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JP4960055B2 - Contamination measurement method - Google Patents
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JP4960055B2 - Contamination measurement method - Google Patents

Contamination measurement method Download PDF

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JP4960055B2
JP4960055B2 JP2006268404A JP2006268404A JP4960055B2 JP 4960055 B2 JP4960055 B2 JP 4960055B2 JP 2006268404 A JP2006268404 A JP 2006268404A JP 2006268404 A JP2006268404 A JP 2006268404A JP 4960055 B2 JP4960055 B2 JP 4960055B2
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vibration element
measurement
piezoelectric vibration
atmosphere
contamination
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JP2008089348A (en
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浩章 飯田
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Kyocera Crystal Device Corp
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Description

本発明はクリーンルーム等の閉鎖空間内の雰囲気中に含有する塵埃等のコンタミネーションの有無又は発塵を測定する方法に関する。 The present invention relates to how you measure the presence or dusting of contamination such as dust contained in the atmosphere in the closed space such as a clean room.

現在、半導体素子や精密機器の製造工程や医療現場では、空間内部の雰囲気中に含まれる微細な塵埃や、雰囲気中の酸や塩基分子に起因する汚染不純物などのコンタミネーションを強制的に除去して、雰囲気の清浄度を高くした所謂クリーンルームが多用されている。最近では清浄度を極限まで引き上げたスーパークリーンルームなども用いられるようになり、その空間内の雰囲気中に含まれるコンタミネーションの測定管理が重要視されるように成っている。   Currently, in the manufacturing process of semiconductor elements and precision equipment and in the medical field, contaminants such as fine dust contained in the atmosphere inside the space and contamination impurities caused by acid and base molecules in the atmosphere are forcibly removed. Thus, so-called clean rooms with high atmosphere cleanliness are often used. Recently, a super clean room with the cleanliness raised to the limit has come to be used, and the measurement management of contamination contained in the atmosphere in the space is regarded as important.

このような雰囲気中のコンタミネーションを測定する方法としては、従来から以下のような方法が用いられてきた。まずコンタミネーションの測定を所望する空間内雰囲気を一定量サンプリングし、そのサンプリングした雰囲気を各種フィルタを通し、各フィルタに対応するコンタミネーションを収集し、フィルタ内のコンタミネーションを溶液中に抽出させその成分を分析したり、パーティクルカウンタを用いて数量を計測したりする。   Conventionally, the following method has been used as a method for measuring the contamination in such an atmosphere. First, a certain amount of the atmosphere in the space where the contamination measurement is desired is sampled, the sampled atmosphere is passed through various filters, the contamination corresponding to each filter is collected, and the contamination in the filter is extracted into the solution. Analyze the components and measure the quantity using a particle counter.

又、他の測定方法としては、レーザー光を使用し、レーザー光でサンプル雰囲気中を走査することで、雰囲気中に塵埃等のコンタミネーションが存在した場合、そのコンタミネーションにレーザー光が当たり散乱光を発生する。その散乱光をCCDカメラにより検出し、そのサンプルから検出した散乱光の発生数により、被測定空間中のコンタミネーションの総量を計算により導出する方法も用いられている。   Another measurement method is to use laser light and scan the sample atmosphere with the laser light. If there is contamination such as dust in the atmosphere, the laser light hits the contamination and the scattered light. Is generated. A method is also used in which the scattered light is detected by a CCD camera, and the total amount of contamination in the measured space is derived by calculation based on the number of scattered light detected from the sample.

上述したようなコンタミネーションの測定方法については、以下のような先行技術文献に開示がある。
特開2000−180348号公報 特開平7−209146号公報 特開平7−229826号公報
Contamination measurement methods as described above are disclosed in the following prior art documents.
JP 2000-180348 A JP-A-7-209146 Japanese Patent Laid-Open No. 7-229826

尚、出願人は前記した先行技術文献情報で特定される先行技術文献以外には、本発明に関連する先行技術文献を、本件出願時までに発見するに至らなかった。   In addition, the applicant has not found any prior art documents related to the present invention by the time of filing of the present application other than the prior art documents specified by the above prior art document information.

