CN104535449A - Non-contact electrode piezoelectric transducer device for monitoring strongly-corrosive gas and method - Google Patents
Non-contact electrode piezoelectric transducer device for monitoring strongly-corrosive gas and method Download PDFInfo
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Abstract
The invention discloses a non-contact electrode piezoelectric transducer device for monitoring a strongly-corrosive gas and a method. The non-contact electrode piezoelectric transducer device comprises a piezoelectric quartz wafer, an exciting electrode, an adsorption measurement tank, a controller and an impedance analyzer. According to the invention, a piezoelectric transducer is adopted to monitor the interaction process of the strongly-corrosive gas and a solid surface; adsorbance measurement errors caused by corrosion of a silver-film or a gold-film electrode originally sprayed onto the surface of the quartz wafer is radically eliminated; after separation of the exciting electrode from the quartz wafer, the mass loading capacity of a quartz crystal resonator is enhanced, and the mass change linearity range detected by the transducer is expanded; and superior light transmittance of quartz is restored, a circular ring metal electrode is used in a matching manner, and optical fibers are additionally mounted in the circular ring to be connected with a spectral measurement instrument, so that information of both mass and spectral changes of the quartz surface can be determined at the same time.
Description
Technical field
The present invention relates to a kind of noncontacting electrode piezoelectric sensor arrangement and method of monitoring severe corrosive gas.
Background technology
From nineteen fifty-nine roentgen Sauerbrey, QCM (Quartz Crystal Microbalance) (Quartz Crystal Microbalance is proposed, QCM) since detecting instrument technology, the sensor of this Surface Quality change in elevation sensitivity obtains widespread use in environmental monitoring, chemical-biological sensing etc., and becomes the powerful of observation interface transport phenomenon.The core devices of QCM (Quartz Crystal Microbalance) is piezoelectric quartz crystal plate, its resonance frequency is with the increase linear decline relation under certain condition of surface quality, Sauerbrey is deduced the resonance frequency of QCM and the relation of mass loading, is called as Sauerbrey equation, that is:
ΔF＝-2.26×10
-6F
0 2×Δm/A (1)
F in formula
0be the fundamental frequency (Hz) of quartz crystal, Δ m is mass change (g), and A is the area (cm of one side resonance range
2)
The sensitizing range of QCM concentrates on the lap of wafer surface two electrode, and therefore electrode surface must with extraneous contact with the mass transport process at perception interface.Although still use silverskin to prepare exciting electrode in many QCM, the serviceable life of this sensor is shorter, usually because silver electrode is corroded, its stability is declined, therefore is used for disposable sensor.The electrode material current with the QCM in bio-sensing field for chemistry mostly is golden film, but because golden film is more weak at the adhesion of quartz surfaces, affect the reusability of sensor, for the adhesion increased between golden film and quartz surfaces can bear comparatively harsh experiment condition (surface treatment etc. in chemical-biological sensing), usual elder generation is at strand DNA on Surface of Quartz crystal vacuum evaporating titanium (Ti) or chromium (Cr) transition bed, and then vacuum evaporating gold film electrode, quartz-crystal resonator prepared by this process conditions has increased substantially the serviceable life of QCM, become the senser element of standard configuration in various QCM instrument, but because technique comparatively complexity add that production scale is little, the price of this qcm sensor is higher.
Utilize QCM can study the characterization of adsorption of various membraneous material, but the material adsorbed can not have strong corrosivity, otherwise will electrode corrosion be caused, on the one hand the mensuration of disturb adsorption amount, affect the serviceable life of sensor on the other hand.Such as, after the corrosive gas such as iodine, sulfuretted hydrogen is modified at the thin film adsorbs of strand DNA on Surface of Quartz crystal, golden film or silverskin that film and then corrosion are plated in plane of crystal can be penetrated, very easily cause the corrosion of the instability of QCM resonance frequency and golden film or silverskin and cause significant measuring error.So the present invention devises the noncontacting electrode piezoelectric sensor arrangement and method that can monitor severe corrosive gas.
