JP2001308044A - Oxide cerium polishing agent and polishing method for substrate - Google Patents
Oxide cerium polishing agent and polishing method for substrateInfo
- Publication number
- JP2001308044A JP2001308044A JP2000131551A JP2000131551A JP2001308044A JP 2001308044 A JP2001308044 A JP 2001308044A JP 2000131551 A JP2000131551 A JP 2000131551A JP 2000131551 A JP2000131551 A JP 2000131551A JP 2001308044 A JP2001308044 A JP 2001308044A
- Authority
- JP
- Japan
- Prior art keywords
- cerium oxide
- polishing
- slurry
- substrate
- insulating film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
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- Grinding-Machine Dressing And Accessory Apparatuses (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
Description
【0001】[0001]
【発明の属する技術分野】本発明は、酸化セリウム研磨
剤及び基板の研磨方法を提供するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention provides a cerium oxide abrasive and a method for polishing a substrate.
【0002】[0002]
【従来の技術】従来、半導体装置の製造工程において、
プラズマ−CVD、低圧−CVD等の方法で形成される
酸化珪素2絶縁膜等無機絶縁膜層を平坦化するための化
学機械研磨剤として、ヒュームドシリカ系の研磨剤が一
般的に検討されている。ヒュームドシリカ系の研磨剤
は、シリカ粒子を四塩化珪酸の熱分解等の方法で粒成長
させ、アンモニア等のアルカリ金属を含まないアルカリ
溶液でpH調整を行って製造している。しかしながら、こ
の様な研磨剤は無機絶縁膜の研磨速度が充分な速度を持
たず、実用化には低研磨速度という技術課題がある。2. Description of the Related Art Conventionally, in the manufacturing process of a semiconductor device,
As a chemical mechanical polishing agent for flattening an inorganic insulating film layer such as a silicon oxide 2 insulating film formed by a method such as plasma-CVD or low pressure-CVD, a fumed silica-based polishing agent is generally studied. I have. Fumed silica-based abrasives are produced by growing silica particles by a method such as thermal decomposition of silicic acid tetrachloride and adjusting the pH with an alkaline solution containing no alkali metal such as ammonia. However, such a polishing agent does not have a sufficient polishing rate for the inorganic insulating film, and there is a technical problem of a low polishing rate for practical use.
【0003】一方、フォトマスク用ガラス表面研磨とし
て、酸化セリウム研磨剤が用いられている。酸化セリウ
ム粒子はシリカ粒子やアルミナ粒子に比べ硬度が低く、
したがって研磨表面に傷が入りにくいことから仕上げ鏡
面研磨に有用である。また、酸化セリウムは強い酸化剤
として知られるように、化学的活性な性質を有してい
る。この利点を活かし、絶縁膜用化学機械研磨剤への適
用が有用である。On the other hand, cerium oxide abrasives have been used for polishing the glass surface for photomasks. Cerium oxide particles have lower hardness than silica particles and alumina particles,
Therefore, it is useful for finish mirror polishing because the polishing surface is hardly damaged. Cerium oxide also has chemically active properties, as is known as a strong oxidizing agent. Taking advantage of this advantage, application to a chemical mechanical polishing agent for an insulating film is useful.
【0004】しかしながら、フォトマスク用ガラス表面
研磨用酸化セリウム研磨剤をそのまま無機絶縁膜研磨に
適用すると、1次粒子径が大きく、そのため絶縁膜表面
に目視で観察できる研磨傷が入ってしまう。また、酸化
セリウム粒子は理論比重が7.2と大きいことから沈降
しやすい。そのことから研磨時の研磨剤供給濃度むら、
供給管での詰まり等の問題が生じる。However, when a cerium oxide abrasive for polishing a glass surface for a photomask is used as it is for polishing an inorganic insulating film, the primary particle diameter is large, and polishing scratches that can be visually observed are formed on the surface of the insulating film. Further, the cerium oxide particles have a large theoretical specific gravity of 7.2, and thus easily settle. As a result, the abrasive supply concentration unevenness during polishing,
Problems such as clogging in the supply pipe occur.
【0005】[0005]
【発明が解決しようとする課題】請求項1〜5記載の発
明は分散性が良く、研磨傷の発生を抑制し、酸化珪素絶
縁膜等の被研磨面を平坦に研磨することが可能な酸化セ
リウム研磨剤を提供するものである。請求項6〜7記載
の発明は高品位で高信頼性の半導体用基板を容易に歩留
まりよく得ることの可能な基板の研磨方法を提供するも
のである。The invention according to claims 1 to 5 has good dispersibility, suppresses the occurrence of polishing scratches, and makes it possible to flatten a surface to be polished such as a silicon oxide insulating film. A cerium abrasive is provided. The invention according to claims 6 to 7 provides a substrate polishing method capable of easily obtaining a high-quality and high-reliability semiconductor substrate with good yield.
【0006】[0006]
【課題を解決するための手段】本発明は、酸化セリウム
と酸化セリウムに付着した分散剤の重量比が1対0.0
02から1対0.005の範囲であるスラリーからなる
酸化セリウム研磨剤に関する。また、本発明は、スラリ
ーが、酸化セリウムに付着していない分散剤を含む前記
の酸化セリウム研磨剤に関する。また、本発明は、スラ
リーが媒体として水を含む前記の酸化セリウム研磨剤に
関する。According to the present invention, a weight ratio of cerium oxide to a dispersant attached to cerium oxide is 1 to 0.0.
Cerium oxide abrasive comprising a slurry ranging from 02 to 1 to 0.005. The present invention also relates to the cerium oxide abrasive, wherein the slurry contains a dispersant that is not attached to cerium oxide. The present invention also relates to the cerium oxide abrasive, wherein the slurry contains water as a medium.
【0007】また、本発明は、分散剤が水溶性有機高分
子、水溶性陰イオン性界面活性剤、水溶性非イオン性界
面活性剤及び水溶性アミンから選ばれる少なくとも1種
の化合物である前記の酸化セリウム研磨剤に関する。ま
た、本発明は、pHが7〜10である前記の酸化セリウム
研磨剤に関する。Further, in the present invention, the dispersant is at least one compound selected from a water-soluble organic polymer, a water-soluble anionic surfactant, a water-soluble nonionic surfactant and a water-soluble amine. Cerium oxide abrasive. The present invention also relates to the cerium oxide abrasive having a pH of 7 to 10.
【0008】また、本発明は、前記の酸化セリウム研磨
剤で、所定の基板を研磨することを特徴とする基板の研
磨方法に関する。また、本発明は、所定の基板が酸化珪
素絶縁膜の形成された半導体素子である前記の基板の研
磨方法に関する。The present invention also relates to a method for polishing a substrate, comprising polishing a predetermined substrate with the cerium oxide abrasive. The present invention also relates to the above-mentioned substrate polishing method, wherein the predetermined substrate is a semiconductor element having a silicon oxide insulating film formed thereon.
