CN101923043A - Accurate measurement method for interface energy release rate of coating film-substrate structure - Google Patents

Accurate measurement method for interface energy release rate of coating film-substrate structure Download PDF

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CN101923043A
CN101923043A CN 201010245009 CN201010245009A CN101923043A CN 101923043 A CN101923043 A CN 101923043A CN 201010245009 CN201010245009 CN 201010245009 CN 201010245009 A CN201010245009 A CN 201010245009A CN 101923043 A CN101923043 A CN 101923043A
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radius
film
coating film
release rate
energy release
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CN101923043B (en
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孙俊贻
许劲
何晓婷
郑周练
胡建力
耿欢欢
朱海桥
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CHONGQING ZHONGKE CONSTRUCTION (GROUP) Co Ltd
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Chongqing University
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Abstract

The invention discloses an accurate measurement method for the interface energy release rate of a coating film-substrate structure. The method comprises the following steps of: opening an aperture with the radius of d on the substrate of a film-substrate structure; clamping a film by using a circular clamping plate with the radius of b (b is less than d) on the central part of an aperture area so that the film in the clamped area cannot be deformed; slowly applying an external force F to the film by using the circular clamping plate to separate a coating film from a substrate and form a bubble with the radius of a and the height of wm; increasing measurement density; measuring bubble heights w1, w2,..., wm-1 and wm and corresponding external forces F1, F2,..., Fm-1 and Fm thereof as much as possible; and calculating the interface energy release rate of the coating film in the area separated from the substrate (namely in a circular ring with the radius of a-d) by using the measurement data. The measurement method for the interface energy release rate of the coating film-substrate structure of the invention has the characteristics of simple and feasible operation, few measurement parameters, and high accuracy of obtained energy release rate.