Summary of the invention
The present invention is in order to solve the problem, propose a kind of noncontacting electrode piezoelectric sensor arrangement and method of monitoring severe corrosive gas, this device can the process of Real-Time Monitoring quartz and finishing film absorption severe corrosive gas, be conducive to the stability improving its resonance frequency, completely eliminate the adsorbance measuring error because quartz wafer plated surface silverskin or golden film are corroded and cause.
To achieve these goals, the present invention adopts following technical scheme:
Monitor a noncontacting electrode piezoelectric sensor arrangement for severe corrosive gas, comprise piezoelectric quartz crystal plate, exciting electrode, absorption measuring cell, controller and electric impedance analyzer; Two exciting electrodes are installed on piezoelectric quartz crystal plate upper and lower respectively, and be separated with piezoelectric quartz crystal plate, form excitation electrical field, wherein going up exciting electrode is encapsulated in thin-walled glass pipe, be placed in absorption measuring cell, lower exciting electrode is placed in bottom absorption measuring cell, and excitation electrical field is applied on piezoelectric quartz crystal plate by the conduction of glass and air and makes its resonance, its resonance frequency is measured by electric impedance analyzer, and carries out data acquisition, analysis and storage by controller.
Described controller calculates the mass change amount of strand DNA on Surface of Quartz crystal by Sauerbrey equation:
ΔF＝-2.26×10
-6F
0 2×Δm/A
In formula, F
0be the fundamental frequency (Hz) of quartz crystal, Δ m is mass change (g), and A is the area (cm of one side resonance range
2).
Described piezoelectric quartz crystal plate is AT cut type piezoelectric quartz crystal, and surface is electrodeless, is naked piezoelectric quartz crystal plate, has excellent light transmission after polishing, simultaneously for quality and spectroscopic assay, can be placed on bottom absorption measuring cell during mensuration.
Described exciting electrode material comprises copper, aluminium, graphite, iron, stainless steel or titanium, and shape comprises disk, cylinder, ball-type, wire gauze and tubulose.
Described upper exciting electrode applies corrosion-resistant coating as required or is encapsulated in thin-walled glass pipe on surface, avoid electrode corrosion.
If do not adopt anticorrosive measure, directly electrode is exposed in absorption measuring cell, even if there is slighter electrode corrosion, only otherwise change electrode separation size, also can not cause the change of quartz-crystal resonance frequency, suffer the electrode of surface corrosion not affect it and use.
Described lower exciting electrode is disk metal electrode, is placed in below quartz wafer.
The shape of upper and lower exciting electrode, area, material can be identical or different, both center can with the center of circle of piezoelectric quartz crystal plate on the same line, also can be placed on asymmetric position.
The center of described upper exciting electrode, lower exciting electrode and the center of circle of piezoelectric quartz crystal plate on the same line time, incident parallel light is radiated at quartz wafer center resonance region by the light transmitting fiber being placed in hollow edged electrode, transmitted light goes out to spectrometer by the outgoing photoconduction Conductivity of Fiber in another hollow edged electrode, carries out the mensuration of quality and spectrum simultaneously.
Based on the method for work of said apparatus, comprise the following steps:
(1) upper and lower exciting electrode, piezoelectric quartz crystal are fixed in measuring cell; Optimize after electrode position, two electrodes and electric impedance analyzer are connected, the reference point that mensuration calculates as quality of forming film without the resonance frequency of film quartz wafer;
(2) at the film of piezoelectric quartz crystal surface preparation material to be studied; Put it in same absorption measuring cell, upwards, after mensuration film forming, the resonance frequency of quartz wafer, is calculated to be film quality and thickness by frequency variation to face;
(3) component upon adsorption is added, monitoring piezoelectric quartz crystal resonance frequency curve over time; Resonance frequency according to piezoelectric quartz crystal changes, and by Sauerbrey equation gauging surface quality, measures relevant dynamics and thermodynamic parameter;
(4) in piezoelectric sensing and spectrum Simultaneously test are tested, piezoelectric quartz crystal is placed in the mensuration light path of sub-ray spectrometer or fluorophotometer, or utilizes light transmitting fiber to carry out light conduction;
(5) cleaning absorption measuring cell, changes piezoelectric quartz crystal, measures next time.