【0009】[0009]
【発明の実施の形態】一般に酸化セリウムは、炭酸塩、
硫酸塩、蓚酸塩等のセリウム化合物を焼成することによ
って得られる。TEOS−CVD法等で形成される酸化
珪素絶縁膜は1次粒子径が大きく、かつ結晶歪が少ない
ほど、すなわち結晶性がよいほど高速研磨が可能である
が、研磨傷が入りやすい傾向がある。そこで、本発明で
用いる酸化セリウム粒子は、あまり結晶性を上げないで
作製される。また、半導体チップ研磨に使用することか
ら、アルカリ金属およびハロゲン類の含有率は1ppm以
下に抑えることが好ましい。DETAILED DESCRIPTION OF THE INVENTION Generally, cerium oxide is a carbonate,
It is obtained by calcining cerium compounds such as sulfates and oxalates. The silicon oxide insulating film formed by a TEOS-CVD method or the like has a large primary particle diameter and a small crystal distortion, that is, a high crystallinity, so that high-speed polishing can be performed, but polishing scratches tend to occur. . Therefore, the cerium oxide particles used in the present invention are produced without increasing crystallinity. Further, since it is used for polishing a semiconductor chip, the content of alkali metals and halogens is preferably suppressed to 1 ppm or less.
【0010】本発明の研磨剤は高純度のもので、Na、
K、Si、Mg、Ca、Zr、Ti、Ni、Cr、Fe
はそれぞれ1ppm以下、Alは10ppm以下である。The abrasive of the present invention is of high purity, and contains Na,
K, Si, Mg, Ca, Zr, Ti, Ni, Cr, Fe
Is 1 ppm or less, and Al is 10 ppm or less.
【0011】本発明において、酸化セリウム粒子を作製
する方法として焼成法が使用できる。ただし、研磨傷が
入らない粒子を作製するために、できるだけ結晶性を上
げない低温焼成が好ましい。セリウム化合物の酸化温度
が300℃であることから、焼成温度は600℃以上9
00℃以下が好ましい。炭酸セリウムを600℃以上9
00℃以下で60〜120分、空気中で焼成することが
好ましい。In the present invention, a firing method can be used as a method for producing cerium oxide particles. However, in order to produce particles that do not cause polishing scratches, low-temperature firing that does not increase the crystallinity as much as possible is preferable. Since the oxidation temperature of the cerium compound is 300 ° C., the firing temperature is 600 ° C. or more and 9 ° C.
00 ° C or lower is preferred. Cerium carbonate over 600 ℃ 9
It is preferable to bake in air at a temperature of 00 ° C. or lower for 60 to 120 minutes.
【0012】焼成された酸化セリウムは、ジェットミル
等の乾式粉砕、ビ−ズミル等の湿式粉砕で粉砕すること
ができる。ジェットミルは例えば化学工業論文集第6巻
第5号(1980)527〜532頁に説明されている。The calcined cerium oxide can be pulverized by dry pulverization such as a jet mill or wet pulverization such as a bead mill. The jet mill is described, for example, in Chemical Industry Transactions, Vol. 6, No. 5, (1980), pp. 527-532.
【0013】焼成酸化セリウムをジェットミル等の乾式
粉砕等で粉砕した酸化セリウム粒子には、一次粒子(結
晶子)サイズの小さい粒子と一次粒子(結晶子)サイズ
まで粉砕されていない多結晶体が含まれ、この多結晶体
は一次粒子(結晶子)が再凝集した凝集体とは異なって
おり、2つ以上の一次粒子(結晶子)から構成され結晶
粒界を有している。この結晶粒界を有す多結晶体を含む
研磨剤で研磨を行うと、研磨時の応力により破壊され活
性面を発生すると推定され、酸化珪素絶縁膜等の被研磨
面を傷なく高速に研磨することに寄与していると考えら
れる。The cerium oxide particles obtained by pulverizing the calcined cerium oxide by dry pulverization such as a jet mill or the like include particles having a small primary particle (crystallite) size and polycrystals not pulverized to the primary particle (crystallite) size. This polycrystal is different from an aggregate in which primary particles (crystallites) are re-agglomerated, and is composed of two or more primary particles (crystallites) and has a crystal grain boundary. When polishing is performed with an abrasive containing a polycrystal having a crystal grain boundary, it is presumed that the surface is destroyed due to stress during polishing and an active surface is generated, and the surface to be polished such as a silicon oxide insulating film is polished at high speed without damage. It is thought that it contributes to doing.
【0014】本発明における酸化セリウムスラリーは、
上記の方法により製造された酸化セリウム粒子を含有す
る水溶液又はこの水溶液から回収した酸化セリウム粒
子、水及び必要に応じて分散剤からなる組成物を分散さ
せることによって得られる。ここで、酸化セリウム粒子
の濃度に制限は無いが、懸濁液(研磨剤)の取り扱い易
さから0.5〜10重量%の範囲が好ましい。さらに、
保存安定性を得るためには1〜5重量%の範囲が好まし
い。[0014] The cerium oxide slurry in the present invention comprises:
It is obtained by dispersing an aqueous solution containing cerium oxide particles produced by the above method or a composition comprising cerium oxide particles recovered from this aqueous solution, water and, if necessary, a dispersant. Here, the concentration of the cerium oxide particles is not limited, but is preferably in the range of 0.5 to 10% by weight from the viewpoint of easy handling of the suspension (abrasive). further,
In order to obtain storage stability, a range of 1 to 5% by weight is preferable.
【0015】また分散剤としては、水溶性有機高分子、
水溶性陰イオン性界面活性剤、水溶性非イオン性界面活
性剤及び水溶性アミンがある。例えば、アクリル酸アン
モニウム塩とアクリル酸メチルの共重合体、特に重量平
均分子量1000〜20000のアクリル酸アンモニウ
ム塩とアクリル酸メチルの共重合体がある。なお、重量
平均分子量は、ゲルパーミエーションクロマトグラフィ
ーで測定し、標準ポリスチレン換算した値である。As the dispersant, a water-soluble organic polymer,
There are water-soluble anionic surfactants, water-soluble nonionic surfactants and water-soluble amines. For example, there is a copolymer of ammonium acrylate and methyl acrylate, particularly a copolymer of ammonium acrylate and methyl acrylate having a weight average molecular weight of 1,000 to 20,000. The weight average molecular weight is a value measured by gel permeation chromatography and converted to standard polystyrene.
【0016】これらの分散剤の添加量は、スラリー中の
粒子の分散性及び沈降防止性等から、酸化セリウム粒子
100重量部に対して0.01〜5重量部の範囲が好ま
しく、その分散効果を高めるためには、分散処理時に分
散機の中に粒子と同時に入れることが好ましい。The amount of the dispersant added is preferably in the range of 0.01 to 5 parts by weight based on 100 parts by weight of the cerium oxide particles in view of the dispersibility of the particles in the slurry and the anti-settling property. In order to increase the particle size, it is preferable to put the particles into a disperser at the same time as the particles are dispersed.
