CN115876299A - Device and method for quartz crystal microbalance mass calibration at low temperature - Google Patents
Device and method for quartz crystal microbalance mass calibration at low temperature Download PDFInfo
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Abstract
The invention discloses a device and a method for calibrating the mass of a quartz crystal microbalance at low temperature, which comprises the following steps: the device comprises a low-temperature sealed cavity, ellipsometer equipment, a temperature control unit and a pressure and component control unit; a low-temperature cold stage, an emission electrode and a target material are arranged in the low-temperature sealing cavity, the low-temperature cold stage is used for placing a quartz crystal oscillator, and the target material is uniformly deposited on the surface of the quartz crystal oscillator through the emission electrode of magnetron sputtering; the ellipsometer equipment comprises a polarizer and an analyzer, wherein the polarizer and the analyzer are respectively arranged on two side walls of the low-temperature sealed cavity; the temperature control unit is arranged at the lower part of the low-temperature cooling table and is used for controlling the temperature of the cold surface of the low-temperature cooling table within a set range; and the pressure and component control unit is used for controlling the low-temperature sealed cavity to reach the vacuum degree required by the experiment and providing the atmosphere required by the experiment. By utilizing the method, the relationship curve between the frequency of the quartz crystal oscillator and the deposition quality on the surface of the quartz crystal oscillator under the low-temperature condition can be obtained, and the aim of low-temperature quality calibration is fulfilled.
Description
Technical Field
The invention relates to the technical field of quartz crystal oscillators, in particular to a device and a method for calibrating the mass of a quartz crystal microbalance at low temperature.
Background
In 1880 Pieer Curie and Jack Curie brothers found that tourmaline has piezoelectric effect. In the next year, the inverse piezoelectric effect is verified through experiments, and the positive and inverse piezoelectric constants are obtained. The piezoelectric effect means that when some dielectrics are deformed by external force in a certain direction, polarization phenomenon is generated in the dielectrics, and charges with opposite positive and negative polarities are generated on two opposite surfaces of the dielectrics. With the progress of research, more and more substances are found to have piezoelectric effect, including quartz crystals.
In 1959, sauerbrey applied piezoelectric quartz crystals as an ultrasensitive weighing device, and proposed that the mass per unit area of the surface of the quartz crystal is proportional to the resonance frequency shift, namely a Sauerbrey equation. The mass sensitivity constant in the equation depends only on the thickness and inherent properties of the quartz crystal plate, including its density and shear modulus. The equation is satisfied only when the rigid film is uniformly distributed on the surface and has a thickness sufficiently thinner than the quartz crystal plate. Quartz Crystal Microbalances (QCMs) are sensors that measure mass deposition or desorption caused by changes in crystal resonance. At small mass loads, the Sauerbrey equation relates the change in sample mass linearly to the change in resonance of the sensing crystal.
Quartz crystal microbalances have numerous advantages in practical applications. The quartz crystal oscillator is used as a core component, has stable frequency and strong anti-interference capability, and is widely used as a standard frequency source in the fields of remote communication, satellite communication, precise measurement instruments and the like; and the quartz crystal oscillator has the characteristics of miniaturization and chip type, has low manufacturing cost, is convenient to integrate in various products, and can carry out in-situ measurement when being applied to the field of quality detection.
Quartz crystal microbalances have become a particularly attractive device in many scientific fields. In the field of physical chemistry, additional information can be provided for analyzing the characteristics of the tested liquid and the thin film; in the field of aerospace, a novel quartz crystal microbalance device Twin-QCM with temperature control is used to evaluate outgassing characteristics during spacecraft development. In the low-temperature field, nanogram-level precision measurement of the quartz crystal microbalance provides a feasible idea for detecting trace water desublimation.
For example, chinese patent publication No. CN107290240a discloses a quartz crystal microbalance, which includes: the device comprises a quartz crystal, a high-frequency oscillator and a data processing device, wherein the quartz crystal microbalance obtains the quantity of substances of an object to be detected by measuring the oscillation frequency change of the quartz crystal before and after the object to be detected is adsorbed.