Principle of work of the present invention is: be placed on by piezoelectric quartz crystal plate between two exciting electrodes, exciting electrode is separated with quartz crystal, excitation electrical field is applied on quartz crystal by glass and air transmitted and makes its resonance, its resonance frequency has sensitive response to the mass loading change on quartz surfaces, Monitoring lower-cut is lower than nanogram, the mass change in quartz surfaces and modified membrane and external influence process can be detected in real time, obtain the information of dynamics about mechanism and thermodynamics aspect.Such as, when studying metal organic frame (MOFs) material ZIF-8 film and iodine vapor mechanism, if use the QCM of surface band exciting electrode to monitor iodine vapor, the tool corrosive gass such as sulfuretted hydrogen are in the adsorption process of ZIF-8 film, because the intermolecular forces of they and exciting electrode is strong, iodine vapor, sulfuretted hydrogen etc. both adsorbed on film, also directly to adsorb at electrode surface, this absorption occurring in electrode surface disturbs MOFs film to iodine vapor on the one hand, the detection of the adsorbances such as sulfuretted hydrogen, the corrosion of exciting electrode is caused to cause this piezoelectric quartz crystal sensor to be scrapped on the other hand.Adopt the electrode design of separate type, effectively can avoid electrode adsorption and be corroded the impact that adsorbance is measured, increase the mass loading ability of sensor, expand the range of linearity that sensor mass detects, can be used for the interaction process of monitoring severe corrosive gas and solid surface.In addition, after exciting electrode is separated with quartz wafer, excellent light transmittance of quartz itself can be utilized, with the use of round loop electrode, introduce light transmitting fiber wherein and spectrum measurement instruments is connected, can the information of quality on Simultaneously test quartz surfaces and spectrum change.Utilize the mass change in the mechanism of this device monitoring iodine vapor and ZIF-8 film and spectrum change, shown this sensor, in the absorption of monitoring severe corrosive gas, there is certain application prospect.
Beneficial effect of the present invention is:
(1) realize the interaction process with noncontacting electrode piezoelectric sensor monitoring severe corrosive gas and solid surface, completely eliminate the corrosion because of silverskin or golden film and the adsorbance error at measurment that causes;
(2), after exciting electrode being separated with quartz wafer, reducing the mass loading of previous spraying plating at the exciting electrode of strand DNA on Surface of Quartz crystal itself, expand the range of linearity of the measurable mass change of this sensor;
(3) use without the quartz wafer of exciting electrode, recovered itself light transmission quartzy, with the use of round loop electrode, introducing light transmitting fiber and spectrum measurement instruments are connected wherein, can the information of quality on Simultaneously test quartz surfaces and spectrum change.
Accompanying drawing explanation
Fig. 1 is the cross-sectional view of noncontacting electrode piezoelectric sensor of the present invention;
Fig. 2 is the schematic diagram of the incident quartz wafer of spectrum of the present invention.
Wherein: 1, well; 2, the upper exciting electrode of Anti-corrosion design is with; 3, glass absorption measuring cell; 4, film to be measured; 5, piezoelectric quartz crystal plate; 6, lower exciting electrode; 7, electric impedance analyzer; 8, controller; 9, light source; 10, incident light transmitting fiber; 11, hollow edged electrode; 12, outgoing light transmitting fiber; 13, detecting device.
Embodiment:
Below in conjunction with accompanying drawing and embodiment, the invention will be further described.
As shown in Figure 1, a kind of noncontacting electrode piezoelectric sensor arrangement of monitoring severe corrosive gas, comprises piezoelectric quartz crystal plate 5, the upper exciting electrode 2 of band Anti-corrosion design, lower exciting electrode 6, absorption measuring cell 3, controller 8 and electric impedance analyzer 7; Two exciting electrodes are installed on piezoelectric quartz crystal plate upper and lower respectively, and be separated with piezoelectric quartz crystal plate, upper exciting electrode 2 wherein with Anti-corrosion design is encapsulated in thin-walled glass pipe, be placed in absorption measuring cell, lower exciting electrode 6 is placed in bottom absorption measuring cell, excitation electrical field is applied on piezoelectric quartz crystal plate 5 by the conduction of glass and air and makes its resonance, and its resonance frequency is measured by electric impedance analyzer 7, and carries out data acquisition, analysis and storage by controller 8.