しかし、上述したようなコンタミネーションの測定方法は、コンタミネーションの成分や量を測定することには有効であるが、コンタミネーションを含む雰囲気サンプルを採取し、そのサンプルを分析装置にかけコンタミネーションを測定する手法のため、測定結果を得るまでに時間がかかり、コンタミネーションの有無や発生を即時に測定することが難しい。又、レーザを用いた測定方法では、測定システム自体を前もってクリーンルーム等に組み込んでいる必要が有り又測定システムが大規模になってしまうので、測定自体のコスト高、複雑化を招く虞がある。   However, the contamination measurement method as described above is effective for measuring the content and amount of contamination, but an atmospheric sample containing the contamination is collected and the sample is applied to an analyzer to measure the contamination. Therefore, it takes time to obtain measurement results, and it is difficult to immediately measure the presence or absence of contamination. In addition, in the measurement method using a laser, the measurement system itself needs to be incorporated in a clean room or the like in advance, and the measurement system becomes large-scale, which may lead to an increase in cost and complexity of the measurement itself.

本発明は上記課題を解決するために成されたものであり、被測定雰囲気中のコンタミネーションの有無又は発生を測定する方法において、被測定雰囲気中に、圧電振動素子を被測定雰囲気よりも低い気圧で気密に密閉された容器内空間に搭載し、圧電振動素子の表裏主面にそれぞれ形成した励振用電極と電気的に接続する外部接続用端子を形成し、且つ容器内外を遮断するシャッター手段とこのシャッター手段の開閉形態を制御する制御部を有する測定端末体を用意する工程Aと、内部に圧電振動素子を搭載し且つシャッター手段を閉じ容器内空間を気密状態とした測定端末体を被測定雰囲気中に少なくとも1つ以上配置し、外部接続用端子及び制御部の所定の端子を測定制御解析処理用の電子機器又は/及び電子計算機に電気的に接続する工程Bと、接続した電子機器又は/及び電子計算機により、測定端末体内の圧電振動素子から、基準となる圧電振動素子のドライブ電流値−クリスタルインピーダンス値間の特性データ値を測定する工程Cと、接続した電子機器又は/及び電子計算機から制御部に制御信号を入力し、シャッター手段を開き、被測定雰囲気を測定端末体内に流入させる工程Dと、所定の時間後に、接続した電子機器又は/及び電子計算機により、測定端末体内の圧電振動素子から、比較対象となる圧電振動素子のドライブ電流値−クリスタルインピーダンス値間の特性データ値を測定する工程Eと、前記工程Cで取得した基準となる圧電振動素子特性のドライブ電流値−クリスタルインピーダンス値間のデータ値と、前記工程Eで取得した比較対象となる圧電振動素子のドライブ電流値−クリスタルインピーダンス値間の特性データ値とを比較解析し、そのデータ値の差異から被測定雰囲気中に有形コンタミネーション物質の有無を判定する工程Fとを具備することを特徴とするコンタミネーションの測定方法である。 The present invention has been made to solve the above problems, and in a method for measuring the presence or absence of contamination in a measured atmosphere, the piezoelectric vibration element is lower than the measured atmosphere in the measured atmosphere. Shutter means that is mounted in a space inside a container that is airtightly sealed with atmospheric pressure, forms external connection terminals that are electrically connected to excitation electrodes formed on the front and back main surfaces of the piezoelectric vibration element, and blocks the inside and outside of the container And a step A for preparing a measurement terminal body having a control unit for controlling the opening / closing mode of the shutter means, and a measurement terminal body in which a piezoelectric vibration element is mounted and the shutter means is closed to make the space in the container airtight. At least one or more terminals are arranged in the measurement atmosphere, and the external connection terminal and the predetermined terminal of the control unit are electrically connected to the measurement control analysis processing electronic device and / or electronic computer. Degree and B, by connecting the electronic device and / or computer, a piezoelectric vibrating element of the measuring device body, the drive current value of the piezoelectric vibrating element as a reference - a step C of measuring the characteristic data values between the crystal impedance value, A control signal is input from the connected electronic device or / and the electronic computer to the control unit, the shutter means is opened, and the process D for causing the measured atmosphere to flow into the measurement terminal body, and after a predetermined time, the connected electronic device or / and the electronic computer, from the piezoelectric vibrating element of the measuring device body, compared drive current value subject to the piezoelectric vibrating element - a and step E of determining characteristic data values between the crystal impedance value, the reference obtained in the step C piezoelectric drive current value of the vibration element characteristics - and data values between the crystal impedance value, the piezoelectric to be compared obtained in the step (E) Drive current value of the dynamic element - comparatively analyzed the characteristic data values between the crystal impedance value, characterized by including a determining step F whether tangible contaminants into the atmosphere to be measured from the difference of the data value This is a contamination measuring method.

