyphenylacetic acid, phenoxyacetic acid, and the like. Further, specific examples of the organic sulfuric acid include methanesulfonic acid, ethanesulfonic acid, isethionic acid, and the like. These acids may be used alone or in combination of two or more.

9-2 有關表面活性劑 9-2 related surfactants

本實施形態之精加工研磨用組成物及前研磨用組成物可添加表面活性劑。表面活性劑如陰離子性或非離子性表面活性劑，其中較佳為非離子性表面活性劑。 A surfactant can be added to the finishing polishing composition and the pre-polishing composition of the present embodiment. A surfactant such as an anionic or nonionic surfactant is preferred as the nonionic surfactant.

例如，聚乙二醇、聚丙二醇、聚四甲二醇等之氧基烯烴聚合物，或聚環氧乙烷烷基醚、聚環氧乙烷烷基苯基醚、聚環氧乙烷烷基胺、聚環氧乙烷脂肪酸酯、聚環氧乙烷甘油基醚脂肪酸酯、聚環氧乙烷山梨糖醇脂肪酸酯等之聚環氧烷加成物、或複數種烷二醇共聚物(二嵌段型、三嵌段型、無規型、交互型)等之非離子性表面活性劑。 For example, an oxyalkylene polymer such as polyethylene glycol, polypropylene glycol, or polytetramethylene glycol, or a polyethylene oxide alkyl ether, a polyethylene oxide alkyl phenyl ether, or a polyethylene oxide alkane. a polyalkylene oxide adduct of a base amine, a polyethylene oxide fatty acid ester, a polyethylene oxide glyceryl ether fatty acid ester, a polyethylene oxide sorbitol fatty acid ester, or a plurality of alkane A nonionic surfactant such as an alcohol copolymer (diblock type, triblock type, random type, interactive type).

非離子性表面活性劑之具體例如，氧基乙烯 (EO)與氧基丙烯(PO)之嵌段共聚物(二嵌段物、PEO-PPO-PEO型三嵌段物、PPO-PEO-PPO型三嵌段物等)、EO與PO之無規共聚物、聚氧基乙二醇、聚環氧乙烷丙基醚、聚環氧乙烷丁基醚、聚環氧乙烷戊基醚、聚環氧乙烷己基醚、聚環氧乙烷辛基醚、聚環氧乙烷-2-乙基己基醚、聚環氧乙烷壬基醚、聚環氧乙烷癸基醚、聚環氧乙烷異癸基醚、聚環氧乙烷十三烷基醚、聚環氧乙烷月桂基醚、聚環氧乙烷十六烷基醚、聚環氧乙烷硬脂醯醚、聚環氧乙烷異硬脂醯醚、聚環氧乙烷油烯基醚、聚環氧乙烷苯基醚、聚環氧乙烷辛基苯基醚、聚環氧乙烷壬基苯基醚、聚環氧乙烷十二烷基苯基醚、聚環氧乙烷苯乙烯化苯基醚、聚環氧乙烷月桂基胺、聚環氧乙烷硬脂醯胺、聚環氧乙烷油基胺、聚環氧乙烷硬脂醯胺、聚環氧乙烷油基醯胺、聚環氧乙烷單月桂酸酯、聚環氧乙烷單硬脂酸酯、聚環氧乙烷二硬脂酸酯、聚環氧乙烷單油酸酯、聚環氧乙烷二油酸酯、單月桂酸聚環氧乙烷山梨糖醇酐、單棕櫚酸聚環氧乙烷山梨糖醇酐、單硬脂酸聚環氧乙烷山梨糖醇酐、單油酸聚環氧乙烷山梨糖醇酐、三油酸聚環氧乙烷山梨糖醇酐、四油酸聚環氧乙烷雙脫水山梨糖醇、聚環氧乙烷篦麻油、聚環氧乙烷硬化蓖麻油等。其中較佳之表面活性劑如，EO與PO之嵌段共聚物(特別是PEO-PPO-PEO型三嵌段物)、EO與PO之無規共聚物，及聚環氧乙烷烷基醚(例如聚環氧乙烷癸基醚)。 Specific examples of the nonionic surfactant are, for example, oxyethylene Block copolymer of (EO) and oxypropylene (PO) (diblock, PEO-PPO-PEO type triblock, PPO-PEO-PPO type triblock, etc.), EO and PO Copolymer, polyoxyethylene glycol, polyethylene oxide propyl ether, polyethylene oxide butyl ether, polyethylene oxide pentyl ether, polyethylene oxide hexyl ether, polyethylene oxide Alkyl octyl ether, polyethylene oxide-2-ethylhexyl ether, polyethylene oxide decyl ether, polyethylene oxide decyl ether, polyethylene oxide isodecyl ether, polyethylene oxide Alkyl tridecyl ether, polyethylene oxide lauryl ether, polyethylene oxide cetyl ether, polyethylene oxide stearyl ether, polyethylene oxide isostearyl ether, polycyclic ring Oxyethane ethane alkenyl ether, polyethylene oxide phenyl ether, polyethylene oxide octyl phenyl ether, polyethylene oxide nonylphenyl ether, polyethylene oxide dodecyl phenyl Ether, polyethylene oxide styrenated phenyl ether, polyethylene oxide laurylamine, polyethylene oxide stearylamine, polyethylene oxide oleylamine, polyethylene oxide stearin Amine, polyethylene oxide oleylamine, polyethylene oxide monolaurate, polyethylene oxide monostearate, poly Ethoxyethane distearate, polyethylene oxide monooleate, polyethylene oxide dioleate, monolaurate polyethylene oxide sorbitan, monopalmitate polyethylene oxide Sorbitol, monostearate polyethylene oxide sorbitan, monooleic acid polyethylene oxide sorbitan, trioleic acid polyethylene oxide sorbitan, tetraoleic acid polycyclic ring Oxygen ethane sorbitan, polyethylene oxide castor oil, polyethylene oxide hardened castor oil, and the like. Among the preferred surfactants are block copolymers of EO and PO (especially PEO-PPO-PEO type triblocks), random copolymers of EO and PO, and polyethylene oxide alkyl ethers ( For example, polyethylene oxide decyl ether).

又，陰離子性表面活性劑如，聚環氧乙烷烷 基醚之硫酸酯及其鹽、磺酸及其鹽、羧酸及其鹽，及磷酸酯及其鹽。 Also, an anionic surfactant such as polyethylene oxide Sulfates and their salts, sulfonic acids and salts thereof, carboxylic acids and salts thereof, and phosphates and salts thereof.

