CN111999383B - Quartz crystal microbalance and in-situ regeneration method of sensing chip thereof - Google Patents
Quartz crystal microbalance and in-situ regeneration method of sensing chip thereof Download PDFInfo
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- 238000011069 regeneration method Methods 0.000 title claims abstract description 69
- 238000003380 quartz crystal microbalance Methods 0.000 title claims abstract description 39
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 15
- 230000008929 regeneration Effects 0.000 claims abstract description 61
- 238000001514 detection method Methods 0.000 claims description 42
- 238000000034 method Methods 0.000 claims description 20
- 230000004044 response Effects 0.000 claims description 19
- 238000010926 purge Methods 0.000 claims description 9
- 238000005259 measurement Methods 0.000 claims description 6
- 230000001172 regenerating effect Effects 0.000 claims description 3
- 239000000126 substance Substances 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 6
- 238000009825 accumulation Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 230000010355 oscillation Effects 0.000 description 14
- 238000012545 processing Methods 0.000 description 14
- 238000012360 testing method Methods 0.000 description 11
- 238000011084 recovery Methods 0.000 description 9
- 238000005070 sampling Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 230000035945 sensitivity Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000003795 desorption Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000013076 target substance Substances 0.000 description 2
- 238000009423 ventilation Methods 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- VONWDASPFIQPDY-UHFFFAOYSA-N dimethyl methylphosphonate Chemical compound COP(C)(=O)OC VONWDASPFIQPDY-UHFFFAOYSA-N 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
- G01N29/02—Analysing fluids
- G01N29/022—Fluid sensors based on microsensors, e.g. quartz crystal-microbalance [QCM], surface acoustic wave [SAW] devices, tuning forks, cantilevers, flexural plate wave [FPW] devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B5/00—Cleaning by methods involving the use of air flow or gas flow
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
- G01N29/02—Analysing fluids
- G01N29/036—Analysing fluids by measuring frequency or resonance of acoustic waves
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
- G01N29/22—Details, e.g. general constructional or apparatus details
- G01N29/222—Constructional or flow details for analysing fluids
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
- G01N29/22—Details, e.g. general constructional or apparatus details
- G01N29/24—Probes
- G01N29/2437—Piezoelectric probes
- G01N29/2443—Quartz crystal probes
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2291/00—Indexing codes associated with group G01N29/00
- G01N2291/01—Indexing codes associated with the measuring variable
- G01N2291/014—Resonance or resonant frequency
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2291/00—Indexing codes associated with group G01N29/00
- G01N2291/02—Indexing codes associated with the analysed material
- G01N2291/021—Gases
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2291/00—Indexing codes associated with group G01N29/00
- G01N2291/02—Indexing codes associated with the analysed material
- G01N2291/028—Material parameters
- G01N2291/02809—Concentration of a compound, e.g. measured by a surface mass change
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Acoustics & Sound (AREA)
- Crystallography & Structural Chemistry (AREA)
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
- Measurement Of Mechanical Vibrations Or Ultrasonic Waves (AREA)
Abstract
The invention discloses an in-situ regeneration method of a quartz crystal microbalance sensing chip, and aims to solve the technical problems that an existing sensor needs to be frequently disassembled, is inconvenient to operate and has poor regeneration effect. The invention tracks the resonance frequency of the sensing chip in real time in an in-situ state, synchronously transmits the same-frequency high-energy regenerated radio frequency signal, and removes the residual accumulation of the detected substances on the surface of the sensing chip. The invention has the beneficial effects that: has the advantages of no need of disassembly, rapid regeneration, good effect and environmental protection.
Description
Technical Field
The invention relates to the technical field of sensors, in particular to a quartz crystal microbalance and a sensor chip in-situ regeneration method thereof.
Background
The mass sensor based on the Quartz Crystal Microbalance (QCM) is paid attention to because of the advantages of non-marking, high sensitivity, quick response, low cost and low energy consumption, and the principle is that after the surface of a sensitive film of the quartz crystal sensing chip adsorbs target molecules, the mass of the surface of the quartz crystal sensing chip is changed, so that the resonance frequency of the quartz crystal sensing chip is changed, the concentration of a target substance to be detected is converted into a corresponding frequency signal to be output, and the concentration of the target substance is detected.
