CN110361287A - A kind of quartz crystal microbalance mass sensor that mass sensitivity is uniform - Google Patents
A kind of quartz crystal microbalance mass sensor that mass sensitivity is uniform Download PDFInfo
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Abstract
For the uniformity for improving QCM mass sensitivity, the present invention provides a kind of qcm sensor of asymmetry electrode structure, belongs to electronic technology field.It includes circular quartz chip (1), and upper and lower surface is respectively provided with metal electrode (2) and (3), and upper/lower electrode geometric center normal is overlapped with Circular wafer geometric center normal three；It is characterized in that, the lower metal electrode (3) is the circle electrode that Radius is m；The upper metal electrode (2) is a ring electrode, and the inside radius of this ring electrode is n, outer radius m, and n is approximately equal to (0.3~0.7) * m；The thickness of gold electrode is about (0.3~0.7) * 10 simultaneously‑7Rice or so；And this m value is related with working frequency, fundamental frequency QCM, the m value to 10MHz is about between 1.5~3.0 millimeters, and to the fundamental frequency QCM of 5MHz, m value is about between 3.0~6.0 millimeters.Meet the mass sensitivity distribution that approximate can obtain homogeneous distribution under the conditions of these three, improves the uniformity of QCM mass sensitivity distribution, and then improve the repeatability of its measurement result.
Description
Technical field
The invention belongs to electronic technology fields, are related to quartz crystal microbalance (Quartz Crystal
Mircrobalance, QCM), especially QCM mass sensor.
Background technique
Quartz crystal microbalance (Quartz Crystal Mircrobalance, QCM) is one kind in the 1960s
The novel Tiny Mass detecting instrument risen, core component is QCM mass sensor.QCM mass sensor is a kind of non-
Normal sensitive mass sensor, its quality determination can be as accurate as nanogram level, in physics, chemistry, biology, medicine, agriculture
It is applied in the test problems of the subjects such as industry and engineering.Under certain external condition, when quartz crystal oscillator adsorption its
When its substance, is changed according to the frequency of quartz vibrator and changes this directly proportional principle to the appended material mass of plane of crystal,
The resonance frequency of quartz crystal oscillator will be with the size of adsorbent quality and change.QCM mass sensor is exactly to have in fact
The quartz-crystal resonator of top-bottom electrode structures.Quartz-crystal resonator is because piezoelectric effect can be under dynamic excitation with the humorous of it
Vibration frequency oscillation, QCM mass sensor is exactly to utilize this characteristic of quartz-crystal resonator, in quartz crystal resonator electrode table
One layer of test substance is adsorbed in face, and the quality signal of test substance is converted into what frequency signal was detected.QCM has very high
It is sensitivity, excellent selectivity, required low in cost, and that test device is simple, is easily achieved live continuous detection etc. is numerous
Advantage, so receiving the great attention of countries in the world scientist, it has been widely used for quality, density, degree of being stained with, concentration etc.
Detection field.
However, QCM has a prominent question in the application: the repeatability of measurement result is very low.To obtain higher repetition
Property measurement result, there has been proposed many QCM use when points for attention, such as make being distributed in for sample homogenous rigidity
The entire electrode surface of QCM, the method that can be realized the distribution of sample homogenous rigidity mainly have vacuum coating, plating etc., operation
Process is not only cumbersome but also efficiency is very low.
Currently, it has been recognized that, the inconsistent of QCM mass sensor mass sensitivity distribution curve is to cause its measurement
As a result the main reason for repeated low.Theory and practice is all it was demonstrated that conventional as what Fig. 1 showed has circle electrode structure (m-m type)
QCM mass sensor, mass sensitivity distribution curve be bell-shaped (or Gaussian) as shown in Figure 2, this generates
QCM mass sensor mass sensitivity distribution curve it is inconsistent, bring the low problem of measurement result repeatability.
In order to obtain the QCM mass sensor that mass sensitivity is evenly distributed, electricity of the researcher to QCM mass sensor
Pole structure has carried out this into such as having devised asymmetric circle n-m type electrode, oval-shaped electrode, but this not can solve
Due to the low problem of the inconsistent brought measurement result repeatability of QCM mass sensor mass sensitivity distribution curve.