陰離子性表面活性劑之具體例如，聚環氧乙烷月桂基醚硫酸、聚環氧乙烷肉豆蔻基醚硫酸、聚環氧乙烷棕櫚基醚硫酸；聚環氧乙烷月桂基醚硫酸鈉、聚環氧乙烷月桂基醚硫酸銨、聚環氧乙烷月桂基醚硫酸三乙醇胺、聚環氧乙烷肉豆蔻基醚硫酸鈉、聚環氧乙烷肉豆蔻基醚硫酸銨、聚環氧乙烷肉豆蔻基醚硫酸三乙醇胺、聚環氧乙烷棕櫚基醚硫酸鈉、聚環氧乙烷棕櫚基醚硫酸胺、聚環氧乙烷棕櫚基醚硫酸三乙醇胺、聚環氧乙烷辛基磺酸、聚環氧乙烷十二烷基磺酸、聚環氧乙烷十六烷基磺酸、聚環氧乙烷辛基苯磺酸、聚環氧乙烷十六烷基苯磺酸；聚環氧乙烷辛基磺酸鈉、聚環氧乙烷十二烷基磺酸鈉、聚環氧乙烷十六烷基磺酸鈉、聚環氧乙烷月桂基醚乙酸、聚環氧乙烷十二烷基醚乙酸、聚環氧乙烷辛基醚乙酸；聚環氧乙烷月桂基醚乙酸鈉、聚環氧乙烷月桂基醚乙酸銨、聚環氧乙烷十三烷基醚乙酸鈉、聚環氧乙烷十三烷基醚乙酸銨、聚環氧乙烷辛基醚乙酸鈉、聚環氧乙烷辛基醚乙酸銨、聚環氧乙烷月桂基醚磷酸、聚環氧乙烷烷基(12-15)醚磷酸；聚環氧乙烷月桂基醚磷酸鈉、聚環氧乙烷油烯基醚磷酸鈉、聚環氧乙烷十六烷基醚磷酸鈉、聚環氧乙烷烷基(12-15)醚磷酸鉀、聚環氧乙烷月桂基磺基琥珀酸二鈉鹽、磺基琥珀酸聚環氧乙烷月桂醯基乙醇醯胺二鈉鹽等。 Specific examples of the anionic surfactant are, for example, polyethylene oxide lauryl ether sulfuric acid, polyethylene oxide myristyl ether sulfuric acid, polyethylene oxide palmityl ether sulfuric acid; polyethylene oxide lauryl ether sulfate , polyethylene oxide ammonium lauryl ether sulfate, polyethylene oxide lauryl ether triethanolamine sulfate, polyethylene oxide myristyl ether sulfate, polyethylene oxide myristyl ether ammonium sulfate, polycyclic ring Oxygen ethane myristyl ether triethanolamine sulfate, polyethylene oxide palmitate sodium sulfate, polyethylene oxide palmityl ether sulfate, polyethylene oxide palmityl ether triethanolamine, polyethylene oxide Octyl sulfonic acid, polyethylene oxide dodecyl sulfonic acid, polyethylene oxide hexadecyl sulfonic acid, polyethylene oxide octyl benzene sulfonic acid, polyethylene oxide hexadecyl benzene Sulfonic acid; sodium polyoxyethylene octyl sulfonate, sodium polyethylene oxide dodecyl sulfonate, sodium polyethylene oxide hexadecyl sulfonate, polyethylene oxide lauryl ether acetic acid, Polyethylene oxide lauryl ether acetate, polyethylene oxide octyl ether acetic acid; polyethylene oxide lauryl ether acetate sodium, polyethylene oxide lauryl Ammonium acetate, polyethylene oxide tridecyl ether acetate, polyethylene oxide tridecyl ether ammonium acetate, polyethylene oxide octyl ether acetate, polyethylene oxide octyl ether ammonium acetate , polyethylene oxide lauryl ether phosphate, polyethylene oxide alkyl (12-15) ether phosphate; polyethylene oxide lauryl ether sodium phosphate, polyethylene oxide oleyl ether sodium phosphate, poly Ethylene oxide cetyl ether sodium phosphate, polyethylene oxide alkyl (12-15) ether potassium phosphate, polyethylene oxide lauryl sulfosuccinate disodium salt, sulfosuccinic acid polyepoxy Ethyl lauryl mercaptoethanol guanamine disodium salt and the like.

表面活性劑之重量平均分子量較佳為200以 上，又以250以上為佳，更佳為300以上。藉由增加表面活性劑之重量平均分子量，可提升矽晶圓之研磨速度。 The weight average molecular weight of the surfactant is preferably 200 Above, it is preferably 250 or more, more preferably 300 or more. By increasing the weight average molecular weight of the surfactant, the polishing speed of the tantalum wafer can be increased.

表面活性劑之重量平均分子量較佳為未達10000，更佳為9500以下。藉由減低表面活性劑之重量平均分子量，可提升被研磨面之平滑性。 The weight average molecular weight of the surfactant is preferably less than 10,000, more preferably not more than 9,500. The smoothness of the surface to be polished can be improved by reducing the weight average molecular weight of the surfactant.

9-3 有關螯合劑 9-3 About chelating agents

本實施形態之精加工研磨用組成物及前研磨用組成物可添加螯合劑。螯合劑係藉由捕捉研磨系中之金屬不純物成份以形成錯合物，而抑制矽基板之金屬污染(特別是來自鎳、銅之污染)。 A chelating agent can be added to the finishing polishing composition and the pre-polishing composition of the present embodiment. The chelating agent inhibits metal contamination of the ruthenium substrate (especially from nickel and copper) by capturing the metal impurity components in the abrasive system to form a complex.

螯合劑之具體例如，戊烯二酸等之羧酸系螯合劑、伸乙基二胺、二伸乙基三胺、三甲基四胺等之胺系螯合劑、伸乙基二胺四乙酸、氰基三乙酸、羥基乙基伸乙基二胺三乙酸、三伸乙基四胺六乙酸、二伸乙基三胺五乙酸等之聚胺基聚羧酸系螯合劑、2-胺基乙基膦酸、1-羥基亞乙基-1,1-二膦酸、胺基三(伸甲基膦酸)、伸乙基二胺四(伸甲基膦酸)、二伸乙基三胺五(伸甲基膦酸)、乙烷-1,1-二膦酸、乙烷-1,1,2-三膦酸、甲烷羥基膦酸、1-膦基丁烷-2,3,4-三羧酸等之有機膦酸系螯合劑、苯酚衍生物、1,3-二酮等。該等螯合劑中較佳為有機膦酸系螯合劑，特佳為伸乙基二胺四(伸甲基膦酸)，該等螯合劑可單獨使用一種，或二種以上組合使用。 Specific examples of the chelating agent include a carboxylic acid-based chelating agent such as glutaconic acid, an amine-based chelating agent such as ethylenediamine, di-ethyltriamine or trimethyltetramine, and ethyldiaminetetraacetic acid. Polyaminopolycarboxylic acid chelating agent such as cyanotriacetic acid, hydroxyethyl extended ethyldiaminetriacetic acid, tris-ethyltetraamine hexaacetic acid, di-extended ethyltriaminepentaacetic acid, etc., 2-amino B Phosphonic acid, 1-hydroxyethylidene-1,1-diphosphonic acid, amine tris(methylphosphonic acid), ethyldiamine tetra(methylphosphonic acid), diethylidene triamine Five (methyl phosphonic acid), ethane-1,1-diphosphonic acid, ethane-1,1,2-triphosphonic acid, methane hydroxyphosphonic acid, 1-phosphinobutane-2,3,4 An organic phosphonic acid-based chelating agent such as a tricarboxylic acid, a phenol derivative, or a 1,3-diketone. Among these chelating agents, an organic phosphonic acid-based chelating agent is preferred, and an ethylidene diamine tetra(methylphosphonic acid) is particularly preferred. These chelating agents may be used alone or in combination of two or more.

9-4 有關防黴劑 9-4 About anti-fungal agents

本實施形態之精加工研磨用組成物及前研磨用組成物可添加防黴劑。防黴劑之具體例如，2-噁唑烷-2,5-二酮等之噁唑啉等。 In the finishing polishing composition and the pre-polishing composition of the present embodiment, an anti-fungal agent can be added. Specific examples of the fungicide include, for example, oxazolines such as 2-oxazolidine-2,5-dione.

9-5 有關氧化劑 9-5 About oxidants

本實施形態之精加工研磨用組成物及前研磨用組成物又以實質不含氧化劑為佳。因精加工研磨用組成物及前研磨用組成物中含有氧化劑時，將該研磨用組成物供給研磨對象物(例如矽晶圓)會使該研磨對象物之表面被氧化而生成氧化膜，故需拉長所需研磨時間。此時所指之氧化劑之具體例如，過氧化氫(H2O2)、過硫酸鈉、過硫酸銨、過錳酸鉀、二氯三聚異氰酸鈉等。 The finishing polishing composition and the pre-polishing composition of the present embodiment are preferably substantially free of an oxidizing agent. When the composition for polishing and the composition for pre-polishing contains an oxidizing agent, the polishing composition is supplied to the object to be polished (for example, a tantalum wafer), and the surface of the object to be polished is oxidized to form an oxide film. It is necessary to lengthen the required grinding time. Specific examples of the oxidizing agent referred to at this time include hydrogen peroxide (H 2 O 2 ), sodium persulfate, ammonium persulfate, potassium permanganate, sodium dichlorotrisocyanate, and the like.

