CN104502273A - Method for representing bonding strength of hard film through interfacial stress of elasticoplastic deformation - Google Patents
Method for representing bonding strength of hard film through interfacial stress of elasticoplastic deformation Download PDFInfo
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Abstract
The invention discloses a method for representing the bonding strength of a hard film through interfacial stress of elasticoplastic deformation. The method comprises the following steps: performing circulation pressing testing on a sample of which a metal or hard alloy substrate surface is deposited with the hard film by using a circulation pressing experiment machine, so as to cause elasticoplastic deformation of a film substrate system, and finally strip off the film from the substrate because of interface fatigue; performing finite element modeling analysis according to relevant material property and practical testing conditions, acquiring the shearing stress amplitude acting at the film base interface when the film is stripped off under different circulation loads according to the solving result, and finally quantitatively representing the bonding strength of the film/substrate interface according to shearing stress amplitude-stripping week curved. The method for representing the bonding strength of a film/substrate interface is relatively reasonable and feasible, relatively accurate and quantitative in representation, relatively practical and reliable in result, and applicable to representation and evaluation on the bonding strength of hard films on metal or hard alloy surfaces which are widely used in the conventional industrial fields.
Description
Technical field
The present invention relates to the detection method of a kind of metal or cemented carbide substrate surfaces ganoine thin film performance.
Background technology
The bond strength of film and matrix, as the important performance indexes evaluating film quality, is the necessary condition of process optimization.As a key areas of Surface Engineering research, the evaluation of bond strength and sign receive to be paid close attention to widely.How effective evaluation and characterization of membrane film-substrate binding strength, to improving tool and mould usability further and having extremely important directive significance serviceable life.
At present, measurement evaluation method for film bond strength reaches tens kinds, mainly contain scarification, plunging, pulling method, bending method etc., but correlative study has fully confirmed to show, said method gained test result is subject to the impact of many non-Interface Factors, can only be used for qualitative or sxemiquantitative sign film bond strength.In addition, said method all belongs to disposable loading to be destroyed, and characterization result can not reflect the military service situation of film under actual condition accurately, conscientiously.At present, film dynamic bind intensity evaluation characterizing method has become one of important film substrate bond strength evaluation method, and also applies to some extent in actual industrial, but it still has certain limitation.To report more rolling contact fatigue method, though be that it is often confined to Elastic Contact scope, reckons without the plastic yield of film/matrix by characterizing bond strength with the film close situation that lost efficacy in a Long-Time Service process.And under actual industrial environment, in use often first can there is elastic-plastic deformation in film matrix system, and just gradually because fatigue failure is peeled off from matrix after a period of time that works under the effect of extraneous load, therefore need badly and a kind ofly can tie up to the method occurring to characterize interface bond strength after elastic-plastic deformation by characterization of membrane matrix.
By finding the retrieval of prior art document, also there is not report up to now based on the method for quantitatively characterizing film/basal body interface bond strength after there is elastic-plastic deformation under film matrix system cyclic loading, more can for promoting the use of without a kind of blanket method.
Summary of the invention
The object of this invention is to provide and a kind ofly can tie up to the method that elastic-plastic deformation rear interface bond strength occurs by characterization of membrane matrix, namely use indentation test machine under different loading environment, with spherical indenter, repeatedly test is pressed into the metal or hardmetal samples that deposit ganoine thin film, make film matrix system that elastic-plastic deformation occur, and fatigue failure occurs peel off from matrix, each cycle when recording sheet peels off, the shearing stress amplitude acting on film base interface when film peels off is obtained by FEM (finite element) calculation, draw shearing stress amplitude---peel off cycle curve, finally for quantitatively characterizing ganoine thin film bond strength.
