JP2010216895A - Micro mass sensor - Google Patents
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本発明は、作製が容易であると共に耐熱性や耐久性に優れた湿度センサやアルコールセンサとなる微量質量センサに関する。 The present invention relates to a trace mass sensor that can be easily manufactured and is a humidity sensor or an alcohol sensor that is excellent in heat resistance and durability.
従来、水晶振動子等の固有振動数や共振周波数の変化を利用した湿度センサが知られている。例えば、特許文献１には、単結晶シリコンや水晶等の基板上に、カチオン性高分子膜とアニオン性高分子膜とが積層された湿度センサが提案されている。この湿度センサは、高分子膜に吸着した水分子の微量質量を、水晶振動子等の固有振動数や共振周波数の変化から検出して湿度を測定するものである。 Conventionally, a humidity sensor that utilizes changes in the natural frequency or resonance frequency of a crystal resonator or the like is known. For example, Patent Document 1 proposes a humidity sensor in which a cationic polymer film and an anionic polymer film are laminated on a substrate such as single crystal silicon or quartz. This humidity sensor measures humidity by detecting a minute mass of water molecules adsorbed on a polymer film from changes in the natural frequency or resonance frequency of a crystal resonator or the like.
上記従来の技術には、以下の課題が残されている。
すなわち、特許文献１に示す湿度センサでは、感応膜として高分子膜を採用しているため、耐熱性や耐久性に欠け、高温環境での検知が困難であるという不都合があった。また、高分子膜を積層する必要があるため、成膜工程が多く、製造コストが増大してしまう問題もあった。
The following problems remain in the conventional technology.
That is, the humidity sensor shown in Patent Document 1 employs a polymer film as a sensitive film, and thus has a disadvantage that it lacks heat resistance and durability and is difficult to detect in a high temperature environment. Moreover, since it is necessary to laminate | stack a polymer film, there existed a problem that there were many film-forming processes and manufacturing cost increased.
本発明は、前述の課題に鑑みてなされたもので、耐熱性や耐久性に優れ、さらに作製が容易で製造コストの低い湿度センサ等の微量質量センサを提供することを目的とする。 The present invention has been made in view of the above-described problems, and an object of the present invention is to provide a trace mass sensor such as a humidity sensor that has excellent heat resistance and durability, is easy to manufacture, and is low in manufacturing cost.
本発明は、前記課題を解決するために以下の構成を採用した。すなわち、本発明の微量質量センサは、基板と、該基板上に成膜された金属の電極膜と、該電極膜上に成膜された感応膜と、を備え、該感応膜が、繊維表面を酸化処理して親水化した微細炭素繊維で形成されていることを特徴とする。 The present invention employs the following configuration in order to solve the above problems. That is, the trace mass sensor of the present invention includes a substrate, a metal electrode film formed on the substrate, and a sensitive film formed on the electrode film, and the sensitive film is a fiber surface. It is characterized by being formed of fine carbon fibers hydrophilized by oxidizing.
この微量質量センサでは、感応膜が、繊維表面を酸化処理して親水化した微細炭素繊維で形成されているので、親水化されて親水基を有する微細炭素繊維によって、水分子やＯＨ基（ヒドロキシ基）を有するアルコール等を吸着・脱着して、高感度に水分子やアルコールを検知可能であると共に、高分子膜の感応膜に比べて高い耐熱性及び耐久性を有している。 In this trace mass sensor, the sensitive membrane is formed of fine carbon fibers that are hydrophilized by oxidizing the fiber surface, so that water molecules and OH groups (hydroxyl) are made by the fine carbon fibers that are hydrophilic and have hydrophilic groups. It is possible to detect water molecules and alcohol with high sensitivity by adsorbing and desorbing alcohol having a base), and has higher heat resistance and durability than a sensitive film of a polymer film.