Description

A kind of accurate measurement method of coating film-substrate structural interface energy release rate
Technical field
The present invention relates to the interfacial energy release rate accurate measuring technique of coating film-substrate structure.
Background technology
By the laminate structure that different materials constitutes, promptly the film-substrate structure has obtained application more and more in many advanced technologies.In P.e.c. and encapsulation field, exist a large amount of ultra-thin coating film-substrate structures, adhesion strength between film and the basic unit can be with the adhesion energy evaluation on the unit area, and adhesion energy is not convenient for measurement, therefore, usually the reliability of film-based structures adopts an index evaluation that is referred to as " energy release rate ", promptly allows film on the unit area, breaks away from basic unit's energy needed (being energy to failure).
The measurement of energy release rate is calculated, and adopt static load bubble test (perhaps bloating test) and axle to carry bubble test usually and realize: opening a radius in the basic unit of film-based structures is
Figure 920769DEST_PATH_IMAGE001
Aperture, by aperture laminate structure is loaded, thereby makes film and basic unit's layering, and form a bubbling, record the displacement (degree of disturbing) of film And corresponding load
Figure 114170DEST_PATH_IMAGE003
With the bubbling radius
Figure 399658DEST_PATH_IMAGE004
Calculate external work
Figure 933408DEST_PATH_IMAGE005
,, calculate the elastic strain energy of film then by the Elasticity response of laminate structure
Figure 456793DEST_PATH_IMAGE006
External work Deduct the elastic strain energy of film
Figure 925000DEST_PATH_IMAGE006
Then break away from the energy to failure of basic unit for film, the energy to failure on the unit area is energy release rate.Because the static load bubble test is difficult to control well in test pressure, bubbling radius and bubbling height, therefore axle carries a bubble test and is advocated.
Because the coating film-substrate structure belongs to the superthin layer structure, finding the solution of its mechanical response belongs to the nonlinear mechanics answer usually, in most cases can only provide approximate solution, is difficult to try to achieve accurate analytic solution.Therefore, the testing program that is used for energy release rate measurement calculating is determined, should consider the operability in the test, takes into account the degree of accuracy that the response of superthin layer structural mechanics is found the solution again.This difficulty is perplexing the worldwide scholars in this field always, up to now, does not see one as yet and measures numerical procedure comparatively accurately.
Summary of the invention
In order to overcome the weak point in the existing measurements and calculations, the present invention has provided the accurately technical scheme of measurements and calculations coating film-substrate structural interface energy release rate of a cover.This technical scheme, easy and simple to handle feasible, measurement parameter is few, precision is high.
The object of the present invention is achieved like this: a kind of interfacial energy release rate accurate measurement method of coating film-substrate structure comprises the steps: to open a radius and is in the basic unit of coating film-substrate structure
Figure 465703DEST_PATH_IMAGE001
Aperture, at the opening area core, utilize a radius to be
Figure 374753DEST_PATH_IMAGE007
" circular clamping plate " film is clamped, make the film of clamped region can not produce distortion, by " circular clamping plate " film is slowly applied external force
Figure 506657DEST_PATH_IMAGE003
, make coating film break away from basic unit, and form a radius and be
Figure 501158DEST_PATH_IMAGE004
, highly be Bubbling, strengthen density measurement, as often as possible record the bubbling height And corresponding external force value
Figure 923633DEST_PATH_IMAGE010
, with the following formula of measurement data substitution, calculating coating film (is that radius is in the disengaging base layer region
Figure 874271DEST_PATH_IMAGE011
Annulus in) the interfacial energy release rate
(1)
Wherein,
Figure 171577DEST_PATH_IMAGE013
Be energy release rate,
Figure 114125DEST_PATH_IMAGE004
Be the bubbling radius,
