JPH06194290A - Method and apparatus for evaluating water quality - Google Patents
Method and apparatus for evaluating water qualityInfo
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- JPH06194290A JPH06194290A JP34251492A JP34251492A JPH06194290A JP H06194290 A JPH06194290 A JP H06194290A JP 34251492 A JP34251492 A JP 34251492A JP 34251492 A JP34251492 A JP 34251492A JP H06194290 A JPH06194290 A JP H06194290A
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- water
- weight sensor
- crystal
- electrode
- frequency
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Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は水中の不純物量特に超純
水中に含まれる不純物を蒸発残留物量として測定する方
法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for measuring the amount of impurities in water, especially the impurities contained in ultrapure water as the amount of evaporation residue.
【０００２】[0002]
【従来の技術】従来、超純水の水質は、比抵抗、全有機
炭素（ＴＯＣ）、微粒子、シリカそして生菌によって評
価されてきている。さらに、最近になって溶存酸素濃度
もその項目の中に加わり、主に表１の６項目によって評
価されている。現在、最も高純度と考えられる超純水の
水質を表１に示すが、これらの項目全てが検出感度以下
のレベルにあり、これまでの評価方法（手段）では、そ
の水質の優位差を評価できない状況にある。2. Description of the Related Art Conventionally, the water quality of ultrapure water has been evaluated by specific resistance, total organic carbon (TOC), fine particles, silica and viable bacteria. Furthermore, recently, the dissolved oxygen concentration has been added to the items, and is mainly evaluated by the six items in Table 1. Currently, the water quality of ultrapure water, which is considered to have the highest purity, is shown in Table 1. However, all of these items are below the level of detection sensitivity, and the evaluation methods (means) used so far evaluate the difference in water quality. There is a situation that cannot be done.
【０００３】[0003]
【表１】 [Table 1]
【０００４】そこで、ウォーターマーク法というＬＳＩ
の製造方法に沿った新しい評価方法が提案された。これ
は、シリコンウエハ上に超純水を滴下し、蒸発乾燥後に
残るしみをウォーターマークと称して、顕微鏡にて観察
しその量と色、形等から水質を評価するものである。通
常、超純水はウエハの洗浄工程において薬液等の処理に
よってウエハ上に付着した不純物を除去するために用い
るものであり、超純水リンス後はウエハは乾燥される。
したがって、蒸発・乾燥後に何もウエハ上に残らないこ
とが最良であり、ウォーターマーク法はＬＳＩ用超純水
の評価方法としては、ＬＳＩ製造工程に沿ったものであ
ると考えられる。また、ウエハ表面にできた“しみ”を
コンピューターを用いて画像処理し、その量を定量的に
把握しようとする試みも行われているが、依然、実用の
域には達していない。Therefore, an LSI called a watermark method is used.
A new evaluation method was proposed in line with the manufacturing method of. This is a technique in which ultrapure water is dropped on a silicon wafer, and stains remaining after evaporation and drying are referred to as watermarks, which are observed with a microscope to evaluate the water quality from the amount, color, shape, and the like. Usually, ultrapure water is used to remove impurities adhering to the wafer by a treatment with a chemical solution or the like in the wafer cleaning step, and the wafer is dried after the ultrapure water rinse.
Therefore, it is best that nothing remains on the wafer after evaporation / drying, and the watermark method is considered to be in line with the LSI manufacturing process as an evaluation method of ultrapure water for LSI. In addition, an attempt has been made to image-process the "spots" formed on the wafer surface by using a computer and quantitatively grasp the amount, but it has not reached the practical range.
【０００５】このウォーターマークに関する公知例とし
ては、ケミカルエンジニアリング１９９０年１月号ｐ．
６８がある。As a known example of this watermark, Chemical Engineering, January 1990, p.
There is 68.
【０００６】[0006]
【発明が解決しようとする課題】上記、従来のウォータ
ーマーク法では、マークの有無や大きさ等の定性的な評
価は可能であるが、重量で定量的な評価をすることがで
きなかった。本発明の課題はこれを可能にすることにあ
る。In the above-mentioned conventional watermark method, it is possible to qualitatively evaluate the presence or the size of the mark and the size, but it is not possible to quantitatively evaluate the weight. The object of the invention is to make this possible.
