CN106813718B - A kind of device and method measuring thin film strain and thermal conductivity - Google Patents

A kind of device and method measuring thin film strain and thermal conductivity Download PDF

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CN106813718B
CN106813718B CN201710118131.3A CN201710118131A CN106813718B CN 106813718 B CN106813718 B CN 106813718B CN 201710118131 A CN201710118131 A CN 201710118131A CN 106813718 B CN106813718 B CN 106813718B
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film
strain
thermal conductivity
loading
thin film
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CN106813718A (en
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王海容
陈翰林
张咪
谷汉卿
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Research Institute Of Xi'an Jiaotong University Zhejiang
Xi an Jiaotong University
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Xi an Jiaotong University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01DMEASURING NOT SPECIALLY ADAPTED FOR A SPECIFIC VARIABLE; ARRANGEMENTS FOR MEASURING TWO OR MORE VARIABLES NOT COVERED IN A SINGLE OTHER SUBCLASS; TARIFF METERING APPARATUS; MEASURING OR TESTING NOT OTHERWISE PROVIDED FOR
    • G01D21/00Measuring or testing not otherwise provided for
    • G01D21/02Measuring two or more variables by means not covered by a single other subclass

Abstract

The invention discloses a kind of device and methods for measuring thin film strain and thermal conductivity, device includes a pedestal, one shell being set on the base, the pedestal is equipped with loading end, film sample is placed on loading end and connects with the freely-supported fixing end of shell upper, a precession guide rod is equipped with below loading end, film sample is connected by sputtering test electrode with power supply.By the way that circular membrane is controlled feeding displacement S by precise guide rod at its radius, using the deflection theory of statics balance and elastic sheet, the deflection equation of available intermediate plectane, when radius is equal to R0When, the deflection value of two parts is equal, and by accurate thread stroke, available radius is in R and R0Between plectane i.e. feeding displacement S size, and then calculate intermediate circular membrane circumferential strain and radial strain value, using the thermal conductivity of 3 ω measurement methods measurement film, both realized the measurement of thermal conductivity of the film under differently strained.

Description

A kind of device and method measuring thin film strain and thermal conductivity
Technical field
The present invention relates to micro-electromechanical system (MEMS) device, especially a kind of device for measuring thin film strain and thermal conductivity And method.
Background technique
Along with the fast development of micro-electromechanical system (MEMS) technology, the thin-film device of all kinds of function admirables comes into being, In, the MEMS device type to work under thermal field is more and more, and dosage is also increasing, such as miniature infrared light supply, micro- gas Sensor, high temperature MEMS pressure sensor, operating temperature reaches hundreds of or even thousands of degrees Celsius, and there are alternating temperature-changing fields, this is right Membrane structure and the reliability of material military service are put forward higher requirements.Especially in sensor field, some fundamental physical quantities are measured When, corresponding deformation can inevitably occur for device, generate strain, the strain responses of the film internal state of film, be determine it is thin The important factor of film integrality, and determine one of the important factor that can work normally of device, when the strain of film is excessive, It is possible that fracture, plastic deformation, falling off, make thin film damage, and then entire device is made to lose the job ability, for semiconductor Thin-film material studies have shown that strain the structure of semiconductor nano material and its regulating and controlling effect of property are played it is vital It influences, such as semi-fluorinated single layer of gallium nitride nano thin-film can realize that ferromagneticization and antiferromagneticization mutually turn by straining Become, while the thermal conductivity of thin-film device directly affects device radiating efficiency.
Such as in patent (103822736 B of Authorization Notice No. CN) " under a kind of circular membrane concentrated force that determining periphery clamps In the method for thin film strain value " (He Xiaoting, Sun Junyi, Zheng Zhoulian, Cai Zhenhong etc.), using a band, whether there is or not the flat circles that rubs Column applies a transverse load as loading axis at the center of circular membrane, thin at certain available point by this method Membrane stress value, different radiuses correspond to different stress values, that is, different strains, but at this method different radii Strain be it is unequal, this is not able to satisfy our demands to strain;Such as in patent (Authorization Notice No. CN 102001617 B detailed to elaborate using straight) in " a kind of flexible electronic device displacement loading device and method " (Feng Xue, Jiang Dongjie, Wang Yong) Galvanic electricity source, bracket, guide rail, spring etc. reach the method for the strain of the film of needs, by controlling the size of DC current, The size strained is connect, the strain that this method obtains is not linear, and device is complicated, still can not meet demand.
