Analytical Method for Liquid Phase Measurement of Non-polar Quartz Crystal

Abstract

The present invention discloses an analysis method for polar quartz crystal liquid phase measurement, and relates to the field of polar quartz crystal liquid phase measurement. The present invention comprises the steps of connecting the polar quartz crystal to be measured to a circuit, controlling an alternating voltage across an air gap to drive the crystal to oscillate; collecting resonance waves and processing output signals; adjusting the analysis environment settings of the polar quartz crystal, recollecting resonance waves to process output signals; obtaining a frequency counter to measure frequency changes, and calculating the mass of QCM adsorbents. The present invention realizes stability measurement of the crystal to be measured and improves measurement accuracy through the design of analog modules and component types.

Description

Technical Field

[0001] The invention relates to the field of polar quartz crystal liquid phase measurement, and in particular to an analysis method for polar quartz crystal liquid phase measurement. Background Art

[0002] Challenges in signal measurement methods for non-polar quartz crystal sensors: Signal measurement methods for non-polar quartz crystal sensors include oscillator method, impedance analysis method, QCM-D measurement method, and electromagnetic piezoelectric acoustic measurement method.

[0003] In the process of using a frequency counter to measure frequency changes to monitor the mass of the adsorbent of the polar quartz crystal QCM, due to the energy dissipation in the liquid phase; when the polar quartz crystal oscillates in the liquid phase, the energy dissipation caused by the sine wave radiation into the liquid is much greater than that in the gas, which will cause frequency deviation and affect the oscillation stability. Summary of the invention

[0004] The present invention provides an analytical method for polar quartz crystal liquid phase measurement, which solves the problem of poor oscillation stability in the prior art. The method uses a technical means of adjusting the analysis environment settings of the polar quartz crystal after the crystal oscillates, and re-collecting the resonance wave to process the output signal, thereby obtaining the frequency change under the condition of excellent oscillation stability, and obtaining a more accurate calculation of the mass of the QCM adsorbent.

[0005] In a first aspect, the present invention provides an analytical method for non-polar quartz crystal liquid phase measurement, comprising:

[0006] Connect the non-polarized quartz crystal to be tested to the circuit, and control the alternating voltage across the air gap to drive the crystal to oscillate;

[0007] Collect the resonance wave and process the output signal;

[0008] After adjusting the analysis environment settings of the non-polar quartz crystal, the resonance wave is collected again to process the output signal;

[0009] The frequency counter is used to measure the frequency change and calculate the mass of the QCM adsorbate.

[0010] Furthermore, the step of connecting the non-polar quartz crystal to be tested to the circuit and controlling the alternating voltage across the air gap to drive the crystal to oscillate specifically includes:

[0011] When the quartz crystal contacts the liquid, the phase characteristic changes of the crystal resonator of the quartz crystal are recorded, and the resonant frequency changes of the crystal and the frequency changes of the circuit during the contact process are collected.

[0012] Furthermore, the collecting of the resonance wave and processing of the output signal specifically includes:

[0013] After the output signal is amplified, the waveform function is sorted and the function is transformed. The AC impedance spectrum of the sensor within a preset frequency range near each selected resonance is measured using a network analyzer, and the AC impedance spectrum curve is fitted to analyze the frequency at the maximum value of the conductivity, that is, the resonance frequency, and the bandwidth of the peak;

[0014] The bandwidth measurement of the peak includes: correlating the peak bandwidth with dissipation, and is inversely proportional to the crystal quality factor: FWHMn / fn=D=1 / Q;

[0015] Where D is the dissipation, determined using the QCM-D oscillation technique; Q is the crystal quality factor; FWHM is the bandwidth of the peak, and fn is the resonant frequency;

[0016] When the frequency changes, it is related to the change in mass on one surface of the crystal through the Sauerbrey equation.

[0017] Furthermore, it also includes collecting data on temperature changes generated during the collection of resonance waves, and adding a temperature compensation circuit to compensate for frequency changes caused by temperature changes.

[0018] Furthermore, the method also includes analyzing the changes in the properties of the non-polar quartz crystal material to be tested by measuring the changes in the resonance frequency.

[0019] Furthermore, the data processing of the frequency signal output by the oscillator specifically includes: converting the frequency data into voltage data by means of frequency-to-voltage conversion, and recording the changed voltage signal by means of a driving function recorder.