【0017】これらの酸化セリウム粒子を水中に分散さ
せる方法としては、通常の撹拌機による分散処理の他
に、超音波分散機、ホモジナイザー、ボールミル等を用
いることができる。サブミクロンオーダの酸化セリウム
粒子を分散させるためには、ボールミル、振動ボールミ
ル、遊星ボールミル、媒体撹拌式ミル等の湿式分散機を
用いることが好ましい。また、スラリーのアルカリ性を
高めたい場合には、分散処理時又は処理後に、アンモニ
ア水などの金属イオンを含まないアルカリ性物質を添加
することができる。As a method for dispersing these cerium oxide particles in water, an ultrasonic disperser, a homogenizer, a ball mill or the like can be used in addition to the usual dispersion treatment using a stirrer. In order to disperse cerium oxide particles on the order of submicron, it is preferable to use a wet disperser such as a ball mill, a vibrating ball mill, a planetary ball mill, and a medium stirring mill. When it is desired to increase the alkalinity of the slurry, an alkaline substance not containing metal ions such as aqueous ammonia can be added during or after the dispersion treatment.
【0018】本発明のスラリーに含まれる分散剤にアク
リル酸アンモニウム塩とアクリル酸メチルの共重合体を
用いる場合、分散剤を酸化セリウム粒子100重量部に
対して0.01〜5.00重量部添加することが好まし
く、その重量平均分子量は1000〜20000が好ま
しい。アクリル酸アンモニウム塩とアクリル酸メチルと
のモル比は0.1〜0.9が好ましい。アクリル酸アン
モニウム塩とアクリル酸メチルの共重合体が酸化セリウ
ム粒子100重量部に対して0.01重量部未満では沈
降し易く、5重量部より多いと再凝集による粒度分布の
経時変化が生じやすい。また、重量平均分子量が200
00を超えると再凝集による粒度分布の経時変化が生じ
やすい。When a copolymer of ammonium acrylate and methyl acrylate is used as the dispersant contained in the slurry of the present invention, the dispersant is used in an amount of 0.01 to 5.00 parts by weight based on 100 parts by weight of the cerium oxide particles. It is preferably added, and its weight average molecular weight is preferably from 1,000 to 20,000. The molar ratio of ammonium acrylate to methyl acrylate is preferably from 0.1 to 0.9. If the copolymer of ammonium acrylate and methyl acrylate is less than 0.01 part by weight with respect to 100 parts by weight of cerium oxide particles, sedimentation is easy, and if it is more than 5 parts by weight, the particle size distribution due to reagglomeration tends to change over time. . Further, the weight average molecular weight is 200
If it exceeds 00, the particle size distribution tends to change with time due to re-aggregation.
【0019】本発明のスラリーに分散される結晶粒界を
有する酸化セリウム粒子径の中央値は60〜1500nm
が好ましく、一次粒子(結晶子)径の中央値は30〜2
50nmが好ましい。The median diameter of the cerium oxide particles having crystal grain boundaries dispersed in the slurry of the present invention is 60 to 1500 nm.
Are preferable, and the median value of the primary particle (crystallite) diameter is 30 to 2
50 nm is preferred.
【0020】結晶粒界を有する酸化セリウム粒子径の中
央値が60nm未満、又は一次粒子(結晶子)径の中央値
が30nm未満であれば、酸化珪素絶縁膜等の被研磨面を
高速に研磨することができ難くなる傾向があり、結晶粒
界を有する酸化セリウム粒子径の中央値が1500nmを
越える、又は一次粒子(結晶子)の中央値が250nmを
越えると、酸化珪素絶縁膜等の被研磨面に傷が発生し易
くなる。結晶粒界を有する酸化セリウム粒子径の最大値
が3000nmを超えると、酸化珪素絶縁膜等の被研磨面
に傷が発生し易くなる。結晶粒界を有する酸化セリウム
粒子は、全酸化セリウム粒子の5〜100体積%である
ことが好ましく、5体積%未満の場合は酸化珪素絶縁膜
等の被研磨面に傷が発生し易くなる。If the median diameter of cerium oxide particles having crystal grain boundaries is less than 60 nm, or the median diameter of primary particles (crystallites) is less than 30 nm, a surface to be polished such as a silicon oxide insulating film is polished at high speed. When the median diameter of cerium oxide particles having crystal grain boundaries exceeds 1500 nm, or the median diameter of primary particles (crystallites) exceeds 250 nm, it is difficult to cover silicon oxide insulating films and the like. Scratches are likely to occur on the polished surface. If the maximum value of the diameter of the cerium oxide particles having a crystal grain boundary exceeds 3000 nm, a surface to be polished such as a silicon oxide insulating film is likely to be damaged. The content of the cerium oxide particles having a crystal grain boundary is preferably 5 to 100% by volume of the total cerium oxide particles, and when the content is less than 5% by volume, a surface to be polished such as a silicon oxide insulating film is easily damaged.
【0021】上記の酸化セリウム粒子では、一次粒子
(結晶子)の最大径は600nm以下が好ましく、一次粒
子(結晶子)径は10〜600nmであることが好まし
い。一次粒子(結晶子)が600nmを越えると傷が発生
し易く、10nm未満であると研磨速度が小さくなる傾向
にある。In the above cerium oxide particles, the maximum diameter of the primary particles (crystallites) is preferably 600 nm or less, and the diameter of the primary particles (crystallites) is preferably 10 to 600 nm. If the primary particles (crystallites) exceed 600 nm, scratches tend to occur, and if it is less than 10 nm, the polishing rate tends to decrease.
【0022】本発明のスラリ−のpHは、7以上10以下
が好ましく、8以上9以下がより好ましい。The pH of the slurry of the present invention is preferably from 7 to 10 and more preferably from 8 to 9.
【0023】本発明における分散剤の酸化セリウム付着
量は、たとえばスラリー中の分散剤量とスラリー中の酸
化セリウムに付着していない分散剤量の差で求められ
る。スラリー中の分散剤量はスラリー中の水分を加熱又
は真空乾燥などの方法で取り除いて得られた固形分量と
酸化セリウム重量の差により求められる。スラリー中の
酸化セリウムに付着していない分散剤量は、まずスラリ
ーを遠心分離などの方法で酸化セリウムと上澄みに分離
し、上澄みの水分を加熱又は真空乾燥などの方法で取り
除いて得られた固形分量である。The amount of cerium oxide attached to the dispersant in the present invention is determined, for example, by the difference between the amount of dispersant in the slurry and the amount of dispersant not attached to cerium oxide in the slurry. The amount of the dispersant in the slurry can be determined by the difference between the amount of solid content obtained by removing water in the slurry by heating or vacuum drying and the weight of cerium oxide. The amount of the dispersing agent not adhering to the cerium oxide in the slurry is obtained by first separating the slurry into cerium oxide and the supernatant by a method such as centrifugation, and removing the water in the supernatant by a method such as heating or vacuum drying. It is a quantity.
