CN116222732A - Tracing method for sensing quality value of quartz crystal microbalance by using hard film method and mass comparison method - Google Patents
Tracing method for sensing quality value of quartz crystal microbalance by using hard film method and mass comparison method Download PDFInfo
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Abstract
The tracing method of the quality value sensed by the quartz crystal microbalance (Quartz Crystal Microbalance, QCM for short) by using the hard film method and the quality comparison method can be adopted by a metering technical mechanism and a laboratory of the high-precision quality comparator and the high-precision weight only to trace the source of the quality value sensed by the QCM; the simplification of the QCM sensing quality value tracing method is realized, and wider popularization is obtained; the tracing of QCM in the mass increment range below 16 mug is innovatively solved, the tracing range of the tracing method to the micro mass is expanded, and the measuring range is enlarged to 2 mug to 1000 mug; the enlarged tiny quality traceability range can improve the quality sensitivity of the device, further improve the QCM detection precision, and further bring about huge change and influence.
Description
Technical Field
The invention relates to the technical field of tracing of sensing quality values of quartz crystal microbalances, in particular to a tracing method of sensing quality values of quartz crystal microbalances by using a hard film method and a mass comparison method.
Background
At present, in the process of transferring tiny mass values in China, the mass values with the mass less than 1 kg are needed to be obtained through a component comparison method; when the quality value is subjected to the component comparison and transmission process every time, the relative uncertainty generated by various reasons is remarkably accumulated step by step; for a mass of 1 kg, the relative uncertainty in the measurement of the current mass value is 2×10 -8 The method comprises the steps of carrying out a first treatment on the surface of the When the mass is transferred to milligram magnitude by the component comparison method, the relative uncertainty is increased to 2500 times of the relative uncertainty of 1 kilogram; if the component comparison is performed on smaller mass values, the relative uncertainty will be greater; while uncertainty may reach 10 when the mass value is transferred to the order of 1 nanogram by the component comparison method -12 The kg, i.e. the magnitude of uncertainty, corresponds to 1 nanogram per se; at present, the traceability of the prior art in China to the tiny quality is 50 mug;
quartz crystal microbalance (Quartz Crystal Microbalance, QCM for short) is widely used in the fields of physics and chemistry, life sciences, environmental sciences, aerospace, medical sciences and environmental sciences; the device is developed at the end of the 50 th century of the last 20 th century, is a high-sensitivity quality detection instrument, has the measurement precision of up to the level of nanograms, is 1000 times higher than an electronic balance with the sensitivity of microgram level, and can theoretically detect the quality change equivalent to a fraction of a monolayer or an atomic layer; the quartz crystal microbalance is constructed based on the piezoelectric effect principle of quartz crystals, and converts the tiny mass change delta m of the surface of a quartz crystal electrode into the frequency change delta f of an electric signal output by a quartz crystal oscillating circuit, so that a theoretical model is combined, and high-precision detection data are obtained through other auxiliary equipment such as a computer; based on the mass value measurement principle of QCM, the quantitative analysis of QCM mass measurement results depends on a theoretical model to a great extent, that is to say, the corresponding relation between Deltam and Deltaf cannot be directly traced to the international system of units;
the tracing method of the quartz crystal microbalance sensing quality value in the prior art mainly comprises the step that researchers such as Stambaugh and the like of National Institute of Standards and Technology (NIST) propose a tracing method of QCM sensing quality value by an EFB method; in the foreign prior art, a film is coated on a QCM quartz crystal oscillator wafer, and a high-precision quality comparator is used for determining the quality difference value of the quartz crystal oscillator wafer before and after the film coating to obtain the corresponding relation between the quality increment on the crystal oscillator wafer and the resonance frequency offset of the QCM crystal oscillator wafer;
the corresponding relation between the coating quality increment measured by the QCM method and the crystal oscillator piece resonance frequency offset caused by the coating quality increment is primarily linked to the international system of units in the foreign prior art; the foreign prior art achieves calibration of QCM in the mass increment range of 16.87 μg to 1044.26 μg from the results; and E is used in the process of comparing the reference quality of the real objects 1 The grade real object reference weight is calibrated by an electrostatic force balance (Electrostatic Force Balance, EFB for short) which can trace to the Planck constant h; the relation between the mass increment on the QCM quartz crystal oscillator plate and the corresponding crystal oscillator plate resonant frequency offset can be traced to the Planckian constant through the mass value by a short path in the foreign prior art;
the prior art has the defects that the traditional mass comparison method relies on a physical mass reference weight and a standard weight for mass value measurement, but for mass values below 20 mug, the electrostatic force effect of the weight is dominant gradually along with the reduction of the mass; therefore, for mass values below 20 mug, tracing cannot be performed by using a real standard weight and a mass comparison method;
the implementation of the foreign prior art depends on an EFB device to a great extent, the EFB device is not a device which can be provided by each metering mechanism and a laboratory, the construction and maintenance cost of equipment is high, and inconvenience is easily caused to tracing the QCM sensing quality value; the quality value traced by the EFB device is not compared with the traditional quality value tracing method;
in addition, the tracing method for the QCM sensing quality value, which is proposed by NIST in the United states, only realizes tracing of QCM in the quality increment range of 16.87-1044.26 mug, and can not meet the tracing of smaller QCM crystal oscillator quality increment.