For the detection of trace water desublimation, the deposition of nanogram-grade mass on a quartz crystal oscillator needs to be controlled at low temperature. The difficulty is how to detect the actual quality of the deposit in the low-temperature sealed cavity; meanwhile, since the oscillation frequency of the quartz crystal is greatly affected by the temperature, the temperature control of the cold surface also needs to be accurate enough.
Disclosure of Invention
The invention provides a device and a method for calibrating the mass of a quartz crystal microbalance at low temperature, which can obtain the relation curve between the frequency of a quartz crystal oscillator and the deposited mass on the surface of the quartz crystal oscillator at low temperature so as to achieve the aim of calibrating the mass at low temperature.
An apparatus for low temperature quartz crystal microbalance mass calibration, comprising: the device comprises a low-temperature sealing cavity, ellipsometer equipment, a temperature control unit and a pressure and component control unit;
transparent windows are arranged on two sides of the low-temperature sealed cavity, a low-temperature cold stage, an emission electrode and a target material are arranged inside the low-temperature sealed cavity, the low-temperature cold stage is used for placing a quartz crystal oscillator, and the target material is uniformly deposited on the surface of the quartz crystal oscillator through the emission electrode of magnetron sputtering;
the ellipsometer equipment comprises a polarizer and an analyzer, wherein the polarizer and the analyzer are respectively arranged on the two sides of the low-temperature sealed cavity, which are opposite to the transparent window; detecting light enters the low-temperature sealed cavity after passing through the polarizer, is received by the polarizer after passing through the film layer on the surface of the quartz crystal oscillator, and the thickness of the film layer to be detected is calculated through the forward and backward changes of the amplitude and phase data of the polarized light;
the temperature control unit is arranged at the lower part of the low-temperature cooling table and is used for controlling the temperature of the cold surface of the low-temperature cooling table within a set range;
the pressure and component control unit is used for controlling the low-temperature sealed cavity to reach the vacuum degree required by the experiment and providing the atmosphere required by the experiment.
Furthermore, the low-temperature sealed cavity comprises a vacuum box and an inner cavity arranged in the vacuum box;
the low-temperature cold stage is arranged at the bottom of the inner cavity and comprises a cold surface and a clamping component which is arranged on the cold surface and used for fixing the quartz crystal oscillator; the emitting electrode and the target material are arranged in the inner cavity close to the upper part.
The clamping component is made of high-heat-conductivity ceramics, and a groove for placing a quartz crystal oscillator is formed in the surface of the clamping component.
Transparent windows are arranged on two sides of the vacuum box and the inner cavity and used for an ellipsometer to detect the thickness of a deposit layer on the surface of the quartz crystal oscillator.
The temperature control unit comprises a temperature control component arranged at the lower part of the cold surface and a liquid nitrogen pool arranged at the lower part of the temperature control component; liquid nitrogen enters the liquid nitrogen pool through the liquid inlet pipeline and is discharged through the gas outlet pipeline.
The temperature control assembly comprises a PID control system, a thermometer and a heating rod which are connected with the PID control system; the thermometer is attached to the cold surface and used for collecting temperature information and sending the temperature information to the PID control system; the heating rod is filled at the lower part of the cold surface and used for heating the cold surface under the regulation and control of the PID control system.
The pressure and component control unit comprises a first vacuum pump, a second vacuum pump and a high-purity nitrogen cylinder; the first vacuum pump and the second vacuum pump are respectively communicated with the vacuum box and the inner cavity through pipelines with needle valves; the high-purity nitrogen cylinder is communicated with the inner cavity through an air inlet pipeline with a secondary pressure reducing valve, and the high-purity nitrogen entering the inner cavity is discharged through an exhaust pipeline with a stop valve.
According to the operating condition requirement of the magnetron sputtering device, the inner cavity of the low-temperature sealing cavity needs to be vacuumized and is in an inert gas environment. The vacuum degree of the inner cavity is controlled by combining the vacuum pump and the high-purity nitrogen cylinder, and the high-purity nitrogen is filled to provide an inert gas environment, so that impurities such as water, carbon dioxide and the like remained in the inner cavity can be removed, and the condition that frosting is formed on the surface of the quartz crystal oscillator in the low-temperature calibration process to interfere the frequency acquisition of the quartz crystal oscillator is prevented. The external vacuum box needs to be vacuumized to reduce heat leakage of the inner cavity.
