CN102305777A - Method for detecting adhesiveness of film based on surface wave - Google Patents

Method for detecting adhesiveness of film based on surface wave Download PDF

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CN102305777A
CN102305777A CN201110207915A CN201110207915A CN102305777A CN 102305777 A CN102305777 A CN 102305777A CN 201110207915 A CN201110207915 A CN 201110207915A CN 201110207915 A CN201110207915 A CN 201110207915A CN 102305777 A CN102305777 A CN 102305777A
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surface wave
film
substrate
dispersion curve
adhesiveness
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肖夏
单兴锰
孙远
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Tianjin University
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Tianjin University
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Abstract

The invention belongs to the technical field of film nondestructive detection, and relates to a method for detecting the adhesiveness of a film based on a surface wave. The method comprises the following steps of: constructing a spring hypothetical model representing the adhesive characteristic of a film; establishing a particle displacement expression of the surface wave; substituting a boundary condition of the surface wave spread in a film/base structure into the surface wave particle displacement expression so as to obtain an equation group composed of 6 equations, namely B6*6C6*1=0; causing determinant of a coefficient matrix B6*6 to be zero, and taking KN and KT as parameters influencing a chromatic dispersion curve, so as to obtain the chromatic dispersion curve of the surface wave; exciting the surface wave on the surface of a sample sheet to be detected; collecting surface wave signals from two different positions close to the surface of the sample sheet to be detected; analyzing and processing the surface wave signals, so as to obtain an experimental chromatic dispersion curve of the surface wave; matching the curve with the obtained surface wave dispersion curve, so as to obtain a normal elastic coefficient KN on the surface of the sample sheet to be detected; and determining the adhesiveness between the thin film and the base according to the KN. The detection method provided by the invention can be used for fast and accurately detecting the adhesiveness between the film and the base without loss.