【０００７】[0007]
【課題を解決するための手段】上記課題は、水晶振動子
と電極で構成される水晶重みセンサーを用いて振動子表
面の電極上にウォーターマークを作成し、乾燥前後の水
晶重みセンサーの振動数変化を測定することで解決でき
る。[Means for Solving the Problems] The above problem is that a crystal weight sensor composed of a crystal oscillator and electrodes is used to create a watermark on an electrode on the surface of the oscillator, and the frequency of the crystal weight sensor before and after drying is increased. It can be solved by measuring the change.
【０００８】[0008]
【作用】通常、水晶振動子は固有振動数を持っている
が、その表面に何か付着することによって重量変化が生
じるとその振動数が変化する。また、その振動数は
（１）式に従って減少することが知られている。Operation Normally, a crystal unit has a natural frequency, but if something adheres to the surface of the crystal unit and the weight changes, the frequency changes. Further, it is known that its frequency decreases according to the equation (1).
【０００９】 ΔＦ＝−２．３×１０6 Ｆ2 Δｍ／Ａ （１） ここで、ΔＦは振動数の変化量（Ｈｚ）、Ｆは固有振動
数（ＭＨｚ）を、Δｍは付着物の重量変化（ｇ）を、そ
してＡは電極の面積（ｃｍ2 ）である。したがって、水
晶重みセンサー表面の電極に水滴を滴下し、蒸発乾燥後
と滴下前の振動数の変化を測定することで、サンプル水
中に含まれる不純物を重量で測定することが可能とな
る。ちなみに、固有振動数をＭＨｚ、電極面積を１ｃｍ
2 とすると１Ｈｚの振動数の変化は１２ｎｇに相当する
ことになる。したがって、１０μｇ／１の不純物を含む
超純水の場合約１．２ｍｌ滴下・乾燥することで１Ｈｚ
の振動数変化として測定できることになる。本発明原理
についての公知例としては、ぶんせき１９８９年２月号
があり、現在、水晶重みセンサーの特性を利用すること
で、金属の腐食速度や蒸着速度の測定を目的として研究
が行われている。ΔF = −2.3 × 10 6 F 2 Δm / A (1) where ΔF is the amount of change in frequency (Hz), F is the natural frequency (MHz), and Δm is the weight of the deposit. The change (g), and A is the area of the electrode (cm 2 ). Therefore, it is possible to measure the impurities contained in the sample water by weight by dropping a water drop on the electrode on the surface of the crystal weight sensor and measuring the change in the frequency after evaporation and drying and before the drop. By the way, the natural frequency is MHz and the electrode area is 1 cm.
If it is set to 2 , the change in the frequency of 1 Hz corresponds to 12 ng. Therefore, in the case of ultrapure water containing 10 μg / 1 impurities, about 1.2 ml is dropped and dried to obtain 1 Hz.
It can be measured as the change in frequency. As a publicly known example of the principle of the present invention, there is the Bunseki February 1989 issue, which is currently being studied for the purpose of measuring the corrosion rate and vapor deposition rate of metals by utilizing the characteristics of a quartz weight sensor. There is.
【００１０】しかしながら、（１）式は電極表面に均一
に付着させることが条件であり、不均一な付着の場合は
（１）式は成り立たない。通常の電極表面に蒸発残査を
作成すると、ある一点に集中して残留物が残ることか
ら、残った位置によって振動数の変化が異なってしま
う。そこで、電極表面に凹凸をつけるか吸水性の物質を
付着させることにより、常に同一場所に残留させること
により位置による振動数変化の感度依存性を抑制するこ
とができる。However, the expression (1) is required to be uniformly attached to the electrode surface, and the expression (1) does not hold in the case of non-uniform attachment. When an evaporation residue is created on a normal electrode surface, the residue remains concentrated at a certain point, and the change in frequency varies depending on the remaining position. Therefore, it is possible to suppress the sensitivity dependence of the change in frequency depending on the position by making the electrode surface uneven and adhering a water-absorbing substance so that the electrode always remains at the same place.
