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CN105043922A - Two-parameter detection device and method for quartz crystal microbalance - Google Patents

Two-parameter detection device and method for quartz crystal microbalance Download PDF

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CN105043922A
CN105043922A CN201510442494.3A CN201510442494A CN105043922A CN 105043922 A CN105043922 A CN 105043922A CN 201510442494 A CN201510442494 A CN 201510442494A CN 105043922 A CN105043922 A CN 105043922A
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signal
unit
quartz crystal
crystal microbalance
frequency
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蒋海峰
丁甜
赵斌炎
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Nanjing University of Science and Technology
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Abstract

本发明提供一种石英晶体微天平双参数检测装置,包括驱动信号单元、串联电路单元、信号处理单元、信号切换单元、A/D转换单元、控制单元、绘制单元;驱动信号单元,用于产生峰峰值固定的余弦信号;串联电路单元,包括被测石英晶体微天平和与其串联的电阻,用于在驱动信号单元的驱动下将石英晶体微天平的导纳信息转化为电压信号输出;信号处理单元,用于提取串联电路单元产生的信号的幅值和相位差信息;信号切换单元,用于将信号处理单元产生的信号切换;A/D转换单元,用于将信号切换单元输出的模拟信号转换成数字信号;控制单元,用于底层电路的控制以及数据信号的转发;绘制单元,具有处理功能,用于实现扫频设定和曲线绘制。

The invention provides a dual-parameter detection device for a quartz crystal microbalance, comprising a drive signal unit, a series circuit unit, a signal processing unit, a signal switching unit, an A/D conversion unit, a control unit, and a drawing unit; a drive signal unit for generating A cosine signal with a fixed peak value; a series circuit unit, including the measured quartz crystal microbalance and a resistor connected in series with it, used to convert the admittance information of the quartz crystal microbalance into a voltage signal output under the drive of the drive signal unit; signal processing The unit is used to extract the amplitude and phase difference information of the signal generated by the series circuit unit; the signal switching unit is used to switch the signal generated by the signal processing unit; the A/D conversion unit is used to convert the analog signal output by the signal switching unit Converted into digital signals; the control unit is used for the control of the underlying circuit and the forwarding of data signals; the drawing unit has processing functions and is used for frequency sweep setting and curve drawing.

Description

一种石英晶体微天平双参数检测装置及方法A dual-parameter detection device and method for a quartz crystal microbalance

技术领域technical field

本发明涉及谐振式传感器技术,特别是一种石英晶体微天平双参数检测装置及方法。The invention relates to a resonant sensor technology, in particular to a dual-parameter detection device and method for a quartz crystal microbalance.

背景技术Background technique

石英晶体微天平(QuartzCrystalMicrobalance,简称QCM)是20世纪60年代发展起来的一种谐振式传感器测量技术,其测量精度很高可达纳克级,作为一种质量传感器广泛应用于医学分析,环境检测,分析化学等对测量要求较高的领域。QCM是通过在AT切石英晶片的上下表面镀上金属电极而构成的一种高分辨率的压电传感器。晶体在外加交变电场的作用下会产生振荡,当振动频率与石英晶体的固有频率一致时,便会产生共振,此时振荡稳定且强烈,即发生压电谐振。Quartz Crystal Microbalance (QCM for short) is a resonant sensor measurement technology developed in the 1960s. Its measurement accuracy is as high as nanograms. It is widely used as a quality sensor in medical analysis and environmental detection. , Analytical chemistry and other fields that require high measurement. QCM is a high-resolution piezoelectric sensor formed by plating metal electrodes on the upper and lower surfaces of an AT-cut quartz wafer. The crystal will oscillate under the action of an external alternating electric field. When the vibration frequency is consistent with the natural frequency of the quartz crystal, resonance will occur. At this time, the oscillation is stable and strong, that is, piezoelectric resonance occurs.