Having foreign study, person proposes the QCM mass sensor with a kind of asymmetry electrode structure, as shown in Figure 3,4,
Its top electrode be a kind of circular ring electrode (round loop electrode inside radius is n, outer radius m), lower electrode be still outside one partly
Diameter is the circular electrode of m.QCM mass sensor with this electrode structure, mass sensitivity distribution curve are bimodal shape,
Bimodal recess is apparent, if it is possible to by the filling-in that is recessed, then can get uniform mass sensitivity distribution.For will be bimodal
Between recess filling-in, scientists have done many discussions.1996, Youbok Lee et al. discovery can be by reducing electrode
Mass loading factor makes bimodal recess reduce (Y.Lee, F.Josse, " Radial dependence of mass
Sensitivity for modified-electrode quartz resonators ", Proc.IEEE
Ultrason.Symp, vol.1, pp.321-325,1996 and F.Josse, Y.Lee. " Analysis of the Radial
Dependence of mass sensitivity for modified-electrode quartz resonators ",
Anal.Chem.1998,70,237-247) its provide mass sensitivity distribution curve as shown in figure 5, i.e. work as mass loading system
When number is 0.002, the fluctuation of curve is minimum, about 24% or so, still unevenly, but it is noted that same author's Similar content
The mass sensitivity theoretical values that two articles calculate are one times substantially poor；And in United States Patent (USP) US8215171 in 2012
In, for the QCM chip of the 5MHz of theoretical calculation when mass loading coefficient is 0.0025, curve is substantially flat, but subsequent
Still there is 26% or so fluctuation in confirmatory experiment, still reaches to the requirement uniform less than sensitivity.In short, plating back frequency in resonator
When minimum, mass sensitivity distribution curve has the tendency that reaching unanimity, but (i.e. the plating of chip returns frequency too since R value is too small
It is small), only reduce electrode quality load factor by reducing the method for thickness of electrode, becomes the equivalent resistance of crystal in this way
It is too big, influence to actually use, meanwhile, experiment shows even if reducing R, still without reaching the uniform requirement of sensitivity.
Summary of the invention
In order to improve the uniformity of QCM mass sensor mass sensitivity, the present invention, which provides, has a kind of asymmetry electrode
The QCM mass sensor of structure improves quality spirit by the ratio of coordination electrode mass loading factor and inner and outer ring electrode diameter
The uniformity of sensitivity achievees the purpose that improve QCM measurement accuracy to improve the repeatability of QCM measurement result.
Technical solution of the present invention is as follows:
A kind of quartz crystal microbalance mass sensor that mass sensitivity is uniform, including circular quartz chip (1), it is described
Circular quartz chip (1) upper and lower surface is respectively provided with metal electrode (2) and lower metal electrode (3), by circular quartz chip
(1) normal of geometric center is with the normal Jing Guo upper metal electrode (2) geometric center and by lower metal electrode (3) geometric center
Normal three keep be overlapped；It is characterized in that, the lower metal electrode (3) is the circle electrode that Radius is m；The upper metal
Electrode (2) is a ring electrode, and the inside radius of this ring electrode is n, outer radius m, n < m, and n be approximately equal to (0.3~
0.7) * m, that is, n value m half or so.
QCM mass sensor provided by the invention, shape be still Fig. 3, shown in 4 with the QCM mass of ring-shaped electrode
Sensor, feature be reasonable coordination electrode mass loading factor and inner and outer ring electrode radius ratio and reasonable m value, when adopting
When with gold electrode, thickness of electrode is about (0.3~0.7) * 10-7Rice or so, while its inside radius n is about outer radius m
Half, and m value is related with working frequency, to the fundamental frequency QCM of 10MHz, m value is about between 1.5~3.0 millimeters, and to 5MHz
Fundamental frequency QCM, m value be about to meet these three conditions between 3.0~6.0 millimeters, thus approximate can obtain uniform quality
Sensitivity profile.
It has three classes region as seen from the figure: being respectively non-electrode region (area U), partial electrode area (area P) and full electrode district
(area E), cutoff frequency uses f respectivelyU、fPAnd fEIt indicates.It is required according to energy well theory, the working frequency of the QCM mass sensor
Range is fE< f < fP< fU.Under the operating frequency range, the solution of the particle displacement amplitude of the QCM mass sensor are as follows:
In formula, J0、Y0、I0And K0It is referred to as 0 rank Bessel function of the first kind, 0 rank Bessel function of the second kind, 0 rank
A kind of dummy variables Bessel function and 0 rank the second class dummy variables Bessel function.Connected by particle displacement and strain in r=n, m
It is continuous, available four linear homogeneous equa tion sets at boundary continuity equation group, find out particle displacement amplitude constant C1、C2、C3、
C4。
In this way, just having obtained the expression of A (r), the mass sensitivity S of the QCM mass sensor can be obtained by following formulaf
(r) expression:
(2) C in formulafIt is the mass sensitivity constant of QCM mass sensor.