Description

Adhesion of film property detection method based on surface wave
Technical field
The invention belongs to the film technical field of nondestructive testing, relate to the adhesiveness detection method between a kind of film and the base material.
Background technology
Adhesiveness between film and the substrate is an important mechanical of membraneous material, has a strong impact on the quality and the life-span of product, therefore needs development to characterize the correlation detection technology of adhesion of film property.Usually having adhesive tape to glue to adhesion of film property sign takes off several different methods such as method, scarification, has diversity and complicacy.The sticking method of taking off of adhesive tape uses special adhesive tape to stick on film surface, adopts certain angle and speed that adhesive tape is uncovered, and the situation that viewing film is uncovered by adhesive tape is judged the adhesiveness between film and the substrate with this.This method is a kind of detection technique that diminishes, and reactive film adhesiveness qualitatively.The cut ratio juris is streaked film surface to be measured for the pressure head that adopts nano-scale with given pace, and the pressure at right angle that acts on simultaneously on the pressure head constantly increases, and peels off from substrate up to film.The minimum pressure that film is peeled off from substrate is designated as critical load, characterizes the adhesiveness of film and substrate with this.This technology can cause damage to film equally, and receives the influence of factors such as cut speed, load speed, roughness of film, adhesiveness that therefore can only semiquantitative sign film.Above method all can't realize to adhesion of film property quantitatively, therefore nondestructive characterisation (NDC) just needs a kind ofly can to carry out fast film and substrate adhesion, the new technique of accurate, nondestructive characterisation (NDC).
Summary of the invention
The purpose of this invention is to provide and a kind ofly can detect adhering lossless detection method between film and the substrate quickly and accurately.Technology of the present invention is applied widely, and film thickness can need not treated the test sample sheet and handle especially from tens nanometers to several microns.For this reason, the present invention adopts following technical scheme.
A kind of adhesion of film property detection method based on surface wave comprises the following steps:
(1) establishes surface wave vibration particle along three-dimensional coordinate direction x 1, x 2, x 3Displacement components u 1, u 2, u 3, normal direction spring ratio and tangential elastic force coefficient between film and substrate are respectively K T, K T, foundation characterizes the spring hypothesized model of the adhesion characteristics of film, sets up surface wave particle displacement expression formula u j = Σ C n α j ( n ) exp ( ikb ( n ) x 3 ) exp [ ik ( l 1 x 1 + l 2 x 2 - vt ) ] , Wherein, v is the phase velocity of surface wave along wave number vector k direction, (l 1, l 2, l 3) be the direction cosine of surface wave propagation, for surface wave l 3=0, α jBe the relative amplitude of each harmonic component of surface wave, b is illustrated in the tack wave-amplitude that records on the plane vertical with the direction of propagation and the phase place variable quantity with the degree of depth, C n(n is 1～6 integer) is weighting coefficient;
(2) will set up the boundary condition that the following surface wave of surface wave particle displacement expression formula substitution is propagated in film/underlying structure, obtain a system of equations B who forms by 6 equations 6 * 6C 6 * 1=0;
1) equates at film/substrate interface place stress, i.e.
Figure BDA0000078171330000012
Figure BDA0000078171330000013
2) discontinuous in film/substrate interface place displacement, the relation of stress and displacement is: T 31 = K T [ u ^ 31 - u 31 ] T 33 = K N [ u ^ 33 - u 33 ] ;
3) (film top) stress is zero at the Free Surface place, i.e.
Figure BDA0000078171330000021
Figure BDA0000078171330000022
In the top boundary condition,
Figure BDA0000078171330000023
T 31Be illustrated respectively in film and the substrate, be parallel to x 3=0 plane is along x 1The tangential stress of direction; T 33Be illustrated respectively in film and the substrate, perpendicular to x 3=0 plane is along x 3The normal stress of direction;
Figure BDA0000078171330000025
u 31Be illustrated respectively in film and the substrate, be parallel to x 3=0 plane is along x 1The displacement of direction;