Figure 83218DEST_PATH_IMAGE001
Be the radius of the aperture of opening in basic unit,
Figure 300573DEST_PATH_IMAGE014
Be coating film thickness, Be elastic modulus,
Figure 152171DEST_PATH_IMAGE016
Be Poisson ratio,
Figure 608561DEST_PATH_IMAGE017
, For the radius of circular clamping plate ( ),
Figure 241033DEST_PATH_IMAGE020
Be calculating parameter (can pass through the analytical method accurate Calculation, also can check in roughly) by accompanying drawing provided by the present invention,
Figure 653560DEST_PATH_IMAGE009
For corresponding to external force The bubbling height value,
Figure 925458DEST_PATH_IMAGE004
,
Figure 911869DEST_PATH_IMAGE018
,
Figure 546113DEST_PATH_IMAGE001
, ,
Figure 476208DEST_PATH_IMAGE002
Unit be the millimeter (mm),
Figure 633520DEST_PATH_IMAGE015
Unit be MPa (MPa),
Figure 755060DEST_PATH_IMAGE003
Unit be newton (N),
Figure 656020DEST_PATH_IMAGE013
Unit be 10 -3Joule/square millimeter (10 -3J/mm 2) or Newton/millimeter (N/mm).
" circular clamping plate " in the above constitutes by clamping disk cap (" 1 " among Fig. 1) and loading cylinder punching pin (" 2 " among Fig. 1), also claims by " clamping punching pin ".By " clamping punching pin " film is applied external force
Figure 343353DEST_PATH_IMAGE003
The time, slow down external force as far as possible
Figure 140408DEST_PATH_IMAGE003
The speed that applies (per minute is less than 1 millimeter), produce fracture to avoid film.Make like this related parameter (external force is arranged
Figure 280402DEST_PATH_IMAGE003
, the bubbling radius
Figure 719474DEST_PATH_IMAGE004
, the bubbling height
Figure 261314DEST_PATH_IMAGE002
) measurement conveniently realized.
In order to improve computational accuracy, adopt the surveying instrument of degree of precision as far as possible, accurately measure corresponding to external force
Figure 229270DEST_PATH_IMAGE021
The bubbling height
Figure 856560DEST_PATH_IMAGE022
, wherein,
Figure 99323DEST_PATH_IMAGE023
, and strengthen density measurement (promptly as far as possible Enough big), to guarantee adopting trapezoidal method to calculate the precision of definite integral.So external force
Figure 634526DEST_PATH_IMAGE003
Institute's work
Figure 749113DEST_PATH_IMAGE005
, can calculate by following formula:
Figure 264408DEST_PATH_IMAGE025
（2）
Thin flexible film strain energy in the existing method
Figure 515260DEST_PATH_IMAGE006
Calculating inaccurate.The present invention is (Jun-yi Sun on the basis of previous research work, Jian-li Hu, Xiao-ting He, Zhou-lian, Zheng, 2010. A theoretical study of a clamped punch-loaded blister configuration:the quantitative relation of load and deflection. International Journal of Mechanical Sciences. 52 (7), 928-936.), the accurate Analysis of the circular membrane that the periphery that utilizes a center to have hard-core clamps is separated, and has tried to achieve the thin flexible film strain energy of loading structure shown in Figure 1
Figure 356177DEST_PATH_IMAGE006
Precise calculation.Specific as follows: as to make film produce the external force of distortion
Figure 426902DEST_PATH_IMAGE026
Maximum degree of disturbing with the film generation
Figure 11467DEST_PATH_IMAGE008
Between, should satisfy following formula
Figure 382405DEST_PATH_IMAGE027
(3)
(see Jun-yi Sun for details, Jian-li Hu, Xiao-ting He, Zhou-lian, Zheng, 2010. A theoretical study of a clamped punch-loaded blister configuration:the quantitative relation of load and deflection. International Journal of Mechanical Sciences. 52 (7), 928-936.) therefore, the thin flexible film strain energy
Figure 863065DEST_PATH_IMAGE006
Can obtain by following formula
Figure 952244DEST_PATH_IMAGE028
(4)
Like this, our the interfacial energy release rate computing formula that can finally obtain the coating film-substrate structure is:
Figure 74921DEST_PATH_IMAGE029
(5)
By as can be seen above, energy release rate of the present invention
Figure 300366DEST_PATH_IMAGE013
Computational accuracy, depend primarily on the precision of surveying instrument.As long as surveying instrument has enough measuring accuracy, strengthen density measurement, just can guarantee the external force that formula (2) calculates
Figure 217506DEST_PATH_IMAGE003
Institute's work
Figure 528402DEST_PATH_IMAGE005
Enough computational accuracies are arranged, and the thin flexible film strain energy
Figure 454769DEST_PATH_IMAGE006