Therefore, those skilled in the art have been working to develop a method for tracing the sensing quality value of a quartz crystal microbalance using a hard film method and a mass comparison method, aiming at solving the problems of the prior art.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present invention aims to solve the technical problem that in the prior art, the quality value measurement by the traditional quality comparison method depends on the physical quality reference weight and the standard weight, and for the quality value below 20 μg, the tracing cannot be performed by using the physical standard weight and the quality comparison method; the tracing method of QCM sensing quality value proposed by NIST in the United states depends on the EFB device to a great extent, and the quality value traced by the EFB device is not compared with the traditional quality value tracing method; moreover, the tracing method proposed by NIST in the United states only realizes tracing of QCM in the mass increment range of 16.87-1044.26 mug, and cannot meet the tracing of the mass increment of smaller QCM crystal oscillator.
In order to achieve the above purpose, the invention provides a tracing method for sensing quality values of a quartz crystal microbalance by using a hard film method and a mass comparison method, which comprises the following steps:
step 1, establishing a tracing mechanism of the micro quality of a rigid hard film;
step 3, loading micro mass on the QCM crystal oscillator sheet;
the step 1, the trace-back of the tiny quality of the rigid hard film can be completed according to the classical Sauerbrey equation,
(1) Wherein f q Is the resonant frequency of the QCM crystal oscillator piece, ρ q Is the density, mu of the crystal oscillator piece q The shear modulus of the crystal oscillator piece, and the negative sign refers to the reduction of the QCM resonant frequency;
in the step 1, if the rigid hard film attached to the crystal oscillator wafer is thin enough, the mass Δm of the rigid hard film and the resonance frequency shift Δf of the crystal oscillator wafer are in a linear relationship;
the traceability mechanism established in the step 1 realizes uncertainty introduced in the measurement process;
Before the idle load quality measurement is carried out in the step 2, the crystal oscillator needs to be kept stand for more than 48 hours in a stable environment so as to eliminate the instability of the crystal oscillator sheet, which is influenced by the environment, in the preparation process;
step 3, loading micro mass on the QCM crystal oscillator sheet;
the method for loading the micro mass on the QCM crystal oscillator wafer in the step 3 is a magnetron sputtering method coating;
step 3, loading micro mass on the QCM crystal oscillator wafer to limit the coating area and the uniformity of coating on the QCM crystal oscillator wafer, and designing mask plates with different aperture sizes to realize the loading area of the rigid hard film micro;
in the step 3, in order to obtain different crystal oscillator wafers with additional tiny mass, rigid hard films with different thicknesses are required to be deposited on the crystal oscillator wafers;
in the step 3, when the micro mass loading is carried out, the thickness of the rigid hard film loaded on the QCM crystal oscillator piece is controlled by the film coating time;
the step 3 is to load micro mass on the QCM crystal oscillator plate, and the thickness of the deposited film has influence on the measurement accuracy of the resonance frequency of the crystal oscillator plate, so the thickness of the rigid hard film deposited on the crystal oscillator plate is required to be far smaller than that of the crystal oscillator plate;
the deposited film material selected in the step 3 needs to have a larger density;
After the loading of the micro mass is completed in the step 3, namely, after metal hard films with different masses are uniformly deposited on the QCM crystal oscillator wafer to serve as the load; the micro mass loaded on the QCM crystal oscillator sheet can be measured;
The micro mass measured in the step 4 can be expressed as delta m=m L -m U And Δf=f L -f U Corresponding relation of (3); wherein, the angle marks L and U respectively represent a Loaded state and an Unloaded state;