Figure BDA0000078171330000026
u 33Be illustrated respectively in film and the substrate, perpendicular to x 3=0 plane is along x 3The displacement of direction;
(3) make matrix of coefficients B 6 * 6Determinant be zero, with K NAnd K TAs the parameter that influences dispersion curve,, obtain funtcional relationship, i.e. the dispersion curve of surface wave about speed v and frequency f through numerical evaluation;
(4) at print surface excitation surface wave to be measured, gather its surface wave signal at two diverse location places near its surface, be transferred to computing machine;
(5) the surface wave signal of two diverse location places being gathered carries out analyzing and processing, obtains the experimental dispersion curve of surface wave;
(6) carry out matching ratio with experimental dispersion curve with according to the surface wave dispersion curve that step 4 obtains, obtain the normal direction spring ratio K on print to be measured surface N
(7) according to K NSize is confirmed the adhesiveness between film and the substrate, K NBig more, adhesiveness is good more.
As preferred implementation, in the step (8), if K N＞100PPa/m then judges between film and the substrate to have good adhesive force property.
The present invention has considered the character of membraneous material and base material; Set up the model of accurate sign adhesiveness, laid a good foundation for obtaining accurate measured value, in the actual measurement the influence of surface wave dispersion characteristics; Adopt lossless detection method; Only need to adopt short-pulse laser, do not detect its adhesiveness, be applicable to the online detection in the commercial production and need film separated with substrate through external influence at print surface excitation surface wave.
Description of drawings
Fig. 1 surface wave is at the model synoptic diagram with " spring hypothesis ";
Fig. 2 K NVariation to the influence curve of surface wave dispersion curve;
The dispersion curve that Fig. 3 (a) surface wave is propagated in porous membrane/silicon base structure;
The dispersion curve that Fig. 3 (b) surface wave is propagated in dense film/silicon base structure.
Embodiment
The present invention adopts the short-pulse laser source to go out to have the surface wave signal of big spectrum width at the print surface excitation.Utilize the piezoelectric effect device that the surface wave signal is gathered.Have different normal direction spring ratio (K through software programming calculating N) time the surface wave dispersion curve.Experiment is detected the surface wave dispersion curve obtain and the dispersion curve that Theoretical Calculation obtains mate, thus the K of definite print film and substrate interface NValue, and with the parameter of this value as sign film/substrate adhesion.Specify the present invention below.
Dispersion phenomenon can take place when in film/underlying structure, propagating in surface wave, and promptly surperficial phase velocity of wave is with change of frequency.Aspect theoretical, the dispersion curve of surface wave can obtain through under the boundary condition of " spring hypothesis ", find the solution the wave equation that surface wave propagates in non-piezoelectric dielectric.According to the character of wave equation, surface wave vibration particle is along three-dimensional coordinate direction x 1, x 2, x 3Displacement components u 1, u 2, u 3Separating of following form should be arranged:
u j＝α j?exp(ikbx 3)exp[ik(l 1x 1+l 2x 2+l 3x 3-vt)](j＝1，2，3) (1)
Wherein, v is the phase velocity of surface wave along wave number vector k direction, (l 1, l 2, l 3) be the direction cosine of surface wave propagation.For surface wave l 3=0.α jIt is the relative amplitude of each harmonic component of surface wave.B is illustrated in the variation with the degree of depth of the tack wave-amplitude that records on the plane vertical with the direction of propagation and phase place.
In order to characterize the adhesion characteristics of film, as shown in Figure 1, between film and substrate, introduce " spring hypothesis " model.Through introducing the normal direction spring ratio (K between film and substrate N) and tangential elastic force coefficient (K T) characterize the adhesion issues of film and substrate.Therefore, the boundary condition in film/underlying structure, propagated of surface wave should be:
(1) equates at film/substrate interface place stress, i.e.
Figure BDA0000078171330000031
Figure BDA0000078171330000032
(2) discontinuous in film/substrate interface place displacement, the relation of stress and displacement is: T 31 = K T [ u ^ 31 - u 31 ] T 33 = K N [ u ^ 33 - u 33 ] ;