【0024】本発明のスラリーの酸化セリウムと酸化セ
リウムに付着した分散剤の重量比は、1対0.002か
ら1対0.005の範囲とされ、この範囲外では、分散
性、低傷性、平坦性、生産性、作業性等が劣る。この重
量比は、1対0.0023から1対0.049の範囲が
好ましい。The weight ratio of cerium oxide to the dispersant adhered to cerium oxide in the slurry of the present invention is in the range of 1: 0.002 to 1: 0.005. , Flatness, productivity, workability, etc. are inferior. This weight ratio is preferably in the range of 1: 0.0023 to 1: 0.049.
【0025】本発明の酸化セリウム研磨剤が使用される
無機絶縁膜の作製方法として、定圧CVD法、プラズマ
CVD法等が挙げられる。定圧CVD法による酸化珪素
絶縁膜形成は、Si源としてモノシラン:SiH4、酸
素源として酸素:O2を用いる。このSiH4−O2系酸
化反応を、400℃程度以下の低温で行わせることによ
り得られる。高温リフローによる表面平坦化を図るため
に、リン:Pをドープするときには、SiH4−O2−P
H3系反応ガスを用いることが好ましい。As a method for forming an inorganic insulating film using the cerium oxide abrasive of the present invention, there are a constant pressure CVD method, a plasma CVD method and the like. In forming a silicon oxide insulating film by a constant-pressure CVD method, monosilane: SiH 4 is used as a Si source, and oxygen: O 2 is used as an oxygen source. This SiH 4 —O 2 -based oxidation reaction is obtained by performing the reaction at a low temperature of about 400 ° C. or less. When doping phosphorus: P in order to planarize the surface by high-temperature reflow, SiH 4 —O 2 —P
It is preferable to use an H 3 -based reaction gas.
【0026】プラズマCD法は、通常の熱平衡下では高
温を必要とする化学反応が低温でできる利点を有する。
プラズマ発生法には、容量結合型と誘導結合型の2つが
挙げられる。反応ガスとしては、Si源としてSi
H4、酸素源としてN2Oを用いたSiH4−N2O系ガス
とテトラエトキシシラン(TEOS)を、Si源に用い
たTEOS−O2系ガス(TEOS−プラズマCVD
法)が挙げられる。基板温度は250℃〜400℃、反
応圧力は67〜400Paの範囲が好ましい。このよう
に、本発明の酸化珪素絶縁膜にはリン、ホウ素等の元素
がド−プされていてもよい。The plasma CD method has an advantage that a chemical reaction requiring a high temperature can be performed at a low temperature under normal thermal equilibrium.
The plasma generation method includes two types, a capacitive coupling type and an inductive coupling type. As a reaction gas, Si is used as a Si source.
H 4 , a SiH 4 —N 2 O-based gas using N 2 O as an oxygen source and tetraethoxysilane (TEOS) are used as a TEOS-O 2 -based gas (TEOS-plasma CVD) used as a Si source.
Method). The substrate temperature is preferably in the range of 250 ° C. to 400 ° C., and the reaction pressure is preferably in the range of 67 to 400 Pa. As described above, the silicon oxide insulating film of the present invention may be doped with elements such as phosphorus and boron.
【0027】所定の基板として、半導体基板すなわち回
路素子とアルミニウム配線が形成された段階の半導体基
板、回路素子が形成された段階の半導体基板等の半導体
基板上に酸化珪素絶縁膜層が形成された基板等が使用で
きる。このような半導体基板上に形成された酸化珪素絶
縁膜層を、上記酸化セリウム研磨剤で研磨することによ
って、酸化珪素絶縁膜層表面の凹凸を解消し、半導体基
板全面に渡って平滑な面とする。As a predetermined substrate, a silicon oxide insulating film layer is formed on a semiconductor substrate such as a semiconductor substrate in which circuit elements and aluminum wiring are formed, and a semiconductor substrate in which circuit elements are formed. A substrate or the like can be used. By polishing the silicon oxide insulating film layer formed on such a semiconductor substrate with the cerium oxide abrasive, unevenness on the surface of the silicon oxide insulating film layer is eliminated, and a smooth surface is formed over the entire semiconductor substrate. I do.
【0028】ここで、研磨する装置としては、半導体基
板を保持するホルダーと研磨布(パッド)を貼り付けた
(回転数が変更可能なモータ等を取り付けてある)定盤
を有する一般的な研磨装置が使用できる。研磨布として
は、一般的な不織布、発泡ポリウレタン、多孔質フッ素
樹脂などが使用でき、特に制限がない。また、研磨布に
はスラリーが溜まる様な溝加工を施すことが好ましい。Here, as an apparatus for polishing, a general polishing machine having a holder for holding a semiconductor substrate and a surface plate to which a polishing cloth (pad) is attached (a motor or the like whose rotation speed can be changed) is attached. The device can be used. As the polishing cloth, general nonwoven fabric, foamed polyurethane, porous fluororesin and the like can be used, and there is no particular limitation. Further, it is preferable that the polishing cloth is subjected to a groove processing for storing the slurry.
【0029】研磨条件には制限はないが、ホルダーと定
盤の回転速度は、半導体基板が飛び出さない様にそれぞ
れ100min-1以下の低回転が好ましく、半導体基板に
かける圧力は、研磨後に傷が発生しない様に100kPa
以下が好ましい。研磨している間、研磨布にはスラリー
をポンプ等で連続的に供給する。この供給量に制限はな
いが、研磨布の表面が常にスラリーで覆われていること
が好ましい。The polishing conditions are not limited, but the rotation speeds of the holder and the platen are preferably low rotations of 100 min -1 or less so that the semiconductor substrate does not pop out. 100kPa so that no
The following is preferred. During polishing, the slurry is continuously supplied to the polishing cloth by a pump or the like. Although the supply amount is not limited, it is preferable that the surface of the polishing pad is always covered with the slurry.
【0030】研磨終了後の半導体基板は、流水中で良く
洗浄後、スピンドライヤ等を用いて半導体基板上に付着
した水滴を払い落としてから乾燥させることが好まし
い。このようにして平坦化された酸化珪素絶縁膜層の上
に、第2層目のアルミニウム配線を形成し、その配線間
および配線上に再度上記方法により、酸化珪素絶縁膜を
形成後、上記酸化セリウム研磨剤を用いて研磨すること
によって、絶縁膜表面の凹凸を解消し、半導体基板全面
に渡って平滑な面とする。この工程を所定数繰り返すこ
とにより、所望の層数の半導体を製造する。It is preferable that the semiconductor substrate after polishing is thoroughly washed in running water, and then water drops adhering to the semiconductor substrate are wiped off using a spin drier or the like, and then dried. A second layer of aluminum wiring is formed on the silicon oxide insulating film layer thus planarized, and a silicon oxide insulating film is formed between the wirings and on the wiring again by the above-described method. By polishing using a cerium abrasive, unevenness on the surface of the insulating film is eliminated, and a smooth surface is formed over the entire surface of the semiconductor substrate. By repeating this process a predetermined number of times, a semiconductor having a desired number of layers is manufactured.