[0020] Furthermore, it also includes an anti-interference module, which is used to shield, isolate and fix factors that affect the frequency stability of the oscillator.

[0021] Furthermore, in the process of fitting the AC impedance spectrum curve, it specifically includes:

[0022] According to the collected phase characteristics of the crystal resonator, the corresponding analog resonance module is constructed. The collected crystal resonance frequency changes and circuit frequency changes are applied to train the analog resonance module. After the analog resonance module amplifies the output signal, the waveform function and the impedance spectrum curve after the function transformation are sorted out. The impedance spectrum curve obtained by the network analyzer is used for comparison to verify the similarity. If the similarity exceeds 90%, the training is completed.

[0023] When the similarity is lower than 90%, the impedance spectrum curve is matched by adjusting the parameters of the output signal in amplification and function transformation, or / and the fitted AC impedance spectrum is split, and the AC impedance spectrum at the frequency near the resonance is obtained after splitting, and the frequency domain characteristics are obtained by function transformation, and the parameters are designed according to the frequency characteristics to achieve similarity improvement;

[0024] For the simulated resonance module that meets the similarity after fitting, measurement design is carried out, that is, liquid damping component, non-mass factor component, temperature compensation component, and crystal surface mass component are added to the simulated resonance module, and different component parameters and functions are set according to the rules of different components affecting the stability of the resonance module;

[0025] By using a single control component type and a permutation and combination control component type, the change in oscillation stability of the simulated resonance module caused by all combination results is obtained. The change in oscillation stability is the effect of setting component control on stability, which includes adjusting the corresponding component when other component conditions remain unchanged, and the stability becomes better or worse;

[0026] Export the stability data of the simulated resonant module under the control component.

[0027] Furthermore, after the environment setting of the non-polar quartz crystal is adjusted, the resonant wave is collected again to process the output signal, including:

[0028] The resonance state of the non-polar quartz crystal to be tested is collected;

[0029] By comparing the stability impact data of the simulated resonance module under the control component, the stability impact data corresponding to the resonance state of the current tested polarity quartz crystal is obtained, the multi-component parameters and permutation and combination order of the stability impact data are output, and then added to the environmental settings of the tested polarity quartz crystal, the output result of the resonance state data of the measured polarity quartz crystal after connecting to the environmental settings is obtained for frequency counting.

[0030] The analytical method for measuring the liquid phase of a polar quartz crystal provided by the present invention uses a simulated resonance module to find the influencing components and types of the currently collected data corresponding to the polar quartz crystal to be measured, and then adds the influencing components in the data processing process, and processes the factors affecting the stability qualitatively and quantitatively and adds them to the data processing process, thereby solving the data deviation caused by human design in the liquid phase measurement and omitting the calculation amount of the difference caused by the fitting data in the transmission process;

[0031] The present invention realizes stability measurement of a crystal to be measured and improves measurement accuracy through the design of analog modules and component types. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] The drawings described herein are used to provide a further understanding of the embodiments of the present invention, constitute a part of the present invention, and do not constitute a limitation of the embodiments of the present invention. In the drawings:

[0033] Figure 1 A flow chart of an analytical method for liquid phase measurement of amorphous quartz crystals provided by an exemplary embodiment of the present invention. DETAILED DESCRIPTION

[0034] Exemplary embodiments will be described in detail herein, examples of which are shown in the accompanying drawings. When the following description refers to the drawings, the same numbers in different drawings represent the same or similar elements unless otherwise indicated. The embodiments described in the following exemplary embodiments do not represent all embodiments consistent with the present invention. Instead, they are merely examples of devices and methods consistent with some aspects of the present invention as detailed in the appended claims.

[0035] The present invention trains a simulated resonance module through the content of the actually measured non-polar quartz crystal, and corrects the training similarity, that is, the accuracy, of the simulated resonance module through output signal amplification, waveform function arrangement, and function transformation of the simulated resonance module. Multiple components are set through the corrected simulated resonance module that meets the similarity requirements, and each component has an impact on the resonance stability. Then, the resonator stability results under different component combinations, that is, the stability impact data of the simulated resonance module under the control component, are derived. In the actual measurement environment, the corresponding permutation and combination order is matched in the stability result of the simulated resonance module, and then brought into the software part for data analysis, and the analysis result is added to the stability result data affected by the permutation and combination.

[0036] The analytical method for measuring the liquid phase of amorphous quartz crystals provided by the present invention aims to solve the above technical problems of the prior art.