(3) (film top) stress is zero at the Free Surface place, i.e.
Figure BDA0000078171330000034
Figure BDA0000078171330000035
In the top boundary condition,
Figure BDA0000078171330000036
T 31Be illustrated respectively in film and the substrate, be parallel to x 3=0 plane is along x 1The tangential stress of direction;
Figure BDA0000078171330000037
T 33Be illustrated respectively in film and the substrate, perpendicular to x 3=0 plane is along x 3The normal stress of direction;
Figure BDA0000078171330000038
u 31Be illustrated respectively in film and the substrate, be parallel to x 3=0 plane is along x 1The displacement of direction; u 33Be illustrated respectively in film and the substrate, perpendicular to x 3=0 plane is along x 3The displacement of direction.
According to the character of linear differential equation,, make it satisfy wave equation and boundary condition simultaneously with the stack of surface wave particle displacement expression formula (1) linear weighted function.If weighting coefficient is C n(n is 1～6 integer), separating of wave equation is rewritten as:
u j = Σ C n α j ( n ) exp ( ikb ( n ) x 3 ) exp [ ik ( l 1 x 1 + l 2 x 2 - vt ) ] - - - ( 2 )
Bring formula (2) into above-mentioned boundary condition, can get a system of equations of forming by 6 equations:
B 6×6C 6×1＝0(3)
Matrix B 6 * 6In comprise speed v and frequency f (f can try to achieve with f=vk/2 π), the tangential elastic force COEFFICIENT K T, normal direction spring ratio K N, direction cosine (l 1, l 2, l 3), film Young modulus, Poisson constant, density of film, film thickness, substrate density, the elastic stiffness constant of substrate.Film Young modulus wherein, Poisson constant, density of film, film thickness, substrate density, the elastic stiffness constant of substrate all can detect or in the material handbook, consult through additive method, have only K NAnd K TBecome the parameter that influences dispersion curve.
According to linear algebra knowledge, for making C nUntrivialo solution is arranged, its matrix of coefficients B 6 * 6Determinant be necessary for zero.Therefore, set some K NAnd K TValue, and with it as parameter, find the solution through computer software programming, can obtain funtcional relationship, i.e. the dispersion curve of surface wave about speed v and frequency f.
Aspect experiment, the surface wave that utilizes short-pulse laser can go out to have broad frequency band at print surface excitation to be measured through thermoelastic effect.The surface wave signal is transferred to computing machine and carries out analyzing and processing by the piezoelectric transducer collection.For recording the surface wave experimental dispersion curve, need carry out Fourier transform to these two signals afterwards at two diverse location acquisition tables ground roll signals.Through formula v SAW(f)=Δ x/ ΔΦ (f) can be in the hope of the experimental dispersion curve of surface wave.Wherein, v SAW(f) presentation surface phase velocity of wave, Δ x are two distances between the detection position, and ΔΦ (f) is the difference at phasing degree behind the two signal Fourier transforms.
Theoretical Calculation shows, with respect to the tangential elastic force COEFFICIENT K T, normal direction spring ratio K NInfluence to the surface wave dispersion characteristics is bigger.Accompanying drawing 2 has shown K NIn 5～1000PPa/m (1PPa/m=1 * 10 15Pa/m), in adhesiveness is infinitely-great perfect boundary condition scope, to the influence of surface wave dispersion curve.Work as K N(K when big N＞100PPa/m), the surface wave dispersion curve is tending towards overlapping, explain between film and the substrate at this moment to have good adhesive force property.Based on above-mentioned model, the surface wave dispersion curve negotiating least square method coupling that experiment records and Theoretical Calculation goes out can be obtained the adhesiveness between print film to be measured and the substrate.
Referring to accompanying drawing 3, Fig. 3 (a) is the dispersion curve that porous film material/silicon base upper surface ripple is propagated, its adhesiveness detected value K NBe 8PPa/m; Fig. 3 (b) is the dispersion curve that dense film material/silicon base upper surface ripple is propagated, its adhesiveness detected value K NBe 50PPa/m, the adhesiveness of dense material and substrate is better than porosint.Through scarification two prints are detected, it is used to characterize adhering parameter, and crucial payload values is respectively 2.548 and 10.885mN, thereby instruction card ground roll method can effectively detect the adhesiveness of film.

