JP2003315316A - Method for measuring hydrogen peroxide concentration in circulating slurry - Google Patents

Method for measuring hydrogen peroxide concentration in circulating slurry

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Publication number
JP2003315316A
JP2003315316A JP2002122123A JP2002122123A JP2003315316A JP 2003315316 A JP2003315316 A JP 2003315316A JP 2002122123 A JP2002122123 A JP 2002122123A JP 2002122123 A JP2002122123 A JP 2002122123A JP 2003315316 A JP2003315316 A JP 2003315316A
Authority
JP
Japan
Prior art keywords
concentration
slurry
hydrogen peroxide
measurement
measuring
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.)
Granted
Application number
JP2002122123A
Other languages
Japanese (ja)
Other versions
JP3617977B2 (en
Inventor
Kazuhiro Hirai
和弘 平井
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
MFSI Ltd
Original Assignee
MFSI Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by MFSI Ltd filed Critical MFSI Ltd
Priority to JP2002122123A priority Critical patent/JP3617977B2/en
Publication of JP2003315316A publication Critical patent/JP2003315316A/en
Application granted granted Critical
Publication of JP3617977B2 publication Critical patent/JP3617977B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00Indexing codes associated with group G01N29/00
    • G01N2291/02Indexing codes associated with the analysed material
    • G01N2291/028Material parameters
    • G01N2291/02809Concentration of a compound, e.g. measured by a surface mass change
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00Indexing codes associated with group G01N29/00
    • G01N2291/02Indexing codes associated with the analysed material
    • G01N2291/028Material parameters
    • G01N2291/02872Pressure

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for measuring hydrogen peroxide concentration in a circulating slurry for accurately and economically measuring hydrogen peroxide concentration in a circulating slurry used for polishing to smoothen, for example, a metallic thin film formed on a semiconductor substrate, thereby keeping constant the hydrogen peroxide concentration in the circulating slurry and efficiently and stably providing a high quality semiconductor. <P>SOLUTION: The method for measuring hydrogen peroxide concentration in a circulating slurry includes steps of sealing a part of the circulating slurry so as to provide a measurement system independent from a circulating slurry system, and after allowing a slurry sealed in the measuring system to stand, measuring hydrogen peroxide concentration in the slurry using an ultrasonic concentration meter. <P>COPYRIGHT: (C)2004,JPO

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【発明の属する技術分野】本発明は、循環しているスラ
リー中の過酸化水素水濃度の測定方法に関する。
TECHNICAL FIELD The present invention relates to a method for measuring the concentration of hydrogen peroxide in a circulating slurry.

【0002】[0002]

【従来の技術】従来より、過酸化水素水が含有されたス
ラリーは、例えば、半導体の製造の際には、シリコンウ
ェーハ等の半導体基板上に形成された金属薄膜の研磨に
使用されている。該金属薄膜は、所望の回路を形成する
ために、素子や抵抗等を接続して配線するためのもので
ある。これらの金属薄膜の形成は、一般的には、タング
ステンや銅等の原料物質を真空容器内で加熱・蒸発させ
て半導体基板上に薄膜を形成する真空蒸着法(CVD
法)や、アルゴンイオン等を用いて金属物質をスパッタ
し、それを半導体基板上に堆積させるスパッタ法といっ
た物理気相堆積法(PVD法)が用いられている。
2. Description of the Related Art Conventionally, a slurry containing a hydrogen peroxide solution has been used for polishing a metal thin film formed on a semiconductor substrate such as a silicon wafer when manufacturing a semiconductor. The metal thin film is for connecting and wiring elements, resistors and the like to form a desired circuit. These metal thin films are generally formed by a vacuum evaporation method (CVD) in which a raw material such as tungsten or copper is heated and evaporated in a vacuum container to form a thin film on a semiconductor substrate.
Method) or a physical vapor deposition method (PVD method) such as a sputtering method in which a metal substance is sputtered using argon ions or the like and deposited on a semiconductor substrate.

【0003】上記の方法によって形成された金属薄膜の
表面は平坦ではないため、通常、半導体基板上に金属薄
膜を形成後、シリカ粉末等を研磨剤として用いたスラリ
ーで金属薄膜の表面を研磨することが行なわれている。
更に、この金属薄膜表面の平坦化処理に際しては、研磨
剤による物理的な研磨を行なうと同時に、スラリー中に
過酸化水素水を混入させることで、過酸化水素水で金属
を酸化・溶解させながら、効率的な処理が行なわれてい
る。
Since the surface of the metal thin film formed by the above method is not flat, the metal thin film is usually formed on a semiconductor substrate and then the surface of the metal thin film is polished with a slurry using silica powder or the like as an abrasive. Is being done.
Further, during the flattening treatment of the surface of the metal thin film, physical polishing with an abrasive is performed, and at the same time, the hydrogen peroxide solution is mixed into the slurry to oxidize and dissolve the metal with the hydrogen peroxide solution. , Efficient processing is being performed.

【0004】近年、半導体製品における小型化及び高性
能化は目覚ましいものがあり、一方、半導体製品は非常
に精緻な構造を有するため、上記したような研磨方法で
平坦化される金属薄膜表面の均一性を確保し、及び、大
量生産された各製品間における金属薄膜表面の均一性を
確保することは、半導体製品の高性能維持のための重要
な要素である。このため、金属薄膜を平坦化する際に使
用されるスラリー中における研磨剤の均一性を図ること
は勿論のこと、スラリー中における過酸化水素水の濃度
を一定に保持することが望まれる。
In recent years, miniaturization and high performance of semiconductor products have been remarkable, while semiconductor products have a very fine structure, so that the surface of a metal thin film to be flattened by the above polishing method is uniform. It is an important factor for maintaining the high performance of semiconductor products to secure the uniformity and the uniformity of the surface of the metal thin film among the mass-produced products. For this reason, it is desirable to maintain the concentration of the hydrogen peroxide solution in the slurry to be constant, as well as to make the polishing agent uniform in the slurry used for planarizing the metal thin film.