Absorption measuring cell is glass absorption measuring cell 3, is provided with well 1.
The core devices of QCM (Quartz Crystal Microbalance) is piezoelectric quartz crystal plate, and its resonance frequency linearly declines with the increase of surface quality under certain condition, i.e. Sauerbrey equation:
ΔF＝-2.26×10
-6F
0 2×Δm/A (1)
F in formula
0be the fundamental frequency (Hz) of quartz crystal, Δ m is mass change (g), and A is the area (cm of one side resonance range
2)
The resonance realizing piezoelectric quartz crystal plate need apply the alternating electric field identical with its resonance frequency to it, therefore two exciting electrodes are prepared at strand DNA on Surface of Quartz crystal, electrode material is silver under normal conditions, because silver has good electric conductivity, and it is stronger with the surface conjunction power of quartz, price is also relatively cheap, surface coating technology is ripe, it is electrode material the most frequently used in piezoelectric quartz crystal resonator, but because the chemical stability of silver is poor, usually quartz-crystal resonator is encapsulated in vacuum environment to avoid electrode and extraneous contact.
The sensitizing range of QCM concentrates on the lap of wafer surface two electrode, and therefore electrode surface must with extraneous contact with the mass transport process at perception interface.Although still use silverskin to prepare exciting electrode in many QCM, the serviceable life of this sensor is shorter, usually because silver electrode is corroded, its stability is declined, therefore is used for disposable sensor.The electrode material current with the QCM in bio-sensing field for chemistry mostly is golden film, but because golden film is more weak at the adhesion of quartz surfaces, affect the reusability of sensor, for the adhesion increased between golden film and quartz surfaces can bear comparatively harsh experiment condition (as the liberation of hydrogen in electrochemical reaction or analyse oxygen, surface treatment etc. in chemical-biological sensing), usual elder generation is at strand DNA on Surface of Quartz crystal vacuum evaporating titanium (Ti) or chromium (Cr) transition bed, and then vacuum evaporating gold film electrode, quartz-crystal resonator prepared by this process conditions has increased substantially the serviceable life of QCM, become the senser element of standard configuration in various QCM instrument, but because technique comparatively complexity add that production scale is little, the price of this qcm sensor is higher, usually at 100 ~ 500 yuan/sheet.
In fact as the quartz wafer itself playing sensing effect in QCM, there is good chemical stability, and have certain physical strength, excellent optical property.In the present invention, exciting electrode is separated with piezoelectric quartz crystal, high frequency pumping electric field is applied on wafer by the conduction of adsorbing measurement pool wall and air and makes it produce resonance, adopt the change curve of cordless the real time measure piezoelectric quartz crystal resonance frequency, calculated the mass change amount of strand DNA on Surface of Quartz crystal by Sauerbrey equation.Because exciting electrode and quartz wafer are no longer connected as a single entity, its selection need not consider the surface conjunction power of it and quartz wafer, and thickness of electrode is not also by the restriction of quartz wafer load capacity, the electrode material that corrosion resistance is good can be used, as platinum (Pt), graphite (C) or the metal etc. be encapsulated in glass tube, electrode size, shape, position can arbitrarily be designed, replacing electrode is convenient, exciting electrode in puzzlement QCM practical application can be avoided to subject to corrosion, the problem in the stronger environment of corrosivity can not be used for, under the environmental baseline that there is corrosive gas, there is certain technical advantage.In addition, use without the quartz wafer of exciting electrode, recovered itself light transmission quartzy, with the use of round loop electrode, introducing light transmitting fiber and spectrum measurement instruments are connected wherein, can the information of quality on Simultaneously test quartz surfaces and spectrum change.
