JP2007010523A - Sensor for measuring micromass - Google Patents

Sensor for measuring micromass Download PDF

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JP2007010523A
JP2007010523A JP2005192726A JP2005192726A JP2007010523A JP 2007010523 A JP2007010523 A JP 2007010523A JP 2005192726 A JP2005192726 A JP 2005192726A JP 2005192726 A JP2005192726 A JP 2005192726A JP 2007010523 A JP2007010523 A JP 2007010523A
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measuring
sensor
container
sensor element
mass
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Akira Ito
章 伊藤
Hiroshi Okawa
弘 大川
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Kyocera Crystal Device Corp
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Kyocera Crystal Device Corp
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a sensor for measuring micromass of high reliability constituted by incorporating a circuit in a QCM sensor container. <P>SOLUTION: The sensor element for measuring micromass is provided to the QCM sensor container so that only one main electrode surface thereof is exposed and the side surface of the micromass measuring sensor element is placed in the QCM sensor container by an insulating adhesive. Also, the circuit part electrically connected to the signal output terminal of the micromass measuring sensor element is built in the QCM sensor container in the vicinity of the micromass measuring sensor element. Further, the micromass measuring sensor (QCM sensor) container is composed of glass, quartz, a plastic or a ceramic and the signal input/output terminal of the circuit part in the QCM sensor container is extended to the outer surface of the container. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

本発明は、液相用のQCMセンサー容器の内部に回路が組み込まれた信頼性の高い微少質量測定用センサーに関する。           The present invention relates to a highly reliable sensor for measuring a minute mass, in which a circuit is incorporated in a liquid phase QCM sensor container.

従来より 水晶振動子を使用した微少質量測定用センサー素子(QCM:Quartz Crystal Microbalance センサー素子)は水晶の厚みすべり振動を利用しており、水晶基板の表面に形成される金属膜材料には、水晶基板との密着性を考慮してクロム(Cr)、ニッケルクロム(NiCr)、チタン(Ti)などが使用されているが、このような微少質量測定用センサー素子全体を溶液中に浸漬させた場合、溶液の抵抗力により先述の振動が抑制されて微少質量測定用センサー素子として使用することが出来なくなる。そこで溶液の反応を検出せず液相に接触させない側の水晶基板の金属膜を気相状態とすることにより微少質量測定用センサーを溶液中に浸漬しても振動を検出することが可能となる。           Conventionally, a sensor element for measuring a minute mass (QCM: Quartz Crystal Microbalance sensor element) using a crystal resonator has utilized a thickness shear vibration of crystal, and a metal film material formed on a surface of a crystal substrate includes a crystal film. Chromium (Cr), nickel chrome (NiCr), titanium (Ti), etc. are used in consideration of adhesion to the substrate. When the entire sensor element for measuring such a small mass is immersed in the solution The vibration described above is suppressed by the resistance force of the solution and cannot be used as a sensor element for measuring a minute mass. Therefore, it is possible to detect vibration even if the sensor for measuring a minute mass is immersed in the solution by setting the metal film of the quartz substrate on the side not contacting the liquid phase without detecting the reaction of the solution to the gas phase state. .

水晶基板の片面の金属膜を液相に接触させずに気相状態に保つには、溶液の進入を防ぐために微少質量測定用センサー素子の側面の全周縁部を接着剤などで固定して塞がなければならない。一般的には微少質量測定用センサー素子の振動への影響を出来うるだけ小さなものとするために、接着の応力の小さなシリコン系の絶縁性接着剤が使用されることが多く見受けられる。           In order to keep the metal film on one side of the quartz substrate in a gas phase without being in contact with the liquid phase, the entire periphery of the side surface of the sensor element for measuring the minute mass is fixed with an adhesive or the like to prevent the solution from entering. There must be. In general, in order to make the influence on vibration of the sensor element for measuring a minute mass as small as possible, a silicon-based insulating adhesive having a small bonding stress is often used.