又，精加工研磨用組成物及前研磨用組成物實質不含氧化劑係指，至少意圖上不含氧化劑。因此不可避免含有來自原料及製法等之微量(例如精加工研磨用組成物及前研磨用組成物中氧化劑之莫耳濃度為0.0005莫耳/L以下，又以0.0001莫耳以下為佳，更佳為0.00001莫耳/L以下，特佳為0.000001莫耳/L以下)氧化劑之研磨用組成物(精加工研磨用組成物、前研磨用組成物)可包含於此時所指實質不含氧化劑之研磨用組成物概念中。 Further, the finishing polishing composition and the pre-polishing composition do not substantially contain an oxidizing agent, and at least the oxidizing agent is not intended to be contained. Therefore, it is inevitable to contain a trace amount from a raw material, a production method, etc. (for example, the molar concentration of the oxidizing agent in the composition for finishing polishing and the composition for pre-polishing is 0.0005 mol/L or less, and preferably 0.0001 mol or less, more preferably The polishing composition (finishing polishing composition, pre-polishing composition) having an oxidizing agent of 0.00001 mol/L or less, particularly preferably 0.000001 mol/L or less may be contained in the case where the oxidizing agent is substantially not contained at this time. In the concept of polishing composition.

10.有關矽晶圓之研磨方法 10. Grinding method for germanium wafer

使用本實施形態之精加工研磨用組成物及前研磨用組 成物研磨矽晶圓時，可藉由一般研磨用之研磨裝置及研磨條件進行。例如可使用單面研磨裝置或雙面研磨裝置。 The finishing polishing composition and the front polishing group of the embodiment are used. When the wafer is polished, the wafer can be polished by a general polishing apparatus and polishing conditions. For example, a single-side polishing device or a double-side polishing device can be used.

例如使用單面研磨裝置研磨矽晶圓時，係藉由使用稱為載體之保持器保持矽晶圓下，將單面貼有研磨布之平板壓在矽晶圓之單面後，於供給本實施形態之精加工研磨用組成物或前研磨用組成物的同時回轉底盤以研磨矽晶圓之單面。 For example, when a tantalum wafer is polished by a single-sided polishing apparatus, a flat plate with a polishing cloth is pressed against one side of the silicon wafer by using a holder called a carrier to hold the silicon wafer under the wafer, and then supplied to the substrate. In the embodiment, the polishing composition or the pre-polishing composition is rotated while rotating the chassis to polish one side of the silicon wafer.

又，使用雙面研磨裝置研磨矽晶圓時，係藉由使用稱為載體之保持器保持矽晶圓下，由矽晶圓兩側將貼有研磨布之平板各自壓在矽晶圓雙面後，於供給本實施形態之精加工研磨用組成物或前研磨用組成物的同時回轉兩側平板以研磨矽晶圓雙面。 Moreover, when the silicon wafer is polished by the double-side polishing apparatus, the wafer is attached to the wafer by using a holder called a carrier, and the flat sheets to which the polishing cloth is attached are pressed on both sides of the wafer. Thereafter, while the finishing polishing composition or the pre-polishing composition of the present embodiment is supplied, both side plates are rotated to polish both sides of the crucible wafer.

無論使用任一種研磨裝置，均可藉由摩擦(研磨布及研磨用組成物(精加工研磨用組成物、前研磨用組成物)與矽晶圓之摩擦)之物理性作用，及精加工研磨用組成物、前研磨用組成物相對於矽晶圓之化學性作用而研磨矽晶圓。 Regardless of the use of any type of polishing device, the physical action of rubbing (friction of polishing cloth and polishing composition (finishing polishing composition, pre-polishing composition) and tantalum wafer), and finishing polishing can be performed. The tantalum wafer is polished by the chemical action of the composition and the pre-polishing composition with respect to the tantalum wafer.

研磨布可使用聚胺基甲酸酯、不織布、絨布等各種材質之物。又可使用不同材質之硬度及厚度等物性各自不同之物，另外可使用含有磨粒之物、不含磨粒之物，但以使用不含磨粒之物為佳。又可使用液狀之精加工研磨用組成物及前研磨用組成物般可實施積存之溝加工之物。 As the polishing cloth, various materials such as polyurethane, non-woven fabric, and flannel can be used. Further, it is also possible to use materials having different physical properties such as hardness and thickness of different materials, and it is also possible to use an abrasive-containing material or an abrasive-free material, but it is preferable to use an abrasive-free material. Further, it is also possible to use a liquid-like finishing polishing composition and a pre-polishing composition to carry out the storage of the groove.

另外精加工研磨步驟、前研磨步驟中之任一 研磨條件中研磨荷重(矽晶圓所負荷之壓力)無特別限定，可為5kPa以上50kPa以下，較佳為8kPa以上30kPa以下，更佳為10kPa以上20kPa以下。研磨荷重為該範圍內時可發揮充分之研磨速度，而抑制因荷重而使矽晶圓破損，及使矽晶圓表面發生傷痕等缺陷。 In addition, either the finishing grinding step or the pre-grinding step The polishing load (the pressure applied to the crucible wafer) in the polishing conditions is not particularly limited, and may be 5 kPa or more and 50 kPa or less, preferably 8 kPa or more and 30 kPa or less, and more preferably 10 kPa or more and 20 kPa or less. When the polishing load is within this range, a sufficient polishing rate can be exhibited, and defects such as breakage of the ruthenium wafer due to the load and scratches on the surface of the ruthenium wafer can be suppressed.

又，研磨條件中研磨用之研磨布與矽晶圓之相對速度(線速度)無特別限定，可為10m/分以上300m/分以下，較佳為30m/分以上200m/分以下。研磨布與矽晶圓之相對速度該範圍內時可得充分之研磨速度。又，可抑制因摩擦矽晶圓而使研磨布破損，另外可充分將摩擦力傳至矽晶圓，即可抑制矽晶圓為滑動狀態而充分研磨。 Moreover, the relative speed (linear velocity) of the polishing cloth for polishing and the tantalum wafer in the polishing conditions is not particularly limited, and may be 10 m/min or more and 300 m/min or less, preferably 30 m/min or more and 200 m/min or less. A sufficient polishing speed is obtained when the relative speed of the polishing cloth and the silicon wafer is within this range. Further, it is possible to suppress breakage of the polishing cloth by rubbing the wafer, and to sufficiently transmit the frictional force to the silicon wafer, thereby suppressing the silicon wafer from being in a sliding state and sufficiently polishing.

又，研磨條件中精加工研磨用組成物及前研磨用組成物之供給量會因矽晶圓之種類、研磨裝置之種類、研磨條件而異，可為供給矽晶圓與研磨布之間的精加工研磨用組成物、前研磨用組成物無不均之充分量。精加工研磨用組成物、前研磨用組成物之供給量較少時，將無法將精加工研磨用組成物、前研磨用組成物供給全體之矽晶圓，且精加工研磨用組成物、前研磨用組成物乾燥凝固後會使矽晶圓之表面發生缺陷。相反地精加工研磨用組成物、前研磨用組成物之供給量過多時，除了經濟面，多餘之精加工研磨用組成物、前研磨用組成物(特別是水)恐防害摩擦而阻礙研磨。 Further, the amount of the finishing polishing composition and the pre-polishing composition in the polishing conditions may vary depending on the type of the wafer, the type of the polishing apparatus, and the polishing conditions, and may be between the supply of the wafer and the polishing cloth. The finishing polishing composition and the pre-polishing composition have a sufficient amount without unevenness. When the amount of the finishing polishing composition and the pre-polishing composition is small, the finishing polishing composition and the pre-polishing composition cannot be supplied to the entire wafer, and the polishing composition and the former are finished. After the polishing composition is dried and solidified, defects may occur on the surface of the germanium wafer. On the other hand, when the amount of the finishing polishing composition and the pre-polishing composition is too large, the excess finishing polishing composition and the pre-polishing composition (particularly water) may be prevented from rubbing and hinder the polishing, in addition to the economical surface.

