CN109520828B - Elastic modulus testing method of film - Google Patents

Elastic modulus testing method of film Download PDF

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CN109520828B
CN109520828B CN201811181947.1A CN201811181947A CN109520828B CN 109520828 B CN109520828 B CN 109520828B CN 201811181947 A CN201811181947 A CN 201811181947A CN 109520828 B CN109520828 B CN 109520828B
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elastic modulus
film
indenter
area
pressure head
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CN109520828A (en
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闫五柱
岳珠峰
赵万嘉
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Northwestern Polytechnical University
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    • G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
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    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
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Abstract

The present disclosure provides a method for testing the elastic modulus of a film. The elastic modulus test method of the film comprises the following steps: providing a test piece, wherein the test piece comprises a base body and a thin film, and the thin film covers the surface of the base body; providing a plurality of indenters, and performing an indentation test on the film by using each indenter to obtain an elastic modulus of the film corresponding to each indenter and serve as a reference elastic modulus, wherein the area of a crimping surface on each indenter for contacting with the film is different; fitting the area of the crimping surface and the reference elastic modulus to obtain a fitting function of the area of the crimping surface and the elastic modulus; and determining the elastic modulus when the area of the pressure welding surface is zero as a target elastic modulus according to the fitting function. The method and the device can improve the accuracy of the tested elastic modulus and reduce the testing cost.