【0005】これに対し、半導体基板上に形成された金
属薄膜を平坦化するための研磨処理に使用されている従
来のスラリーでは、研磨処理の系内を循環しているスラ
リー(以下、循環スラリーと呼ぶ)へ過酸化水素水を、
下記のような方法によって随時添加することが行なわれ
ている。先ず、循環スラリー中の過酸化水素水濃度を測
定し、次に、該測定値を用いて所望の過酸化水素水濃度
に対して不足している過酸化水素水量を算出し、この算
出量に応じた過酸化水素水をスラリー中に添加すること
で過酸化水素水の不足分を補い、これによって使用して
いる循環スラリー中の過酸化水素水濃度を一定に保持す
ることが行なわれている。
On the other hand, in the conventional slurry used in the polishing process for flattening the metal thin film formed on the semiconductor substrate, the slurry circulating in the polishing process system (hereinafter, circulating slurry). Hydrogen peroxide solution,
Addition is performed at any time by the following method. First, the concentration of hydrogen peroxide solution in the circulating slurry is measured, and then the amount of hydrogen peroxide solution lacking with respect to the desired concentration of hydrogen peroxide solution is calculated using the measured value. By adding appropriate hydrogen peroxide solution to the slurry, the shortage of hydrogen peroxide solution is compensated, and thereby the concentration of hydrogen peroxide solution in the circulating slurry used is kept constant. .

【0006】[0006]

【発明が解決しようとする課題】しかしながら、本発明
者らの検討によれば、上記した従来の方法では下記に挙
げるような課題があり、循環スラリー中の過酸化水素水
濃度を変動させないで一定の状態に保つことは難しく、
半導体基板上に形成した金属薄膜の平坦化処理をより均
一に、再現性よく行なって品質に優れた半導体製品を得
るためには、更なる改良が必要であることがわかった。
即ち、従来の方法では、循環スラリー中の過酸化水素水
濃度の測定において、その正確さと精度が充分であると
は言えず、測定精度に劣るため、必要とする過酸化水素
水の添加量を正確に求めることができず、過酸化水素水
の添加が正確に行なわれない場合があった。更に、従来
の過酸化水素水の濃度の測定方法には、メンテナンスや
ランニングコストの点でも課題があり、経済性の観点か
らも改良すべき点があった。
However, according to the studies by the present inventors, the above-mentioned conventional methods have the following problems, and the hydrogen peroxide concentration in the circulating slurry is kept constant without changing. Is difficult to maintain
It has been found that further improvement is required in order to obtain a semiconductor product having excellent quality by performing the flattening treatment of the metal thin film formed on the semiconductor substrate more uniformly and with good reproducibility.
That is, in the conventional method, in the measurement of the concentration of hydrogen peroxide solution in the circulating slurry, the accuracy and precision cannot be said to be sufficient, and the measurement accuracy is inferior. There was a case where the hydrogen peroxide solution could not be added accurately because it could not be determined accurately. Further, the conventional method for measuring the concentration of hydrogen peroxide solution has problems in terms of maintenance and running costs, and there is a point to be improved from the economical point of view.

【0007】従って、本発明の目的は、上記した従来技
術の課題を解決し、例えば、半導体基板上に形成された
金属薄膜を平坦化するための研磨処理等に使用される循
環スラリー中の過酸化水素水濃度を、優れた精度で経済
的に測定できる循環スラリー中の過酸化水素水濃度の測
定方法を提供することにある。更に、本発明の目的は、
上記のような優れた過酸化水素水濃度の測定方法を用い
ることで、循環スラリー中の過酸化水素水濃度を常に一
定に保つことを可能とし、これによって高い品質の半導
体製品を効率よく安定して提供することにある。
Therefore, an object of the present invention is to solve the above-mentioned problems of the prior art, for example, to remove excess particles in a circulating slurry used for polishing treatment for flattening a metal thin film formed on a semiconductor substrate. It is an object of the present invention to provide a method for measuring the concentration of hydrogen peroxide water in a circulating slurry, which is capable of economically measuring the concentration of hydrogen oxide water with excellent accuracy. Further, the object of the present invention is to
By using the excellent method of measuring hydrogen peroxide concentration as described above, it is possible to keep the concentration of hydrogen peroxide in the circulating slurry always constant, which enables efficient and stable high quality semiconductor products. To provide.

【0008】[0008]

【課題を解決するための手段】上記の目的は下記の本発
明によって達成される。即ち、本発明は、循環している
スラリー中の過酸化水素水の濃度を測定する循環スラリ
ー中の過酸化水素水濃度の測定方法であって、循環して
いるスラリーの一部を封入することで、循環しているス
ラリーの系から切り離して独立した状態にした測定系を
設け、該測定系内に封入されたスラリーを静置した後、
該スラリー中の過酸化水素水濃度の測定を超音波濃度計
によって行なうことを特徴とする循環スラリー中の過酸
化水素水濃度の測定方法である。本発明の好ましい形態
は、上記において、更に、前記測定系に圧力計が設けら
れ、該圧力計によって過酸化水素水濃度の測定と併行し
て封入されたスラリーの圧力を測定し、得られた圧力測
定値によって超音波濃度計で測定した過酸化水素水濃度
の測定値を補正演算する補正演算機構を有する循環スラ
リー中の過酸化水素水濃度の測定方法である。又、本発
明の好ましい形態は、上記したスラリーが、ウェーハ基
板上に形成された金属膜表面の研磨を行なう際に使用さ
れるスラリーである循環スラリー中の過酸化水素水濃度
の測定方法である。
The above object can be achieved by the present invention described below. That is, the present invention is a method for measuring the concentration of hydrogen peroxide in a circulating slurry for measuring the concentration of hydrogen peroxide in the circulating slurry, wherein a part of the circulating slurry is enclosed. Then, the measurement system which is separated from the system of the circulating slurry and is in an independent state is provided, and after the slurry enclosed in the measurement system is allowed to stand,
The method for measuring the concentration of hydrogen peroxide water in a circulating slurry is characterized in that the concentration of hydrogen peroxide water in the slurry is measured by an ultrasonic densitometer. A preferred embodiment of the present invention is obtained in the above by further providing a pressure gauge in the measurement system, and measuring the pressure of the enclosed slurry in parallel with the measurement of the hydrogen peroxide concentration by the pressure gauge. It is a method for measuring the concentration of hydrogen peroxide solution in a circulating slurry, which has a correction calculation mechanism for correcting and calculating the measurement value of the hydrogen peroxide solution concentration measured by an ultrasonic densitometer based on the pressure measurement value. Further, a preferred embodiment of the present invention is a method for measuring the concentration of hydrogen peroxide solution in a circulating slurry, wherein the above-mentioned slurry is a slurry used when polishing the surface of a metal film formed on a wafer substrate. .