In the application of gas detection by using a quartz crystal microbalance, the sensing chip is subjected to a plurality of detection-recovery cycle processes, so that the sensing chip is subjected to good adsorption (quick response and high sensitivity) -recovery (quick desorption and repeated use) and the residual accumulation of detected substances on the surface of the sensing chip is effectively removed, so that the sensing chip is efficiently regenerated, and the method is an important index for the sensor to meet the practical application performance.
In order to remove the detected substances adsorbed on the surface of the sensing chip, clean gas is generally used for purging, so that the activity is recovered for the next detection cycle, and after the detection-purging recovery cycles are carried out, the detected substances on the surface of the sensing chip cannot be completely removed and accumulated by using a gas purging method, so that the sensitivity and the selectivity of the sensing chip are continuously reduced, and the detection performance of the sensing chip is affected until the sensing chip is disabled. When the purging cannot realize good recovery of the sensing chip, the sensing chip is usually detached from the sensor, and chemical or physical regeneration treatment is carried out to remove residual and accumulation of the detected substances so as to restore the detection function.
The regeneration treatment has the following defects: firstly, the sensing chip needs to be frequently disassembled to carry out chemical or physical regeneration treatment in the detection work, the operation is complex, fine and time-consuming, and even the sensing chip is damaged; secondly, the installation stress generated by repeated disassembly and assembly can cause poor repeatability of the measurement result and influence the measurement accuracy; thirdly, the field operation is needed to be carried out manually, so that the online and unattended detection mode is difficult to realize.
Disclosure of Invention
The invention provides a quartz crystal microbalance and a sensor chip in-situ regeneration method thereof, which are used for solving the technical problems that the existing sensor needs to be frequently disassembled, is inconvenient to operate and has poor regeneration effect.
In order to solve the technical problems, the invention adopts the following technical scheme:
a quartz crystal microbalance is designed comprising: a sensor chip; the sensor chip is connected with the regeneration radio frequency module and the frequency detection module through the change-over switch in time intervals; when the frequency detection module detects that the vibration frequency of the sensor chip is lower than a threshold value, the regeneration radio frequency module outputs a regeneration radio frequency signal with the same vibration frequency as the sensor chip.
By inputting the radio frequency signals with the same frequency as the sensing chip, resonance is formed, residues attached to the chip can be oscillated and desorbed, disassembly is not needed in the process, and the chip performance degradation caused by disassembly is avoided.
Further, the device also comprises a processor module, the input end of the processor module is correspondingly connected with the output end of the frequency detection module, the instruction output end of the processor module is connected with the input end of the regeneration radio frequency module, the output end of the regeneration radio frequency module is correspondingly connected with the change-over switch, the change-over switch comprises a fixed contact, a first movable contact and a second movable contact, the fixed contact is connected with the sensor chip, the first movable contact is connected with the input end of the data acquisition module, and the second movable contact is connected with the output end of the regeneration radio frequency module.
Further, the regeneration radio frequency module comprises a frequency setting unit and an amplitude adjusting unit; the frequency setting unit is used for adjusting the frequency of the regenerated radio frequency signal to be the same as the vibration frequency of the sensor chip, and the amplitude adjusting unit is used for adjusting the voltage of the regenerated radio frequency signal.
The method for in-situ regeneration of the sensor chip by using the quartz crystal microbalance is also designed, and comprises the following steps:
(1) Collecting the eigenfrequency of the quartz crystal microbalance according to claim 1 when the sensor chip is not contacted with the sample, as a reference frequency;
(2) The sample contacts the sensor chip for the first time, and the frequency value is collected as the first measurement frequency after the vibration frequency of the sensor chip is stable;
(3) Purging the sensor chip, and then contacting another sample to be tested with the sensor chip to obtain the vibration frequency variation of the sensor chip before and after contacting the sample as frequency output data of the quartz crystal microbalance;
(4) Repeating the step (3) and comparing the frequency response of the sensor chip after being contacted with the sample with the first-measurement frequency of the step (2) to obtain a difference value, and starting the step (5) when the difference value is larger than a threshold value;
(5) And (3) inputting a regenerated radio frequency signal with the same vibration frequency as that of the sensor chip in real time until the eigenfrequency of the sensor chip is recovered to a set value.