本発明におけるコンタミネーションの測定方法では、表面に物質が付着した場合に共振周波数やクリスタルインピーダンス(以下CIという)値などの特性が変化する圧電振動素子の作用により、測定端末体を配置した被測定雰囲気中の塵埃や、雰囲気中の酸や塩基分子に起因する汚染不純物などのコンタミネーションが、測定端末体内の圧電振動素子表面に付着したときの特性変化を即時に検出することが可能となるので、コンタミネーションの有無や発生をリアルタイムで測定できる。   In the method for measuring contamination according to the present invention, when a substance adheres to the surface, a measurement terminal in which a measurement terminal is arranged by the action of a piezoelectric vibration element whose characteristics such as resonance frequency and crystal impedance (hereinafter referred to as CI) value change. Because it is possible to immediately detect changes in characteristics when contamination such as dust in the atmosphere and contamination impurities due to acid and base molecules in the atmosphere adhere to the surface of the piezoelectric vibration element in the measurement terminal. The presence and occurrence of contamination can be measured in real time.

又、測定端末体の大きさは数センチ角の概略直方体の大きさであり、複数個の測定端末体を測定空間内に後配置も可能のため、測定構成として従来に比べ小規模に構成できるので、測定自体のコストを低く抑え、簡易化を図ることができ、更に測定端末体が小型であるため、半導体素子等の製造装置内の狭小空間内雰囲気中のコンタミネーションの測定も可能となる。   In addition, the size of the measurement terminal body is a size of a roughly rectangular parallelepiped of several centimeters, and a plurality of measurement terminal bodies can be arranged in the measurement space, so that the measurement configuration can be made smaller than before. Therefore, the cost of the measurement itself can be reduced and simplified, and the measurement terminal body is small, so that it is possible to measure the contamination in the atmosphere in the narrow space in the manufacturing apparatus for semiconductor elements and the like. .

又、コンタミネーションの検出をする圧電振動素子は、素子自体が機械的に振動しているので、振動レベルを高くすることで、圧電振動素子表面に付着したコンタミネーションをより高い振動により除去することも可能となるので、測定端末体の再利用も可能となる。   In addition, since the piezoelectric vibration element for detecting contamination is mechanically vibrated, the contamination attached to the surface of the piezoelectric vibration element can be removed by higher vibration by increasing the vibration level. Therefore, the measurement terminal can be reused.

因って、本発明により、測定を所望する空間内雰囲気中のコンタミネーションの有無又は発生を即時に測定でき、且つその測定の構成も小規模且つ安価簡易に形成できるコンタミネーションの測定方法を提供できる効果を奏する。   Therefore, according to the present invention, there is provided a contamination measuring method that can immediately measure the presence / absence or occurrence of contamination in the atmosphere in the space desired to be measured, and that can be easily formed on a small scale and at low cost. There is an effect that can be done.