Computing formula (4) be accurate analytic solution, do not have the error of calculation, therefore, this has just guaranteed the computational accuracy of energy release rate.
Description of drawings
Fig. 1 loads organigram for bubble test, and among the figure, 1-clamps the disk cap, 2-loads basic unit, 4-coating film in cylinder punching pin, the 3-film based structures.1 and 2 constitute " clamping punching pin ".
Figure 269142DEST_PATH_IMAGE004
Be the bubbling radius,
Figure 622763DEST_PATH_IMAGE018
Be the radius of clamping disk and cylinder punching pin,
Figure 420954DEST_PATH_IMAGE001
Be the radius of the aperture of opening in basic unit,
Figure 619854DEST_PATH_IMAGE014
Be the thickness of coating film, Maximum degree of disturbing for deformation of thin membrane.Wherein
Figure 344414DEST_PATH_IMAGE019
Fig. 2 is a calculating parameter With Poisson ratio
Figure 366914DEST_PATH_IMAGE016
With Graph of a relation, promptly
Figure 382460DEST_PATH_IMAGE020
Parameter Map.Among the figure,
Figure 624085DEST_PATH_IMAGE017
Be respectively 0.0001,0.001,0.01,0.1,0.2,0.3,0.4,0.5,0.6,0.7,0.8,0.9, arrange in the direction of the clock.
Embodiment
Figure 430367DEST_PATH_IMAGE031
Measuring samples is made
Opening a radius in the basic unit of test specimen to be measured (being the coating film-substrate structure) is
Figure 604997DEST_PATH_IMAGE001
Aperture.
Figure 940163DEST_PATH_IMAGE032
Install by " clamping punching pin "
To clamp disk cap and cylinder punching pin firm grip, and make the film of clamped region can not produce distortion.
Figure 200243DEST_PATH_IMAGE033
Film is loaded
Film is loaded as far as possible slowly, rupture to avoid film, loading velocity is controlled at per minute less than in 1 millimeter, makes radius of the final formation of film be
Figure 810216DEST_PATH_IMAGE004
, highly be
Figure 308194DEST_PATH_IMAGE008
Bubbling, and circle ring area should have certain big radius
Figure 610999DEST_PATH_IMAGE011
, to guarantee the validity of surveying work.
Figure 92796DEST_PATH_IMAGE034
Measure
The present invention does not do specific requirement to surveying instrument, mainly stresses to provide a method, and according to test condition, the measurement of correlation instrument in this field can be selected for use to the greatest extent.Adopt surveying instrument as far as possible, accurately record the thickness of coating film with degree of precision
Figure 975301DEST_PATH_IMAGE014
, basic unit's perforate radius
Figure 858944DEST_PATH_IMAGE001
, the final bubbling radius that forms of film
Figure 332650DEST_PATH_IMAGE004
, and in the loading procedure corresponding to external force
Figure 301743DEST_PATH_IMAGE010
The bubbling height
Figure 722360DEST_PATH_IMAGE009
Strengthen density measurement, to guarantee adopting trapezoidal method to calculate the precision of definite integral as far as possible.
Energy release rate Calculating
According to the bubbling radius
Figure 295927DEST_PATH_IMAGE004
Calculate
Figure 51394DEST_PATH_IMAGE017
, by Poisson ratio
Figure 644049DEST_PATH_IMAGE016
With
Figure 928400DEST_PATH_IMAGE036
Value, according to our previous research work (Jun-yi Sun, Jian-li Hu, Xiao-ting He, Zhou-lian, Zheng, 2010. A theoretical study of a clamped punch-loaded blister configuration:the quantitative relation of load and deflection. International Journal of Mechanical Sciences. 52 (7), 928-936.), adopt analytical method accurately to determine calculating parameter
Figure 872085DEST_PATH_IMAGE020
, also can check in calculating parameter roughly by accompanying drawing 2 provided by the invention
Figure 431242DEST_PATH_IMAGE020
Utilize elastic modulus And measurement data
Figure 333656DEST_PATH_IMAGE010
And
Figure 764638DEST_PATH_IMAGE009
With the bubbling radius , basic unit's perforate radius , coating film thickness
Figure 55308DEST_PATH_IMAGE014
, calculate energy release rate by following formula:
Figure 442427DEST_PATH_IMAGE037
Wherein,
Figure 343386DEST_PATH_IMAGE015
With
Figure 765140DEST_PATH_IMAGE016
Be known parameter,
Figure 93354DEST_PATH_IMAGE004
,
Figure 702190DEST_PATH_IMAGE018
,
Figure 406840DEST_PATH_IMAGE001
,
Figure 960399DEST_PATH_IMAGE014
,
Figure 928355DEST_PATH_IMAGE002
Unit be the millimeter (mm), elastic modulus
Figure 555645DEST_PATH_IMAGE015
Unit be MPa (MPa), external force
Figure 798408DEST_PATH_IMAGE003
Unit be newton (N), energy release rate Unit be 10 -3Joule/square millimeter (10 -3J/mm 2) or Newton/millimeter (N/mm).