また、本発明の微量質量センサは、前記感応膜が、前記微細炭素繊維の分散液を前記電極膜上に塗布して乾燥させた膜であることを特徴とする。
すなわち、この微量質量センサでは、感応膜が、微細炭素繊維の分散液を電極膜上に塗布して乾燥させた膜であるので、焼成や積層等の工程が不要で、作製が容易であり、製造コストを低く抑えることができる。
In the trace mass sensor of the present invention, the sensitive film is a film obtained by applying and drying the fine carbon fiber dispersion on the electrode film.
That is, in this trace mass sensor, since the sensitive film is a film obtained by applying a fine carbon fiber dispersion liquid on the electrode film and drying it, steps such as firing and lamination are unnecessary, and the production is easy. Manufacturing costs can be kept low.
また、本発明の微量質量センサは、前記微細炭素繊維が、カーボンナノチューブであることを特徴とする。
すなわち、この微量質量センサでは、微細炭素繊維が、カーボンナノチューブであるので、ナノオーダーの繊維が互いに絡み合って、より高い耐久性及び検出感度を有する感応膜が得られる。
Moreover, the trace mass sensor of the present invention is characterized in that the fine carbon fiber is a carbon nanotube.
That is, in this minute mass sensor, since the fine carbon fibers are carbon nanotubes, nano-order fibers are entangled with each other, and a sensitive film having higher durability and detection sensitivity can be obtained.
また、本発明の微量質量センサは、前記基板が、ランガサイト単結晶で形成されていることを特徴とする。
すなわち、この微量質量センサでは、基板が、耐熱性に優れたランガサイト単結晶で形成されているので、ランガサイト振動子となる基板に上記感応膜が形成されて、さらに高い耐熱性及び耐久性を得ることができる。
Moreover, the trace mass sensor of the present invention is characterized in that the substrate is formed of a langasite single crystal.
That is, in this trace mass sensor, since the substrate is formed of a langasite single crystal having excellent heat resistance, the above-mentioned sensitive film is formed on the substrate to be a langasite vibrator, and further higher heat resistance and durability. Can be obtained.
また、本発明の微量質量センサは、前記感応膜に水分子を吸着させて水分を検出する湿度センサであることを特徴とする。
また、本発明の微量質量センサは、前記感応膜にアルコールを吸着させてアルコールを検出するアルコールセンサであることを特徴とする。
The trace mass sensor of the present invention is a humidity sensor that detects water by adsorbing water molecules to the sensitive film.
Moreover, the trace mass sensor of the present invention is an alcohol sensor that detects alcohol by adsorbing alcohol to the sensitive film.
本発明によれば、以下の効果を奏する。
すなわち、本発明に係る微量質量センサによれば、感応膜が、繊維表面を酸化処理して親水化した微細炭素繊維で形成されているので、高い耐熱性及び耐久性を有して高感度に水分子やアルコールを検知可能である。さらに、感応膜を、微細炭素繊維のスラリー又はペーストを電極膜上に塗布して乾燥させた膜とすることで、作製が容易であり、製造コストを低く抑えることができる。したがって、本発明は、高温環境でも使用可能であり、低コストな湿度センサやアルコールセンサとして好適である。
The present invention has the following effects.
That is, according to the micro-mass sensor according to the present invention, the sensitive film is formed of fine carbon fibers obtained by hydrophilizing the fiber surface by oxidation, so that it has high heat resistance and durability and high sensitivity. It can detect water molecules and alcohol. Furthermore, by making the sensitive film a film obtained by applying a fine carbon fiber slurry or paste onto the electrode film and drying it, the production is easy and the manufacturing cost can be kept low. Therefore, the present invention can be used in a high temperature environment and is suitable as a low-cost humidity sensor or alcohol sensor.
以下、本発明に係る微量質量センサの一実施形態を、図１及び図２を参照しながら説明する。なお、以下の説明に用いる各図面では、各部材を認識可能又は認識容易な大きさとするために縮尺を適宜変更している。 Hereinafter, an embodiment of a minute mass sensor according to the present invention will be described with reference to FIGS. 1 and 2. In each drawing used in the following description, the scale is appropriately changed so that each member can be recognized or easily recognized.