【0009】[0009]

【発明の実施の形態】以下、好ましい実施の形態を挙げ
て本発明を更に詳細に説明する。本発明者らは、上記し
た従来技術の課題を解決すべく鋭意検討の結果、例え
ば、半導体基板上の金属薄膜表面を平坦化するための研
磨処理等に使用される循環スラリー中の過酸化水素水の
量を測定し、かかる測定値に応じて過酸化水素水の不足
量を検出し、該検出値に基づいて循環スラリー中に過酸
化水素水を添加して不足分を補ってスラリー中の過酸化
水素水の量を一定に保つようにした従来の構成において
は、特に、循環スラリー中の過酸化水素水の量を測定の
際に、下記に挙げるような問題があることがわかった。
即ち、従来の、スラリー中の過酸化水素水の濃度を測定
し、該測定値に応じて過酸化水素水の不足量を検出する
過酸化水素水濃度(以下、過水濃度と呼ぶ)の管理機構
においては、下記に挙げる課題があることがわかった。
BEST MODE FOR CARRYING OUT THE INVENTION The present invention will be described in more detail below with reference to preferred embodiments. As a result of intensive studies to solve the above-mentioned problems of the prior art, the present inventors have found that, for example, hydrogen peroxide in a circulating slurry used for polishing treatment for flattening the surface of a metal thin film on a semiconductor substrate. The amount of water is measured, and the shortage amount of hydrogen peroxide water is detected according to the measured value, and hydrogen peroxide water is added to the circulating slurry based on the detected value to compensate for the shortage and It has been found that the conventional configuration in which the amount of hydrogen peroxide solution is kept constant has the following problems, particularly when measuring the amount of hydrogen peroxide solution in the circulating slurry.
That is, the conventional management of hydrogen peroxide concentration (hereinafter referred to as perhydrogen concentration) by measuring the concentration of hydrogen peroxide in the slurry and detecting the insufficient amount of hydrogen peroxide according to the measured value. It was found that the mechanism has the following problems.

【0010】(a)従来より、使用されている過酸化水
素水の濃度の測定方法としては、特開2000−117
635公報に記載されているような、過マンガン酸カリ
ウムや硫酸等の試薬を使用する酸化還元滴定法を用いた
自動滴定装置が主流である。しかし、かかる方法の場合
には、試薬消費によるランニングコストの増加と、試薬
定期交換による運用工数の増加という問題、又、測定用
サンプルを採取する際に使用されるシリンジやシリンジ
シール部は、測定対象がスラリーであるために消耗が激
しく、短期間での交換が余儀なくされるといった問題が
あり、経済的な課題があった。
(A) Conventionally, as a method for measuring the concentration of hydrogen peroxide solution that has been used, there is JP-A 2000-117.
An automatic titrator using a redox titration method using a reagent such as potassium permanganate or sulfuric acid as described in Japanese Patent No. 635 is mainly used. However, in the case of such a method, there is a problem that the running cost increases due to the consumption of the reagent and the operation man-hour increases due to the regular replacement of the reagent, and the syringe and the syringe seal part used when collecting the measurement sample are Since the target is slurry, there is a problem that it is consumed so much that it must be replaced in a short period of time, which is an economic problem.

【0011】(b)これに対し、上記した酸化還元滴定
法による自動滴定装置の代替として、ほぼメンテナンス
フリーで、スラリー中の過酸化水素水の濃度が測定でき
る超音波濃度計が使用されるようになってきているが、
この場合に、通常使用されているインライン(スラリー
の循環系に測定装置を配置して、循環させながら測定を
行なうこと)での使用においては、測定試料である循環
スラリーの流量、圧力、温度等の影響を受け易く、測定
値にバラツキを生じ、測定精度に欠けるという問題があ
る。
(B) On the other hand, an ultrasonic densitometer that can measure the concentration of hydrogen peroxide solution in the slurry almost without maintenance is used as an alternative to the above automatic titration apparatus by the redox titration method. Is becoming
In this case, when using in-line (where a measuring device is placed in the circulation system of the slurry to perform measurement while circulating), the flow rate, pressure, temperature, etc. of the circulating slurry that is the measurement sample are used. Are susceptible to the influence of, the measurement value varies, and the measurement accuracy is lacking.

【0012】上記した問題に対して、本発明では、研磨
工程で使用している循環スラリー中の過水濃度を、スラ
リーの循環系から切り離して独立した系とし、且つ、そ
の測定に超音波濃度計を用いることで、正確な精度のよ
い測定を可能とし、得られた過水濃度測定値を用いるこ
とで、不足している過酸化水素水の濃度を正確に精度よ
く検出し、これにより、循環スラリー中に所望する量の
過酸化水素水を正確に添加することを可能とする。以下
に、本発明の循環スラリー中の過水濃度の測定方法を用
いた場合に得られる種々の効果について述べる。
In order to solve the above-mentioned problems, the present invention separates the perhydrogen concentration in the circulation slurry used in the polishing step from the circulation system of the slurry into an independent system, and measures the ultrasonic concentration in the system. By using a meter, it is possible to perform accurate and accurate measurement, and by using the obtained measured value of the concentration of hydrogen peroxide, it is possible to accurately and accurately detect the concentration of hydrogen peroxide solution that is lacking. It makes it possible to accurately add the desired amount of hydrogen peroxide solution into the circulating slurry. The various effects obtained when the method for measuring the concentration of superfluous water in the circulating slurry of the present invention is used will be described below.

【0013】(i)本発明では、過水濃度を、酸化還元
滴定法等を用いた自動滴定装置を使用するのではなく、
超音波濃度計を使用して測定するため、従来の測定方法
置に比べて、ランニングコストの低減、及びメンテナン
ス工数の低減の達成が可能となる。
(I) In the present invention, instead of using an automatic titrator which uses a redox titration method or the like, the perhydrogen concentration is not used.
Since the measurement is performed using the ultrasonic densitometer, it is possible to reduce the running cost and the maintenance man-hour as compared with the conventional measuring method.

【0014】(ii)本発明では、超音波濃度計による過
水濃度の測定を、循環スラリーの一部を封入すること
で、スラリーの循環系から独立した系で行なうため、従
来、インラインで超音波濃度計を使用して測定した場合
において生じていた、測定誤差の原因となる流量や圧力
の変動といった要素を排除でき、この結果、過酸化水素
水の濃度測定の精度を向上させることができる。
(Ii) In the present invention, the measurement of the superfluous water concentration by an ultrasonic densitometer is performed by enclosing a part of the circulating slurry in a system independent of the circulation system of the slurry. It is possible to eliminate the factors such as fluctuations in flow rate and pressure that cause measurement errors, which occurred when measuring using a sonic densitometer, and as a result, it is possible to improve the accuracy of concentration measurement of hydrogen peroxide solution. .