The invention also provides a method for calibrating the mass of the quartz crystal microbalance at low temperature, which comprises the following steps:
the pre-experimental process comprises the following steps: weighing a workpiece with a specific shape by using an electronic balance, wherein the mass m1 of the workpiece is weighed, and the workpiece is fixed at a position in which a quartz crystal oscillator is arranged in a low-temperature sealing cavity; controlling the low-temperature sealed cavity to reach the vacuum degree required by the experiment by using the pressure and component control unit, providing the atmosphere required by the experiment, and depositing the target material on the surface of the workpiece; stopping deposition after a certain time, detecting the thickness of the deposited metal layer by using an ellipsometer, taking out the workpiece from the cavity, and weighing the mass m2 of the workpiece by using an electronic balance; obtaining the volume V of the metal layer through the measured thickness and the area of the deposition surface, and further solving the density rho;
and (3) quality calibration process: the pressure and component control unit controls the low-temperature sealed cavity to reach the vacuum degree required by the experiment and provide the atmosphere required by the experiment, and the temperature control unit accurately controls the temperature of the cold surface; uniformly depositing target particles on the surface of a quartz crystal oscillator through an emission electrode of magnetron sputtering, detecting the thickness of a deposited metal layer by an ellipsometer, calculating the deposition quality according to the density of the metal layer obtained in the pre-experiment process, and simultaneously collecting a frequency signal of the quartz crystal oscillator; and repeating for multiple times to obtain a relation curve of the frequency of the quartz crystal oscillator and the deposition mass on the surface of the quartz crystal oscillator under the low-temperature condition, and completing the mass calibration.
Compared with the prior art, the invention has the following beneficial effects:
the invention combines the magnetron sputtering principle and the principle of measuring the film thickness by polarized light, directly calculates the quality of the deposit by detecting the thickness of the target material uniformly deposited on the surface of the quartz crystal oscillator, ensures that the mass calibration of the quartz crystal microbalance can be carried out in a low-temperature sealed cavity in the whole process, and achieves the aim of low-temperature micro-mass calibration.
Drawings
FIG. 1 is a schematic diagram of the overall structure of a device for low-temperature quartz crystal microbalance mass calibration according to the present invention;
fig. 2 is a schematic structural view of the low-temperature sealed chamber of the present invention.
Detailed Description
The invention will be described in further detail below with reference to the drawings and examples, which are intended to facilitate the understanding of the invention and are not intended to limit it in any way.
Unless defined otherwise, technical or scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The use of the word "comprise" or "comprises", and the like, in the context of this application, is intended to mean that the elements or items listed before that word, in addition to those listed after that word, do not exclude other elements or items. The terms "connected" or "coupled" and the like are not restricted to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "upper", "lower", "left", "right", and the like are used merely to indicate relative positional relationships, and when the absolute position of the object being described is changed, the relative positional relationships may also be changed accordingly.
As shown in fig. 1, a device for calibrating the mass of a quartz crystal microbalance at low temperature comprises a low-temperature sealed cavity 1, an ellipsometer, a temperature control unit, and a pressure and component control unit.
The low-temperature sealed chamber 1 includes a vacuum box 16 and an inner chamber 15 provided in the vacuum box 16. The bottom of the inner cavity 15 is provided with a low-temperature cooling table which comprises a cold surface and a clamping part 21 arranged on the cold surface and used for fixing the quartz crystal oscillator 20. The clamping component 21 is designed into a reference Twin-QCM structure and is provided with two crystal oscillators of a comparison group and an experimental group. In order to ensure that the temperature of the quartz crystal oscillator 20 is consistent with the temperature of the cold surface, the clamping part 21 is made of high heat conduction ceramics, and the surface of the clamping part is provided with a groove for placing the quartz crystal oscillator 20.
