CN103226173B - A kind of method of Measurement accuracy piezoelectric film bulk acoustic wave resonator mass sensitivity - Google Patents
A kind of method of Measurement accuracy piezoelectric film bulk acoustic wave resonator mass sensitivity Download PDFInfo
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Abstract
The invention discloses a kind of method of Measurement accuracy piezoelectric film bulk acoustic wave resonator mass sensitivity, comprise the following steps: (1) measures no-load resonance frequency; (2) construct end to end closed micro-enclosure wall, the surface of piezoelectric film bulk acoustic wave resonator is surrounded; (3) in the region that micro-enclosure wall surrounds, salt solusion is injected; (4) sal volatile solution; (5) the rear resonance frequency of volatilization is measured; (6) micro-enclosure wall enclosing region is cleaned; (7) parameter injecting salt solusion is changed, the resonance frequency of device after the liquid of group more than obtaining all volatilizees; (8) value of calculated mass sensitivity.The surface being deposited in piezoelectric film bulk acoustic wave resonator completely by the whole solutes in salt solusion obtains the mass loading density that can accurately control, thus increase substantially the order of accuarcy of measured mass sensitivity, and measuring process does not have destructiveness to device itself.
Description
Technical field
What the present invention relates to is a kind of method of piezo-electric resonator applied technical field, specifically, is a kind of method of Measurement accuracy piezoelectric film bulk acoustic wave resonator mass sensitivity.
Background technology
Piezoelectric film bulk acoustic wave resonator is the novel micro nanometer resonating device being subject to extensive concern in recent years in radio communication and biochemical sensitive field.In biochemical sensitive field, this device, based on the sensitivity principle of quality of adsorption, produces high-frequency electrical acoustic resonance with piezoelectric membrane, and the change of its resonance frequency, phase place or amplitude detection material is as the response of sensor.This transducer sensitivity is very high, and existing semiconductor technology can be adopted on silicon chip to manufacture, and device volume is little, is applicable to large-scale integrated and forms sensor array.Such sensor is hopeful to be applied to the aspect such as chemical substance analysis and biological gene detection, protein analysis.
For the resonant transducer based on quality of adsorption sensitivity principle, mass sensitivity is an important key property index.The change of resonance frequency when mass sensitivity is defined as loading unit quality in sensor surface unit area, namely resonance frequency variable quantity is to the derivative of load quality density.For piezoelectric film bulk acoustic wave resonator, its mass sensitivity can in theory by the density of each layer film and THICKNESS CALCULATION out.But, in actual applications, the density of institute's deposited thin film material and the theoretical value deviation to some extent of its body material, and in device fabrication there is certain error in the THICKNESS CONTROL of film, and these two factors cause there is larger error between the mass sensitivity of practical devices and the theoretical value of its calculating.Therefore, the mass sensitivity of the actual piezoelectric film bulk acoustic wave resonator of Measurement accuracy is the important technological problems in such device application.
In the process of mass sensitivity measuring actual piezoelectric film bulk acoustic wave resonator, the most key is accurately apply mass loading at device surface.Current technical scheme mainly adopts and applies mass loading by various thin film deposition or growing technology in the method for device surface deposit additional membranes at piezoelectric film bulk acoustic wave resonator.Such as:
The people such as the H.Zhang of American South University of California describe a kind of program and deposit the technical scheme of aluminium as mass loading of different-thickness at device surface by sputtering technology in the article " Afilmbulkacousticresonatorinliquidenvironments " (a kind of thin film bulk acoustic resonator worked under liquid environment) of JOURNALOFMICROMECHANICSANDMICROENGINEERING (micromechanics and micro-engineering magazine) the 15th volume 1911 pages in 2005.
The people such as the JanWeber of Siemens are at IEEETRANSACTIONSONULTRASONICS, ferroelectrics, andfrequencycontrol (IEEE ultrasonics, ferroelectrics, with frequency control proceedings) describe a kind of technical scheme of monox as mass loading being deposited different-thickness at device by the method for physical deposition at device surface in the article " Investigationofthescalingrulesdeterminingtheperformanceo ffilmbulkacousticresonatorsoperatingasmasssensors " (thin film bulk acoustic resonator is as the relation of mass sensor application mesoscale rule with performance) of 2007 years 54 volumes 405 pages.
The shortcoming of technique scheme is, the mass loading being applied to piezoelectric film bulk acoustic wave resonator surface needs to be obtained by the density of institute's deposit film and THICKNESS CALCULATION, but there is certain deviation in the membraneous material actual density obtained by various thin film deposition or growing technology and theoretical value, thus cause the mass loading that calculates inaccurate, and then mass sensitivity numerical value accurately cannot be measured.In addition, owing to constantly depositing additional film at device surface, technique scheme has obvious destructiveness to prototype part, and after test, device cannot reduce and reuse.