Exciting electrode material can be copper, aluminium, graphite, iron, stainless steel, titanium etc., shape comprises disk, cylinder, ball-type, wire gauze, tubulose, top electrode can apply corrosion-resistant coating on surface or be encapsulated in thin-walled glass pipe as required, avoid electrode corrosion, if do not adopt anticorrosive measure, directly electrode is exposed in absorption measuring cell, even if there is slighter electrode corrosion, only otherwise change electrode separation size, also can not cause the change of quartz-crystal resonance frequency, suffer the electrode of surface corrosion not affect it and use.Bottom electrode is disk metal electrode, is placed in below quartz wafer, and the shape of upper and lower exciting electrode, area, material can be identical or different, its center can with the center of circle of piezoelectric quartz crystal plate on the same line, also can be placed on asymmetric position.Use the tubulose exciting electrode with wafer center of circle conllinear, the directional light that light source 9 sends via incident light transmitting fiber 10 conduction and be radiated at quartz wafer 5 center resonance region through hollow edged electrode 11, transmitted light exports on the detecting device 13 of spectrometer by the outgoing light transmitting fiber 12 being placed in another hollow edged electrode, carry out the mensuration of quality and spectrum change, as shown in Figure 2 simultaneously.
Concrete implementation step is:
1, upper and lower exciting electrode, piezoelectric quartz crystal are fixed in measuring cell; Optimize after electrode position, two electrodes and electric impedance analyzer are connected, the reference point that mensuration calculates as quality of forming film without the resonance frequency of film quartz wafer;
2, at the film of piezoelectric quartz crystal plate surface preparation material to be studied; Put it in same absorption measuring cell, face upwards, measures the resonance frequency (F of quartz wafer after film forming
1), be calculated to be film quality and thickness, simultaneously by F by frequency variation
1as the reference point of calculated rate variable quantity.
3, in absorption measuring cell, a certain amount of target substance is added, the frequency F in monitoring piezoelectric quartz crystal plate or the adsorption film carried and target substance mechanism
2, by Δ F=F
2– F
1calculated rate changing value, the surface quality variable quantity corresponding to Sauerbrey equation calculates, according to kinetics of adsorption and isotherm model, calculates relevant parameters.
4, in piezoelectric sensing and spectrum coupling determination experiment, piezoelectric quartz crystal is placed in the mensuration light path of spectrometer, or utilize light transmitting fiber to carry out light conduction, Simultaneously test quality and spectrum change information, for illustrating about absorption or the mechanism of action, providing the chemical information of quality and amount of spectrum aspect.
By reference to the accompanying drawings the specific embodiment of the present invention is described although above-mentioned; but not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendment or distortion that creative work can make still within protection scope of the present invention.
Claims (8)
1. monitor a noncontacting electrode piezoelectric sensor arrangement for severe corrosive gas, it is characterized in that: comprise piezoelectric quartz crystal plate, exciting electrode, absorption measuring cell, controller and electric impedance analyzer; Two exciting electrodes are installed on piezoelectric quartz crystal plate upper and lower respectively, and be separated with piezoelectric quartz crystal plate, form excitation electrical field, wherein going up exciting electrode is encapsulated in thin-walled glass pipe, be placed in absorption measuring cell, lower exciting electrode is placed in bottom absorption measuring cell, and excitation electrical field is applied on piezoelectric quartz crystal plate by the conduction of glass and air and makes its resonance, its resonance frequency is measured by electric impedance analyzer, and carries out data acquisition, analysis and storage by controller.
2. a kind of noncontacting electrode piezoelectric sensor arrangement of monitoring severe corrosive gas as claimed in claim 1, is characterized in that: described controller is by Sauerbrey equation record and show the mass change amount of strand DNA on Surface of Quartz crystal:
ΔF＝-2.26×10
-6F
0 2×Δm/A
In formula, F
0be the fundamental frequency (Hz) of quartz crystal, Δ m is mass change (g), and A is the area (cm of one side resonance range
2).
3. a kind of noncontacting electrode piezoelectric sensor arrangement of monitoring severe corrosive gas as claimed in claim 1, it is characterized in that: described piezoelectric quartz crystal plate is AT cut type piezoelectric quartz crystal, surface is electrodeless, be naked piezoelectric quartz crystal plate, there is excellent light transmission after polishing, simultaneously for quality and spectroscopic assay, can be placed on during mensuration bottom absorption measuring cell.
4. a kind of noncontacting electrode piezoelectric sensor arrangement of monitoring severe corrosive gas as claimed in claim 1, it is characterized in that: described exciting electrode material comprises copper, aluminium, graphite, iron, stainless steel or titanium, and shape comprises disk, cylinder, ball-type, wire gauze and tubulose.