Theoretical calculation is carried out so that AT cuts 10MHz fundamental frequency as an example, electrode material is gold.
Fig. 6 is dispatch from foreign news agency polar radius 2.5mm, interior electrode radius 1.0mm, mass loading factor R=0.0044, thickness of electrode
Mass sensitivity distribution curve at 500 angstroms, it is seen that approximate at this time to realize uniform mass sensitivity distribution.
Fig. 7 is dispatch from foreign news agency polar radius 2.5mm, interior electrode radius 1.0mm, mass loading factor R=0.0088, thickness of electrode
Mass sensitivity distribution curve at 1000 angstroms, it is seen that mass sensitivity distribution fluctuation at this time is just larger.
Fig. 8 is dispatch from foreign news agency polar radius 5.0mm, interior electrode radius 2.0mm, mass loading factor R=0.0044, thickness of electrode
500 angstroms of mass sensitivity distribution curve, it is seen that mass sensitivity distribution fluctuation at this time is just very big.
From theory analysis as it can be seen that garden ring-shaped electrode is meeting its thickness of electrode about (0.3~0.7) * 10-7Rice or so,
Its inside radius n is about the half of outer radius m simultaneously, and m value is related with working frequency, and to the fundamental frequency QCM of 10MHz, m value is about
Between 1.5~3.0 millimeters, and to the fundamental frequency QCM of 5MHz, m value is about between 3.0~6.0 millimeters after such three conditions,
It approximate can theoretically obtain uniform mass sensitivity distribution.
As seen from Figure 6, after meeting condition proposed by the present invention, so that it may approximately realize uniform mass sensitivity point
Cloth.
In conclusion can be improved the uniformity of mass sensitivity using method proposed by the present invention, to improve QCM
The repeatability of measurement result achievees the purpose that improve QCM measurement accuracy.
Detailed description of the invention
Fig. 1 is the longitudinal cross-section signal of the conventional QCM mass sensor with round electrode structure (m-m type) symmetrical above and below
Figure.
Fig. 2 is the mass sensitivity distribution curve of the QCM mass sensor of structure shown in Fig. 1.
Fig. 3 is the longitudinal cross-section schematic diagram with the QCM mass sensor of annular electrode structure.
Fig. 4 is the upper metal electrode structure schematic diagram of the QCM mass sensor shown in Fig. 3 with annular electrode structure.
Fig. 5 is that the mass sensitivity of the QCM mass sensor shown in Fig. 3 reported in the literature with annular electrode structure is bent
Line.Its distribution in the electrodes around heart point is bimodal shape, and with the reduction of R, mass sensitivity distribution curve, which has, to be tended to
Consistent trend, but under the smallest R, it fluctuates still larger.
Fig. 6 is that 10MHzAT cuts fundamental frequency QCM in outer electrode radius 2.5mm, interior electrode radius 1.0mm, mass loading factor R
=0.0044, mass sensitivity distribution curve at 500 angstroms of thickness of electrode, it is seen that approximate at this time to realize uniform quality spirit
Sensitivity distribution.
Fig. 7 is that 10MHz AT cuts fundamental frequency QCM in outer electrode radius 2.5mm, interior electrode radius 1.0mm, mass loading factor R
=0.0088, mass sensitivity distribution curve at 1000 angstroms of thickness of electrode, it is seen that mass sensitivity distribution fluctuation at this time is just
It is big.
Fig. 8 is that 10MHz AT cuts fundamental frequency QCM in outer electrode radius 5.0mm, interior electrode radius 2.0mm, mass loading factor R
=0.0044,500 angstroms of thickness of electrode of mass sensitivity distribution curve, it is seen that mass sensitivity distribution fluctuation at this time is also big
?.
Fig. 9 is the schematic diagram of entire confirmatory experiment.
Specific embodiment
With reference to the accompanying drawings and detailed description, the present invention is further described.
Ring-shaped electrode is processed by the condition of Fig. 6 first, then can be carried out gold-plated film experiment, the schematic diagram of experiment is such as
Shown in Fig. 9:
Experimental procedure is as follows:
A takes the AT of 15 10MHz to cut fundamental frequency piece, is divided into 3 groups, every group 5；
B and then gold-plated film, two sides is symmetrical, and thickness is 500 angstroms, but the garden ring-shaped electrode of electrode processing shown in fig. 6；
Test frequency is distinguished after plated film；
Then 3 garden Zu Jun face centers add one layer of 500 angstroms of thickness of plating to C, and diameter distinguishes the golden film of 1.0mm, 2.0mm, 3.0mm.
Test frequency respectively.