Summary of the invention
The present invention is directed to shortcomings and deficiencies of the prior art, propose a kind of method of Measurement accuracy piezoelectric film bulk acoustic wave resonator mass sensitivity.
The present invention is achieved by the following technical solutions:
A method for Measurement accuracy piezoelectric film bulk acoustic wave resonator mass sensitivity, is characterized in that, comprise the following steps:
(1) measure piezoelectric film bulk acoustic wave resonator and do not apply the no-load resonance frequency in any mass loading situation;
(2) around piezoelectric film bulk acoustic wave resonator, construct end to end closed micro-enclosure wall, surrounded on the surface of piezoelectric film bulk acoustic wave resonator, the area of plane that micro-enclosure wall encloses is A;
(3) in the region that micro-enclosure wall surrounds, inject salt solusion, inject salt solusion parameter: concentration is C, and volume is V, and density is P;
(4) under the device injecting salt solusion being placed in Tempeerature-constant air environment, until the liquid in micro-enclosure wall enclosing region all volatilizees;
(5) measure liquid all volatilize after the resonance frequency of device;
(6) micro-enclosure wall enclosing region is cleaned;
(7) change and inject the parameter of salt solusion, repeat step (3) to (6), obtain many group liquid all volatilize after the resonance frequency of device;
(8) value of calculated mass sensitivity.
The wall width of the micro-enclosure wall described in step (2) is 10 microns to 30 microns, and the height of micro-enclosure wall is 0.3 to 0.6 millimeter.
Salt solusion described in step (3) minimum volume be injected in micro-enclosure wall enclosing region should make salt solusion cover plane that micro-enclosure wall encloses completely, and maximum volume should make the liquid level after injection lower than 3/4ths of the height of micro-enclosure wall.
Described salt solusion does not have corrosivity to the electrode in micro-enclosure wall and piezoelectric film bulk acoustic wave resonator and piezoelectric.
The value of the mass sensitivity described in step (8) is the derivative of resonance frequency difference to load quality density.
Described load quality density is M, and its computing formula is: M=(V × P × C)/A.
The difference of the resonance frequency of device after the poor no-load resonance frequency for piezoelectric film bulk acoustic wave resonator of described resonance frequency and liquid all volatilize.
In the present invention, the volatilization being injected into salt solusion in micro-enclosure wall makes the whole solutes in solution separate out the surface being deposited in piezoelectric film bulk acoustic wave resonator completely, because the concentration of solution can accurately control, the mass loading density being attached to device surface therefore accurately can be controlled.
Compared with technology in the past, beneficial effect of the present invention is, measured by the order of accuarcy of mass sensitivity that obtains increase substantially, and measuring process does not have destructiveness to device itself, and device can repeatedly use after removing micro-enclosure wall and remaining solute completely.
Accompanying drawing explanation
The structural representation of micro-enclosure wall in accompanying drawing 1 specific embodiment.
When to inject concentration of sodium chloride solution in accompanying drawing 2 specific embodiment be 60 mcg/ml, the real-time change figure of piezoelectric film bulk acoustic wave resonator resonance frequency.
Device resonance frequency in accompanying drawing 3 specific embodiment under different loads mass density is poor.
Embodiment
The present invention can be used for the piezoelectric film bulk acoustic wave resonator measuring various structure, as tabula model, air-gap type and solid assembly type etc., also can test the piezoelectric film bulk acoustic wave resonator of p-wave model or shear wave modes or mixed mode work.
In concrete enforcement, the resonance frequency of piezoelectric film bulk acoustic wave resonator can adopt multiple method to measure, as used and device to be connected with network analyzer or electric impedance analyzer and to carry out frequency measurement by the microprobe that mates of device electrode; Or design and the resonant circuit of device matching and frequency-discriminating circuit carry out frequency measurement.
Concrete steps of the invention process are:
(1) measure piezoelectric film bulk acoustic wave resonator and do not apply the no-load resonance frequency in any mass loading situation.For ensureing test accuracy, should fully cleaning device be surperficial and dry before no-load resonance frequency test.