For reaching above object, the present invention takes following technical scheme to be achieved:
Characterize a method for ganoine thin film bond strength with the interfacial stress of elastic-plastic deformation, it is characterized in that, comprise the steps:
(1) adopt circulation indentation test machine repeatedly to circulate to the metal or hardmetal samples surface that deposit film under a certain load being not more than 1000N and be pressed into test, make sample film matrix system elastic-plastic deformation occur until film separation;
(2) the recording sheet press-in cycle that elastic-plastic deformation occurs under this load and peels off;
(3) to the finite element model of spherical indenter and film base Establishing two-dimensional axial symmetric, and grid division; Analysis step is set;
(4) according to material properties, elastic modulus, the Poisson ratio of actual test condition determination pressure head and film matrix system, and according to actual loading situation arrange load peaks, load minimum value, shearing stress is stablized time CYCLIC LOADING cycle, be input in finite element model and calculate; Wherein, described load peaks is for being not more than 1000N;
(5) by calculating finite element model, the associated arguments reflecting film matrix system deformation is obtained: the contact radius of pressure head and film matrix system is with loading the variation tendency of cycle, vickers indentation with loading the variation tendency of cycle, contact radius place film base interfacial shear stress value and shearing stress amplitude with the variation tendency loading cycle;
(6) the described each parameter of com-parison and analysis step (5) all tend towards stability after CYCLIC LOADING cycle, choose the shearing stress amplitude at film base interface, contact radius place under this CYCLIC LOADING cycle;
(7) according to the loading cycle of the actual film separation recorded in step (1) ~ (2), and the contact radius place film base interfacial shear stress amplitude to be obtained by step (6), draw shearing stress amplitude---peel off cycle curve, for quantitatively characterizing ganoine thin film bond strength.
In said method, described load minimum value is not more than 90% of load peaks.
CYCLIC LOADING cycle when step (4) described shearing stress is stablized is 10.CYCLIC LOADING cycle after the described each parameter of step (6) all tends towards stability is 10 times, and the shearing stress amplitude at the film base interface, contact radius place calculated under being chosen at this CYCLIC LOADING cycle carrys out quantitatively characterizing film matrix system interface bond strength as characterization parameter.
Advantage of the present invention is:
(1) after circulation press-in, residual impression is spherical load mould, matrix has afterflow, the inventive method shows that plastic yield is Absorbable organic halogens in 10 cycles, the press-in of its Posterior circle can not cause the change of plastic yield and stress, can with 10 later contact radius place interfacial shear stress width characterization of membrane film-substrate binding strengths.
(2) the inventive method is with circulation press mode, both minimum load and load peaks ratio can have been fixed, change and load peak value and minimum value, also minimum load value and load peaks ratio can be changed, obtain contact radius place film base interfacial shear stress width, thus make method of testing more flexible and convenient.
(3) because matrix during Stress calculation allows certain plastic yield, and elastic deformation can be there is in pressure head, during test, pressure head material can be high, the substantially indeformable adamas of elastic modulus, also intensity can be adopted high but have the stupalith of certain elastic deformation, test condition is flexible, and the hard thin film material for different-thickness, elastic modulus all quantitatively can obtain bond strength.
Accompanying drawing explanation
Fig. 1 is film matrix system impression geometric configuration and size under different cycle.Wherein: (a) figure adopts surface profiler to record; B () figure is that FEM (finite element) calculation obtains.
Fig. 2 is the engineering stress strain curve of matrix (GCr15 steel) in film matrix system.
Fig. 3 is the change curve of amount of plastic deformation with load cycle of matrix in the film matrix system that obtains of FEM (finite element) calculation.
Fig. 4 is that the contact radius size of the pressure head that obtains of FEM (finite element) calculation and film matrix system is with load cycle change curve.
Fig. 5 is that the film matrix system interface shearing stress value that obtains of FEM (finite element) calculation is with load cycle change curve.
Fig. 6 to be load that FEM (finite element) calculation obtains be under 250N film matrix system interface shearing stress amplitude is with load cycle change curve.
Fig. 7 is the MoN film different loads incision stress amplitude of 5.6 μm---peel off cycle curve.
Fig. 8 is the CrN film different loads incision stress amplitude of 2.3 μm---peel off cycle curve.
Embodiment
Below in conjunction with accompanying drawing basis and specific embodiment, the inventive method is described in further detail.
Embodiment 1
Characterize a method for ganoine thin film bond strength with the interfacial stress of elastic-plastic deformation, comprise the steps:
The first step, uses circulation indentation test machine to test sample
(1) employing deposit thickness is the MoN film of 5.6 μm, and matrix material is that the sample of GCr15 steel is tested.Adopt circulation indentation test machine, the diamond spherical pressure head of radius-of-curvature 200 μm, with fixing load peaks and minimum value, loading sample thin film surface circulation and carry out press-in test, there is elastic-plastic deformation under tying up to extraneous load effect in sample film matrix.The upper limit that in circulation indentation test, load peaks is selected, should be less than that disposable press-in causes load value when peeling off 90%.Minimum load should be not more than 90% of load peaks.The present embodiment film once loads and peels off load and be greater than 1000N, therefore load peaks used is respectively 100N, 150N, 200N, 250N, and minimum load is chosen and is 30% of load peaks.For illustrating that finite element simulation calculation result and actual test result have good consistance, it is 250N that spy provides in load, when press-in cycle is respectively 1 time, 5 times, 10 times, the impression geometrical morphology adopting surface profiler to carry out actual measurement to impression and to be obtained by finite element simulation calculation and size, as shown in Figure 1.Can find out that from figure (a) sample obvious plastic yield occurs under the effect of plus load and residual next spherical indentation, it is basicly stable after the geometrical morphology of impression and size are pressed into afterwards at the 5th time, with to measure the vickers indentation size obtained for the tenth time and be close to and overlap, illustrate that now film matrix system plastic yield is basicly stable, amount of plastic deformation is no longer significantly increased.Can find out that from Fig. 1 (b) vickers indentation that finite element simulation calculation obtains and physical dimension just no longer significant change occur equally after the test of experience five circulation press-in cycle, almost completely the same with Fig. 1 actual measured results, and variation tendency is identical.