Further, the set value in the step (5) is 80% -100% of the reference frequency in the step (1),
further, the threshold value in the step (4) is 70-90% of the first frequency value in the step (2).
Further, in the step (5), the voltage of the regenerated radio frequency signal is 2-10V.
Further, after the input time of the regenerated radio frequency signal in the step (5) is over, the eigenfrequency of the sensor chip still cannot be recovered to the preset value, and then the sensor chip is judged to be scrapped.
Further, before judging that the sensor chip is scrapped, repeatedly inputting 1-3 times of regenerated radio frequency signals, wherein the input time lasts for 10-100s each time.
Compared with the prior art, the invention has the beneficial technical effects that:
1. the invention can avoid the operation of manually disassembling and assembling the chip, improve the regeneration efficiency and quality, does not need to decompose the sensor assembly, and keeps the stability of the equipment.
2. The invention does not use chemical reagent, avoids damage to the sensor chip caused by mechanical and heating regeneration, is convenient for realizing remote manual control and automatic control, and is an efficient, green and environment-friendly sensor chip regeneration method.
Drawings
FIG. 1 is a schematic diagram of a regenerating device for a quartz crystal microbalance sensor chip of the invention.
FIG. 2 is a flow chart of the regeneration of the quartz crystal microbalance sensor chip of the invention.
Fig. 3 is a schematic structural diagram of a quartz crystal microbalance gas detector of the invention.
Fig. 4 is a waveform diagram of the reproduced signal of the quartz crystal microbalance sensor of the present invention.
Fig. 5 is a schematic circuit diagram of a radio frequency output module of the quartz crystal microbalance sensor according to the invention.
In the figure, 1 is a central processing unit, 2 is a regeneration radio frequency output module, 3 is a detection oscillation module, 4 is a QCM sensor, 5 is a sensing chip, 6 is a change-over switch, 7 is an air distribution box, 8 is a sampling fan, 9 is a change-over valve A,10 is a change-over valve B,11 is a test gas inlet, 12 is a test gas outlet, 13 is a fresh air inlet, 14 is a fresh air outlet, 15 is a test gas generator, 16 is a gas mixing fan, and 17 is a ventilation fan.
Detailed Description
The following examples are given to illustrate the invention in detail, but are not intended to limit the scope of the invention in any way.
The procedures involved or relied on in the following embodiments are conventional procedures or simple procedures in the technical field, and those skilled in the art can make routine selections or adaptation according to specific application scenarios.
The unit modules, components, structures, mechanisms, sensors, and other devices according to the following examples are commercially available products unless otherwise specified.
In the description of the present application, it should be understood that the terms "upper," "lower," "front," "rear," "left," "right," "top," "bottom," "inner," "outer," and the like indicate an orientation or a positional relationship based on that shown in the drawings, merely for convenience of description and to simplify the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present application. Reference to "first," "second," etc. in this application is for distinguishing between similar objects and not necessarily for describing a particular sequential or chronological order.
Example 1: referring to fig. 1, an output end of a central processing unit 1 of a QCM is connected with a regeneration radio frequency output module 2 and a detection oscillation module 3, meanwhile, the central processing unit 1 controls a change-over switch 6, the change-over switch 6 is single-pole double-throw type and comprises a fixed contact, a movable contact a and a movable contact b, the movable contact a is connected with the detection oscillation module 3, the movable contact b is connected with the regeneration radio frequency output module 2, and the fixed contact of the change-over switch 6 is connected to a sensing chip 5 in the QCM sensor 4 through a wire. The central processing unit 1 can acquire the oscillation frequency of the sensing chip 5 in real time through the data acquisition module.
When the change-over switch 6 is placed in a state, the detection oscillation module 3 drives the sensing chip 5 to be in a detection working state, the sensing chip 5 generates oscillation, the data acquisition module transmits an oscillation frequency signal f2 when the sensing chip 5 works to the central processing unit 1 and records the oscillation frequency signal f2, the data processing module of the central processing unit 1 judges whether the f2 is normal, if the change-over switch is abnormal, the central processing unit 1 generates a control signal and transmits the control signal together with the frequency signal f2 to the regeneration radio frequency output module 2, and meanwhile, the change-over switch is controlled to be placed in a position b, at the moment, the regeneration radio frequency signal f1 which is the same in frequency as the signal f2 and is 2-10 times higher in voltage is transmitted to the sensing chip 5, after the action time of 10-100s is passed, the in-situ regeneration process of the sensing chip 5 is completed, and the change-over switch 6 is placed in the state a after the regeneration is completed, so that the sensing chip 5 is restored to the detection working state.