另外本實施形態之精加工研磨用組成物、前研磨用組成物使用於研磨矽晶圓時，其係可再回收使用於 研磨矽晶圓。再使用精加工研磨用組成物、前研磨用組成物之方法之一例如，以槽回收由研磨裝置排出之精加工研磨用組成物、前研磨用組成物後，再度循環回研磨裝置內使用於研磨之方法。循環使用精加工研磨用組成物、前研磨用組成物時可減少以廢液狀排出之精加工研磨用組成物、前研磨用組成物之量，因此可減少環境負荷，又因可減少精加工研磨用組成物、前研磨用組成物之量，故可抑制研磨矽晶圓所需之製造成本。 Further, when the finishing polishing composition and the pre-polishing composition of the present embodiment are used for polishing a tantalum wafer, they can be reused for use in Grinding the germanium wafer. Further, one of the methods for finishing the polishing composition and the pre-polishing composition, for example, recovering the finishing polishing composition and the pre-polishing composition discharged from the polishing apparatus in a tank, and then recycling it back to the polishing apparatus for use in the polishing apparatus. The method of grinding. When the finishing polishing composition and the pre-polishing composition are recycled, the amount of the finishing polishing composition and the pre-polishing composition discharged in the form of waste liquid can be reduced, thereby reducing the environmental load and reducing the finishing. Since the amount of the polishing composition and the pre-polishing composition is small, the manufacturing cost required for polishing the silicon wafer can be suppressed.

再使用本實施形態之精加工研磨用組成物、前研磨用組成物時，因使用於研磨所消耗、損失之磨粒、水溶性高分子、鹼性化合物、添加劑等之一部分或全部，可藉由添加組成調整劑而再使用。組成調整劑可使用以任意混合比例混合磨粒、水溶性高分子、鹼性化合物、添加劑等所得之物。藉由追加組成調整劑，將精加工研磨用組成物、前研磨用組成物調整為適合再使用之組成後，可進行較佳之研磨。組成調整劑所含有之磨粒、水溶性分子、鹼性化合物及其他添加劑之濃度可任意，無特別限定，可因應槽大小及研磨條件適當調整。 When the finishing polishing composition and the pre-polishing composition of the present embodiment are used, part or all of the abrasive grains, water-soluble polymers, basic compounds, additives, etc., which are consumed and lost by polishing, can be used. It is reused by adding a compositional modifier. As the composition adjusting agent, those obtained by mixing abrasive grains, water-soluble polymers, basic compounds, additives, and the like in an arbitrary mixing ratio can be used. By adjusting the finishing polishing composition and the pre-polishing composition to a composition suitable for reuse by adding a composition adjusting agent, it is possible to perform preferable polishing. The concentration of the abrasive grains, the water-soluble molecules, the basic compound, and other additives contained in the composition adjusting agent can be arbitrary, and is not particularly limited, and can be appropriately adjusted depending on the groove size and the polishing conditions.

又，本實施形態為表示本發明一例之物，本發明非限定於本實施形態。又，本實施形態可進行各種變更或改良，該類變更或改良後之形態也包括於本發明。例如本實施形態之精加工研磨用組成物、前研磨用組成物可為單液型，或以任意比例混合精加工研磨用組成物、前研磨用組成物之部分或全部成分之雙液型等之多液型。又， 研磨矽晶圓時可直接使用本實施形態之精加工研磨用組成物、前研磨用組成物之原液進行研磨，或使用以水等之稀釋液將原液稀釋為例如10倍以上精加工研磨用組成物、前研磨用組成物稀釋物進行研磨。 Further, the present embodiment is an example of the present invention, and the present invention is not limited to the embodiment. Further, the present embodiment can be variously modified or improved, and such modified or improved forms are also included in the present invention. For example, the finishing polishing composition and the pre-polishing composition of the present embodiment may be a single-liquid type, or a two-liquid type in which a part of the finishing polishing composition or a part of the pre-polishing composition is mixed in an arbitrary ratio. Multi-liquid type. also, When the ruthenium wafer is polished, the raw material for the finishing polishing composition and the pre-polishing composition of the present embodiment can be directly used for polishing, or the stock solution can be diluted to, for example, 10 times or more with a dilution liquid such as water. The material and the pre-grinding composition dilution were ground.

實施例 Example

下面將舉實施例及比較例，於參考表1、表2下更具體說明本發明。 Hereinafter, the present invention will be more specifically described with reference to Tables 1 and 2 in the examples and comparative examples.

混合由平均一次粒徑12nm、25nm或35nm之膠質二氧化矽所形成之磨粒與鹼性化合物與水溶性高分子與表面活性劑與純水，調製前處理用組成物、標準研磨用組成物、前研磨用組成物a、b、c、d、h及精加工研磨用組成物e、f、g、i。各組成物中磨粒、鹼性化合物、水溶性高分子及表面活性劑之含量如表1所記載，又殘部為純水。 Mixing abrasive grains formed with colloidal cerium oxide having an average primary particle diameter of 12 nm, 25 nm or 35 nm with a basic compound and a water-soluble polymer and a surfactant and pure water to prepare a pretreatment composition and a standard polishing composition The pre-grinding compositions a, b, c, d, h and the finishing polishing compositions e, f, g, i. The content of the abrasive grains, the basic compound, the water-soluble polymer, and the surfactant in each composition is as shown in Table 1, and the residual portion is pure water.

所使用之鹼性化合物種類為氨(NH3)或氫氧化鉀(KOH)。所使用之水溶性高分子種類與重量平均分子量如表1所示。又，表1所記載之「HEC」係指羥基乙基纖維素，「PVP」係指聚乙烯基吡喀烷酮。另外所使用之表面活性劑為，環氧乙烷(EO)與環氧丙烷(PO)所形成之嵌段共聚物(PEO-PPO)，或聚環氧乙烷癸基醚(C-PEO)。 The basic compound species used is ammonia (NH 3 ) or potassium hydroxide (KOH). The water-soluble polymer type and weight average molecular weight used are shown in Table 1. Further, "HEC" described in Table 1 means hydroxyethylcellulose, and "PVP" means polyvinylpyrrolidone. Further, the surfactant used is a block copolymer (PEO-PPO) formed of ethylene oxide (EO) and propylene oxide (PO), or polyethylene oxide decyl ether (C-PEO). .

其次求取前研磨用組成物a、b、c、d、h之親水性參數P1及精加工精準度參數P2，與精加工研磨用組成物e、f、g、i之研磨加工性參數F1。結果如表2所示。 Secondly, the hydrophilicity parameter P1 and the finishing precision parameter P2 of the pre-grinding compositions a, b, c, d, h, and the grinding processability parameter F1 of the finishing polishing compositions e, f, g, i are obtained. . The results are shown in Table 2.

下面將說明求取親水性參數P1之標準試驗1，求取精加工精準度P2之標準試驗2，及研磨加工性參數F1之標準試驗3之內容。又，標準試驗1、2、3中求取各參數用之試驗片材質為，與使用前研磨用組成物a、b、c、d、h及精加工研磨用組成物e、f、g、i實施研磨之研磨對象物之矽晶圓同材質。 The following is a description of the standard test 1 for obtaining the hydrophilicity parameter P1, the standard test 2 for obtaining the finishing precision P2, and the standard test 3 for the grinding processability parameter F1. Further, in the standard tests 1, 2, and 3, the test piece material for each parameter was obtained, and the polishing composition a, b, c, d, h and the finishing polishing composition e, f, g, i The material of the polished object to be polished is the same material.

又，標準試驗1、2、3中求取各參數之試驗片及其材料不為與研磨對象物之矽晶圓同一之物，而係使用與研磨對象物之矽晶圓同材質之矽晶圓，但當然可使用與研磨對象物之矽晶圓同一物之試驗片。 Further, in the standard tests 1, 2, and 3, the test piece and the material for which each parameter is obtained are not the same as the wafer of the object to be polished, and the twin crystal of the same material as the wafer of the object to be polished is used. Round, but of course, a test piece identical to the wafer on which the object is polished can be used.