当QCM的电极与待测物质相接触时,待测物质的性质(如:质量、粘度、密度等)就会改变QCM的谐振频率。GuenterSauerbrey和Kanazawa分别推导验证了气相中和液相中石英晶体共振频率与吸附质量之间的公式,公式表明石英晶体的频率变化与晶体表面质量变化成简单线性关系,因此只需检测晶体振荡频率变化就可以测得晶体表面质量的变化,从而实现质量变化转化成频率变化输出然而当QCM用于粘弹性液体检测时,由于粘弹性薄膜的吸附性呈现出明显的柔性吸附特性,只记录谐振频率的变化会使结果产生很大的误差,甚至导致错误的分析结果。此时通记录耗散因子D可以知道吸附在表面的是粘性很大的软质膜,还是刚性结构,因此可以反映更多的结构信息。在粘弹性液体检测中要采用双参数检测法,即同时获得谐振频率变化值Δf和耗散因子D。When the electrodes of the QCM are in contact with the substance to be measured, the properties of the substance to be measured (such as mass, viscosity, density, etc.) will change the resonant frequency of the QCM. GuenterSauerbrey and Kanazawa deduced and verified the formulas between the resonance frequency and adsorption mass of quartz crystals in the gas phase and liquid phase respectively. The formula shows that the frequency change of the quartz crystal has a simple linear relationship with the change of the crystal surface quality, so it is only necessary to detect the crystal oscillation frequency change The change of the surface mass of the crystal can be measured, so as to realize the conversion of mass change into frequency change output. However, when the QCM is used for viscoelastic liquid detection, due to the obvious flexible adsorption characteristics of the viscoelastic film, only the resonance frequency is recorded. Variations can cause large errors in results and even lead to erroneous analysis results. At this time, by recording the dissipation factor D, it can be known whether it is a soft film with a high viscosity or a rigid structure that is adsorbed on the surface, so more structural information can be reflected. In the detection of viscoelastic liquids, a double-parameter detection method is used, that is, the change value of the resonance frequency Δf and the dissipation factor D are simultaneously obtained.

目前主流的能同时获得Δf和D的测量装置是瑞典学者Kasemo、Rodahl等人在Voigt模型和流体力学的基础上提出的QCM-D。测量框图如图1所示。其基本原理为:周期性的连通、断开与QCM传感器和信号源相连的开关,用数字示波器记录其输出电压信号的频率和衰减延迟时间。当驱动信号断开以后,QCM的振荡幅度呈指数形式衰减。该QCM振荡幅度的衰减情况可以分别用数字示波器的高阻或者低阻探头测量得到,这样就可以保证晶体的衰减是在其串联或者并联谐振频率处被记录下来。记录的信号被输入到计算机中,通过数据拟合,可以得到以下形式:其中,频率偏移是直接得到的,Δf=f0-f。而耗散因子D是由以下关系得到: At present, the mainstream measurement device that can simultaneously obtain Δf and D is the QCM-D proposed by Swedish scholars Kasemo, Rodahl, etc. on the basis of Voigt model and fluid mechanics. The measurement block diagram is shown in Figure 1. The basic principle is: periodically connect and disconnect the switch connected to the QCM sensor and signal source, and record the frequency and decay delay time of the output voltage signal with a digital oscilloscope. When the driving signal is disconnected, the oscillation amplitude of the QCM decays exponentially. The attenuation of the QCM oscillation amplitude can be measured with a high-impedance or low-impedance probe of a digital oscilloscope, so as to ensure that the attenuation of the crystal is recorded at its series or parallel resonance frequency. The recorded signal is input into the computer, and through data fitting, the following form can be obtained: Wherein, the frequency offset is obtained directly, Δf=f 0 -f. And the dissipation factor D is obtained from the following relationship:

该方法是目前用得比较多的,但是该方法存在一定的缺陷,主要表现在:This method is widely used at present, but there are certain defects in this method, mainly in:

(1)QCM-D中耗散因子是采用脉冲激励的方式让QCM传感器振荡,然后测量振荡衰减时间计算得到的,这是一种瞬时测量法,容易受到外界扰动的影响,外界的微小干扰都有可能导致测试数据的不准确。同时,因振荡器衰减时间一般是在10-6s量级,故测试仪器的分辨率和精度要求非常高。(1) The dissipation factor in QCM-D is calculated by making the QCM sensor oscillate by means of pulse excitation, and then measuring the oscillation decay time. This is an instantaneous measurement method, which is easily affected by external disturbances. It may lead to inaccurate test data. At the same time, because the decay time of the oscillator is generally on the order of 10 -6 s, the resolution and precision of the test instrument are required to be very high.