(2) around piezoelectric film bulk acoustic wave resonator, construct end to end closed micro-enclosure wall, the surface of piezoelectric film bulk acoustic wave resonator is surrounded.The region that micro-enclosure wall surrounds can be square, circular or any closed polygon.The material of micro-enclosure wall can adopt photoresist, photosensitive polymers, metal or nonmetal, as dimethyl silicone polymer, polyimide, copper, titanium, aluminium, monox, silicon nitride etc.Make the semiconductor processing technology that micro-enclosure wall adopts standard, comprise sputtering, photoetching, plasma and reactive ion etching, wet etching and sacrifice layer process.To combine closely with the substrate of piezoelectric film bulk acoustic wave resonator bottom micro-enclosure wall, to ensure the closure injecting liquid.The wall width of micro-enclosure wall is 10 microns to 30 microns, and the height of enclosure wall is 0.3 to 0.6 millimeter.The area of plane that micro-enclosure wall encloses is A.Can multiple piezoelectric film bulk acoustic wave resonator be had in the scope that micro-enclosure wall surrounds, now can carry out the parallel measurement of multiple device.The electrode of piezoelectric film bulk acoustic wave resonator should have the micro-enclosure wall of component permeate, to be electrically connected.
(3) in the region that micro-enclosure wall surrounds, salt solusion is injected.Inject the aqueous solution or organic solution that salt solusion is salt, its parameter is: concentration is C, and volume is V, and density is P.Salt solusion does not have corrosivity to the electrode in micro-enclosure wall and piezoelectric film bulk acoustic wave resonator and piezoelectric.Generally, better suited salt solusion comprises the chlorate solution of metal, the sulfate liquor of metal and the nitrate solution of metal.Microneedles can be adopted to connect syringe pump for salt solusion or peristaltic pump carries out slow controlled injection.For homogeneity and the accuracy of proof load quality, the salt solusion minimum volume be injected in micro-enclosure wall enclosing region should make salt solusion cover plane that micro-enclosure wall encloses completely, and maximum volume should make the liquid level after injection lower than 3/4ths of the height of micro-enclosure wall.According to the area of plane that the micro-enclosure wall of reality encloses, the volume of the general salt solusion injected is received at hundreds of and is risen to a few microlitre.
(4) under the device injecting salt solusion being placed in Tempeerature-constant air environment, until the liquid in micro-enclosure wall enclosing region all volatilizees.Now, the solute in salt solusion is surperficial at piezoelectric film bulk acoustic wave resonator as mass loading uniform deposition.The environment temperature evaporated in process can be higher to accelerate volatilization process.A resonance frequency long-time stable being masked as device judging that liquid all volatilizees does not change.
(5) measure liquid all volatilize after the resonance frequency of device.The resonance frequency now measured is the resonance frequency after load certain mass, and this frequency comparatively no-load resonance frequency reduces.The environment temperature of now frequency measurement should to measure the environment temperature temperature of no-load resonance frequency identical with step (1).
(6) micro-enclosure wall enclosing region is cleaned.The liquid such as pure water, ethanol can be adopted repeatedly to rinse micro-enclosure wall enclosing region, the solute be deposited on piezoelectric film bulk acoustic wave resonator sensing surface is removed completely, the additional means such as stirring, sonic oscillation, heating can be adopted if desired.This process should notice that adopted cleaning fluid and cleaning means can not destroy micro-enclosure wall and device architecture.One judges that cleaning the resonance frequency being masked as device completely reverts to no-load resonance frequency completely.
(7) change and inject the parameter of salt solusion, repeat step (3) to (6), obtain many group liquid all volatilize after the resonance frequency of device.For the accuracy of sensitivity of ensuring the quality of products, revision test parameter should not be less than five groups.
(8) value of calculated mass sensitivity.The value of mass sensitivity is the derivative of resonance frequency difference to load quality density, and wherein load quality density is M, and its computing formula is: M=(V × P × C)/A; Resonance frequency difference is the difference of the resonance frequency of device after no-load resonance frequency and liquid all volatilize.In concrete enforcement, can make resonance frequency difference and load quality density relationship data point, carry out linear fit to data point, its slope is corresponding mass sensitivity.To resonance frequency difference and the situation of load quality density nonlinearities change, its derived function curve can be calculated and carry out mass sensitivity analysis.
Specific embodiment
The aluminum nitride piezoelectric film bulk acoustic wave resonator of the present embodiment to shear wave modes work carries out mass sensitivity measurement.
This piezoelectric film bulk acoustic wave resonator 1 is solid assembly type structure, adopts the microprobe of two aciculiform formulas that device and network analyzer are carried out frequency measurement.
Under 20 degrees Celsius of environment temperatures, device no-load resonance frequency is 2198.75MHz.