親水性參數P1係由依序進行下述X1步驟~X6步驟之標準試驗1求取。 The hydrophilicity parameter P1 is obtained by sequentially performing the standard test 1 of the following X1 step to X6 steps.

[標準試驗1] [Standard Test 1]

(X1)相對於與研磨對象物之矽晶圓同材質之矽晶圓(本實施例為，直徑300mm、傳導型p型、結晶方位<100>、無結晶缺陷之矽晶圓)實施前處理。即，相對於矽晶圓，使用前處理用組成物進行研磨後，使用標準研磨用組成物進行研磨，再進行洗淨及乾燥。 (X1) pre-processing with respect to a wafer of the same material as the wafer of the object to be polished (in this embodiment, a wafer having a diameter of 300 mm, a conductive p-type, a crystal orientation of <100>, and no crystal defects) . In other words, after polishing with a composition for pretreatment using a composition for pretreatment, the composition is polished using a standard polishing composition, and then washed and dried.

洗淨係使用以體積比1：3：30混合濃度29質量%之氨水、濃度31質量%之過氧化氫水、脫離子水(DIW)所得之洗淨液進行。更具體為，準備2個附有周波數950kHz之超音波發振器之洗淨槽，各自以該第1及第2之洗淨槽收容上述洗淨液且保持於60℃。其次將研磨後之矽晶圓浸漬於發動上述超音波發振器之狀態下之第1洗淨槽中6分鐘，再浸漬於發動超音波發振器之狀態下之收容超純水之清洗槽中進行清洗，其後浸漬於發動上述超音波發振器之狀態下之第2洗淨槽中6分鐘。以下將該類洗淨步驟記為SC-1洗淨。 The washing was carried out using a washing liquid obtained by mixing a concentration of 29:3 mass% of ammonia water, a concentration of 31% by mass of hydrogen peroxide water, and deionized water (DIW) in a volume ratio of 1:3:30. More specifically, two cleaning tanks having ultrasonic waves having a frequency of 950 kHz were prepared, and the cleaning liquid was stored in the first and second cleaning tanks and kept at 60 °C. Next, the polished germanium wafer is immersed in the first cleaning tank in a state where the ultrasonic oscillator is activated for 6 minutes, and then immersed in a cleaning tank for accommodating the ultrapure water in a state where the ultrasonic oscillator is activated. The cleaning was carried out, and then immersed in the second cleaning tank in the state where the ultrasonic oscillator was started for 6 minutes. Hereinafter, this type of washing step is referred to as SC-1 washing.

使用前處理用組成物進行研磨時係使用岡本工作機械製作所股份公司製之研磨機PNX-332B、富吉朋股份公司製之研磨台FP55、其研磨條件為，研磨荷重20kPa、平板回轉速度20rpm、載體回轉速度20rpm、研磨時間2min、前處理用組成物之供給速度1L/min、前處理用組成物之溫度20℃、底盤冷卻水之溫度為20℃ When the pre-treatment composition was used for the polishing, the polishing machine PNX-332B manufactured by Okamoto Machine Tool Co., Ltd. and the polishing table FP55 manufactured by Fujie Pang Co., Ltd. were used, and the polishing conditions were: polishing load 20 kPa, plate rotation speed 20 rpm, carrier Rotation speed 20 rpm, polishing time 2 min, supply rate of pretreatment composition 1 L/min, temperature of pretreatment composition 20 ° C, temperature of chassis cooling water 20 ° C

又，使用標準研磨用組成物進行研磨時係使用岡本工作機械製作所股份公司製之研磨機PNX-332B、 富吉朋股份公司製之研磨台POLYPAS27NX，其研磨條件為，研磨荷重15kPa、底盤回轉速度30rpm、載體回轉速度30rpm、研磨時間2min、標準研磨用組成物之供給速度2L/min、標準研磨用組成物之溫度20℃、底盤冷卻水之溫度20℃。 In addition, when grinding with a standard polishing composition, the grinding machine PNX-332B manufactured by Okamoto Machine Tool Co., Ltd. is used. Grinding table POLYPAS27NX manufactured by Fujitsupeng Co., Ltd., grinding conditions: grinding load 15 kPa, chassis rotation speed 30 rpm, carrier rotation speed 30 rpm, grinding time 2 min, standard polishing composition supply speed 2 L / min, standard polishing composition The temperature is 20 ° C, and the temperature of the chassis cooling water is 20 ° C.

前處理用組成物為，含有0.95質量%之平均一次粒徑35nm之膠質二氧化矽及0.065質量%之氫氧化鉀，且殘部為純水。 The pretreatment composition contained 0.95 mass% of colloidal ceria having an average primary particle diameter of 35 nm and 0.065 mass% of potassium hydroxide, and the residue was pure water.

標準研磨用組成物為，含有0.46質量%之平均一次粒徑35nm之膠質二氧化矽、0.009質量%之氨、0.017質量%之重量平均分子量25萬之羥基乙基纖維素，及0.002質量%之由聚環氧乙烷與聚環氧丙烷所形成之共聚物，且殘部為純水。 The standard polishing composition is composed of 0.46 mass% of colloidal ceria having an average primary particle diameter of 35 nm, 0.009% by mass of ammonia, 0.017 mass% of hydroxyethylcellulose having a weight average molecular weight of 250,000, and 0.002% by mass. A copolymer formed of polyethylene oxide and polypropylene oxide, and the residue is pure water.

(X2)裁切實施前處理後之矽晶圓，製作邊長為60mm之正方形矽薄片試驗片。將該矽薄片試驗片浸漬於濃度3質量%之氟化氫水溶液後，以純水洗淨。 (X2) A silicon wafer having a side length of 60 mm was produced by cutting the wafer after the pre-treatment. The enamel sheet test piece was immersed in a hydrogen fluoride aqueous solution having a concentration of 3 mass%, and then washed with pure water.

(X3)使用前研磨用組成物研磨經X2步驟純水洗淨後之矽薄片試驗片。該矽薄片試驗片進行研磨時係使用日本恩吉斯股份公司製之桌上研磨機EJ-380IN、富吉朋股份公司製之研磨台POLYPAS27NX，其研磨條件為，研磨荷重16kPa、平板回轉速度30rpm、載體回轉速度30rpm、研磨時間2min、前研磨用組成物之供給速度30mL/min、前研磨用組成物之溫度20℃。 (X3) A ruthenium sheet test piece which was washed with pure water in the step X2 was polished by using the composition for polishing before use. The enamel sheet test piece was ground using a table grinder EJ-380IN manufactured by Nippon Co., Ltd., and a polishing table POLYPAS27 NX manufactured by Fujitsupeng Co., Ltd., and the grinding conditions were as follows: a grinding load of 16 kPa, a flat plate turning speed of 30 rpm, The carrier rotation speed was 30 rpm, the polishing time was 2 min, the supply rate of the pre-polishing composition was 30 mL/min, and the temperature of the pre-polishing composition was 20 °C.

(X4)以純水洗淨經X3步驟研磨後之矽薄片 試驗片之表面，以清洗前研磨用組成物。 (X4) Washing the flakes after grinding in the X3 step with pure water The surface of the test piece was used to clean the composition before polishing.

(X5)以該矽薄片試驗片之一方對角線沿著垂直方向般之姿勢靜置經X4步驟純水洗淨後之矽薄片試驗片30秒後，測定對角線中矽薄片試驗片之表面未被純水潤濕之領域之長度，以該長度作為排水距離。 (X5) After the diagonal test piece of one of the enamel sheet test pieces was placed in a vertical direction, the test piece of the ruthenium sheet washed by the X4 step pure water was allowed to stand for 30 seconds, and then the test piece of the ruthenium slice in the diagonal line was measured. The length of the field where the surface is not wetted by pure water, and the length is used as the drainage distance.

(X6)由所測得之排水距離，其於下述式算出前研磨用組成物之親水性參數P1。 (X6) From the measured drainage distance, the hydrophilicity parameter P1 of the pre-polishing composition was calculated by the following formula.