【0015】(iii)更に、本発明の好ましい形態で
は、上記測定系に、循環スラリーの圧力を測定するため
の圧力計を設け、且つ該圧力計を使用して、過水濃度の
測定と併行して封入されたスラリーの圧力を測定するよ
うに構成することで、特に影響が大きい圧力変動による
過水濃度の測定値のバラツキの発生を有効に抑制し、こ
れにより過水濃度の測定精度をより向上させることを可
能とする。
(Iii) Furthermore, in a preferred embodiment of the present invention, the above-mentioned measuring system is provided with a pressure gauge for measuring the pressure of the circulating slurry, and the pressure gauge is used in parallel with the measurement of the concentration of superfluous water. By configuring to measure the pressure of the enclosed slurry, it is possible to effectively suppress the occurrence of variations in the measured value of the superfluid concentration due to pressure fluctuations that have a particularly large effect, and thereby to improve the measurement accuracy of the superfluid concentration. It is possible to further improve.

【0016】以下、上記したような優れた効果が得られ
る本発明の循環スラリー中の過水濃度の測定方法につい
て、更に詳細に説明する。図1は、本発明の過水濃度の
測定方法で使用する測定系の一例を説明するための模式
図である。図中の1はスラリー供給ラインであり、2〜
4はバルブであり、5は圧力計、6は超音波濃度計であ
る。図1に示した例では、測定系に、超音波濃度計6と
共に圧力計5が配置されており、過酸化水素水の濃度の
測定と併行して圧力の測定が行なわれるように構成され
ている。
Hereinafter, the method for measuring the concentration of superfluous water in the circulating slurry of the present invention which achieves the above-mentioned excellent effects will be described in more detail. FIG. 1 is a schematic diagram for explaining an example of a measurement system used in the method for measuring the concentration of superfluous water of the present invention. 1 in the figure is a slurry supply line,
Reference numeral 4 is a valve, 5 is a pressure gauge, and 6 is an ultrasonic densitometer. In the example shown in FIG. 1, the pressure gauge 5 is arranged in the measurement system together with the ultrasonic densitometer 6, and the pressure measurement is performed concurrently with the measurement of the concentration of the hydrogen peroxide solution. There is.

【0017】本発明では、従来のように、過水濃度の測
定を、スラリーが循環している系内で行なわずに、循環
スラリーから一部のスラリーを封入して、これを測定用
試料とすることで、スラリーの循環系から切り離した独
立した系で過水濃度の測定を行なう。上記のように構成
するため、本発明においては、図1に示したように、ス
ラリー供給ライン1の一部にバルブ2〜4を配置する。
そして、過水濃度の測定を行わない時は、これらのバル
ブを使用して、バルブ2及び3を開、バルブ4を閉にし
た状態とし、これによりスラリーを圧力計5を経由して
超音波濃度計6内に導入し、常時循環させる。次に、過
水濃度の測定を行う時は、コントローラー22によっ
て、自動的にバルブ2及びバルブ3を閉の状態にするこ
とで、測定系である圧力計5及び超音波濃度計6に、循
環スラリーの一部を封入する。尚、上記バルブ2及びバ
ルブ3を閉の状態にする動きに連動させてバルブ4を開
にすることで、スラリー供給ライン1におけるスラリー
の循環は、過水濃度等の測定系とは無関係に継続するよ
うに構成されている。従って、研磨処理は、通常通り、
継続して行なわれる。
In the present invention, unlike the prior art, the measurement of the perhydrogen concentration is not carried out in the system in which the slurry is circulated, but a part of the slurry is enclosed from the circulated slurry and this is used as a measurement sample. By doing so, the concentration of superfluous water is measured by an independent system separated from the slurry circulation system. Because of the above-described configuration, in the present invention, as shown in FIG. 1, valves 2 to 4 are arranged in a part of the slurry supply line 1.
Then, when the measurement of the perhydrogen concentration is not performed, the valves 2 and 3 are opened and the valve 4 is closed by using these valves, whereby the slurry is ultrasonically passed through the pressure gauge 5. It is introduced into the densitometer 6 and constantly circulated. Next, when the concentration of superfluous water is measured, the controller 22 automatically closes the valves 2 and 3 to circulate the pressure gauge 5 and the ultrasonic densitometer 6 which are measurement systems. Enclose part of the slurry. By opening the valve 4 in conjunction with the movement of closing the valves 2 and 3, the circulation of the slurry in the slurry supply line 1 is continued regardless of the measurement system such as the concentration of superfluid water. Is configured to. Therefore, the polishing process, as usual,
It will be continued.

【0018】本発明では、上記のようにして圧力計5及
び超音波濃度計6に封入したスラリーについて、圧力及
び過水濃度の測定を静置した後に行なう。具体的には、
コントローラー22によって、予め設定してある測定待
機時間が経過し、測定系が安定した後に行なわれるよう
に制御すればよい。図1に示した例では、上記測定系で
得られた圧力測定値と過水濃度測定値は、コントローラ
ー22に入力され、これらの測定値を用いてコントロー
ラー22で演算が行なわれて、圧力補正がされた過水濃
度の測定値が、コントローラー22に記録されるように
構成されている。本発明では、以上のようにして、測定
系を静置させてから過水濃度を測定するので、超音波濃
度計によって過酸化水素水の濃度を測定した場合に測定
誤差の原因となる、流量と圧力の影響を排除することが
できる。この結果、過酸化水素水の濃度測定を、正確に
且つバラツキのない状態で精度よく行なうことが可能と
なる。
In the present invention, the pressure and the concentration of the perhydrogen of the slurry enclosed in the pressure gauge 5 and the ultrasonic densitometer 6 as described above are measured after standing. In particular,
The controller 22 may be controlled to perform the measurement after the preset measurement standby time has elapsed and the measurement system is stabilized. In the example shown in FIG. 1, the pressure measurement value and the superficial water concentration measurement value obtained by the above measurement system are input to the controller 22, and the controller 22 uses these measurement values to perform an operation to correct the pressure. The measured measured value of the superfluous water concentration is recorded in the controller 22. In the present invention, as described above, the measurement system is allowed to stand and then the concentration of superhydrogen is measured, which causes a measurement error when the concentration of hydrogen peroxide solution is measured by an ultrasonic densitometer. And the effect of pressure can be eliminated. As a result, it becomes possible to measure the concentration of the hydrogen peroxide solution accurately and accurately in the state where there is no variation.