以下に、本発明におけるコンタミネーションの測定方法の実施形態を、図面を参照しながら説明する。
図1は、本発明におけるコンタミネーションの測定方法に使用する測定システムの構成図である。図2は、図1記載の測定端末体を図示したものであり、(a)は開口部形成面側から見た半分は平面図であり残りの半分は内部構造図であり、(b)は(a)記載の仮想切断線A−A′間で切断した場合の断面図である。図3は、測定端末体内の圧電振動素子にコンタミネーションが付着した際に圧電振動素子の特性の変化を示した、ドライブ電流−CI値間の特性グラフであり、その変化の形態を(a)、(b)及び(c)に示したグラフである。
尚、各図では、説明を明りょうにするため構造体の一部を図示せず、また寸法も一部誇張して図示している。特に各部分の厚み寸法は誇張して図示している。
Hereinafter, an embodiment of a method for measuring contamination according to the present invention will be described with reference to the drawings.
FIG. 1 is a configuration diagram of a measurement system used in a contamination measurement method according to the present invention. FIG. 2 illustrates the measurement terminal body shown in FIG. 1, (a) is a plan view of the half viewed from the opening forming surface side, and the other half is an internal structure diagram. It is sectional drawing at the time of cut | disconnecting between the virtual cutting lines AA 'of (a) description. FIG. 3 is a characteristic graph between the drive current and the CI value, showing the change in the characteristics of the piezoelectric vibration element when contamination adheres to the piezoelectric vibration element in the measurement terminal. The form of the change is shown in FIG. It is the graph shown to (b) and (c).
In each of the drawings, a part of the structure is not shown, and some dimensions are exaggerated for the sake of clarity. In particular, the thickness dimension of each part is exaggerated.

まず、本発明におけるコンタミネーションの測定方法に使用する測定端末体20を説明する。測定端末体20を構成する容器体22内は、測定前の状態では被測定空間10内の被測定雰囲気よりも低い気圧で気密に密閉されており、その容器体22内空間に概略円形の主面外形形状を有する平板状の圧電振動素子21が搭載されている。本実施例においては、圧電振動素子を構成する圧電材として水晶を用いたものを例示する。   First, the measurement terminal body 20 used for the contamination measuring method in the present invention will be described. The inside of the container body 22 constituting the measurement terminal body 20 is hermetically sealed at a lower pressure than the atmosphere to be measured in the space to be measured 10 in the state before measurement, and the main space in the container body 22 has a substantially circular main shape. A plate-like piezoelectric vibration element 21 having a surface outer shape is mounted. In the present embodiment, an example using a crystal as a piezoelectric material constituting the piezoelectric vibration element is illustrated.

この圧電振動素子21の表裏主面には、圧電振動素子21と同心の外形形状が円形の励振用電極23が形成されており、それぞれの励振用電極23から表裏主面間で180°異なる方向の圧電振動素子21の縁部へ向かって延設された引出電極24が形成されており、この引出電極24は圧電振動素子21を間に介して対向して設けられている金属製の2本の支持部25にそれぞれで電気的に接続されるのと同時に、それぞれの支持部25に設けたスリット部26に圧電振動素子21の外周縁部の一部を嵌め込むことで、圧電振動素子21を容器体22内の所定の位置で保持している。又、支持部25は容器体22内の支持部台27を介して容器体22外へ導出され素子接続用電極端子と接続されている。   Excitation electrodes 23 having a circular outer shape concentric with the piezoelectric vibration element 21 are formed on the front and back main surfaces of the piezoelectric vibration element 21, and directions different from each excitation electrode 23 by 180 ° between the front and back main surfaces. An extraction electrode 24 extending toward the edge of the piezoelectric vibration element 21 is formed, and the two extraction electrodes 24 are made of metal and are opposed to each other with the piezoelectric vibration element 21 interposed therebetween. At the same time as being electrically connected to each support portion 25, a part of the outer peripheral edge portion of the piezoelectric vibration element 21 is fitted into the slit portion 26 provided in each support portion 25, thereby the piezoelectric vibration element 21. Is held at a predetermined position in the container body 22. The support portion 25 is led out of the container body 22 via a support portion base 27 in the container body 22 and connected to the element connection electrode terminal.

この圧電振動素子21は、例えば圧電材として水晶を用いた場合では、所謂ATカットアングルで水晶結晶体よりカット研磨した円形平板状の水晶片の両主面に、上述したような一対の励振用電極23を被着形成してなり、外部からの交番電圧が一対の励振用電極23を介して水晶片に印加されると、所定の周波数で厚みすべり振動モードを主振動とする振動を起こす。   For example, in the case where crystal is used as the piezoelectric material, the piezoelectric vibration element 21 has a pair of excitation elements as described above on both main surfaces of a circular flat plate crystal piece cut and polished from a crystal crystal at a so-called AT cut angle. When the electrode 23 is deposited and an alternating voltage from the outside is applied to the crystal piece via the pair of excitation electrodes 23, vibration with the thickness-shear vibration mode as the main vibration occurs at a predetermined frequency.