furthermore, the method for loading the micro mass on the QCM crystal oscillator sheet in the step 3 can also use pulse laser deposition, chemical vapor deposition, sol-gel, electroplating and chemical dip plating;
further, in the step 3, gold, silver and copper can be selected as coating materials for the deposited film materials when the QCM crystal oscillator wafer is loaded with micro mass;
further, in the step 3, when the micro mass is loaded on the QCM crystal oscillator wafer, the thickness of the mask is related to the uniformity of the metal hard film, and the thickness of the mask can be smaller than 0.1mm or a mask with sharp edges can be adopted;
further, before the quality measurement of the loaded QCM crystal oscillator sheet is carried out, the loaded QCM crystal oscillator sheet needs to be kept stand for more than 48 hours in a stable environment so as to eliminate the instability of the crystal oscillator sheet caused by the environment in the preparation process;
further, the measurement of the empty and loaded masses of steps 2, 4 may use a high precision mass comparator and a high precision standard weight;
by adopting the scheme, the tracing method for sensing the quality value of the quartz crystal microbalance by using the hard film method and the mass comparison method has the following advantages:
(1) The tracing method for the quartz crystal microbalance sensing quality value by using the hard film method and the mass comparison method realizes the simplification of the tracing method for the QCM sensing quality value and obtains wider popularization; the method of the invention ensures that the method can be adopted by a metering technical mechanism and a laboratory only with a high-precision quality comparator and a high-precision weight with lower cost and wider popularization on the premise of not depending on an EFB device, thereby realizing the tracing of QCM sensing quality values;
(2) According to the tracing method for sensing the quality value of the quartz crystal microbalance by using the hard film method and the quality comparison method, the micro-mass is loaded on the QCM quartz wafer by using the vacuum magnetron sputtering method, so that the loaded micro-mass is combined with the quartz wafer into a whole through the interatomic force, and the action of electrostatic force is avoided in the mass range below 20 mug; the method creatively solves the tracing of QCM in the mass increment range below 16 mug, expands the tracing range of micro mass by the tracing method, and expands the measuring range to 2 mug to 1000 mug; the enlarged tiny quality traceability range can improve the quality sensitivity of the device, further improve the QCM detection precision, and further bring about huge change and influence;
in summary, the tracing method for sensing the quality value by using the hard film method and the mass comparison method for the quartz crystal microbalance disclosed by the invention ensures that the tracing of the QCM sensing quality value can be realized only by adopting the method of the invention for a high-precision mass comparator, a metering technical mechanism of a high-precision weight and a laboratory; the simplification of the QCM sensing quality value tracing method is realized, and wider popularization is obtained; the tracing of QCM in the mass increment range below 16 mug is innovatively solved, the tracing range of the tracing method to the micro mass is expanded, and the measuring range is enlarged to 2 mug to 1000 mug; the enlarged tiny quality traceability range can improve the quality sensitivity of the device, further improve the QCM detection precision, and further bring about huge change and influence;
the conception, specific technical scheme, and technical effects produced by the present invention will be further described in conjunction with the specific embodiments below to fully understand the objects, features, and effects of the present invention.
Drawings
FIG. 1 is a schematic flow chart of a tracing method of sensing quality values of a quartz crystal microbalance according to the present invention;
FIG. 2 is a schematic diagram of the structure of a 14mm sharp edge mask used in example 1 of the present invention for tracing the sensing quality value of a quartz crystal microbalance;
FIG. 3 is a schematic diagram of the structure of a 25mm sharp edge mask used in example 1 of the present invention for tracing the sensing quality value of a quartz crystal microbalance.