Claims (1)

1. the accurate measurement method of a coating film-substrate structural interface energy release rate, it is characterized in that: opening a radius in the basic unit of film-based structures is
Figure 2010102450090100001DEST_PATH_IMAGE001
Aperture, at the opening area core, utilize a radius to be
Figure 745788DEST_PATH_IMAGE002
" circular clamping plate " film is clamped, make the film of clamped region can not produce distortion, by " circular clamping plate " film is slowly applied external force
Figure DEST_PATH_IMAGE003
, make coating film break away from basic unit, and form a radius and be
Figure 407713DEST_PATH_IMAGE004
, highly be
Figure DEST_PATH_IMAGE005
Bubbling, strengthen density measurement, as often as possible record the bubbling height
Figure 77729DEST_PATH_IMAGE006
And corresponding external force value
Figure DEST_PATH_IMAGE007
, with the following formula of measurement data substitution, calculate coating film in the disengaging base layer region, promptly radius is
Figure 457895DEST_PATH_IMAGE008
Annulus in the interfacial energy release rate
Figure DEST_PATH_IMAGE009
Wherein,
Figure 504348DEST_PATH_IMAGE010
Be energy release rate,
Figure 20780DEST_PATH_IMAGE004
Be the bubbling radius,
Figure 861697DEST_PATH_IMAGE001
Be the radius of the aperture of opening in basic unit,
Figure DEST_PATH_IMAGE011
Be coating film thickness, Be elastic modulus,
Figure DEST_PATH_IMAGE013
Be Poisson ratio,
Figure 313724DEST_PATH_IMAGE014
, For the radius of circular clamping plate (
Figure 215821DEST_PATH_IMAGE016
),
Figure DEST_PATH_IMAGE017
Be calculating parameter,
Figure 227640DEST_PATH_IMAGE006
For corresponding to external force
Figure 316818DEST_PATH_IMAGE007
The bubbling height value, ,
Figure 930519DEST_PATH_IMAGE015
,
Figure 113239DEST_PATH_IMAGE001
,
Figure 892976DEST_PATH_IMAGE011
, Unit be millimeter,
Figure 164874DEST_PATH_IMAGE012
Unit be MPa,
Figure 518495DEST_PATH_IMAGE003
Unit be newton,
Figure 785529DEST_PATH_IMAGE010
Unit be 10 -3Joule/square millimeter or Newton/millimeter.
CN2010102450090A 2010-08-04 2010-08-04 Accurate measurement method for interface energy release rate of coating film-substrate structure Expired - Fee Related CN101923043B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103063571A (en) * 2012-12-24 2013-04-24 湘潭大学 Method and system for measuring interface binding energy of thin-film material with bulge method
CN105675484A (en) * 2016-04-26 2016-06-15 重庆大学 Method for determining elastic energy of circular membrane with rigid slab in center and under uniformly distributed load

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JPS612171A (en) * 1984-06-14 1986-01-08 Toshiba Corp Output device of color picture
CN1077027A (en) * 1993-04-16 1993-10-06 冶金工业部钢铁研究总院 The measuring method of material surface film and basal body binding force and device
CN1654950A (en) * 2004-02-05 2005-08-17 Snecma发动机公司 Method of measuring the adhesion of a coating to a substrate
JP2005274423A (en) * 2004-03-25 2005-10-06 Osaka Gas Co Ltd Method and device for evaluating adhesion strength of coating film
CN101122561A (en) * 2007-08-02 2008-02-13 上海交通大学 Back penetration measuring method for film base binding performance
CN101144770A (en) * 2007-08-02 2008-03-19 上海交通大学 Method for measuring silicon base body and membrane base combination intensity

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS612171A (en) * 1984-06-14 1986-01-08 Toshiba Corp Output device of color picture
CN1077027A (en) * 1993-04-16 1993-10-06 冶金工业部钢铁研究总院 The measuring method of material surface film and basal body binding force and device
CN1654950A (en) * 2004-02-05 2005-08-17 Snecma发动机公司 Method of measuring the adhesion of a coating to a substrate
JP2005274423A (en) * 2004-03-25 2005-10-06 Osaka Gas Co Ltd Method and device for evaluating adhesion strength of coating film
CN101122561A (en) * 2007-08-02 2008-02-13 上海交通大学 Back penetration measuring method for film base binding performance
CN101144770A (en) * 2007-08-02 2008-03-19 上海交通大学 Method for measuring silicon base body and membrane base combination intensity

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103063571A (en) * 2012-12-24 2013-04-24 湘潭大学 Method and system for measuring interface binding energy of thin-film material with bulge method
CN105675484A (en) * 2016-04-26 2016-06-15 重庆大学 Method for determining elastic energy of circular membrane with rigid slab in center and under uniformly distributed load
CN105675484B (en) * 2016-04-26 2018-02-16 重庆大学 The determination method of the annular membrane elasticity energy of center band rigid plate under uniform load

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