また、測定される反応物が水晶振動子の表面に付着・乖離する際の微少な重量変化を水晶振動子の周波数変化としてとらえるが、この反応物が水晶振動子の表面に付着するために、基本的には微少質量測定用センサー(以下QCMセンサーとも呼ぶ)は使い捨ての方式が採用されており、その解析精度においては、温度制御の安定度や単位重量当たりの周波数変化量が大きい高周波帯での測定が有効とされているが、ノイズの影響により希望する測定精度が得られない場合があった。           In addition, a minute change in weight when the reactant to be measured adheres to or separates from the surface of the crystal unit is considered as a frequency change of the crystal unit, but because this reactant attaches to the surface of the crystal unit, Basically, a sensor for measuring minute mass (hereinafter also referred to as a QCM sensor) uses a disposable method. In terms of analysis accuracy, the stability of temperature control and the frequency change amount per unit weight are large. However, there are cases where the desired measurement accuracy cannot be obtained due to the influence of noise.

このようにQCMセンサーを用いた測定においてノイズの影響で希望する測定精度が得られない場合があるために、発振器などを含む解析装置とQCMセンサー素子とは多くの場合、ソケットなどの接続具を介して電気的に接続する。その一方でQCM解析装置は生態化学反応による水晶振動子表面への反応物の付着・乖離の状態を計測することが目的であり、温度による反応の形態が個々に異なることから高精度に温度制御された環境下での測定が求められる。           In this way, in the measurement using the QCM sensor, the desired measurement accuracy may not be obtained due to the influence of noise. Therefore, in many cases, the analysis device including the oscillator and the QCM sensor element are connected with a connector such as a socket. Through the electrical connection. On the other hand, the purpose of the QCM analyzer is to measure the state of attachment / dissociation of reactants on the surface of the quartz crystal due to ecochemical reactions. Measurement in a controlled environment is required.

特開2001−153777号公報JP 2001-153777 A 特開平11−14525号公報Japanese Patent Laid-Open No. 11-14525

なお、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 did not find 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.

しかしながら、温度制御された液相系の反応相のなかに先述のソケット部を浸すことは当然ながら電気的短絡(ショート)を起こすために困難であり、またQCMセンサーと解析装置までの中間に位置する回路部である発振回路までの物理的距離が長い場合、温度制御などに起因する電気的ノイズの影響を受けてQCMセンサーを用いた測定精度を著しく低下させてしまうおそれがあった。           However, it is of course difficult to immerse the socket part in the temperature-controlled liquid phase reaction phase because an electrical short circuit is caused, and it is located between the QCM sensor and the analyzer. When the physical distance to the oscillation circuit, which is a circuit unit, is long, there is a possibility that the measurement accuracy using the QCM sensor may be significantly reduced due to the influence of electrical noise caused by temperature control or the like.

本発明は、以上のような技術的背景のもとでなされたものであり、従がってその目的は、液相用のQCMセンサーの容器内部に回路が組み込まれた信頼性の高い微少質量測定用センサー(QCMセンサー)を提供することである。           The present invention has been made under the technical background as described above. Accordingly, the object of the present invention is to provide a highly reliable small mass in which a circuit is incorporated in a container of a liquid phase QCM sensor. It is to provide a sensor for measurement (QCM sensor).

上記の目的を達成するために本発明は、QCMセンサー容器に微少質量測定用センサー素子が、その一方の主電極面だけが露出し、かつ微少質量測定用センサー素子側面で絶縁性接着剤によりQCMセンサー容器内に載置され、微少質量測定用センサー素子近傍に微少質量測定用センサー素子の信号出力端と電気的に接続した回路部をQCMセンサー容器に内蔵することを特徴とする           In order to achieve the above object, the present invention provides a QCM sensor container in which a sensor element for measuring a minute mass is exposed by QCM using an insulating adhesive on the side of the sensor element for measuring a minute mass with only one main electrode surface exposed. A QCM sensor container includes a circuit unit that is placed in the sensor container and is electrically connected to the signal output terminal of the sensor element for measuring the minute mass in the vicinity of the sensor element for measuring the minute mass.

また、微少質量測定用センサー(QCMセンサー)容器がガラス、水晶、プラスチック、若しくはセラミックからなることを特徴とする。           Further, the sensor for measuring a minute mass (QCM sensor) is made of glass, crystal, plastic, or ceramic.