(2)上图QCM的激励信号是由信号发生器产生的固定频率信号。当QCM表面附着薄膜后,其串联谐振频率发生了变化(新的谐振频率未知),如果仍用原来的固定频率信号去激励QCM,所得到的数据不一定能准确反映出薄膜的真实特性。(2) The excitation signal of the QCM in the above figure is a fixed frequency signal generated by a signal generator. When a film is attached to the surface of the QCM, its series resonance frequency changes (the new resonance frequency is unknown). If the original fixed frequency signal is still used to excite the QCM, the obtained data may not accurately reflect the true characteristics of the film.

发明内容Contents of the invention

本发明的目的在于提供一种石英晶体微天平双参数检测装置及方法,本发明基于稳态法以实现对QCM吸附物质前后频率变化和耗散因子的测量。The object of the present invention is to provide a quartz crystal microbalance dual-parameter detection device and method. The present invention is based on the steady-state method to realize the measurement of the frequency change and dissipation factor before and after QCM adsorbed substances.

一种石英晶体微天平双参数检测装置,包括驱动信号单元、串联电路单元、信号处理单元、信号切换单元、A/D转换单元、控制单元、绘制单元。所述驱动信号单元,用于产生峰峰值固定的余弦信号;所述串联电路单元,包括被测石英晶体微天平和与其串联的电阻,用于在驱动信号单元的驱动下将石英晶体微天平的导纳信息转化为电压信号输出;所述信号处理单元,用于提取串联电路单元产生的信号的幅值和相位差信息;所述信号切换单元,用于将信号处理单元产生的信号切换;所述A/D转换单元,用于将信号切换单元输出的模拟信号转换成数字信号;所述控制单元,用于底层电路的控制,以及数据信号的转发;所述绘制单元,具有处理功能,用于实现扫频设定和曲线绘制。A quartz crystal microbalance dual-parameter detection device includes a drive signal unit, a series circuit unit, a signal processing unit, a signal switching unit, an A/D conversion unit, a control unit, and a drawing unit. The drive signal unit is used to generate a cosine signal with a fixed peak-to-peak value; the series circuit unit includes the measured quartz crystal microbalance and a resistor connected in series with it, and is used to drive the quartz crystal microbalance to The admittance information is converted into a voltage signal output; the signal processing unit is used to extract the amplitude and phase difference information of the signal generated by the series circuit unit; the signal switching unit is used to switch the signal generated by the signal processing unit; The A/D conversion unit is used to convert the analog signal output by the signal switching unit into a digital signal; the control unit is used for the control of the underlying circuit and the forwarding of the data signal; the drawing unit has a processing function and uses It is used to realize frequency sweep setting and curve drawing.

根据上述装置,本发明采用如下方法完成石英晶体微天平双参数检测,具体方法为:对空载和负载状态下的石英晶体微天平产生的两路余弦信号进行以下处理:According to the above-mentioned device, the present invention adopts the following method to complete the dual parameter detection of the quartz crystal microbalance, and the specific method is: the two-way cosine signals produced by the quartz crystal microbalance under no-load and load states are processed as follows:

(1)确定一频率,采用自相关和互相关处理,获得两路余弦信号各自的幅值及两者的相位差,根据两路余弦信号的幅值及相位差获得该频率下的电导值,(1) Determine a frequency, adopt autocorrelation and cross-correlation processing, obtain the respective amplitudes and phase differences of the two cosine signals, and obtain the conductance value at the frequency according to the amplitude and phase difference of the two cosine signals,

(2)更改频率,获取不同频率下的电导值,(2) Change the frequency to obtain the conductance value at different frequencies,

(3)构建电导值和频率之间的关系,(3) Construct the relationship between conductance value and frequency,

(4)获取谐振频率变化,及空载或负载状态下耗散因子。(4) Obtain the change of resonant frequency, and the dissipation factor under no-load or load state.

经过上述装置和方法,获得石英晶体微天平的谐振频率变化为空载和负载状态下电导峰值之间频率差;Through the above-mentioned device and method, the resonant frequency change of the quartz crystal microbalance is obtained as the frequency difference between the conductance peak values under no-load and load states;

经过上述装置和方法,获得石英晶体微天平的空载状态下耗散因子为空载状态下半边半功率带宽两倍与谐振频率的比值;Through the above-mentioned device and method, the dissipation factor of the quartz crystal microbalance under the no-load state is obtained as the ratio of half half power bandwidth twice to the resonant frequency under the no-load state;

经过上述装置和方法,获得石英晶体微天平的负载状态下耗散因子为负载状态下半边半功率带宽两倍与谐振频率的比值。Through the above device and method, the dissipation factor of the quartz crystal microbalance under load is obtained as the ratio of twice the half power bandwidth under load to the resonant frequency.