親水性參數P1={(矽薄片試驗片之對角線長度[mm])-(排水距離[mm])}/(矽薄片之對角線長度[mm])×100 Hydrophilic parameter P1={(diagonal length [mm] of the sheet test piece) - (drainage distance [mm])} / (diagonal length of the sheet [mm]) × 100

精加工精準度參數P2係由依序進行下述Y1步驟~Y5步驟之標準試驗2求取。 The finishing precision parameter P2 is obtained by sequentially performing the standard test 2 of the following Y1 step to Y5 step.

[標準試驗2] [Standard Test 2]

(Y1)相對於與研磨對象物之矽晶圓同材質之矽晶圓試驗片(本實施例為，直徑300mm、傳導型P型、結晶方位<100>，無結晶缺陷之矽晶圓試驗片)實施與標準試驗1之X1步驟相同之前處理。即，相對於矽晶圓試驗片，使用前處理用組成物進行研磨後，使用標準研磨用組成物進行研磨，其後進行SC-1洗淨及乾燥以實施前處理。 (Y1) A wafer test piece of the same material as the wafer of the object to be polished (in this embodiment, a wafer having a diameter of 300 mm, a conductive type P, a crystal orientation of <100>, and no crystal defects) The treatment was carried out in the same manner as the X1 procedure of Standard Test 1. In other words, the ruthenium wafer test piece was polished using the composition for pretreatment, and then polished using a standard polishing composition, and then SC-1 was washed and dried to carry out pretreatment.

(Y2)使用前處理用組成物再度研磨經Y1步驟實施前處理後之矽晶圓試驗片。該研磨係使用岡本工作機械製作所股份公司製之研磨機PNX-332B、富吉朋股份 公司製之研磨台FP55，其研磨條件為，研磨荷重20kPa、平板回轉速度20rpm、載體回轉速度20rpm、研磨時間2min、前處理用組成物之供給速度1L/min、前處理用組成物之溫度20℃、平板冷卻水之溫度20℃。 (Y2) The ruthenium wafer test piece subjected to the pretreatment in the Y1 step was re-polished using the pretreatment composition. This grinding system uses a grinder PNX-332B manufactured by Okamoto Machine Works Co., Ltd. Grinding table FP55 manufactured by the company has a grinding condition of 20 kPa, a flat rotation speed of 20 rpm, a carrier rotation speed of 20 rpm, a grinding time of 2 min, a supply speed of the pretreatment composition of 1 L/min, and a temperature of the pretreatment composition of 20 °C, the temperature of the plate cooling water is 20 °C.

(Y3)使用前研磨用組成物研磨實施Y2步驟之研磨後之矽晶圓試驗片。研磨該矽晶圓試驗片時係使用岡本工作機械製作所股份公司製之研磨機PNX-332B、富吉朋股份公司製之研磨台POLYPAS27NX。又，研磨該矽晶圓試驗片之研磨條件為，研磨荷重15kPa、底盤回轉速度30rpm、載體回轉速度30rpm、研磨時間2min、前研磨用組成物之供給速度2L/min、前研磨用組成物之溫度20℃、底盤冷卻水之溫度20℃。 (Y3) The ruthenium wafer test piece after the polishing in the Y2 step was polished by using the composition for polishing before use. In the case of grinding the enamel wafer test piece, a grinding machine PNX-332B manufactured by Okamoto Machine Tool Co., Ltd., and a polishing table POLYPAS27NX manufactured by Fujitsupeng Co., Ltd. were used. Further, the polishing conditions for polishing the silicon wafer test piece were: a polishing load of 15 kPa, a chassis rotation speed of 30 rpm, a carrier rotation speed of 30 rpm, a polishing time of 2 minutes, a supply rate of the front polishing composition of 2 L/min, and a pre-polishing composition. The temperature was 20 ° C, and the temperature of the chassis cooling water was 20 ° C.

(Y4)使用標準研磨用組成物研磨實施Y2步驟之研磨後之矽晶圓試驗片。研磨該矽晶圓試驗片時係使用岡本工作機械製作所股份公司製之研磨機PNX-332B、富吉朋股份公司製之研磨台POLYPAS27NX。又，研磨該矽晶圓試驗片之研磨條件為，研磨荷重15kPa、平板回轉速度30rpm、載體回轉速度30rpm、研磨時間2min、標準研磨用組成物之供給速度2L/min、標準研磨用組成物之溫度20℃、平板冷卻水之溫度20℃。 (Y4) The polished silicon wafer test piece subjected to the Y2 step was polished using a standard polishing composition. In the case of grinding the enamel wafer test piece, a grinding machine PNX-332B manufactured by Okamoto Machine Tool Co., Ltd., and a polishing table POLYPAS27NX manufactured by Fujitsupeng Co., Ltd. were used. Further, the polishing conditions for polishing the tantalum wafer test piece were: a polishing load of 15 kPa, a flat plate rotation speed of 30 rpm, a carrier rotation speed of 30 rpm, a polishing time of 2 min, a supply rate of a standard polishing composition of 2 L/min, and a standard polishing composition. The temperature was 20 ° C, and the temperature of the plate cooling water was 20 ° C.

(Y5)相對於經Y3步驟研磨後之矽晶圓試驗片與經Y4步驟研磨後之矽晶圓試驗片各自進行SC-1洗淨及乾燥後，使用KLA公司製之表面異物檢查裝置SURFSCAN SP2，以DWO方式測定各矽晶圓試驗片表面 之濁度。由經Y3步驟研磨後之矽晶圓試驗片表面之濁度h2，與經Y4步驟研磨後之矽晶圓試驗片表面之濁度α，基於下述式算出前研磨用組成物之精加工精準度參數P2。 (Y5) The surface foreign matter inspection device SURFSCAN SP2 manufactured by KLA Co., Ltd. is used after the SC-1 cleaning and drying of the silicon wafer test piece after the Y3 step polishing and the Y4 step polishing. , measuring the surface of each wafer test piece by DWO method Turbidity. The turbidity h2 of the surface of the test piece of the silicon wafer after the Y3 step is polished, and the turbidity α of the surface of the test piece of the silicon wafer after the Y4 step is ground, and the precision of the finishing of the front polishing composition is calculated based on the following formula. Degree parameter P2.

精加工精準度參數P2=h2/α×100 Finishing precision parameter P2=h2/α×100

研磨加工性參數F1係由依序進行下述Z1步驟~Z6步驟之標準試驗3求取。 The polishing process parameter F1 is obtained by sequentially performing the following standard test 3 of the Z1 step to the Z6 step.

[標準試驗3] [Standard Test 3]

(Z1)相對於與研磨對象物之矽晶圓同材質之矽晶圓試驗片(本實施例為，直徑200mm、傳導型P型、結晶方位<100>，無結晶缺陷之矽晶圓試驗片)實施前處理，即，相對於矽晶圓試驗片，使用前處理用組成物進行研磨後，使用標準研磨用組成物進行研磨，其後進行SC-1洗淨及乾燥。 (Z1) A wafer test piece of the same material as the wafer of the object to be polished (in this embodiment, a wafer having a diameter of 200 mm, a conductive type P, a crystal orientation of <100>, and no crystal defects) Pre-implementation treatment, that is, polishing with a composition for pre-treatment with respect to a silicon wafer test piece, polishing with a standard polishing composition, followed by SC-1 washing and drying.

使用前處理用組成物進行研磨時係使用岡本工作機械製作所股份公司製之研磨機PNX-322、富吉朋股份公司製之研磨台FP55，其研磨條件為，研磨荷重15kPa、平板回轉速度30rpm、載體回轉速度30rpm、研磨時間3min、前處理用組成物之供給速度0.55L/min、前處理用組成物之溫度20℃、平板冷卻水之溫度20℃。 When the pre-treatment composition was used for the polishing, the grinding machine PNX-322 manufactured by Okamoto Machine Tool Co., Ltd. and the polishing table FP55 manufactured by Fujie Pang Co., Ltd. were used, and the polishing conditions were as follows: grinding load 15 kPa, plate rotation speed 30 rpm, carrier The rotation speed was 30 rpm, the polishing time was 3 min, the supply rate of the pretreatment composition was 0.55 L/min, the temperature of the pretreatment composition was 20 ° C, and the temperature of the flat cooling water was 20 ° C.