上述するような圧電振動素子21が内部に搭載されている容器体22において、圧電振動素子21の一方の主面が対向する容器体22の一平面には、圧電振動素子21と同心で且つ励振用電極23とほぼ同じサイズの開口部28が形成されており、この開口部28付近の容器体22内面上には、開口部28を塞ぐことで容器体22内外を気密に遮断するシャッター手段29が設けられている。又、容器体22には、このシャッター手段29の開閉形態を制御する制御部30が併設されている。尚、上述した素子接続用電極端子とシャッター手段29を制御する制御信号を入出力するための制御部30に設けられた制御信号用電極端子は、容器体22に設けられた電極端子ユニット31として一組にまとめられた形態となっている。   In the container body 22 in which the piezoelectric vibration element 21 as described above is mounted, a plane of the container body 22 facing one main surface of the piezoelectric vibration element 21 is concentric with the piezoelectric vibration element 21 and excited. An opening 28 having substantially the same size as the electrode 23 is formed. On the inner surface of the container body 22 in the vicinity of the opening 28, shutter means 29 for blocking the inside and outside of the container body 22 by closing the opening 28. Is provided. The container body 22 is also provided with a control unit 30 for controlling the opening / closing mode of the shutter means 29. The control signal electrode terminal provided in the control unit 30 for inputting and outputting the control signal for controlling the element connecting electrode terminal and the shutter means 29 is an electrode terminal unit 31 provided in the container body 22. It is the form put together in one set.

以下に、上述した測定端末体20を用いたコンタミネーションの測定方法を説明する。
まず、工程Aとして複数個の測定端末体20を用意する。
次に、工程Bとして、上述したような形態の測定端末体20を複数個、クリーンルーム等のコンタミネーションの発生が懸念されるような被測定空間10内の被測定雰囲気中に、シャッター手段29を密閉して測定端末体20の容器体22内空間を気密状態とした状態で配置し、電極端子ユニット31を被測定空間10外に設けた測定制御解析処理用の電子計算機40に電気的に接続する。尚、本実施例では被測定空間10内に配置した複数個の測定端末体20の各電極端子ユニットと接続した信号コードは、被測定空間10内に設けた中継ユニット11にすべて接続し、その中継ユニット11から被測定空間10外へは別の信号コードで接続した形態を用いている。
Hereinafter, a method for measuring contamination using the measurement terminal body 20 described above will be described.
First, as the process A, a plurality of measurement terminal bodies 20 are prepared.
Next, as step B, the shutter unit 29 is placed in the measurement atmosphere in the measurement space 10 where there is a concern about the occurrence of contamination of a plurality of measurement terminal bodies 20 having the above-described form, such as a clean room. The space inside the container body 22 of the measurement terminal body 20 is hermetically sealed, and the electrode terminal unit 31 is electrically connected to an electronic computer 40 for measurement control analysis processing provided outside the space to be measured 10. To do. In this embodiment, the signal cords connected to the electrode terminal units of the plurality of measurement terminals 20 arranged in the measured space 10 are all connected to the relay unit 11 provided in the measured space 10. A form in which another signal cord is connected from the relay unit 11 to the outside of the measured space 10 is used.

次に、工程Cとして、接続した電子計算機40により、各々の測定端末体20内の圧電振動素子21の、圧電振動素子21に印加する励振ドライブ電流値を10μAから1mAへスイープし、更に1mAから10μAへスイープしたときのCI値データを測定する。このとき取得した特性データは、コンタミネーションが圧電振動素子に付着していないときの基準特性データ値となる。   Next, as step C, the excitation drive current value applied to the piezoelectric vibration element 21 of the piezoelectric vibration element 21 in each measurement terminal body 20 is swept from 10 μA to 1 mA by the connected electronic computer 40, and further from 1 mA. Measure CI value data when swept to 10 μA. The characteristic data acquired at this time is a reference characteristic data value when the contamination is not attached to the piezoelectric vibration element.