[0037] The technical solution of the present invention and how the technical solution of the present invention solves the above-mentioned technical problems are described in detail below with specific embodiments. The following specific embodiments can be combined with each other, and the same or similar concepts or processes may not be repeated in some embodiments. The embodiments of the present invention will be described below in conjunction with the accompanying drawings.

[0038] Example 1: Figure 1 As shown, this embodiment provides an analytical method for measuring the liquid phase of a non-polar quartz crystal, comprising the following steps:

[0039] A1. Connect the non-polar quartz crystal to be tested to the circuit and control the alternating voltage across the air gap to drive the crystal to oscillate;

[0040] When the quartz crystal contacts the liquid, the phase characteristic changes of the crystal resonator of the quartz crystal are recorded, and the resonant frequency changes of the crystal and the frequency changes of the circuit during the contact process are collected.

[0041] A2, collect the resonance wave and process the output signal; after recording the original data, in the process of processing the output signal from step A2, execute the generation and training content of the corresponding analog resonance module: construct the corresponding analog resonance module according to the collected phase characteristics of the crystal resonator, apply the collected crystal resonance frequency changes and circuit frequency changes, train the analog resonance module, and organize the waveform function and the impedance spectrum curve after the function transformation after amplifying the output signal of the analog resonance module, and use the impedance spectrum curve obtained by the network analyzer for comparison, verify the similarity, and the training is completed when the similarity exceeds 90%;

[0042] Export the training results, design the components of the crystal resonator that has been successfully verified for similarity, find the sorting combination of the corresponding components from the stability impact data of the simulated resonance module under the control components based on the measured data of the non-polar quartz crystal to be tested, and load the corresponding components and component contents into the analysis process.

[0043] A3. After adjusting the analysis environment settings of the non-polar quartz crystal, re-collect the resonance wave to process the output signal;

[0044] A4. Obtain a frequency counter to measure the frequency change and calculate the mass of the QCM adsorbate.

[0045] In the several embodiments provided by the present invention, it should be understood that the disclosed systems and methods can be implemented in other ways. For example, the system embodiments described above are only illustrative, for example, the division of the modules is only a logical function division, and there may be other division methods in actual implementation, such as multiple modules or components can be combined or integrated into another system, or some features can be ignored or not executed.

[0046] The modules described as separate components may or may not be physically separated, and the components shown as modules may or may not be physical modules, that is, they may be located in one place or distributed on multiple network modules. Some or all of the modules may be selected according to actual needs to achieve the purpose of the solution of this embodiment.

[0047] In addition, each functional module in each embodiment of the present invention may be integrated into one processing module, or each module may exist physically separately, or two or more modules may be integrated into one module. The above-mentioned integrated module may be implemented in the form of hardware or in the form of hardware plus software functional modules.

[0048] Those skilled in the art will appreciate that the embodiments of the present invention may be provided as methods or systems. Therefore, the present invention may take the form of a complete hardware embodiment, a complete software embodiment, or an embodiment combining software and hardware aspects.

[0049] It should also be noted that the terms "include", "comprises" or any other variations thereof are intended to cover non-exclusive inclusion, so that a process, method, commodity or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, commodity or device. In the absence of more restrictions, the elements defined by the sentence "comprises a ..." do not exclude the existence of other identical elements in the process, method, commodity or device including the elements.

[0050] The above are only embodiments of the present invention and are not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent substitution, improvement, etc. made within the spirit and principle of the present invention should be included in the scope of the claims of the present invention.

[0051] Those skilled in the art will readily appreciate other embodiments of the present invention after considering the specification and practicing the invention disclosed herein. The present invention is intended to cover any variations, uses or adaptations of the present invention that follow the general principles of the present invention and include common knowledge or customary techniques in the art that are not disclosed by the present invention. The description and examples are to be considered exemplary only, and the true scope and spirit of the present invention is indicated by the claims above.

[0052] It should be understood that the present invention is not limited to the exact construction that has been described above and shown in the drawings, and that various modifications and changes may be made without departing from the scope thereof. The scope of the present invention is limited only by the appended claims.