(2) under different loads, carry out circulation press-in test to sample and finally cause peeling off of film, cycle that film peels off under the effect of 250N load is 8.0 × 10 to use optical photography instrument observed and recorded to obtain
3secondary; Be 1.4 × 10 under 200N
4secondary; Be 4.0 × 10 under 150N
4secondary; Be 1.0 × 10 under 100N
5secondary.
Second step, sets up finite element model
(1) use general ABAQUS software to set up pressure head and film matrix system two-dimensional axial symmetric model, definition pressure head, film, matrix material attribute, and determine film matrix system elastic modulus, Poisson ratio, yield strength etc.The present embodiment definition diamond penetrator is rigidity; MoN film is elasticity: elastic modulus is 540GPa, and Poisson ratio is 0.25; Matrix GCr15 steel is elastoplasticity: elastic modulus is 210GPa, and Poisson ratio is 0.3, plastic stress---strain input quantity is according to GCr15 steel engineering stress strain curve (Fig. 2).
(2) limit pressure head around Z X-axis rotate with along the displacement of X-axis coordinate direction, restriction sample axis of symmetry is along the displacement of X-coordinate direction of principal axis and sample bottom surface along the displacement of Y-coordinate direction of principal axis.
(3) rigid pressure head selects 2 node linear discrete rigid unit lattice RAX2 to carry out the division of grid, sample selects 4 Node Quadrilateral Finite Element linear decrement integral unit lattice CAX4R to carry out the division of grid, the refined net adopting precision high near pressure head and sample contacts, ensures the accuracy of result of calculation.
(4) way of contact is face-face contact, and wherein interarea is diamond penetrator surface, is film outside surface from face, and contact attribute is hard contact, without friction.
(5) set up analysis step, in the step module of ABAQUS software, set up loading analysis step, smallest incremental is defined as 0.01, and maximal increment is defined as 0.1.
3rd step, selects load parameter according to reality test
(1) load minimum value is 30% of load peaks, and because indentation shape after load cycle 10 times tends towards stability, shearing stress also should be stablized, therefore setting circulation cycle is 10 times.
(2) load parameter is inputted finite element model to solve, obtain the change curve of amount of plastic deformation with load cycle of film matrix system, the contact radius size of film matrix system with load cycle change curve, interface shearing stress value with load cycle change curve and interface shearing stress amplitude with load cycle change curve (Fig. 3 ~ Fig. 6).
As can be seen from Figure 3, the remaining certain plastic yield of matrix after first time unloading, unload plastic yield afterwards at every turn and have a small amount of to increase but trend slows down, plastic yield tends towards stability substantially, once 5% is less than before loading the change comparatively of rear plastic strain value for 5th time, continue to load and no longer produce obvious plastic yield, substantially enter elastic deformation stage.
As can be seen from Figure 4, contact radius presents maximal value when first time loads, but reduce gradually after the work hardening effect due to matrix and tend towards stability, after loading for the 5th time, the size of contact radius value no longer changes substantially, illustrates that the contact of now pressure head and sample is basicly stable.
As can be seen from Figure 5, repeatedly in process of press in, with the increase of circulation cycle, the contact interface place shearing stress peak value size in compression and decompression process tends towards stability gradually, and is finally substantially tending towards constant and no longer changes with cycle.
As can be seen from Figure 6, shearing stress amplitude Changing Pattern is consistent with other each parameter, tend towards stability gradually with the increase of circulation cycle, after the 5th press-in, shearing stress amplitude size variation is less than 0.5%, therefore can be considered as final evaluation ganoine thin film bond strength stress parameter.