次に、工程Dとして、接続した電子計算機40から各測定端末体20の制御部30に制御信号を入力し、シャッター手段29を開き、被測定空間10内の被測定雰囲気を測定端末体20の容器体22内に流入させる。シャッター手段29の開口前の容器体内気圧は、容器体外の被測定空間10内の気圧より僅かに低く設定してあるので、シャッター手段29が開くと同時に被測定空間10内の被測定雰囲気が各測定端末体20の容器体22内に自動的に流入し、仮に被測定雰囲気中にコンタミネーションが含まれていた場合、流入する気体と一緒に容器体22内に進入し、容器体22内に搭載されている圧電振動素子21の表面に付着することとなる。   Next, as step D, a control signal is input from the connected electronic computer 40 to the control unit 30 of each measurement terminal body 20, the shutter means 29 is opened, and the measurement atmosphere in the measurement space 10 is changed to the measurement terminal body 20. It flows into the container body 22. Since the pressure inside the container before the opening of the shutter means 29 is set slightly lower than the pressure inside the measured space 10 outside the container body, the measured atmosphere in the measured space 10 varies as soon as the shutter means 29 opens. If the measurement terminal body 20 automatically flows into the container body 22 and contamination is contained in the atmosphere to be measured, the measurement terminal body 20 enters the container body 22 together with the flowing gas, and enters the container body 22. It will adhere to the surface of the mounted piezoelectric vibration element 21.

次に、工程Eとして、シャッター手段29を開口後に、接続した電子計算機40により、被測定空間10内の各所に配置した各測定端末体20内の圧電振動素子21の、圧電振動素子21に印加する励振ドライブ電流値を10μAから1mAへスイープし、更に1mAから10μAへスイープしたときのCI値データを随時測定する。   Next, as step E, after opening the shutter means 29, the connected electronic computer 40 applies the piezoelectric vibration element 21 in each measurement terminal body 20 arranged at various locations in the measured space 10 to the piezoelectric vibration element 21. CI value data when the excitation drive current value to be swept from 10 μA to 1 mA is swept from 1 mA to 10 μA is measured as needed.

次に、工程Fとして、上記工程Eで取得した測定特性データとシャッター手段29閉口時に測定した基準特性データとをリアルタイムで比較解析する。このとき、測定特性データと基準特性データとの間に差異が無ければ、被測定空間10内の被測定雰囲気中にはコンタミネーションが存在しないこととなる。しかし被測定空間10内の被測定雰囲気中にはコンタミネーションが存在し、測定端末体20内の圧電振動素子21に付着した場合は、付着したコンタミネーションが圧電振動素子21の振動を阻害する作用を及ぼし、図3の各グラフに記載のような特性データ間に差異が生じる。このような特性データ間に差異が生じたことにより、被測定空間10内の被測定雰囲気中にコンタミネーションが存在していることを判定する。   Next, in step F, the measurement characteristic data acquired in step E and the reference characteristic data measured when the shutter unit 29 is closed are compared and analyzed in real time. At this time, if there is no difference between the measured characteristic data and the reference characteristic data, there is no contamination in the measured atmosphere in the measured space 10. However, when there is contamination in the measured atmosphere in the measured space 10 and it adheres to the piezoelectric vibration element 21 in the measurement terminal body 20, the adhered contamination inhibits the vibration of the piezoelectric vibration element 21. Thus, there is a difference between the characteristic data as described in each graph of FIG. Due to the difference between the characteristic data, it is determined that contamination exists in the measured atmosphere in the measured space 10.

又、シャッター手段29が開口した状態の測定端末体20を被測定空間10内に配置しておき、常時上記のような特性データを取得し続けることにより、何らかの原因により被測定空間10内でコンタミネーションが発生してしまった場合に、そのコンタミネーションが測定端末体20内の圧電振動素子21に付着することで、取得していた特性データに変化が生じ、電子計算機40上にコンタミネーションの発生をリアルタイムで通告することができる。   In addition, the measurement terminal body 20 with the shutter means 29 opened is placed in the measured space 10 and the above characteristic data is continuously acquired, so that the contamination in the measured space 10 for some reason. In the case where the nation has occurred, the contamination adheres to the piezoelectric vibration element 21 in the measurement terminal body 20, so that the acquired characteristic data changes, and the occurrence of contamination on the electronic computer 40 occurs. Can be notified in real time.