【００１１】[0011]
【実施例】以下図面を用いて本発明の実施例を詳細に説
明する。Embodiments of the present invention will be described in detail below with reference to the drawings.
【００１２】図１に本発明に係る水晶重みセンサーによ
る水質評価法の一例を示す。本評価装置構成は、水晶振
動子１０１、電極１０２，１０３、発振器１０４、振動
数測定器１０５と演算器１０６より構成される。本装置
の動作は、まず電極１０３表面に何も付着していない状
態での水晶振動子１０１の固定振動数を振動数測定器１
０５により測定する。その後、水晶振動子１０１の上部
電極１０３上にサンプル管１０７を用いてサンプル水１
０８（可能ならば既知量が良い）を滴下する。さらに、
滴下後のサンプル水１０８が乾燥した後に、再度、水晶
振動子１０１の固有振動数を振動数測定器１０５により
測定し、前後の振動数の変化量から演算器１０６によっ
て重量を算出し、サンプル水の量から最終的には水中の
不純物濃度を算出することができる。本装置を用いて、
固有周波数が６ＭＨｚの水晶振動子上に既知濃度（Ｎａ
Ｃｌ）、既知量のサンプル水を滴下・乾燥前後の振動数
変化を測定した結果を図５に示す。ここで、縦軸は振動
数の変化量ΔＦ（Ｈｚ）、横軸はサンプル水中に含まれ
ていたＮａＣｌの重量である。この結果、ΔＦと付着物
重量の間には一次の関係が成立しており、本方式で水中
の不純物量を測定できることがわかる。しかし、水晶重
みセンサーは、付着物の電極表面における位置によって
その振動数変化の感度が大きく異なる。本結果では、特
にその点を考慮しなかったために、結果にばらつきが生
じている。したがって、付着物が均一に付着するか、も
しくは常に同一点に付着物が残留することが必要にな
る。FIG. 1 shows an example of a water quality evaluation method using a crystal weight sensor according to the present invention. The configuration of this evaluation apparatus includes a crystal oscillator 101, electrodes 102 and 103, an oscillator 104, a frequency measuring device 105, and a computing device 106. The operation of this device is as follows. First, the fixed frequency of the crystal unit 101 with nothing attached to the surface of the electrode 103 is measured by the frequency measuring device 1.
It measures by 05. After that, the sample water 1 is placed on the upper electrode 103 of the crystal unit 101 using the sample tube 107.
08 (known amount is good if possible) is dropped. further,
After the sample water 108 after dropping is dried, the natural frequency of the crystal oscillator 101 is measured again by the frequency measuring device 105, and the weight is calculated by the calculator 106 from the amount of change in the frequency before and after. Finally, the impurity concentration in water can be calculated from the amount. With this device,
A known concentration (Na
Cl) and a known amount of sample water were measured for changes in frequency before and after dropping and drying are shown in FIG. Here, the vertical axis represents the amount of change in frequency ΔF (Hz), and the horizontal axis represents the weight of NaCl contained in the sample water. As a result, there is a linear relationship between ΔF and the weight of the deposit, and it can be seen that the amount of impurities in water can be measured by this method. However, the crystal weight sensor has a great difference in the sensitivity of the change in frequency depending on the position of the deposit on the electrode surface. In this result, there is a variation in the result because that point is not taken into consideration. Therefore, it is necessary that the deposit adheres uniformly or that the deposit always remains at the same point.