また、QCMセンサー容器内部の回路部の信号入出力端がこの容器の外面に延在されることを特徴とする。           Further, the signal input / output terminal of the circuit part inside the QCM sensor container extends to the outer surface of the container.

本発明の微少質量測定用センサー(QCMセンサー)によれば、水晶振動子を用いた微少質量測定用センサー素子から発振回路といった回路部までの物理的距離を短くすることが出来、外的ノイズによる影響を著しく軽減することが出来る。           According to the sensor for measuring a minute mass (QCM sensor) according to the present invention, the physical distance from the sensor element for measuring a minute mass using a crystal resonator to a circuit unit such as an oscillation circuit can be shortened. The impact can be significantly reduced.

また、本発明の微少質量測定用センサーによれば、微少質量測定用センサー素子である水晶振動子と回路部を同じ容器内で、高精度に制御された温度環境下で使用することが出来るために、微少質量測定用センサーの測定精度を著しく向上することが出来る。           In addition, according to the sensor for measuring a minute mass of the present invention, the crystal unit that is the sensor element for measuring the minute mass and the circuit unit can be used in the same container in a temperature environment controlled with high accuracy. In addition, the measurement accuracy of the sensor for measuring minute mass can be remarkably improved.

以下に図面を参照しながら本発明の実施の一形態について説明する。なお、各図においての同一の符号は同じ対象を示すものとする。           Hereinafter, an embodiment of the present invention will be described with reference to the drawings. In addition, the same code | symbol in each figure shall show the same object.

図1は本発明の微少質量測定用センサー12(QCMセンサー12)を側面方向からみた概略の側面断面図である。即ち、水晶基板1の表面に金属膜2を形成した水晶振動子を用いた微少質量測定用センサー素子4であり、微少質量測定用センサー容器5にQCMセンサー素子4が、その一方の主電極面6だけが液相側に露出し、かつQCMセンサー素子側面7で絶縁性接着剤8により微少質量測定用センサー容器5内に載置され、QCMセンサー素子4のすぐ近傍にQCMセンサー素子4の信号出力端と電気的に接続した回路部10をQCMセンサー容器5に内蔵した構造のものである。本発明のQCMセンサー12によれば、水晶振動子を用いた微少質量測定用センサー(QCMセンサー)素子4から発振回路といった回路部10までの物理的距離を従来に比べて非常に短くすることが出来、外的ノイズによる影響を著しく軽減することが出来る。           FIG. 1 is a schematic side sectional view of a sensor 12 for measuring a minute mass (QCM sensor 12) of the present invention as viewed from the side. That is, it is a sensor element 4 for measuring a minute mass using a quartz crystal resonator in which a metal film 2 is formed on the surface of a quartz substrate 1, and a QCM sensor element 4 is disposed on a sensor container 5 for measuring a minute mass, on one main electrode surface. 6 is exposed to the liquid phase side, and is placed in the sensor container 5 for measuring the minute mass by the insulating adhesive 8 on the side surface 7 of the QCM sensor element, and the signal of the QCM sensor element 4 is immediately adjacent to the QCM sensor element 4. The circuit unit 10 electrically connected to the output end is built in the QCM sensor container 5. According to the QCM sensor 12 of the present invention, the physical distance from the minute mass measurement sensor (QCM sensor) element 4 using a crystal resonator to the circuit unit 10 such as an oscillation circuit can be made much shorter than before. And the effect of external noise can be significantly reduced.