【0019】更に、過水濃度測定値の信頼性をより向上
させるためには、下記のように構成することが好まし
い。先ず、上記のようにして測定した過水濃度測定値が
コントローラー22に記録された後、再び、バルブ2及
び3を開き、且つバルブ4を閉にすることで、測定系内
にスラリーを循環させる。そして、再び、前述したスラ
リーの封入、各測定、圧力測定値及び過水濃度測定値の
コントローラー22への入力、コントローラー22での
演算後、圧力補正した過水濃度測定値をコントローラー
22へ記録する。そして、この一連の濃度測定動作を数
回繰り返し、数個の濃度記録値が、予め設定しておいた
許容誤差範囲内に入ったときに、これらの数個の濃度記
録値の平均をとり、かかる値を、ある過水濃度測定時間
における濃度測定結果とすることが好ましい。
Further, in order to further improve the reliability of the measured value of the concentration of superfluous water, the following constitution is preferable. First, after the measured value of the superfluous concentration measured as described above is recorded in the controller 22, the valves 2 and 3 are opened again and the valve 4 is closed to circulate the slurry in the measurement system. . Then, again, after the above-mentioned encapsulation of the slurry, each measurement, the input of the measured pressure value and the measured value of the superfluous water concentration to the controller 22 and the calculation by the controller 22, the pressure-corrected measured perhydrogenated water concentration value is recorded in the controller 22. . Then, this series of density measurement operation is repeated several times, and when several density recorded values fall within the preset allowable error range, the average of these several density recorded values is taken, It is preferable to use such a value as the concentration measurement result at a certain perhydrogen concentration measurement time.

【0020】図2に、上記した本発明の循環スラリー中
の過水濃度の測定方法を、ウェーハ基板上に形成された
金属膜表面の研磨を行なう際のスラリー供給システムに
適用した場合の概略構成図を示した。研磨装置26で安
定したウェーハの研磨を行うためには、循環しているス
ラリー中の過水濃度を一定にする必要があるが、上記し
た本発明の過水濃度の測定方法を適用すれば達成するこ
とが可能となる。図2に基づいて説明すると、研磨装置
26へ供給するためのスラリーは、過酸化水素水の添加
機構29(以下、過水添加機構と呼ぶ)によって所定の
過水濃度に調整されてスラリータンク31に貯蔵された
後、スラリータンク31からスラリー供給装置27を経
て、スラリー供給ライン1によって常時循環され、使用
される。スラリー中の過水濃度は、下記に述べるように
して一定に保たれる。図中の28は、先に説明した、本
発明の過水濃度の測定方法を適用した測定系を示してい
る。
FIG. 2 is a schematic configuration of the above-described method for measuring the concentration of superfluous water in a circulating slurry of the present invention applied to a slurry supply system for polishing a surface of a metal film formed on a wafer substrate. The figure is shown. In order to perform stable wafer polishing with the polishing apparatus 26, it is necessary to make the superfluid concentration in the circulating slurry constant, but this is achieved by applying the above-described method for measuring the superfluous concentration of the present invention. It becomes possible to do. To describe with reference to FIG. 2, the slurry to be supplied to the polishing apparatus 26 is adjusted to have a predetermined perhydrogen concentration by a hydrogen peroxide water addition mechanism 29 (hereinafter, referred to as a perhydrogen addition mechanism), and a slurry tank 31. After being stored in, the slurry tank 31 is constantly circulated by the slurry supply line 1 via the slurry supply device 27 and used. The perhydrogen concentration in the slurry is kept constant as described below. Reference numeral 28 in the figure indicates a measurement system to which the above-described method for measuring the perhydrogen concentration of the present invention is applied.

【0021】以下に、図2において、本発明の過水濃度
の測定方法を適用した測定系28と、過水添加機構29
とによって、循環スラリー中の過水濃度を一定にする方
法について説明する。所望する所定の過水濃度の調整
は、下記の一連の操作によってなされる。先ず、コント
ローラー22によって予め設定されている、ある過水濃
度測定時間がきたとき、測定系28によってスラリー中
の過水濃度が測定され、過水濃度の測定結果がコントロ
ーラー22に記録される。この測定系28の濃度測定結
果が、所望の濃度以下の場合には、スラリー中の過水濃
度を所望の濃度にするために、過水添加機構29によっ
て、スラリータンク31中へ不足している過酸化水素水
の添加が行われる。
Hereinafter, referring to FIG. 2, a measuring system 28 to which the method for measuring the concentration of superfluid water of the present invention is applied, and a superfluid water adding mechanism 29.
A method of keeping the perhydrogen concentration in the circulating slurry constant will be described with reference to. The desired predetermined superfluid concentration is adjusted by the following series of operations. First, when a certain amount of superfluous water concentration measurement time preset by the controller 22 arrives, the measurement system 28 measures the superfluous water concentration in the slurry, and the measurement result of the superfluous water concentration is recorded in the controller 22. When the concentration measurement result of the measurement system 28 is equal to or lower than the desired concentration, the excess amount of the excess water in the slurry tank 31 is insufficient in the slurry tank 31 in order to adjust the concentration of the excess water in the slurry to the desired concentration. Hydrogen peroxide solution is added.

【0022】過酸化水素水の添加は、バルブによって、
スラリータンク31中へ直接添加してもよいが、下記の
方式で行なうことがより好ましい。即ち、過酸化水素水
の貯蔵タンクを設け、かかるタンクに対して一定圧力で
の加圧を行なって過酸化水素水の供給を行ない、該供給
流量を流量計によって定量し、これを積算することで過
酸化水素水の添加量を定量しながら添加を行なう方式と
すれば、過酸化水素水の添加を良好に行なうことができ
る。特に、羽根車式流量計を用い、更に、過酸化水素水
の供給経路に、過水添加機構29とスラリータンク31
との設置距離に応じて添加流量を変更でき、添加流量を
一定に維持できる流量制御オリフィスを設け、羽根車式
流量計からのパルスを瞬時に積算することで過酸化水素
水の総添加量の定量を行ないながら過酸化水素水の供給
を行なう方式を用いれば、安価に、しかも、微小流量の
過酸化水素水の添加を、より良好な状態で行なうことが
できる。
The hydrogen peroxide solution is added by a valve.
Although it may be added directly to the slurry tank 31, it is more preferable to add it in the following manner. That is, a storage tank for hydrogen peroxide water is provided, the hydrogen peroxide solution is supplied by pressurizing the tank with a constant pressure, the supply flow rate is quantified by a flow meter, and this is integrated. If the method of adding the hydrogen peroxide solution while quantifying the added amount is used, the hydrogen peroxide solution can be added well. In particular, an impeller type flow meter is used, and further, a hydrogen peroxide water supply path is provided with a superhydrogen addition mechanism 29 and a slurry tank 31.
The addition flow rate can be changed according to the installation distance with the flow rate control orifice that can maintain the addition flow rate constant, and the pulse from the impeller flow meter can be integrated instantaneously to determine the total addition amount of hydrogen peroxide water. By using the method of supplying the hydrogen peroxide solution while performing the quantitative determination, it is possible to inexpensively add the hydrogen peroxide solution at a minute flow rate in a better condition.