An emission electrode and a target 19 are arranged in the inner cavity 15 near the upper part, and the target 19 is uniformly deposited on the surface of the quartz crystal oscillator 20 through the emission electrode of magnetron sputtering.
The left and right side surfaces of the inner cavity 15 are respectively provided with a first transparent window 22 and a second transparent window 23, the left surface of the vacuum box 16 is provided with a third transparent window 24 which is opposite to and parallel to the first transparent window 22, and the right surface is provided with a fourth transparent window 25 which is opposite to and parallel to the second transparent window 23. The transparent window is mainly used for detecting the thickness of a deposition layer on the surface of the quartz crystal oscillator 20 by an ellipsometer.
The ellipsometer equipment comprises a polarizer 12 and an analyzer 13, the polarizer 12 and the analyzer 13 are respectively arranged on two side walls of the low-temperature sealed cavity 11, and the polarizer 12 and the analyzer 13 are connected with a data acquisition unit 14 through data lines. The detection light enters the low-temperature sealed cavity after passing through the polarizer 12, is reflected by the film layer on the surface of the quartz crystal oscillator 20 and then is received by the polarizer 13, the thickness of the film layer to be detected is calculated through the polarization of the light wave in the film layer, the used P, S component of the light wave is calculated, and the polarization state of the light wave can be described by two parameters of amplitude and phase.
In order to enable the ellipsometer to accurately measure the thickness of the deposition layer, the center of the polarizer 12, the center of the transparent window on one side and the center of the quartz crystal oscillator of the experimental group are located on the same straight line; similarly, the center of the analyzer 13, the center of the transparent window on the other side, and the center of the quartz crystal oscillator of the experimental group should be located on the same straight line.
The temperature control unit comprises a temperature control component 18 arranged at the lower part of the cold surface and a liquid nitrogen pool 17 arranged at the lower part of the temperature control component 18, and the mass calibration of the quartz crystal microbalance at different temperatures is completed by controlling the temperature of the cold surface.
The self-pressurization type liquid nitrogen tank 8 is used for providing liquid nitrogen for the liquid nitrogen pool 17, and the liquid nitrogen enters the liquid nitrogen pool 17 through a liquid inlet pipeline 26 with a stop valve 9 and is discharged through a gas outlet pipeline 27.
The temperature control assembly 18 comprises a PID control system 10, and a thermometer and a heating rod which are connected with the PID control system 10; the thermometer is attached to the cold surface and used for collecting temperature information and sending the temperature information to the PID control system 10; the heating rods are filled in the lower part of the cold surface and used for heating the cold surface under the regulation and control of the PID control system 10. The PID control system 10 is connected to a data acquisition unit 14.
In the pressure and composition control unit, a vacuum box 16 and an inner cavity 15 are respectively vacuumized by a first vacuum pump 1 and a second vacuum pump 2 through a needle valve 3 and a needle valve 4. A high-purity nitrogen bottle 5 is used for providing an inert gas environment for the inner cavity 15 through a secondary pressure reducing valve 6, and the high-purity nitrogen entering the inner cavity 15 is discharged through a stop valve 7.
According to the operating condition requirement of the magnetron sputtering device, the inner cavity 15 of the low-temperature sealing cavity needs to be vacuumized and is in an inert gas environment. The vacuum degree of the inner cavity 15 is controlled by combining a vacuum pump and a high-purity nitrogen cylinder, and the high-purity nitrogen is filled to provide an inert gas environment, so that impurities such as water, carbon dioxide and the like remained in the inner cavity can be removed, and the condition that frosting is formed on the surface of the quartz crystal oscillator in the low-temperature calibration process to interfere the frequency acquisition of the quartz crystal oscillator is prevented. The outer vacuum box 16 needs to be evacuated to reduce heat leakage from the cavity.