本发明与现有技术相比,具有以下优点:Compared with the prior art, the present invention has the following advantages:

(1)粘弹性薄膜对QCM的影响就可以通过频率变化和半功率带宽变化直接反映出来,更能真实的反应出QCM表面所吸附的薄膜性质,从理论上保证了分析数据的准确性。(1) The influence of the viscoelastic film on the QCM can be directly reflected by the frequency change and the half-power bandwidth change, which can more truly reflect the properties of the film adsorbed on the surface of the QCM, and theoretically ensure the accuracy of the analytical data.

(2)分析处理的数据时QCM传感器在驱动电路的作用下产生的稳定信号。其谐振频率和半边半功率带宽都是在稳态下获得的,并且记录下的数据都是以频率的方式出现的,谐振频率和半边半功率带宽分别为106Hz和103Hz数量级。这比瞬时测量法得到的衰减延迟时间10-6s量级更容易做到精确测量。(2) The stable signal generated by the QCM sensor under the action of the drive circuit when analyzing the processed data. Its resonant frequency and half-half power bandwidth are obtained in a steady state, and the recorded data appear in the form of frequency. The resonant frequency and half-half power bandwidth are on the order of 10 6 Hz and 10 3 Hz, respectively. This is easier to measure accurately than the 10 -6 s decay delay time obtained by the instantaneous measurement method.

下面结合说明书附图对本发明做进一步描述。The present invention will be further described below in conjunction with the accompanying drawings.

附图说明Description of drawings

图1是QCM-D工作时的结构示意图。Figure 1 is a schematic diagram of the structure of QCM-D when it is working.

图2是本发明石英晶体微天平双参数检测装置的具体结构图。Fig. 2 is a specific structural diagram of the quartz crystal microbalance dual-parameter detection device of the present invention.

图3为本发明的方法流程图。Fig. 3 is a flow chart of the method of the present invention.

图4是本发明石英晶体微天平双参数检测方法中半边半功率带宽获取方法示意图。Fig. 4 is a schematic diagram of a method for obtaining a half-power half-power bandwidth in the dual-parameter detection method of the quartz crystal microbalance of the present invention.

图5是本发明石英晶体微天平双参数检测方法中谐振频率变化获取方法示意图。Fig. 5 is a schematic diagram of a method for acquiring resonance frequency changes in the dual-parameter detection method of the quartz crystal microbalance of the present invention.

具体实施方式Detailed ways

结合图2,一种石英晶体微天平(QCM)双参数检测装置,包括驱动信号单元、串联电路单元、信号处理单元、信号切换单元、A/D转换单元、控制单元、绘制单元。所述驱动信号单元,用于产生峰峰值固定的余弦信号;所述串联电路单元,包括被测石英晶体微天平和与其串联的电阻,用于在驱动信号单元的驱动下将石英晶体微天平的导纳信息转化为电压信号输出;所述信号处理单元,用于提取串联电路单元产生的信号的幅值和相位差信息;所述信号切换单元,用于将信号处理单元产生的信号切换;所述A/D转换单元,用于将信号切换单元输出的模拟信号转换成数字信号;所述控制单元,用于底层电路的控制以及数据信号的转发;所述绘制单元,具有处理功能,用于实现扫频设定和曲线绘制。2, a quartz crystal microbalance (QCM) dual-parameter detection device includes a drive signal unit, a series circuit unit, a signal processing unit, a signal switching unit, an A/D conversion unit, a control unit, and a drawing unit. The drive signal unit is used to generate a cosine signal with a fixed peak-to-peak value; the series circuit unit includes the measured quartz crystal microbalance and a resistor connected in series with it, and is used to drive the quartz crystal microbalance to The admittance information is converted into a voltage signal output; the signal processing unit is used to extract the amplitude and phase difference information of the signal generated by the series circuit unit; the signal switching unit is used to switch the signal generated by the signal processing unit; The A/D conversion unit is used to convert the analog signal output by the signal switching unit into a digital signal; the control unit is used for the control of the underlying circuit and the forwarding of the data signal; the drawing unit has a processing function and is used for Realize frequency sweep setting and curve drawing.