Claims (2)

1. the adhesion of film property detection method based on surface wave comprises the following steps:
(1) establishes surface wave vibration particle along three-dimensional coordinate direction x 1, x 2, x 3Displacement components u 1, u 2, u 3, normal direction spring ratio and tangential elastic force coefficient between film and substrate are respectively K N, K T, foundation characterizes the spring hypothesized model of the adhesion characteristics of film, sets up surface wave particle displacement expression formula u j = Σ C n α j ( n ) exp ( ikb ( n ) x 3 ) exp [ ik ( l 1 x 1 + l 2 x 2 - vt ) ] , Wherein, v is the phase velocity of surface wave along wave number vector k direction, (l 1, l 2, l 3) be the direction cosine of surface wave propagation, for surface wave l 3=0, α jBe the relative amplitude of each harmonic component of surface wave, b is illustrated in the tack wave-amplitude that records on the plane vertical with the direction of propagation and the phase place variable quantity with the degree of depth, C n(n is 1～6 integer) is weighting coefficient;
(2) will set up the boundary condition that the following surface wave of surface wave particle displacement expression formula substitution is propagated in film/underlying structure, obtain a system of equations B who forms by 6 equations 6 * 6C 6 * 1=0;
1) equates at film/substrate interface place stress, i.e.
Figure FDA0000078171320000012
2) discontinuous in film/substrate interface place displacement, the relation of stress and displacement is: T 31 = K T [ u ^ 31 - u 31 ] T 33 = K N [ u ^ 33 - u 33 ] ;
3) stress is zero at the Free Surface place, i.e.
Figure FDA0000078171320000015
In the top boundary condition,
Figure FDA0000078171320000017
T 31Be illustrated respectively in film and the substrate, be parallel to x 3=0 plane is along x 1The tangential stress of direction;
Figure FDA0000078171320000018
T 33Be illustrated respectively in film and the substrate, perpendicular to x 3=0 plane is along x 3The normal stress of direction;
Figure FDA0000078171320000019
u 31Be illustrated respectively in film and the substrate, be parallel to x 3=0 plane is along x 1The displacement of direction;
Figure FDA00000781713200000110
u 33Be illustrated respectively in film and the substrate, perpendicular to x 3=0 plane is along x 3The displacement of direction;
(3) make matrix of coefficients B 6 * 6Determinant be zero, with K NAnd K TAs the parameter that influences dispersion curve,, obtain funtcional relationship, i.e. the dispersion curve of surface wave about speed v and frequency f through numerical evaluation;
(4) at print surface excitation surface wave to be measured, gather its surface wave signal at two diverse location places near its surface, be transferred to computing machine;
(5) the surface wave signal of two diverse location places being gathered carries out analyzing and processing, obtains the experimental dispersion curve of surface wave;
(6) experimental dispersion curve and the surface wave dispersion curve that obtains according to step (3) are carried out matching ratio, obtain the normal direction spring ratio K on print to be measured surface N
(7) according to K NAdhesiveness between size film and the substrate, K NBig more, adhesiveness is good more.
2. method according to claim 1 is characterized in that, in the step (8), if K N＞100PPa/m then judges between film and the substrate to have good adhesive force property.
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104458570A (en) * 2014-11-28 2015-03-25 河海大学常州校区 Method for judging connecting compactness of interface by using spring stiffness coefficient
CN105653784A (en) * 2015-12-28 2016-06-08 天津大学 Method for determining composite parameter that characterizes adhesion of thin film based on cohesion model
CN105651689A (en) * 2015-12-28 2016-06-08 天津大学 Nondestructive testing method for adhesion of thin film based on cohesion model
CN106770654A (en) * 2016-12-08 2017-05-31 天津大学 A kind of method of film adherability quality is judged with adhesiveness criterion value
CN110057911A (en) * 2019-03-08 2019-07-26 天津大学 A kind of surface acoustic wave nondestructive detection system
CN110057910A (en) * 2019-03-08 2019-07-26 天津大学 Using the method for removable dual probe piezoelectric transducer measurement film adherability

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104458570A (en) * 2014-11-28 2015-03-25 河海大学常州校区 Method for judging connecting compactness of interface by using spring stiffness coefficient
CN105653784A (en) * 2015-12-28 2016-06-08 天津大学 Method for determining composite parameter that characterizes adhesion of thin film based on cohesion model
CN105651689A (en) * 2015-12-28 2016-06-08 天津大学 Nondestructive testing method for adhesion of thin film based on cohesion model
CN105651689B (en) * 2015-12-28 2018-10-16 天津大学 A method of the non-destructive testing film adherability based on cohesive zone model
CN105653784B (en) * 2015-12-28 2019-03-12 天津大学 The method of the complex parameter of characterization film adherability is determined based on cohesive zone model
CN106770654A (en) * 2016-12-08 2017-05-31 天津大学 A kind of method of film adherability quality is judged with adhesiveness criterion value
CN110057911A (en) * 2019-03-08 2019-07-26 天津大学 A kind of surface acoustic wave nondestructive detection system
CN110057910A (en) * 2019-03-08 2019-07-26 天津大学 Using the method for removable dual probe piezoelectric transducer measurement film adherability
CN110057911B (en) * 2019-03-08 2021-08-13 天津大学 Surface acoustic wave nondestructive testing system
CN110057910B (en) * 2019-03-08 2021-08-17 天津大学 Method for measuring film adhesion by adopting movable double-probe piezoelectric sensor

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Application publication date: 20120104