Therefore strain and the relationship of the thermal conductivity of material become more and more prominent in research thin-film device, especially film material The thermal conductivity of material and the relationship of strain, directly affect the service performance of material, and thermal conductivity has MEMS device extremely important Effect and potential application value.This is just needed under temperature, and the relationship of research material strain and thermal conductivity, material is answered It is equal requirement that change, which must satisfy measured zone internal strain,.Therefore, a kind of circular membrane receiving that simple supported edge is fixed is studied The device of thin film strain and thermal conductivity of thin film under ring load is concentrated, so that it is simply easily achieved, and theoretical method is mature Reliably become current this field technical problem urgently to be resolved.
Summary of the invention
To solve drawbacks described above existing in the prior art, fixed the purpose of the present invention is to provide a kind of simple supported edge Circular membrane bears to concentrate the device of thin film strain and thermal conductivity of thin film under ring load.
The present invention is realized by following technical proposals.
A kind of device measuring thin film strain and thermal conductivity, including a pedestal, a shell being set on the base, institute Pedestal is stated equipped with loading end, the substrate for being coated with film is placed on loading end and connects with the freely-supported fixing end of shell upper, A precise guide rod is equipped with below loading end, being coated with sputtering in the substrate of film has test electrode and a metal strip, test electricity Pole is connected with the external detection system with locking phase amplification module, and is connected to computer;
Being displaced S by the precession of precise guide rod makes the film being coated in the substrate of film generate strain, by control into The size that thin film strain is controlled to displacement S, by being passed through periodic current I to test electrodeω, computer reads electric from test The ingredient U of 3 ω harmonic waves of pole acquisitionSize obtain the thermal conductivity of film.
Preferably, the shell is round-meshed buckle closure shape, freely-supported fixing end is convex along bottom in circular hole; The loading end be it is discoid, disk top perimeter be equipped in protrusion load annulus hemisphere.
Further, the load annulus hemisphere is contacted with the substrate for being coated with film contacts for line, and contact surface is same In horizontal plane.
Preferably, the film surface, which surveys thermal conductivity of film method according to 3 ω, sputters four pads, using MEMS technology It is that micron-sized metal strip is produced on film surface by a geometric scale, four pads connect metal strip, and the pad includes As test electrode, shape is two pairs of electric current anode and cathode terminals and voltage positive and negative anodes for two electric current pads and two voltage pads Terminal is distributed in metal strip end according to π shape.
Preferably, the maximum compression distance of the loading end is identical as the thickness of film.
Further, the screw pitch accuracy of precise guide rod is with the ratio for the film thickness being coated with no more than 10-2
The present invention accordingly gives a kind of method using described device measurement thin film strain and thermal conductivity, including following steps It is rapid:
1) uniformly deposited in the circular-base that radius is R a layer thickness be t, Young's modulus E, Poisson's ratio be μ to Survey film;
2) it is being less than radius R0Be coated with film substrate surface sputtering test electrode, while using MEMS technology by one Geometric scale is that micron-sized metal strip is produced on film surface, wherein (R0< R) R0It is arrived for the load annulus hemisphere on loading end The distance in the loading end center of circle;
3) a displacement S is applied by precise guide rod, the load annulus hemisphere and freely-supported fixing end for corresponding to loading end exist A corresponding circumferential strain ε is generated on filmθ, the as strain of detected materials;
4) substrate for having prepared step 2) is placed on the load annulus hemisphere surface of device loading end, to test electrode Two electric current pads be passed through periodic current Iω, voltage tester electrode is connected to the external detection electricity with locking phase amplification module Lu Zhong directly reads the data of acquisition using computer, after pending data is stablized, records the ingredient U of 3 ω harmonic waves at this timeIt is big It is small;
5) by control feeding displacement S, carry out the size of controlled strain, to strain as independent variable, 3 read by computer The ingredient U of ω harmonic waveSize obtain the thermal conductivity k of film.