Detailed Description
The following describes a number of preferred embodiments of the present invention to make its technical contents more clear and easy to understand. This invention may be embodied in many different forms of embodiments which are exemplary of the description and the scope of the invention is not limited to only the embodiments set forth herein.
Example 1 Using the method of the present invention to complete the traceability of QCM sensed quality values
The tracing of the QCM sensing quality values implemented in this embodiment 1 is shown in fig. 1; firstly, performing step 1, establishing a tracing mechanism of the micro quality of a rigid hard film;
the step 1, the trace-back of the tiny quality of the rigid hard film can be completed according to the classical Sauerbrey equation,
(1) Wherein f q Is the resonant frequency of the QCM crystal oscillator piece, ρ q Is the density, mu of the crystal oscillator piece q The shear modulus of the crystal oscillator piece, and the negative sign refers to the reduction of the QCM resonant frequency;
in the step 1, if the rigid hard film attached to the crystal oscillator wafer is thin enough, the mass Δm of the rigid hard film and the resonance frequency shift Δf of the crystal oscillator wafer are in a linear relationship;
the traceability mechanism established in the step 1 realizes uncertainty introduced in the measurement process;
Before the idle load quality measurement is carried out in the step 2, the crystal oscillator needs to be kept stand for more than 48 hours in a stable environment so as to eliminate the instability of the crystal oscillator sheet, which is influenced by the environment, in the preparation process;
after the measurement of the empty load quality is completed, step 3, loading the micro mass on the QCM crystal oscillator sheet;
the method for loading the micro mass on the QCM crystal oscillator wafer in the step 3 is a magnetron sputtering method coating;
the method for loading the micro mass on the QCM crystal oscillator sheet in the step 3 can also use pulse laser deposition, chemical vapor deposition, sol-gel, electroplating and chemical dip plating;
step 3, loading micro mass on the QCM crystal oscillator wafer to limit the coating area and the uniformity of coating on the QCM crystal oscillator wafer, and designing mask plates with different aperture sizes to realize the loading area of the rigid hard film micro;
in the step 3, in order to obtain different crystal oscillator wafers with additional tiny mass, rigid hard films with different thicknesses are required to be deposited on the crystal oscillator wafers;
in the step 3, when the micro mass loading is carried out, the thickness of the rigid hard film loaded on the QCM crystal oscillator piece is controlled by the film coating time;
the step 3 is to load micro mass on the QCM crystal oscillator plate, and the thickness of the deposited film has influence on the measurement accuracy of the resonance frequency of the crystal oscillator plate, so the thickness of the rigid hard film deposited on the crystal oscillator plate is required to be far smaller than that of the crystal oscillator plate;
the deposited film material selected in the step 3 needs to have a larger density;
in the step 2, gold, silver and copper can be selected as coating materials for depositing the film materials when the QCM crystal oscillator wafer is loaded with micro mass;
the thickness of the mask is related to the uniformity of the metal hard film when the QCM crystal oscillator sheet is loaded with micro mass, and the thickness of the mask can be smaller than 0.1mm or a mask with sharp edges can be adopted;
when in use, the method of loading the micro mass of the rigid hard film on the QCM crystal oscillator wafer is realized by adopting a vacuum magnetron sputtering method coating method;
in the embodiment 1, the empty load mass and the loaded mass of the QCM crystal oscillator wafer are measured by using a high-precision mass comparator and a high-precision standard weight;
wherein the resolution of the mass comparator reaches 0.1 mug, and the electric weighing range of the mass comparator is 0 to 1100mg; the uncertainty of the synthesis standard of the used high-accuracy standard weight is less than 0.4 mug;
and the measuring apparatus of this example 1, under vacuum conditions, has a vacuum degree of less than 5X 10 at the time of measurement -6 hPa, avoiding the influence of air buoyancy on measurement; under air condition, the uncertainty of air density measurement standard of the air density measurement device is less than 4×10 -5 mg/cm 3 To obtain accurate air buoyancy correction;
before the QCM crystal oscillator sheets which are unloaded and loaded are subjected to quality measurement, standing is carried out for more than 48 hours in a stable environment, so that instability of the crystal oscillator sheets, which is influenced by the environment in the preparation process, is eliminated;