【００１３】図２にそのための本発明に係る水質評価装
置に使用する水晶重みセンサーの電極形状の一例を示
す。ここで、本センサー２００は水晶振動子２０１、下
部電極２０２、上部電極２０３、配線２０４より構成さ
れる。本センサー２００は、その上部電極表面に細かい
凹凸２０５を設けており、この凹凸２０５によって滴下
したサンプル水が凹部に留まり、上部電極２０３上に均
一に残留物を残すことが可能になる。本実施例では、細
かい凹凸をつけたが、その他の方法としては、電極中央
に凹部を設けることで常に同一場所に残留させることが
可能になる。また、逆に中央に凸部を設けても、サンプ
ル水が凸部に付着しながら乾燥していくことから、最終
的には残留物も凸部近傍に残留させることが可能にな
る。FIG. 2 shows an example of the electrode shape of the crystal weight sensor used for the water quality evaluation apparatus according to the present invention. Here, the sensor 200 includes a crystal oscillator 201, a lower electrode 202, an upper electrode 203, and a wiring 204. The sensor 200 is provided with fine irregularities 205 on the surface of the upper electrode, and the irregularity 205 allows the dropped sample water to remain in the concave portions, thereby allowing a residue to be left uniformly on the upper electrode 203. In this embodiment, fine irregularities are formed, but as another method, it is possible to always leave the concave portions at the same place by providing a concave portion at the center of the electrode. On the contrary, even if the convex portion is provided in the center, the sample water is dried while adhering to the convex portion, so that it is possible to leave the residue in the vicinity of the convex portion in the end.
【００１４】図３も本発明に係る水質評価に用いる水晶
重みセンサー電極形状の一例を示す。ここで、本センサ
ー３００は水晶振動子３０１、下部電極３０２、上部電
極３０３、配線３０５，３０６より構成される。本セン
サー３００は、その上部電極３０３の上に水分を吸収で
きる吸水性物質３０４が設置されている。この吸水性物
質３０４にサンプル水を滴下すると、サンプル水は吸水
性物質３０４内に均一に吸い込まれ、乾燥後に残る不純
物も均一に吸水性物質３０４内に残留することになり、
水中の不純物が上部電極３０３に対して均一に残留する
様になる。この吸水性物質の一例としては、布織布や紙
等が挙げられる。FIG. 3 also shows an example of the crystal weight sensor electrode shape used for water quality evaluation according to the present invention. Here, the sensor 300 includes a crystal resonator 301, a lower electrode 302, an upper electrode 303, and wirings 305 and 306. In this sensor 300, a water absorbing substance 304 capable of absorbing water is provided on the upper electrode 303. When the sample water is dropped onto the water-absorbing substance 304, the sample water is evenly sucked into the water-absorbing substance 304, and the impurities remaining after drying also remain uniformly in the water-absorbing substance 304.
Impurities in water will remain uniformly on the upper electrode 303. Examples of this water-absorbing substance include woven cloth and paper.
【００１５】図４に本発明を用いた水質評価システムの
一例を示す。本システムは水質評価装置４００と超純水
装置の生成水配管４０８より構成され、さらに水質評価
装置は、水晶重みセンサー４０１、サンプル水滴下系４
０２、サンプル水乾燥系４０３、発振器４０４、振動数
測定器４０５と演算器４０６より構成される。本システ
ムは超純水生成配管４０８内を流れる超純水を水質評価
装置４００のサンプル水導入部４０９よりサンプル水滴
下系４０２に供給する。ここで、一定量のサンプル水が
水晶重みセンサー４０１の電極上に滴下され、サンプル
水乾燥系４０３よりクリーンな空気できれば高温空気を
吹き付けることによって、サンプル水を乾燥させる。乾
燥後に、水晶重みセンサー４０１の固有振動数を振動数
測定器４０５により測定し、滴下前の振動数測定結果か
らの変化量より演算器４０６によって重量を算出し、サ
ンプル水の量から最終的には水中の不純物濃度を算出
し、モニタリングすることができる。ここで、サンプル
水乾燥系４０３は高温もしくは常温の空気を吹き付ける
ことで乾燥させる例を挙げたが、他の方法でも特に問題
ない。また、本実施例は超純水製造装置の生成水のモニ
タリングを例に挙げたが、他の液体処理装置からの生成
液中の不純物濃度測定もしくはモニタリングにも適用す
ることが可能である。また、上記水質評価装置において
は、振動子表面の蒸発残留物を除去する機構、例えば電
極表面をブラッシングする機構や超純水等にて洗浄する
機構等を設けると、長期的な使用ができ、オンラインで
の測定が可能になる。FIG. 4 shows an example of a water quality evaluation system using the present invention. This system is composed of a water quality evaluation device 400 and a generated water pipe 408 of an ultrapure water device. Further, the water quality evaluation device includes a crystal weight sensor 401 and a sample water dropping system 4.