The beneficial effects of the present invention are:
The apparatus structure is simple, easily operated, and the size and thin film strain for the strain order of magnitude that film generates are at one The characteristics of in determining region without significant change, fully meet measurement film it is differently strained under thermal conductivity requirement;Measurement side Method mature and reliable, and being capable of practical application.
Detailed description of the invention
Fig. 1 is the main view of loading device.
Fig. 2 (a)-(c) is respectively main view, side view and the top view for loading shell.
Fig. 3 is the shape of sputtering test electrode.
Fig. 4 is electrode connection schematic diagram when 3 ω methods measure thermal conductivity of thin film.
Fig. 5 is film, substrate, pad locations schematic diagram.
Fig. 6 is radius R0With strain stress relation figure.
Fig. 7 is guide rod stroke and strain stress relation figure.
In figure: the load annulus hemisphere of 1- measuring device;2- shell;3- pedestal;4 freely-supported fixing ends;5- is coated with film Substrate;6- loading end;7- precise guide rod.
Specific embodiment
The invention will be described in further detail with reference to the accompanying drawings and examples, but is not intended as doing invention any limit The foundation of system.
As shown in Figure 1, Figure 2 shown in (a)-(c), the present invention measures the device of thin film strain and thermal conductivity, including a pedestal 3, One setting shell 2 on the base 3, pedestal 3 are equipped with loading end 6, be coated with film substrate 5 be placed on loading end 6 and with The freely-supported fixing end 4 on 2 top of shell connects, and a precise guide rod 7 is equipped with below loading end 6, is coated in the substrate 5 of film and splashes Test electrode and a metal strip are penetrated, test electrode is connected with the external detection system with locking phase amplification module, and connects To computer;Being displaced S by the precession of precise guide rod 7 makes the film being coated in the substrate 5 of film generate strain, passes through control Feeding is displaced S to control the size of thin film strain, by being passed through periodic current I to test electrodeω, computer reads from test The ingredient U of 3 ω harmonic waves of electrode acquisitionSize obtain the thermal conductivity of film.
The shell of the device is round-meshed buckle closure shape, and freely-supported fixing end 4 is convex along bottom in circular hole;It is described Loading end be it is discoid, disk top perimeter be equipped in protrusion load annulus hemisphere 1.Film sample base material has Higher elasticity modulus, substrate are preferably circle, and upper and lower surface wants enough smooth, guarantees that test material is evenly distributed on substrate Surface, diameter can be determined according to the actual size of device.
As shown in Figure 3, Figure 4, film surface surveys thermal conductivity of film method in strict accordance with 3 ω and sputters four pads, uses A piece geometric scale is that micron-sized metal strip is produced on film surface by MEMS technology, and four pads connect metal strip, pad Including two electric current pads and two voltage pads as test electrodes, shape be two pairs of electric current anode and cathode terminals and voltage just Negative terminal is distributed in metal strip end according to π shape.
Be coated with thin film on 5 surface of substrate for being coated with film, and be coated with film substrate 5 maximum compression distance with The thickness of film is identical.The screw pitch accuracy of precession precise guide rod 7 and the ratio of coating film thickness are not more than 10-2.Load annulus half Ball 1 is contacted with the substrate 5 for being coated with film and is contacted for line, and contact surface is in the same horizontal plane.
The present invention measures thin film strain and the specific method of thermal conductivity is:
It is the circular membranes that t, Young's modulus E, Poisson's ratio μ, radius are R by thickness, using simple supported edge fixed form, It is the hemispheroidal precise guide rod control feeding displacement S of annulus that radius is a by one end, the annulus hemisphere where precise guide rod is applied It should be kept with circular membrane on the same axis when loading lotus, it, can using the deflection theory of statics balance and elastic sheet To obtain the deflection equation of intermediate plectane, analyze to obtain radius in R using similar method0The amount of deflection side of plectane between R Journey is obtained analysis shows the size of strain is only the function for being displaced S by continuity principle, when radius is equal to R0When, two parts Deflection value it is equal, by accurate thread stroke, available radius is in R0The angle value of disturbing of plectane between R (feeds position Move the size of S), and then intermediate circular membrane circumferential strain and radial strain value are calculated, film is measured using 3 ω measurement methods Thermal conductivity, both realized the measurement of thermal conductivity of the film under differently strained.