所述驱动信号单元包括频率合成器、自动控制增益器、放大器、低通滤波器。单片机发出控制信号控制频率合成器,所述频率合成器,用于产生余弦信号;所述自动控制增益器,用于恒定余弦信号峰峰值;所述放大器,用于放大余弦信号;所述低通滤波器,用于滤除余弦信号中的噪声信号。The driving signal unit includes a frequency synthesizer, an automatic control gainer, an amplifier, and a low-pass filter. The single-chip microcomputer sends a control signal to control the frequency synthesizer, and the frequency synthesizer is used to generate a cosine signal; the automatic control gainer is used for constant peak-to-peak value of the cosine signal; the amplifier is used to amplify the cosine signal; the low-pass Filter, used to filter out the noise signal in the cosine signal.

所述信号处理单元包括三路乘法器和低通滤波器串联的信号获取电路。第一路信号获取电路与石英晶体微天平一端连接,用于实现一路余弦信号自相关处理并获得直流电压值;第二路信号获取电路与石英晶体微天平另一端连接,用于实现另一路余弦信号自相关处理并获得直流电压值;第三路信号获取电路与石英晶体微天平两端连接,用于实现两路余弦信号互相关处理并获得相位差信息。The signal processing unit includes a signal acquisition circuit in which a three-way multiplier and a low-pass filter are connected in series. The first signal acquisition circuit is connected to one end of the quartz crystal microbalance to realize autocorrelation processing of one cosine signal and obtain the DC voltage value; the second signal acquisition circuit is connected to the other end of the quartz crystal microbalance to realize another cosine signal Signal autocorrelation processing and obtaining a DC voltage value; the third signal acquisition circuit is connected to both ends of the quartz crystal microbalance for realizing cross-correlation processing of two cosine signals and obtaining phase difference information.

具体的,该装置采用下述部件实现发明目的:Specifically, the device uses the following components to achieve the purpose of the invention:

(1)石英晶体微天平双参数检测装置中控制单元采用单片机凌阳061A;(1) The control unit in the quartz crystal microbalance dual-parameter detection device adopts the single-chip microcomputer Lingyang 061A;

(2)绘制单元为带有运算功能的PC机;(2) The drawing unit is a PC with computing functions;

(3)DDS芯片采用AD公司生产的AD9850,AD9850的创新型高速DDS内核提供一个32位频率控制字,对于125MHz基准时钟输入,输出调谐分辨率可以达到0.0291Hz;(3) The DDS chip adopts AD9850 produced by AD Company. The innovative high-speed DDS core of AD9850 provides a 32-bit frequency control word. For 125MHz reference clock input, the output tuning resolution can reach 0.0291Hz;

(4)AGC模块采用AD8367,AD8367是一款片上集成平方律探测器(Square-LawDetector)的可变增益放大器,运用该芯片可以方便的搭成自动增益控制器(AGC);(4) The AGC module adopts AD8367. AD8367 is a variable gain amplifier with integrated square-law detector (Square-Law Detector) on chip. Using this chip, it can be easily built into an automatic gain controller (AGC);

(5)运算放大器选用的是AD9632;(5) The operational amplifier is AD9632;

(6)低通滤波器采用椭圆形滤波器,滤除所需频率以上的高频信号;(6) The low-pass filter uses an elliptical filter to filter out high-frequency signals above the required frequency;

(7)乘法器部分采用高精度乘法器AD835,多路开关选用DG408,DG408是8通道,本发明中待AD转换的电压为三路完全可以满足要求;(7) multiplier part adopts high-precision multiplier AD835, multi-way switch selects DG408 for use, and DG408 is 8 channels, and the voltage to be converted by AD in the present invention is that three roads can fully meet the requirements;

(8)AD转换芯片选用AD7711,AD7711是24位高精度AD转换芯片,可直接接受来自传感器的低电平信号,并产生串行数字输出,能完成电路设计需求;(8) The AD conversion chip is AD7711. AD7711 is a 24-bit high-precision AD conversion chip, which can directly receive low-level signals from the sensor and generate serial digital output, which can complete the circuit design requirements;

(9)061A与PC机之间的通信是通过RS232来实现的,如PC机上无串口,则可以通过232-USB转换线来实现通信。(9) The communication between 061A and PC is realized through RS232. If there is no serial port on the PC, communication can be realized through 232-USB conversion line.