【0023】一連の過水濃度測定と過酸化水素水の添加
後、予め設定した待機時間を経て、再度、測定系28に
よる前述の過水濃度の測定動作を行い、上記したような
過水添加機構29による添加によって、循環スラリー中
の過水濃度が所望の濃度に到達したか否かを確認する。
所望の濃度に到達していれば、次回の過水濃度測定時間
までは過水添加機構29はアイドリングとなるが、所望
の濃度に到達していない場合には、再び添加動作が行わ
れる。この後も所望の濃度に達したことが確認されるま
で、濃度測定動作と添加動作が繰り返され、この結果、
循環しているスラリー中の過酸化水素水の濃度が一定に
保たれる。
After a series of measurement of the concentration of superfluid water and addition of hydrogen peroxide water, the above-mentioned operation of measuring the superfluid concentration by the measurement system 28 is performed again after a preset waiting time, and the addition of the superfluid water as described above. It is confirmed whether or not the perhydrogen concentration in the circulating slurry has reached the desired concentration by the addition by the mechanism 29.
If the desired concentration has been reached, the per-water addition mechanism 29 will be idle until the next over-hydrogen concentration measurement time, but if the desired concentration has not been reached, the addition operation is performed again. After that, the concentration measurement operation and the addition operation are repeated until it is confirmed that the desired concentration is reached.
The concentration of hydrogen peroxide solution in the circulating slurry is kept constant.

【0024】[0024]

【実施例】次に、好ましい実施例を挙げて、本発明を更
に詳細に説明する。 (1)過水濃度の測定における圧力の影響 図1に示す模式図において、バルブ2からバルブ3の測
定系の配管中に、1、2、3wt%の、濃度が既知であ
る3種類の過酸化水素水を含有したスラリーを用い、こ
れらを表1に示した各圧力で封入し、その状態で、超音
波濃度計6にてスラリー中の過酸化水素水の濃度の測定
を行い、その際に得られる測定値に及ぼす圧力変動の影
響を調べた。表1に、得られた結果を示した。表1中
に、酸化還元滴定法によって測定したスラリー中の過酸
化水素水濃度を記載した。
The present invention will be described in more detail with reference to the preferred examples. (1) Effect of pressure on the measurement of the concentration of superfluid In the schematic diagram shown in FIG. 1, three types of known concentrations of 1, 2, and 3 wt% are contained in the piping of the measurement system from valve 2 to valve 3. Using a slurry containing hydrogen oxide water, these were sealed at each pressure shown in Table 1, and in that state, the concentration of hydrogen peroxide water in the slurry was measured by an ultrasonic densitometer 6, and at that time, The effect of pressure fluctuations on the measured values obtained in the above was investigated. Table 1 shows the obtained results. In Table 1, the hydrogen peroxide concentration in the slurry measured by the redox titration method is described.

【0025】 [0025]

【0026】表1に示したように、この結果から、超音
波濃度計6によって得られる過水濃度の測定結果は、圧
力に比例して高い値となる傾向があることが確認でき
た。そこで、上記表1の結果を用いて、圧力変動によっ
て生じる過水濃度の測定値のバラツキの補正について検
討した。この結果、比例定数を−0.0006と定め、
下記式によって、圧力変動によって生じる過水濃度の測
定値のバラツキを補正すれば、超音波濃度計による精度
の高い測定が可能となることがわかった。式中のTは、
過水濃度の測定を行なった各スラリーが封入されていた
圧力である。
As shown in Table 1, from this result, it was confirmed that the measurement result of the superfluid concentration obtained by the ultrasonic densitometer 6 tends to be a high value in proportion to the pressure. Therefore, using the results of Table 1 above, the correction of the variation in the measured value of the superfluid concentration caused by the pressure fluctuation was examined. As a result, the proportional constant is set to -0.0006,
It has been found that by correcting the variation in the measured value of the concentration of superfluous water caused by the pressure fluctuation by the following formula, it is possible to perform highly accurate measurement with the ultrasonic densitometer. T in the formula is
It is the pressure at which each slurry for which the concentration of hydrogen peroxide was measured was enclosed.

【0027】 [0027]

【0028】上記の式を用いて各圧力Tにおける圧力補
正を施した場合と、施さなかった場合の比較を行い、超
音波濃度計による過水濃度の実測値に対して、圧力補正
を施した場合の効果を確認した。図3〜5は、その結果
を示すグラフである。この結果、濃度が既知である過酸
化水素水を含んだスラリーについて、圧力補正を施さず
に過酸化水素水の濃度を測定した場合は、圧力の上昇に
比例して真値からの誤差が大きくなることが確認でき
た。これに対して、上記した圧力変動に対する補正をす
ることによって、真値からの誤差の少ない状態で、過酸
化水素水の濃度を測定することが可能となることがわか
った。従って、過酸化水素水の濃度の測定と同時にスラ
リーの圧力を測定し、上記した測定値の補正を行なえ
ば、圧力変動による影響を受けることなく、スラリー中
の過酸化水素水の濃度を超音波濃度計により測定した場
合に、精度のよい正確な測定結果を得ることができる。
Using the above equation, a comparison was made between the case where pressure correction was performed at each pressure T and the case where no pressure correction was performed, and the pressure correction was applied to the actual measured value of the perhydrogen concentration measured by the ultrasonic densitometer. The effect of the case was confirmed. 3 to 5 are graphs showing the results. As a result, when the concentration of hydrogen peroxide solution was measured without pressure correction for a slurry containing hydrogen peroxide solution of known concentration, there was a large error from the true value in proportion to the increase in pressure. I was able to confirm. On the other hand, it has been found that by correcting the pressure fluctuations described above, it is possible to measure the concentration of the hydrogen peroxide solution with a small error from the true value. Therefore, if the pressure of the slurry is measured simultaneously with the measurement of the concentration of the hydrogen peroxide solution and the above-mentioned measurement value is corrected, the concentration of the hydrogen peroxide solution in the slurry can be ultrasonically measured without being affected by the pressure fluctuation. When measured by a densitometer, accurate and accurate measurement results can be obtained.

【0029】(2)過水濃度添加機構について 図2に模式的に示した回路を組み、コントローラー22
によって任意の過酸化水素水の吐出量を指定し、原液過
水の貯蔵タンクから、該タンクに接続されている窒素ラ
インを用いて原液過水を加圧排出し、メスシリンダーに
て実際に排出された量を測定した。この際、加圧用窒素
の圧力を一定にした場合と、変動させた場合について試
験し、指定した吐出量に対し、それぞれの場合の原液過
水の排出量がどのようになるか比較実験を行った。表2
及び図6に、その結果を示した。
(2) The controller 22 is constructed by assembling the circuit schematically shown in FIG.
Specify the discharge amount of hydrogen peroxide water by the, and pressurize the stock solution overpressure from the storage tank of the stock solution overpressure using the nitrogen line connected to the tank, and actually discharge it with the graduated cylinder. The measured amount was measured. At this time, the pressure of the pressurizing nitrogen was made constant and varied, and a comparative experiment was conducted to determine the discharge amount of the undiluted solution per flow for the specified discharge amount. It was Table 2
The results are shown in FIG.