4th step, comprehensive 3rd step parametric analysis, for guaranteeing that test result is more reliable, evaluate sign more accurate, the characterization parameter when interface shearing stress amplitude 3650MPa that the present invention calculates after finally choosing and loading for the tenth time is 250N as test load peaks carrys out quantitatively characterizing film matrix system interface bond strength.Characterization parameter when being 250N with load carrys out the identical process of quantitatively characterizing film matrix system interface bond strength, and the contact radius place interfacial shear stress amplitude obtained when film peels off when load peaks is 100N, 150N, 200N is respectively 2770MPa, 3190MPa, 3390MPa.
The shearing stress amplitude obtained according to Fig. 6 FEM (finite element) calculation, with load cycle change curve, can obtain different loads incision stress amplitude---and peel off cycle curve (Fig. 7), quantitative evaluation can characterize film bond strength.
Embodiment 2
Sample changes the CrN film of 2.3 μm into, and operation steps is with embodiment 1.
The first step, uses circulation indentation test machine, with the diamond spherical pressure head of radius-of-curvature 200 μm, tests sample
(1) adopt circulation indentation test machine to carry out press-in test with fixing 60N load peaks to the loading of sample thin film surface circulation, load minimum value selects 15N, 20N, 30N and 40N (ratio of load minimum value and maximal value is respectively 25%, 33%, 50%, 66%) respectively.
(2) under above-mentioned four load ratios, carry out circulation press-in test to sample and finally cause peeling off of film, it is 9.0 × 10 that observed and recorded obtains the cycle that film peels off under 25% load ratio effect
2secondary; Be for 33% time 1.5 × 10
3secondary; Be for 50% time 1.8 × 10
4secondary; Be for 66% time 5.0 × 10
5secondary.
Second step, sets up finite element model with embodiment 1, and the present embodiment definition diamond penetrator is rigidity; CrN film is elasticity: elastic modulus is 400GPa, and Poisson ratio is 0.25; Matrix GCr15 steel is elastoplasticity: elastic modulus is 210GPa, and Poisson ratio is 0.3, plastic stress---strain input quantity is according to GCr15 steel engineering stress strain curve (Fig. 2).
3rd step, selects load parameter according to reality test
(1) load minimum value is 25%, 33%, 50%, 66% of load peaks, and setting circulation cycle is 10 times.
(2) load parameter is inputted finite element model to solve, obtain interface shearing stress amplitude with load cycle change curve.
4th step, comprehensive 3rd step parametric analysis, choose the interface shearing stress amplitude calculated after loading for the tenth time, contact radius place interfacial shear stress amplitude when film peels off under 25%, 33%, 50% and 66% load ratio is respectively 3330MPa, 2710MPa, 2050MPa, 1330MPa.Different loads incision stress amplitude can be obtained in conjunction with peeling off cycle---peel off cycle curve (Fig. 8).
Embodiment 3
Sample and operation steps are with embodiment 1.
The first step, use circulation indentation test machine, pressure head is the Si of radius-of-curvature 400 μm
3n
4ceramic spherical pressure head, with fixing load peaks and minimum value, loads sample thin film surface circulation and carries out press-in test.
(1) the present embodiment load peaks used is respectively 150N, 200N, and minimum load is chosen and is 30% of load peaks.
(2) under above-mentioned two load, carry out circulation press-in test to sample and finally cause peeling off of film, it is 1.3 × 10 that observed and recorded obtains the cycle that film peels off under the effect of 200N load peaks
5secondary; 1.0 × 10 are greater than under 150N
6secondary.
Second step, sets up finite element model with embodiment 1, the present embodiment definition Si
3n
4pottery pressure head is elasticity: elastic modulus is 210GPa, and Poisson ratio is 0.23; MoN film is elasticity: elastic modulus is 540GPa, and Poisson ratio is 0.25; Matrix GCr15 steel is elastoplasticity: elastic modulus is 210GPa, and Poisson ratio is 0.3, plastic stress---strain input quantity is according to GCr15 steel engineering stress strain curve (Fig. 2).
3rd step, selects load parameter according to reality test
(1) load minimum value is 30% of load peaks, and setting circulation cycle is 10 times.
(2) load parameter is inputted finite element model to solve, obtain interface shearing stress amplitude with load cycle change curve.
4th step, comprehensive 3rd step parametric analysis, choose the interface shearing stress amplitude calculated after loading for the tenth time, contact radius place interfacial shear stress amplitude is respectively: be 2180MPa during load peaks 200N, is 1910MPa during load peaks 150N.