The specific method is as follows:
Step 1: as shown in figure 5, uniformly depositing a layer thickness in the circular-base that radius is R is t, Young's modulus E, Poisson's ratio is the film to be measured of μ.
Step 2: as shown in Figure 4 and Figure 5, it is being less than radius R0Be coated with film substrate surface sputtering test electrode, together A piece geometric scale is that micron-sized metal strip is produced on film surface by Shi Caiyong MEMS technology, wherein R0< R, R0For load On end load annulus hemisphere to the loading end center of circle distance.
Step 3: in its radius R0(R0< R) at by precise guide rod apply a lesser displacement S, correspond to loading end Load annulus hemisphere a corresponding circumferential strain ε is generated on film to be measured with freely-supported fixing endθ, as detected materials Strain.It is the hemispheroidal precise guide rod control feeding displacement of annulus that radius is a by one end using simple supported edge fixed form S, the hemisphere in precise guide rod should keep being based on this axis pair in same axial location with circular membrane when applying load The statics and deflection theory for claiming circular membrane problem are analyzed as follows.
First to R0< r < R annulus film substrate is analyzed, and the transverse shearing force that film substrate is subject to is:
It is brought into corresponding equilibrium equation:
Film thickness is t, Young's modulus E, Poisson's ratio μ;The bending stiffness for the circular membrane substrate that D is indicated;ω (r) table Show film substrate deflection equation;QrIndicate the transverse shearing force being subject to;F indicates annulus concentrfated load power.
Three times to r continuous integral, R is obtained0< r < R annulus film substrate deflection equation:
Substitute into corresponding boundary condition:
R=R, ω (r)=0, Mr=0;R=R0,Mr=0
MrThe radial moment of flexure that the circular membrane substrate of expression is subject to.
Obtain R0< r < R annulus film substrate deflection equation is:
Work as r=R0When, S=ω (r) can further obtain the size of annulus concentrfated load F are as follows:
Again to intermediate circular membrane substrate r≤R0It is analyzed, the shearing being subject at this time is:
Qr=0
It is brought into corresponding equilibrium equation:
Three times to r continuous integral, r≤R is obtained0Circular membrane substrate deflection equation:
Substitute into corresponding boundary condition:
R=0, θ1(0)=0;R=R01(R0)=ω (R0),θ1(R0)=θ (R0)
θ1(r) what is indicated is radius no more than R0Circular membrane substrate corner, θ (r) indicate be radius in R and R0 Between annulus film substrate corner.
Knowing the relationship of radial strain and circumferential strain and amount of deflection simultaneously is:
What wherein z was indicated is thickness value of the film substrate apart from neutral surface, if the surface of circular membrane is then:
By learning above, i.e., radial strain and circumferential strain only and C1It is related, obtain r≤R0Circular membrane substrate deflection equation ω1(r) C in1It is:
It finally obtains:
Work as r=R0, utilize S=ω (R0)=ω1(R0) relationship can further can be obtained:
In formula t be the thickness of film, μ be Poisson's ratio, R0To load annulus hemisphere to the loading end center of circle on loading end Distance, R are the radius for loading annulus hemisphere and substrate contact profile, and S is the displacement of precise guide rod.
Conclusion:
(1) what strain at this time indicated is that (radius is not more than R to intermediate film0) strain, it can be seen that the size of strain is Guide rod is displaced the function of S, obtains ε by above formulaθIt is linear relationship with guide rod displacement S;
(2) circumferential strain εθAnnulus hemisphere is loaded to loading end center of circle distance R on loading end0With functional relation. It is displaced S by guide rod screw thread travel, obtains circumferential strain εθ, test electrode is sputtered on circular membrane surface, with circumferential strain εθ As the strain on measurement circular membrane surface, using the thermal conductivity of 3 ω methods measurement film.