本実施形態の微量質量センサ１は、図１及び図２に示すように、感応膜２に水分子を吸着させて水分を検出する湿度センサ又は感応膜２にアルコールを吸着させてアルコールを検出するアルコールセンサであって、基板３と、該基板３の表裏面上に成膜された一対の電極膜４と、これら電極膜４上に成膜された一対の上記感応膜２と、を備えている。 As shown in FIGS. 1 and 2, the trace mass sensor 1 according to the present embodiment detects alcohol by adsorbing alcohol to the humidity sensor or the sensitive film 2 that adsorbs water molecules to the sensitive film 2 and detects moisture. An alcohol sensor, comprising a substrate 3, a pair of electrode films 4 formed on the front and back surfaces of the substrate 3, and a pair of the sensitive films 2 formed on the electrode films 4. Yes.
上記基板３は、ランガサイト単結晶で形成されている。
なお、ランガサイト（Ｌａｎｇａｓｉｔｅ：Ｌａ３Ｇａ５ＳｉＯ１４）単結晶は、キュリー温度が水晶よりも高く高温領域で使用可能な材料であって、温度による弾性波伝搬速度、周波数の変化率が小さく、圧電性の大小を表す電気機械結合係数（電気エネルギーと機械エネルギーの相互変換効率を示す係数）が水晶に比べて大きいことから、圧電デバイス用や弾性波デバイス用の基板材料として優れている。
The substrate 3 is formed of a langasite single crystal.
Note that the Langasite (La 3 Ga 5 SiO 14 ) single crystal is a material that has a Curie temperature higher than that of quartz and can be used in a high temperature region, and has a small elastic wave propagation speed and frequency change rate due to temperature. Since the electromechanical coupling coefficient (coefficient indicating the mutual conversion efficiency between electric energy and mechanical energy) representing the magnitude of piezoelectricity is larger than that of quartz, it is excellent as a substrate material for piezoelectric devices and acoustic wave devices.
上記感応膜２は、繊維表面を酸化処理して親水化した微細炭素繊維で形成されている。また、感応膜２は、微細炭素繊維の分散液を電極膜４上に塗布して乾燥させた膜である。また、上記微細炭素繊維は、カーボンナノチューブである。 The sensitive film 2 is formed of fine carbon fibers obtained by hydrophilizing the fiber surface by oxidation treatment. The sensitive film 2 is a film obtained by applying a fine carbon fiber dispersion on the electrode film 4 and drying it. The fine carbon fiber is a carbon nanotube.
この感応膜２の成膜方法を説明すると、まず、カーボンナノチューブの繊維表面を酸化処理して親水性を付与する。この酸化処理は、例えばカーボンナノチューブに硫酸などの硫黄含有強酸を添加し、硝酸などの酸化剤を加え、このスラリーを加熱しながら攪拌した後、濾過し、残留する酸を洗浄して除去する方法が採用される。この酸化処理により、カルボニル基やカルボキシル基あるいはニトロ基などの極性官能基が形成されて親水化される。 The film forming method of the sensitive film 2 will be described. First, the fiber surface of the carbon nanotube is oxidized to impart hydrophilicity. In this oxidation treatment, for example, a sulfur-containing strong acid such as sulfuric acid is added to carbon nanotubes, an oxidizing agent such as nitric acid is added, the slurry is stirred while heating, and then filtered, and the remaining acid is washed and removed. Is adopted. By this oxidation treatment, a polar functional group such as a carbonyl group, a carboxyl group, or a nitro group is formed and hydrophilized.
次に、この親水化させたカーボンナノチューブをエタノールの溶媒に例えば５ｗｔ％の濃度で入れて、カーボンナノチューブ分散液を作製する。なお、カーボンナノチューブは、表面を酸化処理して親水化させているので、分散剤を使用しなくても溶媒中で良好な分散状態を維持することができる。 Next, this hydrophilic carbon nanotube is placed in an ethanol solvent at a concentration of, for example, 5 wt% to prepare a carbon nanotube dispersion. In addition, since the surface of the carbon nanotube is hydrophilized by oxidation treatment, a good dispersion state can be maintained in the solvent without using a dispersant.