02, a sample water drying system 403, an oscillator 404, a frequency measuring device 405, and a computing device 406. This system supplies the ultrapure water flowing in the ultrapure water generation pipe 408 to the sample water dropping system 402 from the sample water introducing unit 409 of the water quality evaluation apparatus 400. Here, a fixed amount of sample water is dropped on the electrodes of the crystal weight sensor 401, and clean air can be blown from the sample water drying system 403, if possible, to blow hot air to dry the sample water. After drying, the natural frequency of the crystal weight sensor 401 is measured by the frequency measuring device 405, the weight is calculated by the calculator 406 from the amount of change from the frequency measurement result before dropping, and finally the amount of sample water is calculated. Can calculate and monitor the concentration of impurities in water. Here, the sample water drying system 403 has been described as an example in which the sample water drying system 403 is dried by blowing air at high temperature or room temperature, but other methods may be used without any problem. Further, although the present embodiment has exemplified the monitoring of the produced water of the ultrapure water producing apparatus, it can be applied to the measurement or monitoring of the impurity concentration in the produced liquid from another liquid processing apparatus. Further, in the above-mentioned water quality evaluation device, if a mechanism for removing evaporation residue on the vibrator surface, such as a mechanism for brushing the electrode surface, a mechanism for cleaning with ultrapure water, etc., is provided, long-term use is possible, Online measurement is possible.
【００１６】[0016]
【発明の効果】本発明によれば、通常の純水ばかりでな
く超純水中に含まれる蒸発残留物をその重量で測定する
ことで、その水質を測定もしくはモニタリングすること
ができる。特に、ＬＳＩ用の超純水の水質評価法として
は、ＬＳＩ洗浄ではウエハ上に残る残留物が問題である
ことから、本評価法は非常に有効であると考えられる。According to the present invention, the water quality can be measured or monitored by measuring the evaporation residue contained in not only ordinary pure water but also ultrapure water by its weight. In particular, as a water quality evaluation method for ultrapure water for LSI, since the residue remaining on the wafer during LSI cleaning is a problem, this evaluation method is considered to be very effective.
【図面の簡単な説明】[Brief description of drawings]
【図１】本発明に係る水晶重みセンサーによる水質評価
法の一例FIG. 1 is an example of a water quality evaluation method using a crystal weight sensor according to the present invention.
【図２】本発明に係る水質評価に用いる水晶重みセンサ
ー電極形状の一例FIG. 2 is an example of a crystal weight sensor electrode shape used for water quality evaluation according to the present invention.
【図３】本発明に係る水質評価に用いる水晶重みセンサ
ー電極形状の他の一例FIG. 3 is another example of the crystal weight sensor electrode shape used for water quality evaluation according to the present invention.
【図４】本発明を用いた水質評価システムの一例FIG. 4 is an example of a water quality evaluation system using the present invention.
【図５】本発明に係る水質評価法の実験結果の一例FIG. 5: Example of experimental results of water quality evaluation method according to the present invention
１０１…水晶振動子 １０２，１０３…
電極 １０４…発振器 １０５…振動数測
定器 １０６…演算器101 ... Crystal oscillator 102, 103 ...
Electrode 104 ... Oscillator 105 ... Frequency measurement device 106 ... Computing device
───────────────────────────────────────────────────── フロントページの続き (72)発明者 松本隆行 茨城県日立市大みか町七丁目２番１号 株 式会社日立製作所エネルギー研究所内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Takayuki Matsumoto 7-2-1 Omika-cho, Hitachi-shi, Ibaraki Hitachi Energy Research Laboratory, Ltd.