3 ω measurement methods have proven to be a kind of very effective method of testing film thermal conductivity.One relatively thin electricity The metal wire of conduction is deposited on sample to be tested, and Fig. 3 and Fig. 4 are seen in test electrode shape and position.At two of mark electric current The periodic current I that frequency is ω is passed through on padω, this metal strip is both heater and temperature sensor, on metal strip The Joule heat that frequency is 2 ω will be generated, the amplitude and phase of thermal diffusion wave become according to the thermal conductivity k of material and specific heat capacity c Change, includes the ingredient U of one 3 ω harmonic wave by the voltage that heater measures, this portion voltage is exactly the hot physical property of material The information of generation.Correlation theory verified UThere are f (U with k, k) and functional relation
Step 4: the substrate that step 2 has been prepared is placed on the load annulus hemisphere surface of device loading end, to survey Two electric current pads of examination electrode are passed through periodic current Iω, voltage tester electrode, which is connected to outside, has locking phase amplification module In detection circuit, the data of acquisition are directly read using computer, after pending data is stablized, record the ingredient U of 3 ω harmonic waves at this time Size.
Step 5: feeding displacement S by control, carry out the size of controlled strain, machine-readable by calculating to strain as independent variable The ingredient U of the 3 ω harmonic waves takenSize obtain the thermal conductivity k of film to be measured.
The thermal conductivity k of the film and ingredient U of harmonic waveIt is obtained by following formula:
In formula, k is thermal conductivity, and P/l respectively indicates the heating power of metal strip heating film unit length, and Δ T indicates temperature Fluctuation, U0Indicate fundamental voltage, R '0For metal strip initial resistivity value, dR ,/dT indicate resistance variation with temperature rate, UIt indicates Voltage containing 3 ω harmonic waves.
The method theoretical foundation is strong, and the size and thin film strain for the strain order of magnitude that film generates are determining at one Feature in the same size in region, fully meet measurement film it is differently strained under thermal conductivity requirement;Measurement method maturation can It leans on, and being capable of practical application.
Wherein above-mentioned all parameters are all made of the International System of Units.
The present invention is further illustrated to a specific example below.
The material of selection is aluminium, and specific parameter is: radius of load R0=20mm, film radius R=35mm, Poisson's ratio μ =0.33, elastic modulus E=68.9Gpa, thickness t=0.8mm.
Selection guide rod feeding length is displaced S=0.2mm at this time, is by the size that corresponding formula obtains F:
F=111.7505N
εrθ=2.8767 × 10-4
By actual calculating and analysis, the size order meet demand strained at this time.
Then it is calculated with multiple numerical value, at this time R0Until uniformly increasing 1mm to 20mm since 5mm, Fig. 6 is obtained.
Another theoretical test condition is: R0It is 20mm, film radius R=35mm, Poisson's ratio μ=0.33, elastic modulus E =68.9Gpa, thickness t=0.8mm.Guide rod stroke (compression distance, displacement S or ω1(r) deflection value) from 0.05mm to Between 0.3mm, draws, obtained such as Fig. 7 every 0.01mm.
Interpretation of result: radius R0Relationship with thin film strain is logarithmic function relationship, guide rod stroke (compression distance, displacement S Or ω1(r) deflection value) with thin film strain be linear relationship, and strain size fully meet requirement.
Finally using the thermal conductivity of 3 ω measurement methods measurement film, the I of the electric current being passed through at this timeω, test voltage U, Finally obtain the functional relation f (ε, k) of strain stress Yu thermal conductivity k.
By embodiment as can be seen that the present invention measures thin film strain and the method for thermal conductivity passes through thermal conductivity and strain Relationship can determine the internal state of film, meet the needs of to strain;What effectively solution device can work normally asks Topic.