尚、本発明は上述の実施形態に限定されるものではなく、本発明の要旨を逸脱しない範囲において種々の変更、改良等が可能である。例えば、例えば、上述した実施形態においては、圧電振動素子を構成する圧電素材として水晶を用いた測定端末体を説明したが、圧電素材としては、ニオブ酸リチウム、タンタル酸リチウムまたは、圧電セラミックスを用いたものでも構わない。又、圧電振動素子から取得する特性データとして、励振ドライブ電流値−クリスタルインピーダンス値間の特性データを用いたが、他に、励振ドライブ電流値−共振周波数値間の特性データや、共振周波数値−等価リアクタンス値間の特性データ用いても、本発明と同様な効果を奏することができる。更に、上記実施形態では各測定端末体の特性データを測定解析する装置として電子計算機を用いた形態を開示したが、他に電子計算機の代わりにインピーダンスアナライザやネットワークアナライザ等の電子機器を用いた場合や、これら電子機器と電子計算機を組み合わせて構築した測定システムを使用しても良い。   In addition, this invention is not limited to the above-mentioned embodiment, A various change, improvement, etc. are possible in the range which does not deviate from the summary of this invention. For example, in the above-described embodiment, the measurement terminal body using crystal as the piezoelectric material constituting the piezoelectric vibration element has been described. However, as the piezoelectric material, lithium niobate, lithium tantalate, or piezoelectric ceramics is used. It doesn't matter what you have. In addition, as the characteristic data acquired from the piezoelectric vibration element, the characteristic data between the excitation drive current value and the crystal impedance value is used. In addition, the characteristic data between the excitation drive current value and the resonance frequency value, and the resonance frequency value − Even if the characteristic data between the equivalent reactance values is used, the same effect as the present invention can be obtained. Furthermore, in the above-described embodiment, a form using an electronic computer as an apparatus for measuring and analyzing the characteristic data of each measurement terminal body has been disclosed. However, in the case where an electronic device such as an impedance analyzer or a network analyzer is used instead of the electronic computer Alternatively, a measurement system constructed by combining these electronic devices and electronic computers may be used.

図1は、本発明におけるコンタミネーションの測定方法に使用する測定システムの構成図である。FIG. 1 is a configuration diagram of a measurement system used in a contamination measurement method according to the present invention. 図2は、図1記載の測定端末体を図示したものであり、(a)は開口部形成面側から見た半分は平面図であり残りの半分は内部構造図であり、(b)は(a)記載の仮想切断線A−A′間で切断した場合の断面図である。FIG. 2 illustrates the measurement terminal body shown in FIG. 1, (a) is a plan view of the half viewed from the opening forming surface side, and the other half is an internal structure diagram. It is sectional drawing at the time of cut | disconnecting between the virtual cutting lines AA 'of (a) description. 図3は、測定端末体内の圧電振動素子にコンタミネーションが付着した際に圧電振動素子の特性の変化を示した、ドライブ電流−CI値間の特性グラフであり、その変化の形態を(a)、(b)及び(c)に示したグラフである。FIG. 3 is a characteristic graph between the drive current and the CI value, showing the change in the characteristics of the piezoelectric vibration element when contamination adheres to the piezoelectric vibration element in the measurement terminal. The form of the change is shown in FIG. It is the graph shown to (b) and (c).