又，使用標準研磨用組成物進行研磨時係使用岡本工作機械製作所股份公司製之研磨機PNX-322、富吉朋股份公司製之研磨台POLYPAS27NX，其研磨條件 為，研磨荷重15kPa、平板回轉速度30rpm、載體回轉速度30rpm、研磨時間4min、標準研磨用組成物之供給速度0.4L/min、標準研磨用組成物之溫度20℃、平板冷卻水之溫度20℃。 In addition, the polishing machine PNX-322 manufactured by Okamoto Machine Manufacturing Co., Ltd. and the polishing table POLYPAS27NX manufactured by Fujitsupeng Co., Ltd. were used for the polishing using the standard polishing composition. The polishing load is 15 kPa, the plate rotation speed is 30 rpm, the carrier rotation speed is 30 rpm, the polishing time is 4 min, the supply rate of the standard polishing composition is 0.4 L/min, the temperature of the standard polishing composition is 20 ° C, and the temperature of the flat cooling water is 20 ° C. .

(Z2)測定實施Z1步驟之前處理後之矽晶圓試驗片之質量。其次將矽晶圓試驗片浸漬於濃度3質量%之氟化氫水溶液後，以純水洗淨。 (Z2) The mass of the silicon wafer test piece after the treatment before the Z1 step was measured. Next, the silicon wafer test piece was immersed in a hydrogen fluoride aqueous solution having a concentration of 3 mass%, and then washed with pure water.

(Z3)使用精加工研磨用組成物研磨經Z2步驟之純水洗淨後之矽晶圓試驗片。研磨該矽晶圓試驗片時係使用岡本工作機械製作所股份公司製之研磨機PNX-322、富吉股份公司製之研磨台POLYPAS27NX。又，研磨該矽晶圓試驗片之研磨條件為，研磨荷重15kPa、底盤回轉速度30rpm、載體回轉速度30rpm、研磨時間15min、精加工研磨用組成物之供給速度0.4L/min、精加工研磨用組成物之溫度20℃、底盤冷卻水之溫度20℃。 (Z3) A silicon wafer test piece which was washed with pure water of the Z2 step was polished using a finishing polishing composition. When grinding the test piece of the tantalum wafer, the grinding machine PNX-322 manufactured by Okamoto Machine Tool Co., Ltd. and the polishing table POLYPAS27NX manufactured by Fujie Co., Ltd. were used. Further, the polishing conditions for polishing the tantalum wafer test piece were: a polishing load of 15 kPa, a chassis rotation speed of 30 rpm, a carrier rotation speed of 30 rpm, a polishing time of 15 minutes, a supply speed of a finishing polishing composition of 0.4 L/min, and a finishing polishing. The temperature of the composition was 20 ° C, and the temperature of the chassis cooling water was 20 ° C.

(Z4)使用標準研磨用組成物研磨經Z2步驟之純水洗淨後之矽晶圓試驗片。研磨該矽晶圓試驗片時係使用岡本工作機械製作所股份公司製之研磨機PNX-322、富吉朋股份公司製之研磨台POLYPAS27NX。又，研磨該矽晶圓試驗片之研磨條件為，研磨荷重15kPa、平板回轉速度30rpm、載體回轉速度30rpm、研磨時間15min、標準研磨用組成物之供給速度0.4L/min、標準研磨用組成物之溫度20℃、平板冷卻水之溫度20℃。 (Z4) A silicon wafer test piece which was washed with pure water of the Z2 step was polished using a standard polishing composition. When grinding the test piece of the tantalum wafer, the grinder PNX-322 manufactured by Okamoto Machine Tool Co., Ltd. and the polishing table POLYPAS27NX manufactured by Fujitsupeng Co., Ltd. were used. Further, the polishing conditions for polishing the tantalum wafer test piece were a polishing load of 15 kPa, a flat plate rotation speed of 30 rpm, a carrier rotation speed of 30 rpm, a polishing time of 15 minutes, a supply rate of a standard polishing composition of 0.4 L/min, and a standard polishing composition. The temperature is 20 ° C, and the temperature of the flat cooling water is 20 ° C.

(Z5)相對於經Z3步驟研磨後之矽晶圓試 驗片與經Z4步驟研磨後之矽晶圓試驗片各自進行SC-1洗淨及乾燥後，測定質量。 (Z5) Relative to the wafer test after grinding in the Z3 step The test piece and the ruthenium wafer test piece polished by the Z4 step were each subjected to SC-1 washing and drying, and then the mass was measured.

(Z6)由Z2步驟測得之矽晶圓試驗片之質量與Z5步驟測得之矽晶圓試驗片之質量的差，各自算出Z3步驟之研磨之矽磨速度R與Z4步驟之研磨之研磨速度β。其次基於下述式算出精加工研磨用組成物之研磨加工性參數F1。 (Z6) The difference between the mass of the wafer test piece measured by the Z2 step and the mass of the wafer test piece measured by the Z5 step, and the grinding of the grinding speed of the Z3 step and the grinding of the Z4 step are respectively calculated. Speed β. Next, the polishing processability parameter F1 of the finishing polishing composition is calculated based on the following formula.

研磨加工性參數F1=R/β×100 Grinding processability parameter F1=R/β×100

適當組合該類前研磨用組成物a、b、c、d、h與精加工研磨用組成物e、f、g、i，製作實施例1~4及比較例1~4之研磨用組成物套組(參考表2)。其次使用該等研磨用組成物套組研磨研磨對象物之矽晶圓，研磨後測定矽晶圓表面之濁度。矽晶圓之研磨方法為，備有使用前處理用組成物進行研磨之第1次研磨步驟，與使用前研磨用組成物進行研磨之前研磨步驟(第二次研磨步驟)，與使用精加工研磨用組成物進行精加工研磨步驟之方法。 The polishing compositions of Examples 1 to 4 and Comparative Examples 1 to 4 were produced by appropriately combining the pre-grinding compositions a, b, c, d, and h and the finishing polishing compositions e, f, g, and i. Set (refer to Table 2). Next, the wafer of the object to be polished is polished using the polishing composition set, and the turbidity of the surface of the wafer is measured after polishing. The polishing method of the ruthenium wafer includes a first polishing step of polishing the composition before use, a polishing step before the polishing using the polishing composition before use (second polishing step), and a finishing polishing process. A method of finishing a grinding step with a composition.

下面將具體說明矽晶圓之研磨方法及濁度之測定方法。 The method of polishing the ruthenium wafer and the method of measuring the turbidity will be specifically described below.

(1)首先相對於直徑300mm、傳導型P型、結晶方位<100>、無結晶缺陷之矽晶圓實施與標準試驗1之X1步驟相同之前處理。即，相對於矽晶圓，使用前處理用組成物進行研磨後，使用標準研磨用組成物進行研磨，其後進行SC-1洗淨及乾燥而實施前處理。 (1) First, the wafer was subjected to the same treatment as the X1 step of the standard test 1 with respect to the wafer having a diameter of 300 mm, a conductive type P, a crystal orientation of <100>, and no crystal defects. In other words, after polishing with a composition for pretreatment using a composition for pretreatment, the composition is polished using a standard polishing composition, and then SC-1 is washed and dried to carry out pretreatment.

(2)其次使用前處理用組成物再度研磨實施 (1)之步驟之前處理後的矽晶圓。研磨該矽晶圓時所使用之研磨裝置及研磨台與標準試驗2之Y2步驟相同。又，研磨該矽晶圓之研磨條件與標準試驗2之Y2步驟相同。 (2) The second use of the pre-treatment composition is re-ground (1) The processed germanium wafer before the step. The polishing apparatus and polishing table used in polishing the wafer were the same as the Y2 procedure of Standard Test 2. Further, the polishing conditions for polishing the tantalum wafer were the same as the Y2 procedure of Standard Test 2.