结合图2,具体地,上述装置的连接方式如下:With reference to Figure 2, specifically, the connection method of the above-mentioned devices is as follows:

单片机输出端连接频率合成器DDS输入端,频率合成器DDS输出端连接自动控制增益器AGC输入端,自动控制增益器AGC输出端连接放大器AMP输入端,放大器AMP输出端连接低通滤波器LPF输入端,低通滤波器LPF输出端连接石英晶体微天平QCM第一端,石英晶体微天平QCM第二端连接电阻R,所述三路信号获取电路中第一路乘法器的两个输入端均连接石英晶体微天平QCM第一端,第二路乘法器的两个输入端分别连接石英晶体微天平QCM第一端和第二端,第三路乘法器两个输入端均连接石英晶体微天平(QCM)第二端,所述三路信号获取电路中的低通滤波器分别与三路开关中的不同开关连接,三路开关输出端与A/D转换器连接,A/D转换器输出端与单片机连接,单片机与PC机连接。The MCU output is connected to the frequency synthesizer DDS input, the frequency synthesizer DDS output is connected to the automatic gain control AGC input, the automatic gain control AGC output is connected to the amplifier AMP input, and the amplifier AMP output is connected to the low-pass filter LPF input end, the output end of the low-pass filter LPF is connected to the first end of the quartz crystal microbalance QCM, the second end of the quartz crystal microbalance QCM is connected to the resistor R, and the two input ends of the first multiplier in the three-way signal acquisition circuit are both Connect the first terminal of the quartz crystal microbalance QCM, the two input terminals of the second multiplier are respectively connected to the first terminal and the second terminal of the quartz crystal microbalance QCM, and the two input terminals of the third multiplier are connected to the quartz crystal microbalance (QCM) second end, the low-pass filter in the three-way signal acquisition circuit is respectively connected with different switches in the three-way switch, the three-way switch output terminal is connected with the A/D converter, and the A/D converter outputs The terminal is connected with the single-chip microcomputer, and the single-chip microcomputer is connected with the PC.

结合图3,一种石英晶体微天平双参数检测方法,对空载和负载状态下的石英晶体微天平产生的两路余弦信号进行以下处理:Combined with Figure 3, a dual-parameter detection method for a quartz crystal microbalance, the following processing is performed on the two-way cosine signals generated by the quartz crystal microbalance under no-load and load conditions:

步骤S101,确定一频率,对QCM产生的两路余弦信号进行自相关和互相关处理,获得两路余弦信号各自的幅值及两者的相位差,Step S101, determining a frequency, performing autocorrelation and cross-correlation processing on the two cosine signals generated by the QCM, and obtaining the respective amplitudes and phase differences of the two cosine signals,

步骤S102,根据两路余弦信号的幅值及相位差获得该频率下的电导值,Step S102, obtaining the conductance value at the frequency according to the amplitude and phase difference of the two cosine signals,

步骤S103,更改频率,重复步骤S101和步骤S102,获取不同频率下的电导值,Step S103, change the frequency, repeat step S101 and step S102, obtain conductance values at different frequencies,

步骤S104,构建电导值和频率之间的关系,Step S104, constructing the relationship between conductance value and frequency,

步骤S105,获取谐振频率变化,及空载或负载状态下耗散因子。Step S105, obtaining the change of the resonant frequency, and the dissipation factor under no-load or load state.

具体地,LPF滤除信号中的高频噪声后,至此信号产生完毕,设为同时电阻R上电压此时QCM的导纳可以表示为:Specifically, after the LPF filters out the high-frequency noise in the signal, the signal is generated so far, and it is set to At the same time, the voltage across the resistor R At this time, the admittance of the QCM can be expressed as:

YY == 11 ZZ == ii ·&Center Dot; uu ·&Center Dot; 11 == uu ·&Center Dot; 11 RR ** 11 uu ·&Center Dot; 11 -- uu ·&Center Dot; 22 == 11 RR ** 11 uu ·&Center Dot; 11 uu ·&Center Dot; 22 -- 11 -- -- -- (( 11 ))

将u1和u2的表达式代入式(1)得到:Substitute the expressions of u 1 and u 2 into formula (1) to get:

将复数用欧拉公式展开可得:pluralize It can be expanded by Euler's formula:

相应的,电导值G和电纳值B为Correspondingly, the conductance value G and the susceptance value B are

通过式(4)、(5)所示。由幅值u1、u2以及两路信号的相位差便可得到QCM的电导和电纳。后续的信号处理部分将完成幅值和相位差信息的提取,这部分采用的是相关性原理,相关性原理部分的实现是乘法器加低通滤波器,利用自相关实现幅值信息的获取,利用互相关实现相位差信息的提取。Through the formula (4), (5) shown. From the amplitude u 1 , u 2 and the phase difference of the two signals The conductance and susceptance of the QCM can be obtained. Subsequent signal processing part will be completed The extraction of amplitude and phase difference information, this part uses the correlation principle, the realization of the correlation principle part is a multiplier plus a low-pass filter, using autocorrelation to realize the acquisition of amplitude information, and using cross-correlation to realize the phase difference information extraction.

自相关部分:Autocorrelation part:

uu 1111 == 11 TT ∫∫ 00 TT uu 11 (( tt )) 22 dd tt == 11 TT ∫∫ 00 TT (( uu 11 coscos ww tt )) 22 dd tt == 11 22 uu 11 22 -- -- -- (( 77 ))

互相关部分:Cross-correlation part:

此时at this time

uu 11 == 22 uu 1111 -- -- -- (( 1010 ))

uu 22 == 22 uu 22twenty two -- -- -- (( 1111 ))

将式(10)、(11)以及(13)分别代入式(4)、式(5)得到:Substitute equations (10), (11) and (13) into equations (4) and (5) respectively to get:

GG == 11 AA RR (( uu 1212 uu 22twenty two -- 11 )) -- -- -- (( 1414 ))

BB == 11 AA RR uu 1111 uu 22twenty two ·&Center Dot; 11 -- uu 1212 22 uu 1111 uu 22twenty two -- -- -- (( 1515 ))

AA == uu 1111 uu 22twenty two -- 22 uu 1212 uu 22twenty two ++ 11 -- -- -- (( 1616 ))

由于R为已知量,所以只需测得u11、u12以及u22便可得到此频率下QCM电导和电纳值,当改变信号的频率,便可得到不同频率下的电导和电纳值,以频率值为横坐标,电导电纳值为纵坐标便可得到电导电纳关于频率的曲线,还可以获得导纳圆。分析电导和电纳曲线可以获得QCM此时的谐振频率、半边半功率带宽等信息。Since R is a known quantity, it is only necessary to measure u 11 , u 12 and u 22 to obtain the conductance and susceptance of QCM at this frequency. When changing the frequency of the signal, the conductance and susceptance at different frequencies can be obtained value, the frequency value is the abscissa, and the conductance value is the ordinate, the curve of the conductance relative to the frequency can be obtained, and the admittance circle can also be obtained. Analyzing the conductance and susceptance curves can obtain information such as the resonant frequency and half-power half-power bandwidth of the QCM at this time.

当QCM处于工作状态时(即表面吸附物质),开始新的一轮频率扫描与数据采集,便可得到工作状态下的谐振频率、半边半功率带宽,再与空载时的作比较,便可得到Δf。When the QCM is in the working state (that is, the surface adsorbed substances), start a new round of frequency scanning and data acquisition, and then you can get the resonant frequency and half-half power bandwidth in the working state, and compare them with those at no-load. Get Δf.

结合图4,假设一次扫描后获得的导纳曲线如图3所示。取所获得的电导的峰值的并过此值作一水平线,此时它与曲线所交的点称为半功率点,图中A、B两点,Γ则称为半边半功率带宽,其中为电导值为最大电导值Gmax时所对应的频率,f为谐振频率。根据即可得到此时耗散因子D。In combination with FIG. 4 , it is assumed that the admittance curve obtained after one scan is shown in FIG. 3 . Take the peak value of the conductance obtained as And pass this value to draw a horizontal line. At this time, the point where it intersects with the curve is called the half-power point. In the figure, A and B are two points, and Γ is called the half-side half-power bandwidth. in is the conductance value of the maximum conductance value G max When the corresponding frequency, f is the resonant frequency. according to The dissipation factor D at this time can be obtained.