The experimental results showed that B groups of frequency variations are approximately 4 times of A groups, C groups of frequency variations are approximately 9 times of A groups,
In view of 4 times that B groups of mass changes are A groups, C groups of mass changes are 9 times of A groups, and i.e. explanation is with shown in fig. 6 in this way
The mass sensitivity distribution of the QCM of garden ring electrode is approximate uniform, because its corresponding frequency of the variation of three kinds of quality changes
All approximately linears.
Claims (6)
1. a kind of quartz crystal microbalance mass sensor that mass sensitivity is uniform, including circular quartz chip (1), the circle
Shape quartz wafer (1) upper and lower surface is respectively provided with metal electrode (2) and lower metal electrode (3), by circular quartz chip (1)
The normal of geometric center is with the normal Jing Guo upper metal electrode (2) geometric center and by lower metal electrode (3) geometric center
Normal three keeps being overlapped；It is characterized in that, the lower metal electrode (3) is the circle electrode that Radius is m；The upper metal electricity
Pole (2) is a ring electrode, and the inside radius of this ring electrode is n, outer radius m, n < m, and n be approximately equal to (0.3~
0.7) * m, that is, n value m half or so.
2. quartz crystal microbalance mass sensor according to claim 1, which is characterized in that the upper metal electrode
(2) and lower metal electrode (3) material is gold or chromium+gold, and thickness is about (0.3~0.7) * 10-7Rice or so.
3. quartz crystal microbalance mass sensor according to claim 1 or 2, which is characterized in that the ring-shaped electrode
Radius m in the range of 1.0 millimeters to 5.0 millimeters.And this m value is related with working frequency, to the fundamental frequency QCM, m of 10MHz
Value is about between 1.5~3.0 millimeters, and to the fundamental frequency QCM of 5MHz, m value is about between 3.0~6.0 millimeters.
4. quartz crystal microbalance mass sensor according to claim 1,2 or 3, which is characterized in that the quartz-crystal
The diameter of piece (1) is in the range of 7.0mm to 14.0mm.
5. quartz crystal microbalance mass sensor according to claim 1,2,3 or 4, which is characterized in that the quartz
Chip (1) is that AT cuts quartz wafer, and corner cut range is ° 25 ' from 35 ° 08 ' to 35.
6. quartz crystal microbalance mass sensor according to claim 1,2,3 or 4, which is characterized in that the quartz
The nominal frequency of crystal microbalance mass sensor is 5MHz, 10MHz or 11MHz etc., work overtone number be fundamental frequency, 3 times it is general
Sound or 5 overtones etc..
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115112208A (en) * | 2022-06-08 | 2022-09-27 | 南京理工大学 | Novel quartz crystal microbalance with concave platform annular structure |
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|---|---|---|---|---|
| US8215171B1 (en) * | 2008-08-26 | 2012-07-10 | University Of South Florida | Uniform mass sensitivity thickness shear mode quartz resonator |
| CN102967521A (en) * | 2012-11-15 | 2013-03-13 | 电子科技大学 | Quartz crystal microbalance (QCM) mass sensor |
| CN102967522A (en) * | 2012-11-15 | 2013-03-13 | 电子科技大学 | Quartz crystal microbalance (QCM) mass sensor |
| CN103048210A (en) * | 2013-01-11 | 2013-04-17 | 东南大学 | Quartz crystal microbalance detecting device |
| CN106153718A (en) * | 2016-08-18 | 2016-11-23 | 中国工程物理研究院总体工程研究所 | A kind of piezoelectric crystal gas transducer with double working modes |
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2018
- 2018-04-10 CN CN201810308560.1A patent/CN110361287A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8215171B1 (en) * | 2008-08-26 | 2012-07-10 | University Of South Florida | Uniform mass sensitivity thickness shear mode quartz resonator |
| CN102967521A (en) * | 2012-11-15 | 2013-03-13 | 电子科技大学 | Quartz crystal microbalance (QCM) mass sensor |
| CN102967522A (en) * | 2012-11-15 | 2013-03-13 | 电子科技大学 | Quartz crystal microbalance (QCM) mass sensor |
| CN103048210A (en) * | 2013-01-11 | 2013-04-17 | 东南大学 | Quartz crystal microbalance detecting device |
| CN106153718A (en) * | 2016-08-18 | 2016-11-23 | 中国工程物理研究院总体工程研究所 | A kind of piezoelectric crystal gas transducer with double working modes |
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Cited By (1)
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|---|---|---|---|---|
| CN115112208A (en) * | 2022-06-08 | 2022-09-27 | 南京理工大学 | Novel quartz crystal microbalance with concave platform annular structure |
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