The change-over switch 6 may be mechanical, e.g. a relay, or electronic, e.g. a transistor. The regeneration radio frequency output module 2 may be a digital oscillation circuit functional unit, including DDS, FPGA and analog circuit functional unit, in this embodiment, the circuit structure shown in fig. 5 is adopted, the single-chip controller C8051F130 generates three commands of frequency control, waveform setting and duty cycle adjustment according to the input parameters of the central processing unit 1, the radio frequency generator MAX038 receives the commands to generate radio frequency signals with required frequencies, and then the voltage of the signals is raised to 2-10 times higher than the F2 signal through amplitude adjustment, which is the required regeneration radio frequency signals, and in general, the final voltage value of the regeneration signals is 2-10V; the central processing unit 1 can be connected to the terminal equipment in a wireless mode, so that remote control is convenient.
Referring to fig. 2, in the process of regenerating the sensor of the quartz crystal microbalance, (1) after the quartz crystal microbalance is started, a sensing chip is arranged in a detection working condition, and an instrument is preheated and self-inspected; (2) After preheating, stabilizing a frequency baseline, and keeping a frequency fluctuation value between +/-0.5 Hz; (3) Collecting and storing the intrinsic frequency value of the sensing chip by the central processing unit 1 and built-in QCM data processing software, and pre-storing the value as a reference frequency value; (4) Sampling and testing the detected substance, measuring and storing a first detection frequency response value, and setting the value as the first detection frequency response value; (5) The performance of the sensing chip 5 is reduced after 10-100 repeated detection-recovery cycles, the frequency response is reduced, and the system is instantly compared with the first-measurement frequency response value; (6) Setting the frequency response value to be invalid when the detection frequency response value is less than 85% of the first detection frequency response value; (7) A regeneration instruction set is sent to the regeneration radio frequency output module 2 in an automatic or manual operation mode, wherein the instruction set comprises real-time frequency setting, voltage setting and an instruction for switching the sensing chip 5 to a regeneration working condition; (8) The regeneration radio frequency output module 2 tracks the real-time frequency of the sensing chip and transmits a high-energy regeneration radio frequency signal which has the same value as the real-time frequency and has the voltage 2-10 times higher than the working voltage of the sensing chip 5, and the transmission time is 10-100s; (9) The change of the frequency of the sensing chip is tracked and measured in real time, and the central processing unit 1 and QCM data processing software are compared with a pre-stored reference frequency value; (10) After the tracking and measuring sensing chip is restored to the reference frequency value, an ending instruction is sent to realize accumulation and removal of residues of detected substances on the surface of the sensing chip, and in-situ regeneration of the sensing chip is completed; (11) If the regenerated radio frequency signal is input for 1-3 times and the sensing chip still cannot be restored to 90% -100% of the reference frequency, the sensing chip is judged to be scrapped.
Example 2: a quartz crystal microbalance gas detector, see fig. 3, using the experimental test gas DMMP (dimethyl methylphosphonate) at a concentration of 30ppb. The QCM sensor 4 is arranged between the switching valves a and B. The experimental procedure and results were as follows:
injecting a certain amount of dimethyl methyl phosphate (DMMP) liquid into the test gas generator 15, gasifying at 185 ℃, releasing the liquid into the gas distribution box 7, starting the gas mixing fan 16 to obtain air+DMMP mixed gas (experimental test gas) with the concentration of 30ppb, starting the sampling fan to enable the test gas to enter from the test gas inlet 11, leading out from the test gas outlet 12 for 10-60 seconds, switching the valve to a state that the fresh air inlet 13 is communicated with fresh air 14, and continuously purging for 10-300 seconds; the above process is repeated for 20 times, the DMMP gas is repeatedly sampled for 20 times through the QCM sensor 4, and the QCM sensor chip 5 is purged and recovered after each sampling, and the detection signal is detected by the QCM central processing unit and the control system, so that the detection signal is reduced to 62Hz from the initial 80Hz, the detection response value is reduced by 23%, and the fact that the surface residues of the sensor chip are more is prompted, so that the sensitivity is reduced. At this time, the QCM sensing chip 4 is disconnected from the detection oscillation module 3 and communicated with the regeneration radio frequency output module 2, 10V is applied for 30 seconds with the same resonance frequency, and then the sensing chip is communicated with the sensing chip oscillation module 2 again, and the detection result is as follows: the resonance frequency of the sensing chip is increased by about 55Hz, the response value of the DMMP with the detection concentration of 30ppb is 78Hz, the regeneration effect of nearly 98 percent is achieved, and compared with the last detection before regeneration, the recovery time is reduced from 400 seconds to 255 seconds, and the reduction amplitude is 36 percent. After the detection is finished, the ventilation fan 17 is started, the fresh air inlet 13 and the fresh air outlet 14 are opened, and the air distribution box 7 is cleaned.