Description

Elastic modulus testing method of film
Technical Field
The disclosure relates to the technical field of materials, in particular to a method for testing the elastic modulus of a film.
Background
The film is widely applied to the fields of machinery, microelectronics, optics, medical treatment and the like. The preparation of the film on the substrate is beneficial to prolonging the service life of the substrate, improving the hardness, wear resistance and friction performance of the substrate and enhancing the corrosion resistance and oxidation resistance of the substrate.
The modulus of elasticity is the most important property evaluation index for films. When the nano indentation method is adopted to test the elastic modulus of the film, a pressure head is required to apply a pressure load to the film. Since the membrane is often coated on the substrate surface, the applied compressive load is carried by both the membrane and the substrate. In order to eliminate the influence of the substrate on the test to improve the accuracy of the test, the indentation test needs to be performed by using an indenter with a smaller size. However, the smaller size indenter is costly to machine. Meanwhile, for a thin film with small thickness, the size of the required pressure head is very small, and the existing processing equipment cannot meet the requirement, so that the accuracy of the test is reduced.
It is to be noted that the information disclosed in the above background section is only for enhancement of understanding of the background of the present disclosure, and thus may include information that does not constitute prior art known to those of ordinary skill in the art.
Disclosure of Invention
The invention aims to provide a method for testing the elastic modulus of a film, which can not only improve the accuracy of the tested elastic modulus, but also reduce the testing cost.
According to one aspect of the present disclosure, a method for testing an elastic modulus of a film is provided. The elastic modulus test method of the film comprises the following steps: providing a test piece, wherein the test piece comprises a base body and a thin film, and the thin film covers the surface of the base body; providing a plurality of indenters, and performing an indentation test on the film by using each indenter to obtain an elastic modulus of the film corresponding to each indenter and serve as a reference elastic modulus, wherein the area of a crimping surface on each indenter for contacting with the film is different; fitting the area of the crimping surface and the reference elastic modulus to obtain a fitting function of the area of the crimping surface and the elastic modulus; and determining the elastic modulus when the area of the pressure welding surface is zero as a target elastic modulus according to the fitting function.
In an exemplary embodiment of the disclosure, the fitting the area of the crimping surface and the reference elastic modulus, and obtaining a fitting function of the area of the crimping surface and the elastic modulus includes: and fitting by using a least square method by using the area of the crimping surface as an independent variable and the reference elastic modulus as a dependent variable to obtain the fitting function.
In an exemplary embodiment of the present disclosure, the performing an indentation test on the film using each of the indenters to obtain an elastic modulus of the film corresponding to each of the indenters includes: applying an indentation load to the film by using each indenter to obtain a relation curve of the indentation load and the indentation depth of the film corresponding to each indenter; determining the initial unloading rigidity of the film corresponding to each pressure head according to the curve of the film corresponding to the indentation load and the indentation depth of each pressure head; and obtaining the elastic modulus of the film corresponding to each pressure head according to the initial unloading rigidity of the film corresponding to each pressure head and the area of the pressure joint surface of each pressure head.
In an exemplary embodiment of the present disclosure, the obtaining the elastic modulus of the film corresponding to each of the indenters according to the initial unload stiffness of the film corresponding to each of the indenters and the area of the crimping surface of each of the indenters includes: substituting the initial unloading rigidity and the area of the crimping surface into a preset formula to obtain the elastic modulus, wherein the preset formula is as follows:
Figure BDA0001825215270000021
wherein S isiFor the initial unload stiffness, M, of the film corresponding to the ith indenteriThe area of the pressure contact surface of the ith pressure head, EiThe modulus of elasticity of the film corresponding to the ith indenter.
In an exemplary embodiment of the present disclosure, an indentation load applied to the film by each of the indenters increases for a first preset time and decreases for a second preset time.
In an exemplary embodiment of the present disclosure, the first preset time is equal to the second preset time.
In an exemplary embodiment of the present disclosure, the first preset time and the second preset time are both 1 s.
In an exemplary embodiment of the present disclosure, the indenter has a cylindrical structure, and the crimping surface is a bottom surface of the indenter.
In an exemplary embodiment of the present disclosure, the test piece has a cubic structure, and one tenth of the edge length of the test piece is greater than or equal to the radius of the bottom surface of the indenter.
This beneficial effect that prior art was compared to the disclosure lies in:
according to the method for testing the elastic modulus of the film, the elastic modulus when the area of the compression joint surface is zero can be obtained according to the fitting function of the area of the compression joint surface and the elastic modulus, so that the accuracy of the tested elastic modulus is improved; meanwhile, the testing method can avoid processing the pressure head with smaller size, and reduces the testing cost.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the disclosure.
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The above and other features and advantages of the present disclosure will become more apparent by describing in detail exemplary embodiments thereof with reference to the attached drawings. It is to be understood that the drawings in the following description are merely exemplary of the disclosure, and that other drawings may be derived from those drawings by one of ordinary skill in the art without the exercise of inventive faculty.
FIG. 1 is a flow chart of a mode of elastic modulus testing of a film in an embodiment of the present disclosure;
FIG. 2 is a schematic view of an indenter and a test piece in an embodiment of the present disclosure;
FIG. 3 is a flow chart of step 12 of a mode of elastic modulus testing of a film in an embodiment of the present disclosure;
FIG. 4 is a graph of the change in indentation load over time in an embodiment of the disclosure;
FIG. 5 is a graph of indentation load versus indentation depth for an embodiment of the disclosure;
FIG. 6 is a plot of the modulus of elasticity fitted to the radius of the indenter in an embodiment of the present disclosure.
In the figure: 1. a test piece; 101. a film; 102. a substrate; 2. and (4) pressing head.
Detailed Description