符号の説明Explanation of symbols

10・・・被測定空間
20・・・測定端末体
21・・・圧電振動素子
22・・・容器体
23・・・励振用電極
24・・・引出電極
25・・・支持部
26・・・スリット部
27・・・支持部台
28・・・開口部
29・・・シャッター手段
30・・・制御部
31・・・電極端子ユニット
40・・・電子計算機
DESCRIPTION OF SYMBOLS 10 ... Measuring space 20 ... Measurement terminal body 21 ... Piezoelectric vibration element 22 ... Container body 23 ... Excitation electrode 24 ... Extraction electrode 25 ... Support part 26 ... Slit part 27 ... Supporting part base 28 ... Opening part 29 ... Shutter means 30 ... Control part 31 ... Electrode terminal unit 40 ... Computer

Claims (1)

被測定雰囲気中のコンタミネーションの有無又は発生を測定する方法において、
被測定雰囲気中に、圧電振動素子を該被測定雰囲気よりも低い気圧で気密に密閉された容器内空間に搭載し、該圧電振動素子の表裏主面にそれぞれ形成した励振用電極と電気的に接続する外部接続用端子を形成し、且つ容器内外を遮断するシャッター手段と該シャッター手段の開閉形態を制御する制御部を有する測定端末体を用意する工程Aと、
内部に圧電振動素子を搭載し且つシャッター手段を閉じ容器内空間を気密状態とした該測定端末体を被測定雰囲気中に少なくとも1つ以上配置し、該外部接続用端子及び該制御部の所定の端子を測定制御解析処理用の電子機器又は/及び電子計算機に電気的に接続する工程Bと、
接続した電子機器又は/及び電子計算機により、該測定端末体内の圧電振動素子から、基準となる圧電振動素子のドライブ電流値−クリスタルインピーダンス値間の特性データ値を測定する工程Cと、
接続した電子機器又は/及び電子計算機から制御部に制御信号を入力し、シャッター手段を開き、被測定雰囲気を該測定端末体内に流入させる工程Dと、
所定の時間後に、接続した電子機器又は/及び電子計算機により、該測定端末体内の圧電振動素子から、比較対象となる圧電振動素子のドライブ電流値−クリスタルインピーダンス値間の特性データ値を測定する工程Eと、
工程Cで取得した基準となる圧電振動素子のドライブ電流値−クリスタルインピーダンス値間の特性データ値と該工程Eで取得した比較対象となる圧電振動素子のドライブ電流値−クリスタルインピーダンス値間の特性データ値とを比較解析し、そのデータ値の差異から被測定雰囲気中に有形コンタミネーション物質の有無を判定する工程Fと
を具備することを特徴とするコンタミネーションの測定方法。
In a method for measuring the presence or occurrence of contamination in the atmosphere to be measured,
A piezoelectric vibration element is mounted in a space in a container hermetically sealed at a lower air pressure than the measurement atmosphere in the measurement atmosphere, and is electrically connected to the excitation electrodes respectively formed on the front and back main surfaces of the piezoelectric vibration element. Step A of preparing a measurement terminal body having a shutter means for forming an external connection terminal to be connected and blocking the inside and outside of the container and a control unit for controlling the opening / closing mode of the shutter means;
At least one or more measurement terminal bodies each having a piezoelectric vibration element mounted therein and the shutter means closed and the space inside the container being hermetically sealed are disposed in the atmosphere to be measured, and the external connection terminal and the predetermined control unit Step B for electrically connecting the terminal to an electronic device or / and an electronic computer for measurement control analysis processing;
A step C of measuring a characteristic data value between a drive current value and a crystal impedance value of a reference piezoelectric vibration element from the piezoelectric vibration element in the measurement terminal by a connected electronic device or / and an electronic computer;
A step D of inputting a control signal to the control unit from the connected electronic device or / and electronic computer, opening the shutter means, and allowing the atmosphere to be measured to flow into the measurement terminal body;
A step of measuring a characteristic data value between a drive current value and a crystal impedance value of a piezoelectric vibration element to be compared from the piezoelectric vibration element in the measurement terminal by a connected electronic device or / and electronic computer after a predetermined time. E and
Drive current value of the piezoelectric vibrating element as a reference obtained in the step C - and the characteristic data values between the crystal impedance value, the drive current value of the piezoelectric vibrating elements to be compared obtained in the step E - between the crystal impedance value of A method of measuring contamination, comprising: a step F of comparing and analyzing characteristic data values and determining the presence or absence of a tangible contaminant in the atmosphere to be measured from the difference between the data values.
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