このカーボンナノチューブ分散液を基板３の表裏面上に塗布し、乾燥機で例えば１００℃５分の条件で乾燥させることで、実用強度のある感応膜２が成膜できる。本実施形態では、約１０μｍの膜厚で感応膜２が形成されている。
なお、カーボンナノチューブ分散液に結着剤を加えてスラリー又はペーストにして、上記塗布を行っても構わない。結着剤としては、例えばポリフッ化ビニリデン（ＰＶｄＦ）、カルボキシメチルセルロース（ＣＭＣ）などが採用可能である。
The carbon nanotube dispersion liquid is applied onto the front and back surfaces of the substrate 3 and dried with a dryer at, for example, 100 ° C. for 5 minutes, whereby the sensitive film 2 having practical strength can be formed. In the present embodiment, the sensitive film 2 is formed with a film thickness of about 10 μm.
The coating may be performed by adding a binder to the carbon nanotube dispersion to form a slurry or paste. As the binder, for example, polyvinylidene fluoride (PVdF), carboxymethyl cellulose (CMC) and the like can be employed.
上記電極膜４は、金属膜であって、例えば表面側がＡｕで形成されていると共に裏面側がＣｒで形成されている。
この微量質量センサ１では、振動モードとして例えばランガサイト振動子となる基板３の厚み方向の上下表面がそれぞれ対向方向にすべるような振動モードである厚みすべり振動を利用して、数ＭＨｚ〜数百ＭＨｚ帯域の周波数をカバーして共振周波数の変化を検出可能である。
The electrode film 4 is a metal film. For example, the front surface side is made of Au and the back surface side is made of Cr.
In this trace mass sensor 1, several MHz to several hundreds are utilized by utilizing thickness shear vibration, which is a vibration mode in which the upper and lower surfaces in the thickness direction of the substrate 3 serving as a Langasite vibrator, for example, slide in opposite directions as vibration modes. A change in resonance frequency can be detected by covering the frequency in the MHz band.
このように本実施形態の微量質量センサ１では、感応膜２が、繊維表面を酸化処理して親水化した微細炭素繊維で形成されているので、親水化されて親水基を有する微細炭素繊維によって、水分子やＯＨ基（ヒドロキシ基）を有するアルコール等を吸着・脱着して、高感度に水分子やアルコールを検知可能であると共に、高分子膜の感応膜に比べて高い耐熱性及び耐久性を有している。 Thus, in the trace mass sensor 1 of the present embodiment, the sensitive film 2 is formed of fine carbon fibers that are hydrophilized by oxidizing the fiber surface. Therefore, the fine carbon fibers that are hydrophilic and have hydrophilic groups are used. Adsorbs and desorbs water molecules and alcohols with OH groups (hydroxy groups) to detect water molecules and alcohol with high sensitivity, and has higher heat resistance and durability compared to polymer membrane sensitive membranes. have.
特に、微細炭素繊維が、カーボンナノチューブであるので、ナノオーダーの繊維が互いに絡み合って、より高い耐久性及び検出感度を有する感応膜が得られる。
さらに、基板３が、耐熱性に優れたランガサイト単結晶で形成されているので、ランガサイト振動子となる基板３に上記感応膜２が形成されて、さらに高い耐熱性及び耐久性を得ることができる。例えば、５００℃の高温環境でも湿度センサ又はアルコールセンサとして機能可能である。
In particular, since the fine carbon fibers are carbon nanotubes, nano-order fibers are entangled with each other, and a sensitive film having higher durability and detection sensitivity can be obtained.
Furthermore, since the substrate 3 is formed of a langasite single crystal having excellent heat resistance, the sensitive film 2 is formed on the substrate 3 to be a langasite vibrator to obtain higher heat resistance and durability. Can do. For example, it can function as a humidity sensor or an alcohol sensor even in a high temperature environment of 500 ° C.