The oscillation frequency of the quartz crystal microbalance sensing chip is shown in fig. 4, (1) is a sampling point before regeneration, (1-1) is a sampling point after regeneration, (4) is a regeneration starting point, (4-1) is a regeneration ending point, (5) is a baseline increase value after regeneration of 55Hz, and (6) is the noise frequency generated during the switching of detection-regeneration working conditions; (2) fresh air purging recovery time before regeneration is 400 seconds; (3) the detection response value before regeneration is 63Hz; (2-1) the fresh air recovery time after regeneration is 255 seconds; (3-1) is the post-regeneration detection response value 78 Hz; compared with the method (2), the method (2-1) reduces 145 seconds, and shortens the fresh air recovery time by 36%; (3-1) was increased by 16Hz over (3) by 26%. The test results show that after the same-frequency oscillation regeneration treatment, the detection sensitivity and fresh air purging desorption performance of the chip are improved, and the residues of detected substances are also removed well, so that the service life of the chip is prolonged.
Therefore, the DMMP gas is repeatedly sampled 20 times by the QCM sensor before regeneration, and is detected by the QCM central processing unit 1 and the control system, the response value of the detection signal is 63Hz, and the detection period is 400 seconds. At this time, the sensing chip is disconnected from the oscillation module, an alternating voltage of 10V with the same resonance frequency is applied for 30 seconds (data acquisition is suspended), then the sensing chip is connected with the QCM again, and the detection result is as follows: the resonance frequency of the sensing chip is raised by about 57Hz, the detection response value of DMMP with the detection concentration of 30ppb after regeneration is 78Hz, the response value is increased by 23.8% compared with the detection signal response value before regeneration, the detection period is reduced from 400 seconds to 300 seconds, and the detection period is shortened by 25%.
While the present invention has been described in detail with reference to the drawings and the embodiments, those skilled in the art will understand that various specific parameters in the above embodiments may be changed without departing from the spirit of the invention, and a plurality of specific embodiments are common variation ranges of the present invention, and will not be described in detail herein.
Claims (8)
1. A quartz crystal microbalance, comprising a sensor chip; the sensor chip is connected with the regeneration radio frequency module and the frequency detection module through the change-over switch in time intervals; when the frequency detection module detects that the vibration frequency of the sensor chip is lower than a threshold value, the regeneration radio frequency module outputs a regeneration radio frequency signal with the same vibration frequency as the sensor chip to the sensor chip; the regeneration radio frequency module comprises a frequency setting unit and an amplitude adjusting unit; the frequency setting unit is used for adjusting the frequency of the regenerated radio frequency signal so that the frequency is the same as the vibration frequency of the sensor chip in real time, and the amplitude adjusting unit is used for adjusting the voltage of the regenerated radio frequency signal.
2. The quartz crystal microbalance according to claim 1, further comprising a processor module, wherein the input of the processor module is correspondingly connected to the output of the frequency detection module, the instruction output of the processor module is connected to the input of the regeneration radio frequency module, the output of the regeneration radio frequency module is correspondingly connected to the change-over switch, the change-over switch comprises a stationary contact, a first movable contact and a second movable contact, the stationary contact is connected to the sensor chip, the first movable contact is connected to the input of the data acquisition module, and the second movable contact is connected to the output of the regeneration radio frequency module.