【0031】本発明の酸化セリウム研磨剤は、半導体基
板に形成された酸化珪素絶縁膜だけでなく、所定の配線
を有する配線板に形成された酸化珪素絶縁膜、ガラス、
窒化ケイ素等の無機絶縁膜、フォトマスク・レンズ・プ
リズム等の光学ガラス、ITO等の無機導電膜、ガラス
及び結晶質材料で構成される光集積回路・光スイッチン
グ素子・光導波路、光ファイバ−の端面、シンチレ−タ
等の光学用単結晶、固体レ−ザ単結晶、青色レ−ザ用L
EDサファイア基板、SiC、GaP、GaAS等の半
導体単結晶、磁気ディスク用ガラス基板、磁気ヘッド等
を研磨するために使用される。The cerium oxide abrasive of the present invention can be used not only for a silicon oxide insulating film formed on a semiconductor substrate but also for a silicon oxide insulating film formed on a wiring board having predetermined wiring, glass,
Inorganic insulating films such as silicon nitride, optical glasses such as photomasks, lenses, and prisms; inorganic conductive films such as ITO; optical integrated circuits, optical switching elements, optical waveguides, and optical fibers composed of glass and crystalline materials. End face, single crystal for optical such as scintillator, single crystal for solid laser, L for blue laser
It is used for polishing ED sapphire substrates, semiconductor single crystals such as SiC, GaP, and GaAs, glass substrates for magnetic disks, and magnetic heads.
【0032】このように本発明において所定の基板と
は、酸化珪素絶縁膜が形成された半導体基板、酸化珪素
絶縁膜が形成された配線板、ガラス、窒化ケイ素等の無
機絶縁膜、フォトマスク・レンズ・プリズム等の光学ガ
ラス、ITO等の無機導電膜、ガラス及び結晶質材料で
構成される光集積回路・光スイッチング素子・光導波
路、光ファイバ−の端面、シンチレ−タ等の光学用単結
晶、固体レ−ザ単結晶、青色レ−ザ用LEDサファイア
基板、SiC、GaP、GaAs等の半導体単結晶、磁
気ディスク用ガラス基板、磁気ヘッド等を含む。As described above, in the present invention, the predetermined substrate is a semiconductor substrate on which a silicon oxide insulating film is formed, a wiring board on which a silicon oxide insulating film is formed, glass, an inorganic insulating film such as silicon nitride, a photomask or the like. Optical glasses such as lenses and prisms, inorganic conductive films such as ITO, optical integrated circuits, optical switching elements, optical waveguides composed of glass and crystalline materials, optical fiber end faces, optical single crystals such as scintillators , A solid laser single crystal, a blue laser LED sapphire substrate, a semiconductor single crystal such as SiC, GaP, GaAs, a magnetic disk glass substrate, a magnetic head, and the like.
【0033】[0033]
【実施例】次に、実施例により本発明を説明する。Next, the present invention will be described by way of examples.
【0034】実施例1 (酸化セリウム粒子の作製)炭酸セリウム水和物2kgを
白金製容器に入れ、800℃で2時間空気中で焼成する
ことにより黄白色の粉末を約1kg得た。この粉末をX線
回折法で相同定を行ったところ酸化セリウムであること
を確認した。焼成粉末粒子径は30〜100μmであっ
た。焼成粉末粒子表面を走査型電子顕微鏡で観察したと
ころ、酸化セリウムの粒界が観察された。粒界に囲まれ
た酸化セリウム一次粒子(結晶子)径を測定したとこ
ろ、その分布の中央値が190nm、最大値が500nmで
あった。Example 1 (Preparation of Cerium Oxide Particles) 2 kg of cerium carbonate hydrate was placed in a platinum container and calcined at 800 ° C. for 2 hours in the air to obtain about 1 kg of yellowish white powder. When this powder was subjected to phase identification by an X-ray diffraction method, it was confirmed that the powder was cerium oxide. The particle diameter of the calcined powder was 30 to 100 μm. When the surface of the fired powder particles was observed with a scanning electron microscope, grain boundaries of cerium oxide were observed. When the diameter of primary particles (crystallite) of cerium oxide surrounded by the grain boundaries was measured, the median of the distribution was 190 nm and the maximum was 500 nm.
【0035】酸化セリウム粉末1kgをジェットミルを用
いて乾式粉砕を行った。この多結晶体は走査型電子顕微
鏡で観察したところ、一次粒子(結晶子)径と同等サイ
ズの小さな粒子の他に、1μmから3μmの大きな多結
晶体と0.5から1μmの多結晶体が混在していた。こ
れらの多結晶体は、一次粒子(結晶子)が再凝集した凝
集体とは異なっており、2つ以上の一次粒子(結晶子)
から構成され結晶粒界を有していることがわかった。さ
らに多結晶体の比表面積をBET法により測定した結
果、17m2/gであることがわかった。1 kg of cerium oxide powder was dry-pulverized using a jet mill. Observation of this polycrystal with a scanning electron microscope revealed that in addition to the small particles having the same size as the primary particles (crystallites), a large polycrystal of 1 μm to 3 μm and a polycrystal of 0.5 to 1 μm were obtained. It was mixed. These polycrystals are different from aggregates in which primary particles (crystallites) are re-agglomerated, and two or more primary particles (crystallites)
, And has a crystal grain boundary. Further, the specific surface area of the polycrystal was measured by the BET method and found to be 17 m 2 / g.
【0036】(酸化セリウムスラリーの作製)上記、酸
化セリウム粒子の作製で作製した酸化セリウム粒子10
00gとアクリル酸とアクリル酸メチルを3:1で共重
合した分子量10,000のポリアクリル酸アンモニウ
ム塩水溶液(40重量%)23gと脱イオン水8977
gを混合し、撹拌をしながら超音波分散を行った。超音
波周波数は40kHzで、分散時間10分で分散を行っ
た。得られたスラリーを30ミクロンフィルターでろ過
し、さらに脱イオン水を加えることにより5.0重量%
の酸化セリウムスラリー研磨剤を得た。酸化セリウムス
ラリーのpHは8.5であった。酸化セリウムスラリーの
粒度分布をレーザー回折式粒度分布計で調べたところ、
平均粒子径は1.29μmであった。(Preparation of Cerium Oxide Slurry) The cerium oxide particles 10 prepared in the above-described preparation of cerium oxide particles
23 g of an aqueous solution of polyacrylic acid ammonium salt (40% by weight) having a molecular weight of 10,000 obtained by copolymerizing 00 g with acrylic acid and methyl acrylate at a ratio of 3: 1 and deionized water 8977
g were mixed and ultrasonically dispersed while stirring. Dispersion was performed at an ultrasonic frequency of 40 kHz and a dispersion time of 10 minutes. The resulting slurry was filtered through a 30 micron filter, and 5.0 wt% was added by adding deionized water.