また、感応膜２が、微細炭素繊維の分散液を電極膜４上に塗布して乾燥させた膜であるので、焼成や積層等の工程が不要で、作製が容易であり、製造コストを低く抑えることができる。 In addition, since the sensitive film 2 is a film obtained by applying a fine carbon fiber dispersion on the electrode film 4 and drying it, steps such as firing and lamination are not required, and the production is easy and the manufacturing cost is low. Can be suppressed.
次に、本発明に係る微量質量センサを、上記実施形態に基づいて実際に作製した実施例により評価した結果を具体的に説明する。 Next, the result of having evaluated the trace mass sensor based on this invention by the Example actually produced based on the said embodiment is demonstrated concretely.
まず、上記本実施形態の微量質量センサを実際に作製した実施例を湿度センサとして使用して、湿度感応性として経過時間に対する共振周波数について評価した結果を、図３に示す。この評価では、測定雰囲気の湿度を３０分毎に変化させたときの共振周波数を調べた。また、測定雰囲気の湿度は、４７％ＲＨ、５７％ＲＨ、６７％ＲＨ、７７％ＲＨの順に変化させている。
この評価結果から、本実施例の微量質量センサ（湿度センサ）では、時間と共に変化する湿度に応じて高い応答性を有して共振周波数が変化していることがわかる。
First, FIG. 3 shows the result of evaluating the resonance frequency with respect to the elapsed time as humidity sensitivity using an example in which the minute mass sensor of the present embodiment was actually manufactured as a humidity sensor. In this evaluation, the resonance frequency was examined when the humidity of the measurement atmosphere was changed every 30 minutes. The humidity of the measurement atmosphere is changed in the order of 47% RH, 57% RH, 67% RH, and 77% RH.
From this evaluation result, it can be seen that in the trace mass sensor (humidity sensor) of this example, the resonance frequency changes with high responsiveness according to the humidity that changes with time.
また、本実施例の微量質量センサ（湿度センサ）について、湿度に対する共振周波数の平均値について評価した結果を、図４に示す。この評価結果から、本実施例の微量質量センサ（湿度センサ）では、湿度が高いほど共振周波数が低くなることがわかる。このように本実施例の微量質量センサは、湿度センサとして十分な湿度感応性を有していることわかる。 In addition, FIG. 4 shows the result of evaluating the average value of the resonance frequency with respect to the humidity of the trace mass sensor (humidity sensor) of this example. From this evaluation result, it can be seen that in the trace mass sensor (humidity sensor) of this example, the higher the humidity, the lower the resonance frequency. Thus, it can be seen that the trace mass sensor of the present example has sufficient humidity sensitivity as a humidity sensor.
次に、本実施例の微量質量センサをアルコールセンサとして使用して、アルコール感応性として経過時間に対する共振周波数の変化について評価した結果を、図５に示す。この評価では、密閉容器内に微量質量センサ（アルコールセンサ）を設置し、そこへ各種アルコールを１滴投入したときの共振周波数の変化を測定した。なお、測定に使用したアルコールは、メタノール（ＭｅＯＨ）、エタノール（ＥｔＯＨ）、イソプロパノール（ＩＰＡ）である。 Next, FIG. 5 shows the results of evaluating the change in resonance frequency with respect to elapsed time as alcohol sensitivity using the trace mass sensor of this example as an alcohol sensor. In this evaluation, a minute mass sensor (alcohol sensor) was installed in an airtight container, and the change in resonance frequency was measured when one drop of various alcohols was added thereto. In addition, the alcohol used for the measurement is methanol (MeOH), ethanol (EtOH), and isopropanol (IPA).