3. A method for in-situ regeneration of a sensor chip using the quartz crystal microbalance of claim 1, comprising the steps of:
(1) Collecting the eigenfrequency of the quartz crystal microbalance according to claim 1 when the sensor chip is not contacted with the sample, as a reference frequency;
(2) The method comprises the steps that a sample contacts the sensor chip for the first time, a frequency value is acquired after the vibration frequency of the sensor chip is stable, and the frequency value is used as a first measurement frequency;
(3) Purging the sensor chip, and then contacting another sample to be tested with the sensor chip to obtain the vibration frequency variation of the sensor chip before and after contacting the sample as frequency output data of the quartz crystal microbalance;
(4) Repeating the step (3) and comparing the frequency response of the sensor chip after the sensor chip is contacted with the sample with the first measured frequency in the step (2) to obtain a difference value, and starting the step (5) when the difference value is larger than a threshold value;
(5) And (3) inputting a regenerated radio frequency signal with the same vibration frequency as the real-time one to the sensor chip until the intrinsic frequency of the sensor chip is recovered to a set value.
4. The method of in-situ regeneration of a sensor chip according to claim 3, wherein the set value in step (5) is 80% -100% of the reference frequency in step (1).
5. A method of regenerating a sensor chip in situ according to claim 3, wherein the threshold value in step (4) is 70-90% of the first frequency value in step (2).
6. The method of in-situ regeneration of a sensor chip according to claim 3, wherein the regenerated rf signal in step (5) has a voltage of 2-10V.
7. The method for in-situ regeneration of a sensor chip according to claim 3, wherein after the end of the time for inputting the regenerated rf signal in step (5), the intrinsic frequency of the sensor chip cannot be restored to a predetermined value, and the sensor chip is determined to be scrapped.
8. The method for in-situ regeneration of a sensor chip according to claim 7, wherein the regeneration radio frequency signal is repeatedly input 1 to 3 times for 10 to 100 seconds before the sensor chip is judged to be scrapped.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1286668A (en) * | 1998-11-20 | 2001-03-07 | 普拉乌道株式会社 | Method of treating liquid, liquid treatment apparatus, and liquid treatment system |
| TWI220687B (en) * | 2003-08-29 | 2004-09-01 | Ind Tech Res Inst | A quartz crystal microbalance apparatus |
| CN200982958Y (en) * | 2006-07-07 | 2007-11-28 | 中国科学技术大学 | Measurement device of quartz crystal micro balance attenuation factor with controllable surge range |
| CN103646873A (en) * | 2013-11-29 | 2014-03-19 | 上海华力微电子有限公司 | A method for removing photoresist |
| CN104048893A (en) * | 2014-06-19 | 2014-09-17 | 中国科学院理化技术研究所 | Quartz crystal microbalance sensor for detecting HCN gas and manufacturing method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI354777B (en) * | 2007-12-28 | 2011-12-21 | Tatung Co | Dual mode measurement system with quartz crystal m |
-
2020
- 2020-09-08 CN CN202010932417.7A patent/CN111999383B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1286668A (en) * | 1998-11-20 | 2001-03-07 | 普拉乌道株式会社 | Method of treating liquid, liquid treatment apparatus, and liquid treatment system |
| TWI220687B (en) * | 2003-08-29 | 2004-09-01 | Ind Tech Res Inst | A quartz crystal microbalance apparatus |
| CN200982958Y (en) * | 2006-07-07 | 2007-11-28 | 中国科学技术大学 | Measurement device of quartz crystal micro balance attenuation factor with controllable surge range |
| CN103646873A (en) * | 2013-11-29 | 2014-03-19 | 上海华力微电子有限公司 | A method for removing photoresist |
| CN104048893A (en) * | 2014-06-19 | 2014-09-17 | 中国科学院理化技术研究所 | Quartz crystal microbalance sensor for detecting HCN gas and manufacturing method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| Microfluidic quartz-crystal-microbalance (QCM) sensors with specialized immunoassays for extended measurement range and improved reusability;J.-W. Thies 等;《Microelectronic Engineering》;第25-30页 * |
| 石英晶体微天平传感器在生物和化学领域的应用;崔学晨等;《现代科学仪器》;第68-76页 * |
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