Claims

1. An analytical method for measuring the liquid phase of amorphous quartz crystals, characterized in that: include: Connect the non-polarized quartz crystal to be tested to the circuit, and control the alternating voltage across the air gap to drive the crystal to oscillate; Collect the resonance wave and process the output signal, including: After the output signal is amplified, the waveform function is sorted and the function is transformed. The AC impedance spectrum of the sensor within a preset frequency range near each selected resonance is measured using a network analyzer, and the AC impedance spectrum curve is fitted to analyze the frequency at the maximum value of the conductivity, that is, the resonance frequency, and the bandwidth of the peak; The bandwidth measurement of the peak includes: correlating the peak bandwidth with dissipation, and is inversely proportional to the crystal quality factor: FWHMn / fn=D=1 / Q; Where D is the dissipation, determined using the QCM-D oscillation technique; Q is the crystal quality factor; FWHM is the bandwidth of the peak, and fn is the resonant frequency; When the frequency changes, it is related to the change in mass on the surface of one side of the crystal through the Sauerbrey equation; The process of fitting the AC impedance spectrum curve specifically includes: According to the collected phase characteristics of the crystal resonator, the corresponding analog resonance module is constructed. The collected crystal resonance frequency changes and circuit frequency changes are applied to train the analog resonance module. After the analog resonance module amplifies the output signal, the waveform function and the impedance spectrum curve after the function transformation are sorted out. The impedance spectrum curve obtained by the network analyzer is used for comparison and the similarity is verified. If the similarity exceeds 90%, the training is completed. When the similarity is lower than 90%, the impedance spectrum curve is matched by adjusting the parameters of the output signal in amplification and function transformation, or / and the fitted AC impedance spectrum is split, and the AC impedance spectrum at the frequency near the resonance is obtained after splitting, and the frequency domain characteristics are obtained by function transformation, and the parameters are designed according to the frequency characteristics to achieve similarity improvement; For the simulated resonance module that meets the similarity after fitting, measurement design is carried out, that is, liquid damping component, non-mass factor component, temperature compensation component, and crystal surface mass component are added to the simulated resonance module, and different component parameters and functions are set according to the rules of different components affecting the stability of the resonance module; By using a single control component type and a permutation and combination control component type, the change in oscillation stability of the simulated resonance module caused by all combination results is obtained. The change in oscillation stability is the effect of setting component control on stability, which includes adjusting the corresponding component when other component conditions remain unchanged, and the stability becomes better or worse; Export the stability impact data of the simulated resonance module under the control component; After adjusting the analysis environment settings of the non-polar quartz crystal, re-collect the resonance wave and process the output signal, including: The resonance state of the non-polar quartz crystal to be tested is collected; By comparing the stability impact data of the simulated resonance module under the control component, the stability impact data corresponding to the resonance state of the current non-polar quartz crystal to be tested is obtained, and the multi-component parameters and the arrangement and combination sequence of the stability impact data are output, and then added to the environmental setting of the non-polar quartz crystal to be tested, and the output result of the resonance state data of the measured non-polar quartz crystal after access to the environmental setting is obtained for frequency counting; The frequency counter is used to measure the frequency change and calculate the mass of the QCM adsorbate.

2. The analytical method for non-polar quartz crystal liquid phase measurement according to claim 1, characterized in that: The step of connecting the non-polarized quartz crystal to be tested to the circuit and controlling the alternating voltage across the air gap to drive the crystal to oscillate specifically includes: When the quartz crystal contacts the liquid, the phase characteristic changes of the crystal resonator of the quartz crystal are recorded, and the resonant frequency changes of the crystal and the frequency changes of the circuit during the contact process are collected.

3. The analytical method for non-polar quartz crystal liquid phase measurement according to claim 2, characterized in that: It also includes collecting data on temperature changes generated during the collection of resonance waves, and adding a temperature compensation circuit to compensate for frequency changes caused by temperature changes.

4. The analytical method for non-polar quartz crystal liquid phase measurement according to claim 3, characterized in that: The method also includes analyzing the change of the properties of the non-polar quartz crystal material to be tested by measuring the change of the resonance frequency.

5. The analytical method for non-polar quartz crystal liquid phase measurement according to claim 4, characterized in that: The data processing of the frequency signal output by the oscillator specifically includes: converting the frequency data into voltage data by means of frequency-voltage conversion, and recording the changed voltage signal by means of a driving function recorder.

6. The analytical method for non-polar quartz crystal liquid phase measurement according to claim 5, characterized in that: It also includes an anti-interference module, which is used to shield, isolate and fix factors that affect the frequency stability of the oscillator.

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