Of cerium oxide slurry was obtained. The pH of the cerium oxide slurry was 8.5. When the particle size distribution of the cerium oxide slurry was examined with a laser diffraction type particle size distribution meter,
The average particle size was 1.29 μm.
【0037】研磨剤を6ヶ月間5℃〜40℃で保管し
た。その後、攪拌により均一な濃度分布の酸化セリウム
スラリーに戻し、レーザー回折粒度分布測定を行ったと
ころ、作製直後と同一の粒度分布であることを確認でき
た。また研磨時に攪拌することにより、この酸化セリウ
ムスラリーには濃度むらが生じなかった。酸化セリウム
スラリーの濃度はスラリーの重量中、酸化セリウム粒子
の重量が占める割合から求めた。酸化セリウム粒子の重
量は、スラリーを150℃で加熱して水を蒸発させて残
った固形分重量とした。The abrasive was stored at 5 ° C. to 40 ° C. for 6 months. Thereafter, the slurry was returned to a cerium oxide slurry having a uniform concentration distribution by stirring, and a laser diffraction particle size distribution measurement was performed. As a result, it was confirmed that the particle size distribution was the same as that immediately after the preparation. Further, by stirring during the polishing, there was no concentration unevenness in the cerium oxide slurry. The concentration of the cerium oxide slurry was determined from the ratio of the weight of the cerium oxide particles to the weight of the slurry. The weight of the cerium oxide particles was determined as the weight of the solid content remaining after the slurry was heated at 150 ° C. to evaporate water.
【0038】(酸化セリウムと酸化セリウムに付着した
分散剤の重量比の測定)上記、酸化セリウムスラリーの
作製で作製した酸化セリウムスラリー10gを150℃
で1時間加熱して水分をすべて蒸発させた。固形分重量
は0.542gでスラリー中の分散剤量は0.042g
となった。また酸化セリウムスラリーの作製で作製した
酸化セリウムスラリー10gを別に取り、遠心分離機で
酸化セリウムと上澄みに分離し、上澄みを150℃で1
時間加熱して水分をすべて蒸発させた。固形分重量は
0.0305gであり、酸化セリウムスラリー10g中
の酸化セリウムに付着した分散剤量は0.042gと
0.0305gの差から0.0115gと求められた。
酸化セリウムスラリー10g中の酸化セリウム重量は
0.5gなので上記、酸化セリウムスラリーの作製で作
製した酸化セリウムスラリーの酸化セリウムと酸化セリ
ウムに付着した分散剤の重量比は1対0.0023と求
められた。(Measurement of Weight Ratio of Cerium Oxide and Dispersant Attached to Cerium Oxide) 10 g of the cerium oxide slurry prepared in the preparation of the cerium oxide slurry was heated at 150 ° C.
For 1 hour to evaporate all the water. The solid content is 0.542 g and the amount of dispersant in the slurry is 0.042 g.
It became. Separately, 10 g of the cerium oxide slurry prepared in the preparation of the cerium oxide slurry was separately separated into a cerium oxide and a supernatant by a centrifugal separator.
Heating was performed for a period of time to evaporate all water. The solid content weight was 0.0305 g, and the amount of the dispersant attached to cerium oxide in 10 g of the cerium oxide slurry was determined to be 0.0115 g from the difference between 0.042 g and 0.0305 g.
Since the weight of cerium oxide in 10 g of cerium oxide slurry is 0.5 g, the weight ratio of cerium oxide and the dispersant attached to cerium oxide in the cerium oxide slurry prepared in the preparation of cerium oxide slurry is determined to be 1: 0.0023. Was.
【0039】(絶縁膜層の研磨)TEOS−プラズマC
VD法で作製した酸化珪素絶縁膜を形成させたSiウエ
ハをセットし、多孔質ウレタン樹脂製の研磨パッドを貼
り付けた定盤上に、絶縁膜面を下にしてホルダーを載
せ、さらに加工荷重が30kPaになるように重しを載せ
た。上記の酸化セリウムスラリーを脱イオン水で5倍に
希釈したスラリー(固形分:1重量%)を容器に入れ、
攪拌しながらポンプで配管を通じて定盤上に供給できる
ようにした。このとき、容器、配管内ともに沈降は見ら
れなかった。(Polishing of Insulating Film Layer) TEOS-Plasma C
The Si wafer on which the silicon oxide insulating film formed by the VD method was formed was set, and the holder was placed with the insulating film face down on a surface plate on which a polishing pad made of a porous urethane resin was attached. Was set to 30 kPa. A slurry (solid content: 1% by weight) obtained by diluting the above cerium oxide slurry by 5 times with deionized water is put in a container,
It was possible to supply the solution onto the surface plate through a pipe with a pump while stirring. At this time, no sedimentation was observed in both the container and the piping.
【0040】定盤上にスラリーを50cc/minの速度で滴
下しながら、定盤を30min-1で2分間回転させ、絶縁
膜を研磨した。研磨後ウエハをホルダーから取り外し
て、流水で良く洗浄後、超音波洗浄機によりさらに20
分間洗浄した。洗浄後、ウエハをスピンドライヤーで水
滴を除去し、120℃の乾燥機で10分間乾燥させた。
光干渉式膜厚測定装置を用いて、研磨前後の膜厚変化を
測定した結果、この研磨によりそれぞれ400nm(研磨
速度:400nm/min)の絶縁膜が削られ、ウエハ全面に
渡って均一の厚みになっていることがわかった。また、
光学顕微鏡を用いて絶縁膜表面を観察したところ、明確
な傷は見られなかった。While the slurry was dropped on the platen at a rate of 50 cc / min, the platen was rotated at 30 min -1 for 2 minutes to polish the insulating film. After polishing, the wafer is removed from the holder, washed well with running water, and then further cleaned with an ultrasonic cleaner.
Washed for minutes. After the cleaning, water droplets were removed from the wafer with a spin dryer, and the wafer was dried with a dryer at 120 ° C. for 10 minutes.
As a result of measuring the change in film thickness before and after polishing using an optical interference type film thickness measuring device, the insulating film of each 400 nm (polishing rate: 400 nm / min) was removed by this polishing, and the uniform thickness was obtained over the entire surface of the wafer. It turned out to be. Also,
When the surface of the insulating film was observed using an optical microscope, no clear scratch was found.