Embodiment 4
Sample changes the TiAlN thin film of thickness 9.6 μm on M2 high speed steel substrate into, and operation steps is with embodiment 1.Pressure head changes the diamond spherical pressure head of radius-of-curvature 500 μm into, with fixing load peaks and minimum value, loads carry out press-in test to sample thin film surface circulation.
(1) the present embodiment load peaks used is respectively 800N and 200N, and minimum load is 10N.
(2) under above-mentioned two load, carry out circulation press-in test to sample and finally cause peeling off of film, it is 15 times that observed and recorded obtains the cycle that film peels off under the effect of 800N load peaks; The cycle peeled off under the effect of 200N load peaks is 160 times;
Second step, sets up finite element model with embodiment 1, and TiAlN thin film is elasticity: elastic modulus is 450GPa, and Poisson ratio is 0.25; Matrix M2 high-speed steel is elastoplasticity: elastic modulus is 210GPa, and Poisson ratio is 0.3.
3rd step, selects load parameter according to reality test
(1) load minimum value is 10N, and setting circulation cycle is 10 times.
(2) load parameter is inputted finite element model to solve, obtain interface shearing stress amplitude with load cycle change curve.
4th step, comprehensive 3rd step parametric analysis, choose the interface shearing stress amplitude calculated after loading for the tenth time, contact radius place interfacial shear stress amplitude is respectively: be 4480MPa during load peaks 800N, is 3120MPa during load peaks 200N.
Described above is only specific embodiment of the invention case; do not represent limitation of the present invention; with under the same case of the above-mentioned case study on implementation inventive concept of the present invention, technical scheme does not have substantial conversion, improvement or equivalently to replace, and all should be considered as within protection scope of the present invention.
Claims (4)
1. characterize a method for ganoine thin film bond strength with the interfacial stress of elastic-plastic deformation, it is characterized in that, comprise the steps:
(1) adopt circulation indentation test machine repeatedly to circulate to the metal or hardmetal samples surface that deposit film under a certain load being not more than 1000N and be pressed into test, make sample film matrix system elastic-plastic deformation occur until film separation;
(2) the recording sheet press-in cycle that elastic-plastic deformation occurs under this load and peels off;
(3) to the finite element model of spherical indenter and film base Establishing two-dimensional axial symmetric, and grid division; Analysis step is set;
(4) according to material properties, elastic modulus, the Poisson ratio of actual test condition determination pressure head and film matrix system, and according to actual loading situation arrange load peaks, load minimum value, shearing stress is stablized time CYCLIC LOADING cycle, be input in finite element model and calculate; Wherein, described load peaks is for being not more than 1000N;
(5) by calculating finite element model, the associated arguments reflecting film matrix system deformation is obtained: the contact radius of pressure head and film matrix system is with loading the variation tendency of cycle, vickers indentation with loading the variation tendency of cycle, contact radius place film base interfacial shear stress value and shearing stress amplitude with the variation tendency loading cycle;
(6) the described each parameter of com-parison and analysis step (5) all tend towards stability after CYCLIC LOADING cycle, choose the shearing stress amplitude at film base interface, contact radius place under this CYCLIC LOADING cycle;
(7) according to the loading cycle of the actual film separation recorded in step (1) ~ (2), and the contact radius place film base interfacial shear stress amplitude to be obtained by step (6), draw shearing stress amplitude---peel off cycle curve, for quantitatively characterizing ganoine thin film bond strength.
2. the method characterizing ganoine thin film bond strength with the interfacial stress of elastic-plastic deformation as claimed in claim 1, it is characterized in that, described load minimum value is not more than 90% of load peaks.
3. the method characterizing ganoine thin film bond strength with the interfacial stress of elastic-plastic deformation as claimed in claim 1, it is characterized in that, CYCLIC LOADING cycle when step (4) described shearing stress is stablized is 10.
4. the method characterizing ganoine thin film bond strength with the interfacial stress of elastic-plastic deformation as claimed in claim 1, it is characterized in that, CYCLIC LOADING cycle after the described each parameter of step (6) all tends towards stability is 10 times, and the shearing stress amplitude at the film base interface, contact radius place calculated under being chosen at this CYCLIC LOADING cycle carrys out quantitatively characterizing film matrix system interface bond strength as characterization parameter.
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Effective date of registration: 20190418 Address after: No. 721 Yanhu Road, Jiangshan Town, Yinzhou District, Ningbo City, Zhejiang Province, 315000 Patentee after: Ningbo Yuntu Technology Co., Ltd. Address before: 710049 Xianning West Road, Xi'an, Xi'an, Shaanxi Patentee before: Xi'an Jiaotong University |
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