in the embodiment 1, the deposited film material selected in the step 3 is gold as a film coating material; the selected method for loading the rigid hard film micro mass on the QCM crystal oscillator plate is realized by adopting a vacuum magnetron sputtering method coating method;
in the embodiment 1, the vacuum magnetron sputtering method is used for loading the micro mass on the QCM quartz wafer, so that the loaded micro mass is combined with the electrode of the quartz wafer into a whole through the interatomic force, and the influence of electrostatic force on mass measurement is avoided in the mass range below 20 mug;
wherein, the thickness of the mask is related to the uniformity of the metal hard film, in order to avoid penumbra effect of the mask, in this embodiment 1, the mask with sharp edges is adopted respectively;
the mask used in this example 1 is shown in FIGS. 2 and 3 below, where FIG. 2 is a sharp edge mask having a diameter of 14mm and FIG. 3 is a sharp edge mask having a diameter of 25 mm;
in the test process, the embodiment 1 uses a sharp edge mask plate with the diameter of 14mm and 25mm, and can be applied to QCM crystal oscillator plates with the diameter of 14mm and 25 mm;
the outer edge diameter and the inner edge diameter of the mask plate can be adjusted, so that the QCM crystal oscillator plates with different diameters and crystal oscillator plate working face electrodes with different area sizes can be respectively matched in the embodiment 1;
then, the step 4 is completed, and the tiny mass loaded on the QCM crystal oscillator sheet in the step 3 is measured
After the loading of the micro mass is completed in the step 3, namely, after metal hard films with different masses are uniformly deposited on the QCM crystal oscillator wafer to serve as the load; the micro mass loaded on the QCM crystal oscillator sheet can be measured;
The micro mass measured in the step 4 can be expressed as delta m=m L -m U And Δf=f L -f U Corresponding relation of (3); wherein, the angle marks L and U respectively represent a Loaded state and an Unloaded state;
before quality measurement is carried out on the loaded QCM crystal oscillator wafer, the loaded QCM crystal oscillator wafer needs to be kept stand for more than 48 hours in a stable environment so as to eliminate instability of the crystal oscillator wafer, which is influenced by the environment, in the preparation process;
the measurement of the idle mass and the loaded mass in the steps 2 and 4 can use a high-precision mass comparator and a high-precision standard weight; the tracing of the QCM sensing quality value is completed;
in summary, the technical scheme of the patent realizes simplification of the QCM sensing quality value tracing method and obtains wider popularization; the method of the invention ensures that the method can be adopted by a metering technical mechanism and a laboratory only with a high-precision quality comparator and a high-precision weight with lower cost and wider popularization on the premise of not depending on an EFB device, thereby realizing the tracing of QCM sensing quality values; the vacuum magnetron sputtering method is used for loading the micro mass on the QCM quartz wafer, so that the loaded micro mass is combined with the quartz wafer into a whole through the interatomic force, and the action of electrostatic force is avoided in the mass range below 20 mug; the method creatively solves the tracing of QCM in the mass increment range below 16 mug, expands the tracing range of micro mass by the tracing method, and expands the measuring range to 2 mug to 1000 mug; the enlarged tiny quality traceability range can improve the quality sensitivity of the device, further improve the QCM detection precision, and further bring about huge change and influence.
The foregoing describes in detail preferred embodiments of the present invention. It should be understood that numerous modifications and variations can be made in accordance with the concepts of the invention by one of ordinary skill in the art without undue burden. Therefore, all technical solutions which can be obtained by logic analysis, reasoning or limited experiments based on the prior art by a person skilled in the art according to the inventive concept shall be within the scope of protection defined by the claims.
Claims (9)
1. A tracing method for sensing quality values of a quartz crystal microbalance (Quartz Crystal Microbalance, QCM for short) by using a hard film method and a mass comparison method is characterized by comprising the following steps:
step 1, establishing a tracing mechanism of the micro quality of a rigid hard film;
step 2, measuring the mass of the empty-load QCM crystal oscillator wafer;
step 3, loading micro mass on the QCM crystal oscillator sheet;
and 4, measuring the tiny mass loaded on the QCM crystal oscillator sheet in the step 3.