【0030】 [0030]

【0031】表2に示したように、貯蔵タンクから窒素
ラインを用いて過水を加圧排出する際の加圧用窒素の圧
力が一定の場合に比べて、該圧力が変動した場合には、
明らかに、指定した吐出量に対して排出量が少なく、誤
差が大きくなることが確認できた。逆に言えば、貯蔵タ
ンクを使用すれば吐出圧力を一定にすることが可能であ
り、更に、このようにすれば、スラリーへの過酸化水素
水の添加にあたって、所望する量を、正確に精度よく添
加できることが確認された。
As shown in Table 2, in the case where the pressure of nitrogen for pressurization at the time of discharging the pressurized hydrogen from the storage tank using a nitrogen line is constant, when the pressure fluctuates,
Obviously, it was confirmed that the discharge amount was smaller than the specified discharge amount and the error was large. Conversely, if a storage tank is used, it is possible to make the discharge pressure constant, and further, in this way, when adding the hydrogen peroxide solution to the slurry, the desired amount can be accurately adjusted. It was confirmed that they could be added well.

【0032】実施例1 図2に示したような試験プラントを作成した。そして過
酸化水素水を添加することなくスラリーを循環させた。
スラリーには、タングステン研磨用シリカスラリー(キ
ャボット・マイクロエレクトロニクス・コーポレーショ
ン社製 Semi−Sperse W2000)に対し
て、1.73wt%及び1.84wt%の既知の濃度の
過酸化水素水を添加したものを使用し、下記のようにし
て過水濃度の測定を行なった。測定は、超音波濃度計
(富士工業(株)社製 超音波液体濃度計FUD−1
MODEL−11)を用い、又、同時に測定系に封入し
たスラリーの圧力を、圧力計(サーパス工業(株)社製
プレッシャーセンサーTPL−5A−N)によって測
定した。そして、先に説明した式によって、圧力変動に
よって生じる過水濃度の測定値のバラツキを補正し、得
られた結果をコントローラー22に記録した。
Example 1 A test plant as shown in FIG. 2 was prepared. Then, the slurry was circulated without adding hydrogen peroxide solution.
The slurry was prepared by adding a hydrogen peroxide solution having a known concentration of 1.73 wt% and 1.84 wt% to a silica slurry for polishing tungsten (Semi-Space W2000 manufactured by Cabot Microelectronics Corporation). It was used and the measurement of the perhydrogen concentration was carried out as follows. The measurement is performed by an ultrasonic densitometer (Ultrasonic liquid densitometer FUD-1 manufactured by Fuji Industry Co., Ltd.).
MODEL-11), and at the same time, the pressure of the slurry enclosed in the measurement system was measured by a pressure gauge (pressure sensor TPL-5A-N manufactured by Surpass Industry Co., Ltd.). Then, the variation in the measured value of the superfluid concentration caused by the pressure fluctuation was corrected by the above-described formula, and the obtained result was recorded in the controller 22.

【0033】上記のようにして、過水濃度が1.73w
t%と1.84wt%である既知のスラリーを各々循環
させて、超音波濃度計による測定を3回繰り返した。得
られた結果を表3に示した。その平均値は、それぞれ
1.73wt%、1.83wt%であり、測定結果は真
値に近く、正確な測定が行なわれることが確認できた。
又、その標準偏差は、それぞれ0.013wt%、0.
006wt%であり、繰り返し測定の際のバラツキが小
さく、精度のよい測定がなされていることが確認でき
た。
As described above, the perhydrogen concentration is 1.73 w.
The known slurries of t% and 1.84 wt% were circulated, respectively, and the measurement by the ultrasonic densitometer was repeated three times. The results obtained are shown in Table 3. The average values were 1.73 wt% and 1.83 wt%, respectively, and the measurement results were close to the true values, confirming that accurate measurement was performed.
The standard deviations are 0.013 wt% and 0.
It was 006 wt%, and it was confirmed that there was little variation during repeated measurements and that accurate measurements were made.

【0034】 [0034]

【0035】使用例1 過水添加機構29を構成している容量2Lの貯蔵タンク
からスラリータンク31へと過酸化水素水を添加しなが
ら、スラリーを循環させた。この際、スラリー供給装置
27によって、3L/minの速度でスラリーが循環す
るように供給した。又、本使用例では、スラリーに添加
された過酸化水素水の添加量を定量するために、羽根車
式流量計(東京計装(株)社製 ミニホイールフローメ
ーターW812−1−T)を用いた。更に、流量制御オ
リフィス(φ1.5mm)を用いた。又、コントローラ
ーには、(横河電機(株)社製 プログラマブルコント
ローラーFA−M3)を用いた。
USE EXAMPLE 1 The slurry was circulated while adding hydrogen peroxide solution from the 2 L capacity storage tank constituting the perhydrogen addition mechanism 29 to the slurry tank 31. At this time, the slurry was supplied by the slurry supply device 27 so as to circulate at a rate of 3 L / min. Further, in this example of use, an impeller flow meter (Mini Wheel Flow Meter W812-1-T manufactured by Tokyo Keiso Co., Ltd.) was used to quantify the amount of hydrogen peroxide added to the slurry. Using. Further, a flow rate control orifice (φ1.5 mm) was used. A programmable controller FA-M3 manufactured by Yokogawa Electric Corp. was used as the controller.

【0036】上記した構成で、スラリーを循環させた。
又、コントローラーに入力する所望の過酸化水素水の濃
度を2.00wt%とした。そして、スラリータンク中
の過水濃度を所望の濃度より低めに調整し、先に説明し
た、過水濃度の測定と、過酸化水素水の添加の一連の動
作によって、スラリー中の過水濃度を所望の濃度に調整
することを、3回試みた。表4に、その結果を示した。
この結果、表4に示した通り、所望の濃度2.00wt
%に対して、±0.02wt%の範囲内で、正確に且つ
精度よく、過水濃度をコントロールできることが確認で
きた。
With the above constitution, the slurry was circulated.
Further, the concentration of the desired hydrogen peroxide solution input to the controller was set to 2.00 wt%. Then, adjusting the perhydrogen concentration in the slurry tank to be lower than the desired concentration, and measuring the perhydrogen concentration and the series of operations of adding hydrogen peroxide water described above, Attempts to adjust to the desired concentration were made three times. The results are shown in Table 4.
As a result, as shown in Table 4, the desired concentration was 2.00 wt.
It was confirmed that the perhydrogen concentration can be accurately and accurately controlled within the range of ± 0.02 wt% with respect to%.