図2は本発明のQCMセンサー12を微少質量測定用センサー素子4の露出した一方の主面方向からみた概略の上面模式図である。図示されたような形状のために、左右に張り出した部分に作業者が指を掛けてコネクターへの本発明のQCMセンサー12の抜き差しが著しく簡便となるといった効果を奏するものである。また、本発明のQCMセンサー12の筒部の空洞は、微少質量測定用センサー素子4の片面の金属膜2を液相に接触させずに気相状態に保ち、液相の溶液進入を防ぐためにQCMセンサー素子側面7の全周縁部を接着剤などで固定して塞ぐ必要があるが、QCMセンサー素子側面7において絶縁性接着剤8を用いて微少質量測定用センサー容器5内に固定、載置する際に絶縁性接着剤8から発生するガスを抜くために設けられたものである。           FIG. 2 is a schematic top view of the QCM sensor 12 of the present invention as viewed from the direction of one main surface where the sensor element 4 for measuring a minute mass is exposed. Due to the shape as shown in the figure, an effect is obtained in that an operator puts his / her finger on the left and right protruding portions and the insertion / removal of the QCM sensor 12 of the present invention into the connector is remarkably simplified. In addition, the hollow of the cylindrical portion of the QCM sensor 12 of the present invention is to keep the metal film 2 on one side of the sensor element 4 for measuring a minute mass in a gas phase without contacting the liquid phase, and to prevent the liquid phase from entering the solution. Although it is necessary to fix and close the entire periphery of the side surface 7 of the QCM sensor element with an adhesive or the like, the QCM sensor element side surface 7 is fixed and placed in the sensor container 5 for measuring a minute mass using the insulating adhesive 8. This is provided to remove the gas generated from the insulating adhesive 8 during the process.

図3は本発明のQCMセンサー12にコネクター14を接続した様子を示す微少質量測定用センサー素子4の露出した一方の主面方向からみた概略の上面模式図である。QCMセンサー12を用いた測定作業の効率化を図るために、本発明のQCMセンサー12では、QCMセンサー容器5内部の回路部10の信号入出力端9が容器5の外面に延在されており、このために迅速なQCMセンサー12のコネクター14との着脱が可能な構造となっている。           FIG. 3 is a schematic top view of the micromass measuring sensor element 4 as viewed from the direction of one exposed main surface, showing the connector 14 connected to the QCM sensor 12 of the present invention. In the QCM sensor 12 of the present invention, the signal input / output end 9 of the circuit unit 10 inside the QCM sensor container 5 is extended to the outer surface of the container 5 in order to improve the efficiency of measurement work using the QCM sensor 12. For this reason, the QCM sensor 12 can be quickly attached to and detached from the connector 14.

図4は従来のQCMセンサー素子に水晶振動子を用いた測定系の構成と比較した本発明のQCMセンサー素子に水晶振動子を用いた測定系の構成を示す模式図である。本発明によれば、QCMセンサー素子4である水晶振動子と回路部10を同じ容器内で、この図4の模式図に示されるように高精度に制御された温度環境下で使用することが出来るために、測定精度を著しく向上することが出来る。           FIG. 4 is a schematic diagram showing the configuration of a measurement system using a crystal resonator in the QCM sensor element of the present invention compared with the configuration of a measurement system using a crystal resonator in a conventional QCM sensor element. According to the present invention, it is possible to use the crystal resonator which is the QCM sensor element 4 and the circuit unit 10 in the same container in a temperature environment controlled with high accuracy as shown in the schematic diagram of FIG. Therefore, the measurement accuracy can be remarkably improved.

図5は従来の微少質量測定用センサー素子4単体を側面方向からみた概略の側面断面図である。           FIG. 5 is a schematic side sectional view of a conventional sensor element 4 for measuring a minute mass as viewed from the side.

図6は従来の微少質量測定用センサー素子4単体を斜め上面方向からみた概略の上面斜視図である。従来は、この図6に示されるような微少質量測定用センサー素子4を用いたQCMセンサー12単体と解析装置までの中間に位置する回路部10である発振回路までの物理的距離が長い場合、温度制御などに起因する電気的ノイズや周囲の温度の影響を受けてQCMセンサー12を用いた測定精度を著しく低下させてしまうおそれがあった。           FIG. 6 is a schematic top perspective view of a conventional sensor element 4 for measuring a small mass as seen from an oblique top surface direction. Conventionally, when the physical distance to the oscillation circuit which is the circuit unit 10 located in the middle between the single QCM sensor 12 using the sensor element 4 for measuring a minute mass as shown in FIG. There is a possibility that the measurement accuracy using the QCM sensor 12 may be remarkably lowered under the influence of electrical noise caused by temperature control or the like and the ambient temperature.