この評価結果から、本実施例の微量質量センサ（アルコールセンサ）では、アルコールの滴下後に大きく共振周波数が変化し、その後、アルコールが拡散して一定の濃度に安定したことを示すように、共振周波数の変化が一定のレベルに落ち着いていることがわかる。 From this evaluation result, in the trace mass sensor (alcohol sensor) of this example, the resonance frequency greatly changes after the alcohol is dropped, and then the alcohol is diffused and the resonance frequency is stabilized to indicate that the concentration is stable. It can be seen that the change in is settled to a certain level.
また、本実施例の微量質量センサ（アルコールセンサ）について、エタノール濃度に対する共振周波数の変化について評価した結果を、図６に示す。この評価結果から、本実施例の微量質量センサ（アルコールセンサ）では、エタノール濃度が高いほど共振周波数が低くなることがわかる。このように本実施例の微量質量センサは、アルコールセンサとして十分なアルコール感応性を有していることわかる。 Moreover, the result of having evaluated the change of the resonant frequency with respect to ethanol concentration about the trace mass sensor (alcohol sensor) of a present Example is shown in FIG. From this evaluation result, it can be seen that, in the trace mass sensor (alcohol sensor) of this example, the higher the ethanol concentration, the lower the resonance frequency. Thus, it can be seen that the trace mass sensor of this example has sufficient alcohol sensitivity as an alcohol sensor.
なお、本発明の技術範囲は上記実施形態及び実施例に限定されるものではなく、本発明の趣旨を逸脱しない範囲において種々の変更を加えることが可能である。
例えば、上記実施形態では、ランガサイト単結晶で形成した基板を採用しているが、同様に高温での特性に優れたランガテイト単結晶などの他のランガサイト系単結晶で形成した基板を使用しても構わない。
The technical scope of the present invention is not limited to the above-described embodiments and examples, and various modifications can be made without departing from the spirit of the present invention.
For example, in the above embodiment, a substrate formed of a langasite single crystal is used, but a substrate formed of another langasite single crystal such as a rangate single crystal having excellent characteristics at a high temperature is used. It doesn't matter.
１…微量質量センサ、２…感応膜、３…基板、４…電極膜 DESCRIPTION OF SYMBOLS 1 ... Trace mass sensor, 2 ... Sensitive film, 3 ... Substrate, 4 ... Electrode film
Claims (6)
該基板上に成膜された金属の電極膜と、
該電極膜上に成膜された感応膜と、を備え、
該感応膜が、繊維表面を酸化処理して親水化した微細炭素繊維で形成されていることを特徴とする微量質量センサ。 A substrate,
A metal electrode film formed on the substrate;
A sensitive film formed on the electrode film,
A trace mass sensor, wherein the sensitive film is formed of fine carbon fibers obtained by hydrophilizing the fiber surface by oxidation treatment.
前記感応膜が、前記微細炭素繊維の分散液を前記電極膜上に塗布して乾燥させた膜であることを特徴とする微量質量センサ。 The trace mass sensor according to claim 1,
The micro-mass sensor, wherein the sensitive film is a film obtained by applying the fine carbon fiber dispersion liquid onto the electrode film and drying it.
前記微細炭素繊維が、カーボンナノチューブであることを特徴とする微量質量センサ。 The trace mass sensor according to claim 1 or 2,
A minute mass sensor, wherein the fine carbon fiber is a carbon nanotube.
前記基板が、ランガサイト単結晶で形成されていることを特徴とする微量質量センサ。 In the trace mass sensor according to any one of claims 1 to 3,
A trace mass sensor, wherein the substrate is made of a langasite single crystal.
前記感応膜に水分子を吸着させて水分を検出する湿度センサであることを特徴とする微量質量センサ。 In the trace mass sensor according to any one of claims 1 to 4,
A trace mass sensor, wherein the moisture sensor detects moisture by adsorbing water molecules to the sensitive film.
前記感応膜にアルコールを吸着させてアルコールを検出するアルコールセンサであることを特徴とする微量質量センサ。 In the trace mass sensor according to any one of claims 1 to 4,
A trace mass sensor that is an alcohol sensor that detects alcohol by adsorbing alcohol to the sensitive film.
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