5. a kind of noncontacting electrode piezoelectric sensor arrangement of monitoring severe corrosive gas as claimed in claim 1, is characterized in that: described upper exciting electrode applies corrosion-resistant coating as required or is encapsulated in thin-walled glass pipe on surface, avoid electrode corrosion.
6. a kind of noncontacting electrode piezoelectric sensor arrangement of monitoring severe corrosive gas as claimed in claim 1, is characterized in that: described lower exciting electrode is disk metal electrode, is placed in below quartz wafer.
7. a kind of noncontacting electrode piezoelectric sensor arrangement of monitoring severe corrosive gas as claimed in claim 1, it is characterized in that: the center of described upper exciting electrode, lower exciting electrode and the center of circle of piezoelectric quartz crystal plate on the same line time, incident parallel light is radiated at quartz wafer center resonance region by the light transmitting fiber being placed in hollow edged electrode, transmitted light goes out to spectrometer by the outgoing photoconduction Conductivity of Fiber in another hollow edged electrode, carries out the mensuration of quality and spectrum simultaneously.
8. based on the method for work of the device such as according to any one of claim 1-7, it is characterized in that: comprise the following steps:
(1) upper and lower exciting electrode, piezoelectric quartz crystal are fixed in measuring cell; Optimize after electrode position, two electrodes and electric impedance analyzer are connected, the reference point that mensuration calculates as quality of forming film without the resonance frequency of film quartz wafer;
(2) at the film of piezoelectric quartz crystal surface preparation material to be studied; Put it in same absorption measuring cell, upwards, after mensuration film forming, the resonance frequency of quartz wafer, is calculated to be film quality and thickness by frequency variation to face;
(3) component upon adsorption is added, monitoring piezoelectric quartz crystal resonance frequency curve over time; Resonance frequency according to piezoelectric quartz crystal changes, and by Sauerbrey equation gauging surface quality, measures relevant dynamics and thermodynamic parameter;
(4) in piezoelectric sensing and spectrum Simultaneously test are tested, piezoelectric quartz crystal is placed in the mensuration light path of sub-ray spectrometer or fluorophotometer, or utilizes light transmitting fiber to carry out light conduction;
(5) cleaning absorption measuring cell, changes piezoelectric quartz crystal, measures next time.
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| CN105958958B (en) * | 2016-04-27 | 2018-09-25 | 北京无线电计量测试研究所 | A kind of quartz-crystal resonator and preparation method thereof |
| CN105978525B (en) * | 2016-04-27 | 2018-09-25 | 北京无线电计量测试研究所 | A kind of quartz resonator |
| CN105958961B (en) * | 2016-04-27 | 2018-09-25 | 北京无线电计量测试研究所 | A kind of production method of quartz resonator |
| CN105958961A (en) * | 2016-04-27 | 2016-09-21 | 北京无线电计量测试研究所 | Manufacturing method for quartz resonators |
| CN112543865A (en) * | 2018-08-23 | 2021-03-23 | 株式会社日立制作所 | Corrosion environment monitoring method and corrosion environment monitoring system |
| CN112543865B (en) * | 2018-08-23 | 2023-11-07 | 株式会社日立制作所 | Corrosion environment monitoring method and corrosion environment monitoring system |
| CN109164846A (en) * | 2018-10-06 | 2019-01-08 | 烟台大学 | The temperature regulating device and temperature control method measured for SAW resonance, anti-resonance frequency |
| CN109374731B (en) * | 2018-11-14 | 2021-07-13 | 江苏科技大学 | Quartz crystal microbalance with annular indium tin oxide electrode |
| CN109374731A (en) * | 2018-11-14 | 2019-02-22 | 江苏科技大学 | A kind of quartz crystal microbalance of annular indium-tin oxide electrode |
| CN113281393A (en) * | 2021-03-29 | 2021-08-20 | 江苏科技大学 | Electrodeless miniaturized measuring device for detecting new corona RNA virus |
| CN113281393B (en) * | 2021-03-29 | 2022-11-25 | 江苏科技大学 | Electrodeless miniaturized measuring device for detecting new corona RNA virus |
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