Under the atmosphere of high-purity nitrogen, liquid nitrogen is conveyed from the self-pressurization type liquid nitrogen tank 8 to a liquid nitrogen pool 17 below the cold surface in the low-temperature sealing cavity 11, and the temperature is accurately controlled by matching with the PID temperature control system 10. Through an emitting electrode of magnetron sputtering, particles of the target material 19 are uniformly deposited on the surface of a quartz crystal oscillator 20, a polarizer 12 and an analyzer 13 which are arranged on two sides of a low-temperature sealed cavity 11 pass through a side window of the cavity to detect the thickness of a deposited layer, the deposition quality is calculated, and meanwhile, a frequency signal of the quartz crystal oscillator is collected to calibrate the quality. Specifically, the frequency signal is collected by a frequency collecting device arranged in the low-temperature sealed cavity 11, and the collected frequency signal of the quartz crystal oscillator is sent to the data collecting unit 14.
The density data of the deposition layer is needed in the mass calculation of the embodiment, and the deposition layer density can be obtained through pre-experiments for subsequent mass calibration because the magnetron sputtering can achieve uniform deposition. The preliminary experiment included the following steps:
the density of the metal layer deposited by the magnetron sputtering device is determined through preliminary experiments, and the specific operation is that a workpiece (such as a cube, a cylinder and the like) with a specific shape is taken, and the mass m1 of the workpiece is weighed by an electronic balance. The workpiece is fixed in the position of the inner cavity 15 where the quartz crystal oscillator 20 is placed. Starting the first vacuum pump 1 and the second vacuum pump 2, and ventilating the cavity 15 through a high-purity nitrogen bottle 5 when the pressure is stable. After the chamber 15 reaches the required vacuum degree, the target 19 is deposited on the surface of the workpiece. After a certain time, the deposition is stopped, and the thickness of the deposited metal layer is detected by an ellipsometer. Stopping ventilation, closing the first vacuum pump 1 and the second vacuum pump 2, taking out the workpiece from the cavity 15 when the pressure of the low-temperature sealed cavity 11 is stable, and weighing the mass m2 by using an electronic balance to obtain the mass m = m2-m1 of the metal layer. Meanwhile, the volume V of the metal layer can be obtained through the measured thickness and the area of the deposition surface, and further the density rho = m/V can be obtained.
After the density of the deposition layer is obtained, carrying out mass calibration:
under the atmosphere of high-purity nitrogen, liquid nitrogen is conveyed to a liquid nitrogen pool below the cold surface in the low-temperature sealing cavity, and the temperature of the cold surface is accurately controlled by matching with a temperature control unit;
uniformly depositing target particles to the surface of a quartz crystal oscillator through an emission electrode of magnetron sputtering, detecting the thickness of a deposition layer through polarizers and analyzers arranged at two sides of a low-temperature sealed cavity, and calculating the deposition quality; simultaneously collecting frequency signals of a quartz crystal oscillator;
and repeating for many times to obtain a relation curve between the frequency of the quartz crystal oscillator and the deposition mass on the surface of the quartz crystal oscillator under the low-temperature condition, and completing the mass calibration.
The technical solutions and advantages of the present invention have been described in detail with reference to the above embodiments, it should be understood that the above embodiments are only specific examples of the present invention and should not be construed as limiting the present invention, and any modifications, additions and equivalents made within the scope of the principles of the present invention should be included in the scope of the present invention.
Claims (8)
1. A device for low-temperature quartz crystal microbalance mass calibration is characterized by comprising: the device comprises a low-temperature sealing cavity, ellipsometer equipment, a temperature control unit and a pressure and component control unit;
transparent windows are arranged on two sides of the low-temperature sealed cavity, a low-temperature cold stage, an emission electrode and a target material are arranged inside the low-temperature sealed cavity, the low-temperature cold stage is used for placing a quartz crystal oscillator, and the target material is uniformly deposited on the surface of the quartz crystal oscillator through the emission electrode of magnetron sputtering;
the ellipsometer equipment comprises a polarizer and an analyzer, wherein the polarizer and the analyzer are respectively arranged on the two sides of the low-temperature sealed cavity, which are opposite to the transparent window; detecting light enters the low-temperature sealed cavity after passing through the polarizer, is received by the polarizer after passing through the film layer on the surface of the quartz crystal oscillator, and the thickness of the film layer to be detected is calculated through the forward and backward changes of the amplitude and phase data of the polarized light;
the temperature control unit is arranged at the lower part of the low-temperature cooling table and is used for controlling the temperature of the cold surface of the low-temperature cooling table within a set range;
the pressure and component control unit is used for controlling the low-temperature sealed cavity to reach the vacuum degree required by the experiment and providing the atmosphere required by the experiment.