结合图5,空载和负载状态下扫描得到的电导曲线,其中谐振频率变化Δf为电导峰值之间频率差,半边半功率带宽的获取方式如图4所示,同时图5中还可以获得两次扫描中半边半功率带宽差ΔΓ。Combined with Figure 5, the conductance curves obtained by scanning under no-load and load conditions, in which the resonance frequency change Δf is the frequency difference between the conductance peaks, the half-power half-power bandwidth acquisition method is shown in Figure 4, and two can also be obtained in Figure 5 The half-power half-power bandwidth difference ΔΓ in the sub-scan.

Claims (8)

1. A quartz crystal microbalance double-parameter detection device is characterized by comprising:
the driving signal unit is used for generating a cosine signal with a fixed peak-to-peak value;
the series circuit unit comprises a tested quartz crystal microbalance and a resistor connected with the tested quartz crystal microbalance in series and is used for converting admittance information of the quartz crystal microbalance into a voltage signal to be output under the driving of the driving signal unit;
a signal processing unit for extracting amplitude and phase difference information of the signal generated by the series circuit unit;
the signal switching unit is used for switching the signal generated by the signal processing unit;
the A/D conversion unit is used for converting the analog signal output by the signal switching unit into a digital signal;
the control unit is used for controlling the bottom layer circuit and forwarding the data signal; and
and the drawing unit has a processing function and is used for realizing sweep frequency setting and curve drawing.
2. The quartz crystal microbalance dual parameter detection device of claim 1, wherein the driving signal unit comprises:
a frequency synthesizer for generating a cosine signal;
the automatic gain controller is used for keeping the peak value of the cosine signal constant;
an amplifier for amplifying the cosine signal;
and the low-pass filter is used for filtering the noise signal in the cosine signal.
3. The quartz crystal microbalance double-parameter detection device of claim 1, wherein the signal processing unit comprises a signal acquisition circuit with a three-way multiplier and a low-pass filter connected in series,
the first path of signal acquisition circuit is connected with one end of the quartz crystal microbalance and is used for realizing the autocorrelation processing of a path of cosine signals and acquiring a direct-current voltage value;
the second path of signal acquisition circuit is connected with the other end of the quartz crystal microbalance and is used for realizing the autocorrelation processing of the other path of cosine signal and acquiring a direct-current voltage value;
and the third signal acquisition circuit is connected with two ends of the quartz crystal microbalance and is used for realizing the cross-correlation processing of the two cosine signals and acquiring phase difference information.
4. The quartz crystal microbalance double-parameter detection method adopting the device of any one of the preceding claims is characterized in that the following processing is carried out on two paths of cosine signals generated by the quartz crystal microbalance under no-load and load states:
determining a frequency, obtaining respective amplitudes of the two cosine signals and a phase difference between the two cosine signals by adopting autocorrelation and cross-correlation processing, obtaining a conductance value under the frequency according to the amplitudes and the phase difference of the two cosine signals,
changing the frequency, obtaining the conductance values under different frequencies,
constructing a relationship between the conductance value and the frequency, an
And acquiring the change of the resonant frequency and the dissipation factor in the no-load or load state.
5. The quartz crystal microbalance double parameter detection method according to claim 4,
the resonance frequency changes into a frequency difference between conductance peak values in the no-load and load states;
the dissipation factor in the no-load state is the ratio of twice half-power bandwidth to resonant frequency in the no-load state;
the dissipation factor under the load state is the ratio of twice half-power bandwidth under the load state to the resonant frequency.
6. The quartz crystal microbalance double parameter detection method of claim 5, wherein the half-side half-power bandwidthWhereinThe conductance value is the maximum conductance value GmaxIs/are as followsThe frequency corresponding to the time, f is the resonance frequency.
7. The quartz crystal microbalance double-parameter detection method according to claim 4, wherein the respective direct current voltage values obtained after the autocorrelation processing of the two cosine signals are
u 11 = 1 2 u 1 2
u 22 = 1 2 u 2 2
Wherein u is1、u2Is the cosine signal amplitude;
the phase difference obtained after the two cosine signals are processed in a cross-correlation way
Wherein u is12A dc signal output for cross-correlation.
8. The quartz crystal microbalance double parameter detection method of claim 7, wherein the conductance value is G = 1 AR ( u 12 u 22 - 1 ) , Wherein,r is an and stoneResistance values of quartz crystal microbalances connected in series.
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