【0037】 [0037]

【0038】[0038]

【発明の効果】上記したように、本発明によれば、例え
ば、半導体基板上に形成された金属薄膜を平坦化するた
めの研磨処理等に使用される循環スラリー中の過水濃度
を、優れた精度で経済的に測定できる循環スラリー中の
過水濃度の測定方法が提供される。更に、本発明によれ
ば、上記のような優れた過水濃度の測定方法を用いるこ
とで、循環スラリー中の過水濃度を常に一定に保つこと
が可能となる結果、高い品質の半導体製品を効率よく安
定して提供することを可能にできる。
As described above, according to the present invention, for example, it is possible to improve the concentration of superfluous water in a circulating slurry used for polishing treatment for flattening a metal thin film formed on a semiconductor substrate. Provided is a method for measuring the concentration of superfluid water in a circulating slurry, which can be economically measured with high accuracy. Furthermore, according to the present invention, by using the above-mentioned excellent method for measuring the concentration of superfluous water, it becomes possible to always keep the concentration of superfluous water in the circulating slurry constant, resulting in high quality semiconductor products. It can enable efficient and stable provision.

【図面の簡単な説明】[Brief description of drawings]

【図1】本発明の方法に用いる測定系を模式的に説明す
る図である。
FIG. 1 is a diagram schematically illustrating a measurement system used in the method of the present invention.

【図2】 本発明の方法をスラリー供給システムに適用
した場合の概略構成図である。
FIG. 2 is a schematic configuration diagram when the method of the present invention is applied to a slurry supply system.

【図3】超音波濃度計による過水濃度の実測値に対し
て、圧力補正の有無による違いを示す結果の図である。
FIG. 3 is a diagram showing a result showing a difference between the actual measurement value of the concentration of superfluous water measured by an ultrasonic densitometer and the presence / absence of pressure correction.

【図4】超音波濃度計による過水濃度の実測値に対し
て、圧力補正の有無による違いを示す結果の図である。
FIG. 4 is a diagram showing a result showing a difference between the presence or absence of pressure correction with respect to an actual measurement value of the concentration of superfluous water measured by an ultrasonic densitometer.

【図5】超音波濃度計による過水濃度の実測値に対し
て、圧力補正の有無による違いを示す結果の図である。
FIG. 5 is a diagram showing results showing a difference between the actual measurement value of the superfluous water concentration measured by the ultrasonic densitometer and the presence / absence of pressure correction.

【図6】過酸化水素水の添加の際の圧力変動の有無が添
加量に及ぼす違いを示す結果の図である。
FIG. 6 is a graph showing the results of the difference in the amount of addition of the presence or absence of pressure fluctuation during the addition of hydrogen peroxide solution.

【符号の説明】[Explanation of symbols]

1:スラリー供給ライン 2、3、4:バルブ 5:圧力計 6:超音波濃度計 19:バルブ 21:レベル計 22:コントローラー(PLC) 26:研磨装置 27:スラリー供給装置 28:測定系 29:過水添加機構 31:スラリータンク 1: Slurry supply line 2, 3, 4: Valve 5: Pressure gauge 6: Ultrasonic densitometer 19: Valve 21: Level meter 22: Controller (PLC) 26: Polishing device 27: Slurry supply device 28: Measurement system 29: Overwater addition mechanism 31: Slurry tank

Claims (3)

【特許請求の範囲】[Claims] 【請求項1】 循環しているスラリー中の過酸化水素水
の濃度を測定する循環スラリー中の過酸化水素水濃度の
測定方法であって、循環しているスラリーの一部を封入
することで、循環しているスラリーの系から切り離して
独立した状態にした測定系を設け、該測定系内に封入さ
れたスラリーを静置した後、該スラリー中の過酸化水素
水濃度の測定を超音波濃度計によって行なうことを特徴
とする循環スラリー中の過酸化水素水濃度の測定方法。
1. A method for measuring the concentration of hydrogen peroxide solution in a circulating slurry for measuring the concentration of hydrogen peroxide solution in a circulating slurry, comprising enclosing a part of the circulating slurry. A measurement system that is separated from the system of the circulating slurry and is set in an independent state is provided, and the slurry enclosed in the measurement system is allowed to stand still, and then the concentration of hydrogen peroxide solution in the slurry is measured by ultrasonic waves. A method for measuring the concentration of hydrogen peroxide water in a circulating slurry, which is characterized in that it is carried out by a densitometer.
【請求項2】 更に、前記測定系に圧力計が設けられ、
該圧力計によって過酸化水素水濃度の測定と併行して封
入されたスラリーの圧力を測定し、得られた圧力測定値
によって超音波濃度計で測定した過酸化水素水濃度の測
定値を補正演算する補正演算機構を有する請求項1に記
載の循環スラリー中の過酸化水素水濃度の測定方法。
2. A pressure gauge is further provided in the measurement system,
The pressure of the enclosed slurry is measured in parallel with the measurement of the hydrogen peroxide concentration by the pressure gauge, and the measured value of the hydrogen peroxide concentration measured by the ultrasonic concentration meter is corrected by the obtained pressure measurement value. The method for measuring the concentration of hydrogen peroxide solution in the circulating slurry according to claim 1, further comprising a correction calculation mechanism that
【請求項3】 前記スラリーが、ウェーハ基板上に形成
された金属膜表面の研磨を行なう際に使用されるスラリ
ーである請求項1に記載の循環スラリー中の過酸化水素
水濃度の測定方法。
3. The method for measuring the concentration of hydrogen peroxide water in a circulating slurry according to claim 1, wherein the slurry is a slurry used when polishing the surface of a metal film formed on a wafer substrate.
JP2002122123A 2002-04-24 2002-04-24 Measuring method of hydrogen peroxide concentration in circulating slurry Expired - Fee Related JP3617977B2 (en)

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JP3617977B2 JP3617977B2 (en) 2005-02-09

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Country Link
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101868771B1 (en) * 2018-03-22 2018-07-17 성락규 Solution for Detecting Concentration of CMP Slurry and Preparation thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101868771B1 (en) * 2018-03-22 2018-07-17 성락규 Solution for Detecting Concentration of CMP Slurry and Preparation thereof

Also Published As

Publication number Publication date
JP3617977B2 (en) 2005-02-09

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