本発明の微少質量測定用センサー(QCMセンサー)を側面方向からみた概略の側面断面図である。It is the side sectional view of the outline which looked at the sensor for minute mass measurement (QCM sensor) of the present invention from the side. 本発明のQCMセンサーを微少質量測定用センサー素子の露出した一方の主面方向からみた概略の上面模式図である。FIG. 3 is a schematic top view of the QCM sensor of the present invention as viewed from the direction of one main surface where a sensor element for measuring a minute mass is exposed. 本発明のQCMセンサーにコネクターを接続した様子を示す微少質量測定用センサー素子の露出した一方の主面方向からみた概略の上面模式図である。It is a schematic top view as seen from the direction of one exposed main surface of the sensor element for measuring a minute mass, showing a state where the connector is connected to the QCM sensor of the present invention. 従来のQCMセンサーを用いた測定系の構成と比較した本発明のQCMセンサーを用いた測定系の構成を示す概略図である。It is the schematic which shows the structure of the measurement system using the QCM sensor of this invention compared with the structure of the measurement system using the conventional QCM sensor. 従来の微少質量測定用センサー素子単体を側面方向からみた概略の側面断面図である。It is the general side sectional view which looked at the conventional sensor element for micro mass measurement from the side direction. 従来の微少質量測定用センサー素子単体を斜め上面方向からみた概略の上面斜視図である。It is the general | schematic upper surface perspective view which looked at the conventional sensor element for micro mass measurement from the diagonal upper surface direction.

符号の説明Explanation of symbols

1 水晶基板
2 金属膜
4 微少質量測定用センサー素子
5 微少質量測定用センサー容器
6 主電極面
7 微少質量測定用センサー素子側面
8 絶縁性接着剤
9 信号入出力端
10 回路部
11 微少質量測定用センサー素子容器の外面
12 微少質量測定用センサー
14 コネクター
DESCRIPTION OF SYMBOLS 1 Crystal substrate 2 Metal film 4 Sensor element 5 for minute mass measurement Sensor container 6 for minute mass measurement Main electrode surface 7 Sensor element side surface 8 for minute mass measurement Insulating adhesive 9 Signal input / output terminal 10 Circuit unit 11 For minute mass measurement External surface 12 of sensor element container Sensor 14 for measuring minute mass Connector

Claims (3)

水晶基板の表面に金属膜を形成して成る水晶振動子を用いた微少質量測定用センサー素子において、
微少質量測定用センサー容器に該微少質量測定用センサー素子が、その一方の主電極面だけが露出し、かつ該微少質量測定用センサー素子側面で絶縁性接着剤により該微少質量測定用センサー容器内に載置され、該微少質量測定用センサー素子近傍に該微少質量測定用センサー素子の信号出力端と電気的に接続した回路部を該微少質量測定用センサー容器に内蔵することを特徴とする微少質量測定用センサー。
In a sensor element for measuring micro mass using a crystal resonator formed by forming a metal film on the surface of a quartz substrate,
Only one main electrode surface of the sensor element for measuring the minute mass is exposed to the sensor container for measuring the minute mass, and the inside of the sensor container for measuring the minute mass with an insulating adhesive on the side of the sensor element for measuring the minute mass And a circuit part electrically connected to the signal output terminal of the sensor element for measuring the minute mass in the vicinity of the sensor element for measuring the minute mass is incorporated in the sensor container for measuring the minute mass Sensor for mass measurement.
該微少質量測定用センサー容器がガラス、水晶、プラスチック、若しくはセラミックから成ることを特徴とする請求項1に記載の微少質量測定用センサー。           2. The sensor for measuring micro mass according to claim 1, wherein the sensor container for measuring micro mass is made of glass, quartz, plastic, or ceramic. 該微少質量測定用センサー容器内部の回路部の信号入出力端が該容器の外面に延在されることを特徴とする請求項1に記載の微少質量測定用センサー。           2. The sensor for measuring a minute mass according to claim 1, wherein a signal input / output terminal of a circuit portion inside the sensor container for measuring a minute mass extends to an outer surface of the container.
JP2005192726A 2005-06-30 2005-06-30 Sensor for measuring micromass Pending JP2007010523A (en)

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