Claims (5)
成される水晶重みセンサーの電極表面にサンプル水を滴
下し、滴下・乾燥前後の水晶重みセンサーの振動数変化
から、サンプル水中に含まれる不純物もしくは全蒸発残
留物の量を測定することを特徴とする水質評価方法。1. The sample water is dropped on the electrode surface of a crystal weight sensor composed of a crystal oscillator having a natural frequency and an electrode, and is included in the sample water from the frequency change of the crystal weight sensor before and after dropping and drying. A method for evaluating water quality, which comprises measuring the amount of impurities or total evaporation residue.
成される水晶重みセンサーの電極表面にサンプル水を滴
下し、滴下・乾燥前後の水晶重みセンサーの振動数変化
から、サンプル水中に含まれる不純物もしくは全蒸発残
留物の量を測定することを特徴とする水質評価用の水晶
重みセンサーにおいて、その発振周波数と蒸発乾燥後の
付着物重量の間に相関がある様に電極を設けたことを特
徴とする水晶重みセンサー。2. The sample water is dropped on the electrode surface of a crystal weight sensor composed of a crystal oscillator having a fixed frequency and an electrode, and is included in the sample water from the frequency change of the crystal weight sensor before and after dropping and drying. In the quartz weight sensor for water quality evaluation, which is characterized by measuring the amount of impurities or total evaporation residue, electrodes are provided so that there is a correlation between the oscillation frequency and the weight of deposits after evaporation and drying. Crystal weight sensor characterized by.
その発振周波数が付着物重量と相関があるようにサンプ
ル水を乾燥させる機構として、電極の中央もしくは表面
全体に凹凸を有していることを特徴とする水晶重みセン
サー。3. The crystal weight sensor according to claim 2, wherein
A crystal weight sensor characterized by having irregularities in the center or the entire surface of the electrode as a mechanism for drying the sample water so that the oscillation frequency has a correlation with the weight of the deposit.
その発振周波数が付着物重量と相関があるようにサンプ
ル水を乾燥させる機構として、電極が吸水性の物質で構
成されるか、もしくは電極表面に吸水性の物質が設置さ
れていることを特徴とする水晶重みセンサー。4. The crystal weight sensor according to claim 2, wherein
As a mechanism for drying the sample water so that the oscillation frequency correlates with the weight of the deposit, the electrode is composed of a water-absorbing substance, or the water-absorbing substance is installed on the electrode surface. A crystal weight sensor that does.
成される水晶重みセンサー、その振動子を発振させる発
振装置と振動数を測定する測定器、その測定値から計算
により重量を求める演算装置、水晶重みセンサー上にサ
ンプル水を滴下する滴下装置および滴下されたサンプル
水を乾燥させる乾燥装置から構成され、サンプル水の滴
下・乾燥前後における水晶重みセンサーの固有振動数の
変化からサンプル水中の不純物もしくは全蒸発残留物量
を測定することを特徴とする水質評価装置。5. A crystal weight sensor composed of a crystal oscillator having a natural frequency and an electrode, an oscillator for oscillating the oscillator, a measuring instrument for measuring the frequency, and a calculation for obtaining the weight by calculation from the measured value. It consists of a device, a dropping device for dropping sample water on the crystal weight sensor, and a drying device for drying the dropped sample water. A water quality evaluation apparatus characterized by measuring the amount of impurities or total evaporation residue.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34251492A JP3178926B2 (en) | 1992-12-22 | 1992-12-22 | Water quality evaluation method and apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34251492A JP3178926B2 (en) | 1992-12-22 | 1992-12-22 | Water quality evaluation method and apparatus |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06194290A true JPH06194290A (en) | 1994-07-15 |
| JP3178926B2 JP3178926B2 (en) | 2001-06-25 |
Family
ID=18354336
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP34251492A Expired - Fee Related JP3178926B2 (en) | 1992-12-22 | 1992-12-22 | Water quality evaluation method and apparatus |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3178926B2 (en) |
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