Claims (8)

1. a kind of device for measuring thin film strain and thermal conductivity, which is characterized in that including a pedestal (3), one is arranged the bottom of at Shell (2) on seat (3), the pedestal (3) are equipped with loading end (6), and the substrate (5) for being coated with film is placed on loading end (6) And connect with the freely-supported fixing end (4) on shell (2) top, it is equipped with a precise guide rod (7) below loading end (6), is coated with thin Sputtering has test electrode and a metal strip, test electrode and the external detection with locking phase amplification module in the substrate (5) of film System is connected, and is connected to computer;
Being displaced S by the precession of precise guide rod (7) makes the film being coated in the substrate (5) of film generate strain, passes through control Feeding is displaced S to control the size of thin film strain, by being passed through periodic current I to test electrodeω, computer reads from test The ingredient U of 3 ω harmonic waves of electrode acquisitionSize obtain the thermal conductivity of film;
The shell (2) is round-meshed buckle closure shape, and freely-supported fixing end (4) is convex along bottom in circular hole;It is described to add Carry end be it is discoid, disk top perimeter be equipped in protrusion load annulus hemisphere (1).
2. a kind of device for measuring thin film strain and thermal conductivity as described in claim 1, which is characterized in that the load annulus Hemisphere (1) is contacted with the substrate (5) for being coated with film to be contacted for line, and contact surface is in the same horizontal plane.
3. a kind of device for measuring thin film strain and thermal conductivity as described in claim 1, which is characterized in that the film surface Thermal conductivity of film method is surveyed according to 3 ω and sputters four pads, uses MEMS technology by a geometric scale for micron-sized metal Item is produced on film surface, and four pads connect metal strip, and the pad includes that two electric current pads and two voltage pads are made To test electrode, shape is distributed in metal strip end according to π shape for two pairs of electric current anode and cathode terminals and voltage anode and cathode terminals.
4. a kind of device for measuring thin film strain and thermal conductivity as described in claim 1, which is characterized in that the loading end (6) maximum compression distance is identical as the thickness of film.
5. a kind of device for measuring thin film strain and thermal conductivity as claimed in claim 4, which is characterized in that precise guide rod (7) Screw pitch accuracy with the ratio of film thickness that is coated with no more than 10-2
6. a kind of method using device as described in claim 1 measurement thin film strain and thermal conductivity, which is characterized in that including under State step:
1) uniformly deposited in the circular-base that radius is R a layer thickness be t, Young's modulus E, Poisson's ratio be μ it is to be measured thin Film;
2) it is being less than radius R0The substrate surface sputtering test electrode for being coated with film, while using MEMS technology by a geometry Scale is that micron-sized metal strip is produced on film surface, wherein R0< R, R0For the load annulus hemisphere on loading end to load Hold the distance in the center of circle;
3) a displacement S is applied by precise guide rod, the load annulus hemisphere and freely-supported fixing end for corresponding to loading end are in film One corresponding circumferential strain ε of upper generationθ, the as strain of detected materials;
4) substrate for having prepared step 2) is placed on the load annulus hemisphere surface of device loading end, to the two of test electrode A electric current pad is passed through periodic current Iω, voltage tester electrode is connected to the external detection circuit with locking phase amplification module In, the data of acquisition are directly read using computer, after pending data is stablized, record the ingredient U of 3 ω harmonic waves at this timeSize;
5) by control feeding displacement S, carry out the size of controlled strain, to strain as independent variable, 3 ω read by computer are humorous The ingredient U of waveSize obtain the thermal conductivity k of film.
7. it is according to claim 6 measurement thin film strain and thermal conductivity method, which is characterized in that it is described obtain strain with Displacement S has following relationship:
In formula t be the thickness of film, μ be Poisson's ratio, R0To load distance of the annulus hemisphere to the loading end center of circle, R on loading end For the radius for loading annulus hemisphere and substrate contact profile, S is the displacement of precise guide rod.
8. the method for measurement thin film strain and thermal conductivity according to claim 6, which is characterized in that the thermal conductivity of the film The ingredient U of rate k and harmonic waveIt is obtained by following formula:
In formula, k is thermal conductivity, and P/l respectively indicates the heating power of metal strip heating film unit length, and Δ T indicates temperature fluctuation, U0Indicate fundamental voltage, R '0For metal strip initial resistivity value, dR '/dT indicates resistance variation with temperature rate, UExpression contains 3 The voltage of ω harmonic wave.
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CN108844990B (en) * 2018-04-10 2020-05-22 西安交通大学 MEMS (micro-electromechanical system) process based film strain thermal conductivity testing device and method

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