【0041】実施例2 (酸化セリウム粒子の作製)炭酸セリウム水和物2kgを
白金製容器に入れ、800℃で2時間空気中で焼成する
ことにより黄白色の粉末を約1kg得た。この粉末をX線
回折法で相同定を行ったところ酸化セリウムであること
を確認した。焼成粉末粒子径は30〜100μmであっ
た。焼成粉末粒子表面を走査型電子顕微鏡で観察したと
ころ、酸化セリウムの粒界が観察された。粒界に囲まれ
た酸化セリウム一次粒子(結晶子)径を測定したとこ
ろ、その分布の中央値が190nm、最大値が500nmで
あった。Example 2 (Preparation of Cerium Oxide Particles) 2 kg of cerium carbonate hydrate was put in a platinum container and calcined at 800 ° C. for 2 hours in the air to obtain about 1 kg of yellowish white powder. When this powder was subjected to phase identification by an X-ray diffraction method, it was confirmed that the powder was cerium oxide. The particle diameter of the calcined powder was 30 to 100 μm. When the surface of the fired powder particles was observed with a scanning electron microscope, grain boundaries of cerium oxide were observed. When the diameter of primary particles (crystallite) of cerium oxide surrounded by the grain boundaries was measured, the median of the distribution was 190 nm and the maximum was 500 nm.
【0042】酸化セリウム粉末1kgをジェットミルを用
いて乾式粉砕を行った。この多結晶体は走査型電子顕微
鏡で観察したところ、一次粒子(結晶子)径と同等サイ
ズの小さな粒子の他に、1μmから3μmの大きな多結
晶体と0.5から1μmの多結晶体が混在していた。こ
れらの多結晶体は、一次粒子(結晶子)が再凝集した凝
集体とは異なっており、2つ以上の一次粒子(結晶子)
から構成され結晶粒界を有していることがわかった。さ
らに多結晶体の比表面積をBET法により測定した結
果、17m2/gであることがわかった。1 kg of cerium oxide powder was dry-pulverized using a jet mill. Observation of this polycrystal with a scanning electron microscope revealed that in addition to the small particles having the same size as the primary particles (crystallites), a large polycrystal of 1 μm to 3 μm and a polycrystal of 0.5 to 1 μm were obtained. It was mixed. These polycrystals are different from aggregates in which primary particles (crystallites) are re-agglomerated, and two or more primary particles (crystallites)
, And has a crystal grain boundary. Further, the specific surface area of the polycrystal was measured by the BET method and found to be 17 m 2 / g.
【0043】(酸化セリウムスラリーの作製)上記、酸
化セリウム粒子の作製で作製した酸化セリウム粒子10
00gとアクリル酸とアクリル酸メチルを3:1で共重
合した分子量10,000のポリアクリル酸アンモニウ
ム塩水溶液(40重量%)23gと脱イオン水8977
gを混合し、撹拌をしながら超音波分散を行った。超音
波周波数は40kHzで、分散時間10分で分散を行っ
た。得られたスラリーを0.3ミクロンフィルターでろ
過し、さらに脱イオン水を加えることにより5.0重量
%の酸化セリウムスラリー研磨剤を得た。酸化セリウム
スラリーのpHは8.5であった。酸化セリウムスラリー
の粒度分布をレーザー回折式粒度分布計で調べたとこ
ろ、平均粒子径は0.16μmであった。(Preparation of Cerium Oxide Slurry) The cerium oxide particles 10 prepared in the above-described preparation of cerium oxide particles
23 g of an aqueous solution of polyacrylic acid ammonium salt (40% by weight) having a molecular weight of 10,000 obtained by copolymerizing 00 g with acrylic acid and methyl acrylate at a ratio of 3: 1 and deionized water 8977
g were mixed and ultrasonically dispersed while stirring. Dispersion was performed at an ultrasonic frequency of 40 kHz and a dispersion time of 10 minutes. The resulting slurry was filtered through a 0.3 micron filter, and further deionized water was added to obtain a 5.0% by weight cerium oxide slurry abrasive. The pH of the cerium oxide slurry was 8.5. When the particle size distribution of the cerium oxide slurry was examined with a laser diffraction type particle size distribution analyzer, the average particle size was 0.16 μm.
【0044】研磨剤を6ヶ月間5℃〜40℃で保管し
た。その後、攪拌により均一な濃度分布の酸化セリウム
スラリーに戻し、レーザー回折粒度分布測定を行ったと
ころ、作製直後と同一の粒度分布であることを確認でき
た。また研磨時に攪拌することにより、この酸化セリウ
ムスラリーには濃度むらが生じなかった。酸化セリウム
スラリーの濃度はスラリーの重量中、酸化セリウム粒子
の重量が占める割合から求めた。酸化セリウム粒子の重
量は、スラリーを150℃で加熱して水を蒸発させて残
った固形分重量とした。The abrasive was stored at 5 ° C. to 40 ° C. for 6 months. Thereafter, the slurry was returned to a cerium oxide slurry having a uniform concentration distribution by stirring, and a laser diffraction particle size distribution measurement was performed. As a result, it was confirmed that the particle size distribution was the same as that immediately after the preparation. Further, by stirring during the polishing, there was no concentration unevenness in the cerium oxide slurry. The concentration of the cerium oxide slurry was determined from the ratio of the weight of the cerium oxide particles to the weight of the slurry. The weight of the cerium oxide particles was determined as the weight of the solid content remaining after the slurry was heated at 150 ° C. to evaporate water.
【0045】(酸化セリウムと酸化セリウムに付着した
分散剤の重量比の測定)上記、酸化セリウムスラリーの
作製で作製した酸化セリウムスラリー10gを150℃
で1時間加熱して水分をすべて蒸発させた。固形分重量
は0.616gでスラリー中の分散剤量は0.116g
となった。また酸化セリウムスラリーの作製で作製した
酸化セリウムスラリー10gを別に取り、遠心分離機で
酸化セリウムと上澄みに分離し、上澄みを150℃で1
時間加熱して水分をすべて蒸発させた。固形分重量は
0.0915gであり、酸化セリウムスラリー10g中
の酸化セリウムに付着した分散剤量は0.116gと
0.0915gの差から0.0245gと求められた。
酸化セリウムスラリー10g中の酸化セリウム重量は
0.5gなので上記、酸化セリウムスラリーの作製で作
製した酸化セリウムスラリーの酸化セリウムと酸化セリ
ウムに付着した分散剤の重量比は1対0.0049と求
められた。(Measurement of Weight Ratio of Cerium Oxide and Dispersant Attached to Cerium Oxide) 10 g of the cerium oxide slurry prepared in the preparation of the cerium oxide slurry was heated at 150 ° C.
For 1 hour to evaporate all the water. The solid weight is 0.616 g and the amount of dispersant in the slurry is 0.116 g.