2. The device for low-temperature quartz crystal microbalance mass calibration according to claim 1, wherein the low-temperature sealed cavity comprises a vacuum box and an inner cavity arranged in the vacuum box;
the low-temperature cold stage is arranged at the bottom of the inner cavity and comprises a cold surface and a clamping component which is arranged on the cold surface and used for fixing the quartz crystal oscillator; the emitting electrode and the target material are arranged in the inner cavity close to the upper part.
3. The device for calibrating the mass of the quartz crystal microbalance at the low temperature according to claim 2, wherein the clamping component is made of high heat conduction ceramics, and the surface of the clamping component is provided with a groove for placing a quartz crystal oscillator.
4. The device for low-temperature quartz crystal microbalance mass calibration according to claim 2, wherein transparent windows are arranged on both sides of the vacuum box and the inner cavity.
5. The apparatus for low-temperature quartz crystal microbalance mass calibration according to claim 2, wherein the temperature control unit comprises a temperature control component disposed at the lower part of the cold surface and a liquid nitrogen pool disposed at the lower part of the temperature control component; liquid nitrogen enters the liquid nitrogen pool through the liquid inlet pipeline and is discharged through the gas outlet pipeline.
6. The device for low-temperature quartz crystal microbalance mass calibration according to claim 5, wherein the temperature control assembly comprises a PID control system and a thermometer and a heating rod connected with the PID control system; the thermometer is attached to the cold surface and used for collecting temperature information and sending the temperature information to the PID control system; the heating rod is filled at the lower part of the cold surface and used for heating the cold surface under the regulation and control of the PID control system.
7. The apparatus for low temperature quartz crystal microbalance mass calibration according to claim 2, wherein the pressure and composition control unit comprises a first vacuum pump, a second vacuum pump and a high purity nitrogen gas cylinder; the first vacuum pump and the second vacuum pump are respectively communicated with the vacuum box and the inner cavity through pipelines with needle valves; the high-purity nitrogen cylinder is communicated with the inner cavity through an air inlet pipeline with a secondary pressure reducing valve, and the high-purity nitrogen entering the inner cavity is discharged through an exhaust pipeline with a stop valve (7).
8. A method for calibrating the mass of a quartz crystal microbalance at low temperature, which is characterized in that the device for calibrating the mass of the quartz crystal microbalance at low temperature according to any one of claims 1 to 7 is used, and comprises the following steps:
the process of the preliminary experiment: weighing a workpiece with a specific shape by using an electronic balance, wherein the mass m1 of the workpiece is weighed, and the workpiece is fixed at a position in which a quartz crystal oscillator is arranged in a low-temperature sealing cavity; controlling the low-temperature sealed cavity to reach the vacuum degree required by the experiment by using the pressure and component control unit, providing the atmosphere required by the experiment, and depositing the target material on the surface of the workpiece; stopping deposition after a certain time, detecting the thickness of the deposited metal layer by using an ellipsometer, taking out the workpiece from the cavity, and weighing the mass m2 of the workpiece by using an electronic balance; obtaining the volume V of the metal layer through the measured thickness and the area of the deposition surface, and further solving the density rho;
and (3) quality calibration process: the pressure and component control unit controls the low-temperature sealed cavity to reach the vacuum degree required by the experiment and provide the atmosphere required by the experiment, and the temperature control unit accurately controls the temperature of the cold surface; uniformly depositing target particles on the surface of a quartz crystal oscillator through an emission electrode of magnetron sputtering, detecting the thickness of a deposited metal layer by an ellipsometer, calculating the deposition quality according to the density of the metal layer obtained in the pre-experiment process, and simultaneously collecting a frequency signal of the quartz crystal oscillator; and repeating for many times to obtain a relation curve between the frequency of the quartz crystal oscillator and the deposition mass on the surface of the quartz crystal oscillator under the low-temperature condition, and completing the mass calibration.
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