2. The method for tracing a sensing quality value according to claim 1,
the step 1, the trace source of the tiny quality of the rigid hard film is completed according to the classical Sauerbrey equation,
(1) Wherein f q Is the resonant frequency of the QCM crystal oscillator piece, ρ q Is the density, mu of the crystal oscillator piece q The shear modulus of the crystal oscillator piece, and the negative sign refers to the reduction of the QCM resonant frequency;
in the step 1, if the rigid hard film attached to the crystal oscillator wafer is sufficiently thin, the mass Δm of the rigid hard film and the resonance frequency shift Δf of the crystal oscillator wafer are in a linear relationship.
3. The method for tracing a sensing quality value according to claim 1,
step 2, firstly, obtaining the empty load mass m of the empty load QCM crystal oscillator wafer by a mass comparison method U And using QCM to obtain its resonance frequency f at no-load U The method comprises the steps of carrying out a first treatment on the surface of the Wherein, the corner mark U represents an empty (Unloaded) state;
and (2) before carrying out no-load quality measurement, standing for more than 48 hours in a stable environment to eliminate instability of the crystal oscillator wafer, which is influenced by the environment in the preparation process.
4. The method for tracing a sensing quality value according to claim 1,
the method for loading the micro mass on the QCM crystal oscillator wafer in the step 3 is a magnetron sputtering method coating;
step 3, loading micro mass on the QCM crystal oscillator wafer to limit the coating area and the uniformity of coating on the QCM crystal oscillator wafer, and designing mask plates with different aperture sizes to realize the loading area of the rigid hard film micro;
in the step 3, in order to obtain different crystal oscillator wafers with additional tiny mass, rigid hard films with different thicknesses are required to be deposited on the crystal oscillator wafers.
5. The method for tracing a sensing quality value according to claim 1,
in the step 3, when the micro mass loading is carried out, the thickness of the rigid hard film loaded on the QCM crystal oscillator piece is controlled by the film coating time;
the step 3 is to load micro mass on the QCM crystal oscillator plate, and the thickness of the deposited film has influence on the measurement accuracy of the resonance frequency of the crystal oscillator plate, so the thickness of the rigid hard film deposited on the crystal oscillator plate is required to be far smaller than that of the crystal oscillator plate;
the deposited film material selected in the step 3 needs to have a relatively high density.
6. The method for tracing a sensing quality value according to claim 1,
after the loading of the micro mass is completed in the step 3, namely, after metal hard films with different masses are uniformly deposited on the QCM crystal oscillator wafer to serve as the load; the micro mass loaded on the QCM crystal oscillator sheet can be measured;
step 4 is to measure the loading mass m of the wafer after coating L Then QCM is used to obtain the resonance frequency f of the crystal oscillator sheet when the crystal oscillator sheet is loaded qL ；
The micro mass measured in the step 4 can be expressed as delta m=m L -m U And Δf=f L -f U Corresponding relation of (3); wherein, the corner mark L represents a Loaded state;
before quality measurement is carried out on the loaded QCM crystal oscillator wafer, the loaded QCM crystal oscillator wafer needs to be kept stand for more than 48 hours in a stable environment so as to eliminate instability of the crystal oscillator wafer, which is influenced by the environment, in the preparation process.
7. The method for tracing a sensing quality value according to claim 1,
and 3, when the QCM crystal oscillator sheet is loaded with micro mass, the thickness of the mask is related to the uniformity of the metal hard film, and the thickness of the mask can be smaller than 0.1mm or a mask with sharp edges can be adopted.
8. The method for tracing a sensing quality value according to claim 1,
the method for loading the micro mass on the QCM crystal oscillator sheet in the step 3 can also use pulse laser deposition, chemical vapor deposition, sol-gel, electroplating and chemical dip plating;
and in the step 3, gold, silver and copper can be selected as coating materials for depositing the film materials when the QCM crystal oscillator plate is loaded with micro mass.
9. The method for tracing a sensing quality value according to claim 1,
the measurement of the empty and loaded masses of steps 2, 4 may use a high precision mass comparator and a high accuracy standard weight.
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