It became. Separately, 10 g of the cerium oxide slurry prepared in the preparation of the cerium oxide slurry was separately separated into a cerium oxide and a supernatant by a centrifugal separator.
Heating was performed for a period of time to evaporate all water. The solid content weight was 0.0915 g, and the amount of the dispersant attached to cerium oxide in 10 g of the cerium oxide slurry was determined to be 0.0245 g from the difference between 0.116 g and 0.0915 g.
Since the weight of cerium oxide in 10 g of cerium oxide slurry is 0.5 g, the weight ratio of cerium oxide to the dispersant attached to cerium oxide in the cerium oxide slurry prepared in the preparation of the cerium oxide slurry is determined to be 1: 0.0049. Was.
【0046】(絶縁膜層の研磨)TEOS−プラズマC
VD法で作製した酸化珪素絶縁膜を形成させたSiウエ
ハをセットし、多孔質ウレタン樹脂製の研磨パッドを貼
り付けた定盤上に、絶縁膜面を下にしてホルダーを載
せ、さらに加工荷重が30kPaになるように重しを載せ
た。上記の酸化セリウムスラリーを脱イオン水で5倍に
希釈したスラリー(固形分:1重量%)を容器に入れ、
攪拌しながらポンプで配管を通じて定盤上に供給できる
ようにした。このとき、容器、配管内ともに沈降は見ら
れなかった。(Polishing of Insulating Film Layer) TEOS-Plasma C
The Si wafer on which the silicon oxide insulating film formed by the VD method was formed was set, and the holder was placed with the insulating film face down on a surface plate on which a polishing pad made of a porous urethane resin was attached. Was set to 30 kPa. A slurry (solid content: 1% by weight) obtained by diluting the above cerium oxide slurry by 5 times with deionized water is put in a container,
It was possible to supply the solution onto the surface plate through a pipe with a pump while stirring. At this time, no sedimentation was observed in both the container and the piping.
【0047】定盤上にスラリーを50cc/minの速度で滴
下しながら、定盤を30min-1で2分間回転させ、絶縁
膜を研磨した。研磨後ウエハをホルダーから取り外し
て、流水で良く洗浄後、超音波洗浄機によりさらに20
分間洗浄した。洗浄後、ウエハをスピンドライヤーで水
滴を除去し、120℃の乾燥機で10分間乾燥させた。
光干渉式膜厚測定装置を用いて、研磨前後の膜厚変化を
測定した結果、この研磨によりそれぞれ160nm(研磨
速度:80nm/min)の絶縁膜が削られ、ウエハ全面に渡
って均一の厚みになっていることがわかった。また、光
学顕微鏡を用いて絶縁膜表面を観察したところ、明確な
傷は見られなかった。While the slurry was dropped on the platen at a rate of 50 cc / min, the platen was rotated at 30 min -1 for 2 minutes to polish the insulating film. After polishing, the wafer is removed from the holder, washed well with running water, and then further cleaned with an ultrasonic cleaner.
Washed for minutes. After the cleaning, water droplets were removed from the wafer with a spin dryer, and the wafer was dried with a dryer at 120 ° C. for 10 minutes.
As a result of measuring the change in film thickness before and after polishing using an optical interference type film thickness measuring device, the insulating film of 160 nm (polishing rate: 80 nm / min) was respectively removed by this polishing, and the uniform thickness was obtained over the entire surface of the wafer. It turned out to be. When the surface of the insulating film was observed using an optical microscope, no clear damage was found.
【0048】[0048]
【発明の効果】請求項1〜5記載の酸化セリウム研磨剤
は分散性が良く、研磨傷の発生を抑制し、酸化珪素絶縁
膜等の被研磨面を平坦に研磨することが可能なものであ
る。請求項6〜7記載の基板の研磨方法は高品位で高信
頼性の半導体用基板を容易に歩留まりよく得ることの可
能なものである。The cerium oxide abrasive according to any one of claims 1 to 5 has a good dispersibility, can suppress the occurrence of polishing scratches, and can polish a surface to be polished such as a silicon oxide insulating film flat. is there. The method for polishing a substrate according to the sixth and seventh aspects is capable of easily obtaining a high-quality, high-reliability semiconductor substrate with good yield.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 FI テーマコート゛(参考) C09K 3/14 550 C09K 3/14 550Z ──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat ゛ (Reference) C09K 3/14 550 C09K 3/14 550Z
Claims (7)
分散剤の重量比が1対0.002から1対0.005の
範囲であるスラリーからなる酸化セリウム研磨剤。1. A cerium oxide abrasive comprising a slurry having a weight ratio of cerium oxide to a dispersant attached to cerium oxide in the range of 1: 0.002 to 1: 0.005.
ない分散剤を含む請求項1記載の酸化セリウム研磨剤。2. The cerium oxide abrasive according to claim 1, wherein the slurry contains a dispersant that is not attached to cerium oxide.
又は2記載の酸化セリウム研磨剤。3. The slurry according to claim 1, wherein the slurry contains water as a medium.
Or the cerium oxide abrasive according to 2.
オン性界面活性剤、水溶性非イオン性界面活性剤及び水
溶性アミンから選ばれる少なくとも1種の化合物である
請求項1、2又は3記載の酸化セリウム研磨剤。4. The dispersant is at least one compound selected from the group consisting of a water-soluble organic polymer, a water-soluble anionic surfactant, a water-soluble nonionic surfactant and a water-soluble amine. Or the cerium oxide abrasive according to 3.
は4記載の酸化セリウム研磨剤。5. The cerium oxide abrasive according to claim 1, wherein the pH is 7 to 10.
セリウム研磨剤で、所定の基板を研磨することを特徴と
する基板の研磨方法。6. A method for polishing a substrate, comprising polishing a predetermined substrate with the cerium oxide abrasive according to claim 1.
た半導体素子である請求項6記載の基板の研磨方法。7. The method according to claim 6, wherein the predetermined substrate is a semiconductor device having a silicon oxide insulating film formed thereon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000131551A JP2001308044A (en) | 2000-04-26 | 2000-04-26 | Oxide cerium polishing agent and polishing method for substrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000131551A JP2001308044A (en) | 2000-04-26 | 2000-04-26 | Oxide cerium polishing agent and polishing method for substrate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2001308044A true JP2001308044A (en) | 2001-11-02 |
Family
ID=18640428
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2000131551A Pending JP2001308044A (en) | 2000-04-26 | 2000-04-26 | Oxide cerium polishing agent and polishing method for substrate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2001308044A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005268799A (en) * | 2004-03-16 | 2005-09-29 | Samsung Corning Co Ltd | Cerium oxide slurry for semiconductor thin film polishing |
-
2000
- 2000-04-26 JP JP2000131551A patent/JP2001308044A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005268799A (en) * | 2004-03-16 | 2005-09-29 | Samsung Corning Co Ltd | Cerium oxide slurry for semiconductor thin film polishing |
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