(3)其次使用研磨用組成物套組之前研磨用組成物，再一次研磨(2)之步驟中使用前處理用組成物再度研磨後之矽晶圓。研磨該矽晶圓時所使用之研磨裝置及研磨台與標準試驗2之Y3步驟相同。又，研磨該矽晶圓之研磨條件與標準試驗2之Y3步驟相同。 (3) Next, the polishing composition is used before the polishing composition is set, and the ruthenium wafer after the polishing is re-polished using the pre-treatment composition in the step of polishing (2). The polishing apparatus and polishing table used in polishing the wafer were the same as the Y3 procedure of Standard Test 2. Further, the polishing conditions for polishing the tantalum wafer were the same as the Y3 procedure of Standard Test 2.

(4)又，使用研磨用組成物套組之精加工研磨用組成物，又一次研磨(3)之步驟中使用前研磨用組成物研磨後之矽晶圓。研磨該矽晶圓時所使用之研磨裝置及研磨台與標準試驗2之Y3步驟相同。又，研磨該矽晶圓之研磨條件與標準試驗2之Y3步驟相同。 (4) Further, the finishing polishing composition is used in the polishing composition set, and the ruthenium wafer after the polishing composition is polished in the step (3). The polishing apparatus and polishing table used in polishing the wafer were the same as the Y3 procedure of Standard Test 2. Further, the polishing conditions for polishing the tantalum wafer were the same as the Y3 procedure of Standard Test 2.

(5)接著相對於(4)之步驟中使用精加工研磨用組成物研磨後之矽晶圓進行SC-1洗淨及乾燥，其後使用KLA公司製之表面異物檢查裝置SURFSCAN SP2以DWO方式測定矽晶圓表面之濁度。 (5) Next, SC-1 is washed and dried with respect to the tantalum wafer polished by the finishing polishing composition in the step (4), and then the surface foreign matter inspection device SURFSCAN SP2 manufactured by KLA Co., Ltd. is used in the DWO manner. The turbidity of the surface of the tantalum wafer was measured

濁度之測定結果如表2所示。使用實施例1~4之研磨用組成物套組研磨後之矽晶圓中，前研磨用組成物之親水性參數P1為未達100、前研磨用組成物之精加工精準度參數P2為1000以下，精加工研磨用組成物之研磨加工性參數F1為80以下，因此可降低精加工研磨後之矽晶圓表面之濁度，得高品質之被研磨面。 The measurement results of turbidity are shown in Table 2. In the tantalum wafer after polishing using the polishing composition set of Examples 1 to 4, the hydrophilicity parameter P1 of the pre-polishing composition was less than 100, and the finishing precision parameter P2 of the pre-polishing composition was 1000. In the following, since the polishing processability parameter F1 of the composition for finishing polishing is 80 or less, the turbidity of the surface of the wafer after finishing polishing can be reduced, and a high-quality surface to be polished can be obtained.

相對地使用比較例1~4之研磨用組成物套組研磨後之矽晶圓中，前研磨用組成物之親水性參數P1、前研磨用組成物之精加工精準度參數P2、及精加工研磨用組成物之研磨加工性參數F1中任一項均無法符合所必需之要件，因此精加工研磨後之矽晶圓表面之濁度較高。 The hydrophilicity parameter P1 of the pre-polishing composition, the finishing precision parameter P2 of the pre-polishing composition, and finishing were relatively used in the polishing wafer after the polishing composition set of Comparative Examples 1 to 4 were used. None of the polishing process parameters F1 of the polishing composition can meet the necessary requirements, so that the surface of the wafer after finishing polishing has a high turbidity.

Claims (8)

一種研磨用組成物套組，其為備有使用於使矽晶圓進行精加工研磨之精加工研磨步驟之精加工研磨用組成物，與使用於前述精加工研磨步驟之前一階段之研磨步驟的前研磨步驟之前研磨用組成物的研磨用組成物套組，標準試驗1所求取之前述前研磨用組成物之親水性參數P1為未達100，標準試驗2所求取之前述前研磨用組成物之精加工精準度參數P2為1000以下，標準試驗3所求取之前述精加工研磨用組成物之研磨加工性參數F1為80以下。 A polishing composition kit, which is a finishing polishing composition for use in a finishing polishing step for finishing polishing a silicon wafer, and a polishing step used in a stage before the finishing polishing step The polishing composition set of the polishing composition before the pre-grinding step, the hydrophilicity parameter P1 of the pre-polishing composition obtained in the standard test 1 is less than 100, and the pre-grinding for the standard test 2 The finishing precision parameter P2 of the composition is 1000 or less, and the grinding processability parameter F1 of the finishing polishing composition obtained in the standard test 3 is 80 or less. 如請求項1之研磨用組成物套組，其中前述精加工研磨用組成物及前述前研磨用組成物均為含有磨粒與鹼性化合物與水溶性高分子。 The polishing composition kit according to claim 1, wherein the finishing polishing composition and the pre-polishing composition both contain abrasive grains, a basic compound, and a water-soluble polymer. 一種前研磨用組成物，其為使用於使矽晶圓進行精加工研磨之精加工研磨步驟之前一階段之研磨步驟的前研磨步驟之前研磨用組成物，標準試驗1所求取之親水性參數P1為未達100，標準試驗2所求取之精加工精準度參數P2為1000以下。 A pre-polishing composition which is a composition for polishing before a pre-polishing step of a polishing step of a stage prior to a finishing polishing step of finishing a tantalum wafer, and a hydrophilic parameter obtained in Standard Test 1 P1 is less than 100, and the precision precision parameter P2 obtained by the standard test 2 is 1000 or less. 如請求項3之前研磨用組成物，其中含有磨粒與鹼性化合物與水溶性高分子。 A composition for polishing prior to claim 3, which comprises abrasive grains and a basic compound and a water-soluble polymer. 一種矽晶圓之研磨方法，其為備有使矽晶圓進行精加工研磨之精加工研磨步驟，與前述精加工研磨步驟之前一階段之研磨步驟的前研磨步驟之矽晶圓之研磨方法，使用如請求項1或2之研磨用組成物套組進行前述精加工 研磨步驟及前述前研磨步驟。 A method for polishing a tantalum wafer, which comprises a finishing polishing step for finishing polishing a tantalum wafer, and a polishing method for a wafer after a pre-grinding step of a grinding step before the finishing polishing step, Performing the aforementioned finishing using the polishing composition kit of claim 1 or 2 The grinding step and the aforementioned pre-grinding step. 一種矽晶圓之研磨方法，其為備有使矽晶圓進行精加工研磨之精加工研磨步驟，與前述精加工研磨步驟之前一階段之研磨步驟的前研磨步驟之矽晶圓之研磨方法，使用如請求項3或4之前研磨用組成物進行前述前研磨步驟。 A method for polishing a tantalum wafer, which comprises a finishing polishing step for finishing polishing a tantalum wafer, and a polishing method for a wafer after a pre-grinding step of a grinding step before the finishing polishing step, The foregoing pre-grinding step is carried out using the composition for grinding prior to claim 3 or 4. 一種精加工研磨用組成物，其為使用於備有使矽晶圓進行精加工研磨之精加工研磨步驟，與前述精加工研磨步驟之前一階段之研磨步驟的前研磨步驟之矽晶圓之研磨方法中前述精加工研磨步驟之精加工研磨用組成物，標準試驗3所求取之研磨加工性參數F1為80以下。 A finishing polishing composition for polishing a wafer prepared by a finishing polishing step for finishing polishing a silicon wafer, and a pre-polishing step of a polishing step before the finishing polishing step In the method, the finishing polishing composition for the finishing polishing step, the grinding processability parameter F1 obtained in the standard test 3 is 80 or less. 如請求項7之精加工研磨用組成物，其中含有磨粒與鹼性化合物與水溶性高分子。 The finishing polishing composition according to claim 7, which comprises abrasive grains and a basic compound and a water-soluble polymer.
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