The structural representation of micro-enclosure wall 2 as shown in Figure 1.The material of micro-enclosure wall 2 is photoresist, adopts general photoetching process to make.For ensureing physical strength and the closure of micro-enclosure wall, after micro-enclosure wall completes, device has carried out the baking of more than three hours under 90 degrees Celsius of environment.The wall width 3 of micro-enclosure wall 2 is 20 microns, and the height 4 of micro-enclosure wall is 0.5 millimeter.The plane that micro-enclosure wall encloses is of a size of 6 millimeters × 1.5 millimeters square.The electrode 5 of piezoelectric film bulk acoustic wave resonator has the micro-enclosure wall 2 of component permeate.Micro-enclosure wall 2 is combined closely with the substrate 6 of piezoelectric film bulk acoustic wave resonator.Inject salt solusion 7 for sodium-chloride water solution, volume is 3 microlitres, and concentration is 20 to 100 mcg/ml, totally five groups of concentration parameters, adopts syringe pump to inject.Pure water irrigation instrument sensing surface is repeatedly adopted between each group of test.Under device after injection is placed in 20 degrees Celsius of environment temperatures, until the liquid in micro-enclosure wall enclosing region all volatilizees.
As shown in Figure 2 for inject concentration of sodium chloride solution be 60 mcg/ml time, the real-time change figure of device resonance frequency.According to formula M=(V × P × C)/A, load quality density M corresponding to this concentration is 2 micro-grams/cm.In the figure, sodium chloride solution injected the 50th second time, was no-load resonance frequency before this, and it is zero that initial resonance frequency differs from 8.After about 300 seconds, the resonance frequency of device is stablized, and now for the sodium chloride particle of precipitation is applied to piezoelectric film bulk acoustic wave resonator surface as mass loading, final resonance frequency differs from 9 for 1.09MHz.
Accompanying drawing 3 is that the device resonance frequency under different loads mass density is poor.Data point being carried out the value that linear fit obtains mass sensitivity is 465Hzcm
2/ ng.
Claims (6)
1. a method for Measurement accuracy piezoelectric film bulk acoustic wave resonator mass sensitivity, is characterized in that, comprises the following steps:
(1) measure piezoelectric film bulk acoustic wave resonator and do not apply the no-load resonance frequency in any mass loading situation;
(2) around piezoelectric film bulk acoustic wave resonator, construct end to end closed micro-enclosure wall, surrounded on the surface of piezoelectric film bulk acoustic wave resonator, the area of plane that micro-enclosure wall encloses is A;
(3) in the region that micro-enclosure wall surrounds, inject salt solusion, inject salt solusion parameter: concentration is C, and volume is V, and density is P;
(4) under the device injecting salt solusion being placed in Tempeerature-constant air environment, until the liquid in micro-enclosure wall enclosing region all volatilizees;
(5) measure liquid all volatilize after the resonance frequency of device;
(6) micro-enclosure wall enclosing region is cleaned;
(7) change and inject the parameter of salt solusion, repeat step (3) to (6), obtain many group liquid all volatilize after the resonance frequency of device;
(8) value of calculated mass sensitivity.
2. the method for a kind of Measurement accuracy piezoelectric film bulk acoustic wave resonator mass sensitivity according to claim 1, it is characterized in that, the wall width of the micro-enclosure wall described in step (2) is 10 microns to 30 microns, and the height of micro-enclosure wall is 0.3 to 0.6 millimeter.
3. the method for a kind of Measurement accuracy piezoelectric film bulk acoustic wave resonator mass sensitivity according to claim 1, it is characterized in that, salt solusion described in step (3) minimum volume be injected in micro-enclosure wall enclosing region should make salt solusion cover plane that micro-enclosure wall encloses completely, and maximum volume should make the liquid level after injection lower than 3/4ths of the height of micro-enclosure wall.
4. the method for a kind of Measurement accuracy piezoelectric film bulk acoustic wave resonator mass sensitivity according to claim 1, is characterized in that, the value of the mass sensitivity described in step (8) is the derivative of resonance frequency difference to load quality density.
5. the method for a kind of Measurement accuracy piezoelectric film bulk acoustic wave resonator mass sensitivity according to claim 4, it is characterized in that, described load quality density is M, and its computing formula is: M=(V × P × C)/A.
6. the method for a kind of Measurement accuracy piezoelectric film bulk acoustic wave resonator mass sensitivity according to claim 4, it is characterized in that, the difference of the resonance frequency of device after the poor no-load resonance frequency for piezoelectric film bulk acoustic wave resonator of described resonance frequency and liquid all volatilize.
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| US5818238A (en) * | 1996-03-15 | 1998-10-06 | Symetrix Corporation | Apparatus for measuring current and other parameters of an electornic device in response to an applied voltage |
| CN101105476A (en) * | 2006-07-14 | 2008-01-16 | 中国科学院声学研究所 | Difference frequency type film acoustic wave resonator based micro-mass sensor |
| CN101477029A (en) * | 2009-01-16 | 2009-07-08 | 中国科学院上海微***与信息技术研究所 | Surface stress sensitization method for improving resonance type ultra-thin cantilever beam transducer sensitivity |
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