Example embodiments will now be described more fully with reference to the accompanying drawings. Example embodiments may, however, be embodied in many different forms and should not be construed as limited to the examples set forth herein; rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of example embodiments to those skilled in the art. The described features, structures, or characteristics may be combined in any suitable manner in one or more embodiments. In the following description, numerous specific details are provided to give a thorough understanding of embodiments of the disclosure. One skilled in the relevant art will recognize, however, that the subject matter of the present disclosure can be practiced without one or more of the specific details, or with other methods, films, devices, etc. In other instances, well-known technical solutions have not been shown or described in detail to avoid obscuring aspects of the present disclosure. The same reference numerals in the drawings denote the same or similar structures, and thus their detailed description will be omitted.
The terms "a," "an," "the," and "said" are used to indicate the presence of one or more elements/components/etc.; the terms "comprising," "having," and "providing" are intended to be inclusive and mean that there may be additional elements/components/etc. other than the listed elements/components/etc.
The embodiment of the disclosure provides a method for testing the elastic modulus of a film. As shown in fig. 1, the method for testing the elastic modulus of the film may include steps S11-S14, in which:
and step S11, providing a test piece, wherein the test piece comprises a substrate and a film, and the film covers the surface of the substrate.
And step S12, providing a plurality of pressure heads, and performing an indentation test on the film by using each pressure head to obtain an elastic modulus of the film corresponding to each pressure head and using the elastic modulus as a reference elastic modulus, wherein the area of a pressure joint surface for contacting with the film on each pressure head is different.
And step S13, fitting the area of the crimping surface and the reference elastic modulus to obtain a fitting function of the area of the crimping surface and the elastic modulus.
Step S14 is to determine the elastic modulus when the area of the pressure contact surface is zero as the target elastic modulus based on the fitting function.
According to the method for testing the elastic modulus of the thin film in the disclosed embodiment, the elastic modulus when the area of the crimping surface is zero can be obtained according to the fitting function of the area of the crimping surface and the elastic modulus, so that the accuracy of the tested elastic modulus is improved; meanwhile, the testing method can avoid processing the pressure head with smaller size, and reduces the testing cost.
The following describes the steps of the method for testing the elastic modulus of a film in the embodiments of the present disclosure in more detail:
in step S11, a test piece is provided, the test piece including a substrate and a film covering a surface of the substrate.
As shown in fig. 2, the thin film 101 is a two-dimensional material formed by depositing atoms, molecules and ions on the surface of the substrate 102, and the thickness thereof is not particularly limited in the embodiments of the present disclosure. The substrate 102 may be a metal material, a ceramic material, or the like, and embodiments of the present disclosure are not listed here. The substrate 102 and the thin film 101 constitute the test piece 1 described above. The test piece 1 may be a cylinder, a rectangular parallelepiped, or other shapes such as a cube.
In step S12, a plurality of indenters are provided, and an indentation test is performed on the film using each of the indenters to obtain an elastic modulus of the film corresponding to each of the indenters, as a reference elastic modulus, wherein the area of the crimping surface for contacting the film on each of the indenters is different.
As shown in fig. 2, the indentation test is a test in which the indenter 2 is brought into contact with the film 101, a pressing load is applied to the film 101 by the indenter 2, the distance by which the indenter 2 is pressed into the film 101 is measured, and the elastic modulus of the film 101 can be determined from the applied pressing load and the distance by which the indenter 2 is pressed into the film 101. The material of the indenter 2 may be diamond to give the indenter 2 a good stiffness. Of course, the material of the ram 2 may also be aluminum-zinc alloy or other materials with good rigidity. The indenter 2 may have a cylindrical shape, but not limited thereto, and may have a square shape, or may have another shape such as a rectangular parallelepiped. The indenter may be sized according to the size of the test body. For example, when the indenter is a cylinder and the test piece is a cube, the radius of the indenter is less than one tenth of the edge length of the test piece. Specifically, as shown in FIG. 3, step S12 may include steps S121-S123, wherein:
and S121, applying an indentation load to the film by using each indenter, and obtaining a relation curve between the indentation load and the indentation depth of the film corresponding to each indenter.
The indentation load isThe pressure load applied to the film by the pressure head in the indentation test. The indentation load is perpendicular to the contact surface of the indenter and the membrane. The indentation load applied by each indenter to the film may be increased for a first predetermined time and may be decreased for a second predetermined time. The first preset time and the second preset time may be equal, and of course, may not be equal. In one embodiment, as shown in FIG. 4, an indenter applies an indentation load FoAt a first preset time t1Linearly increasing and at a second preset time t2Linear decrease and the first predetermined time t1And the second preset time t2All for 1 s. In other embodiments of the present disclosure, the first predetermined time and the second predetermined time may be other values, and are not described in detail herein.
The indentation depth is the distance the indenter is pressed into the film in the indentation test. Taking a plurality of indenters having a cylindrical shape as an example, the bottom surface of the indenter may be used as a pressure contact surface where the indenter contacts the film, and the indentation depth may be used as the distance by which the bottom surface of the indenter is pressed into the film. Wherein the bottom surfaces of the plurality of indenters have different radii so that the area of the pressure contact surface for contacting the film is different for each indenter. And in the process of applying an indentation load to the film by using the pressure head, detecting and recording the indentation depth in real time. And when the indentation load is reduced to 0, taking the applied indentation load as a dependent variable and the recorded indentation depth as an independent variable, and obtaining a relation curve of the indentation load and the indentation depth through a rectangular coordinate system. As shown in FIG. 5, the ith indenter applies an indentation load FiIndentation depth h corresponding to ith indenter of filmiIncludes two curves, one of the two curves is a loading curve Li1Corresponding to indentation load FiThe addition process of (d); the other curve is the unloading curve Li2Corresponding to indentation load FiThe lowering process of (1). Wherein i is a positive integer of 1, 2, 3, 4, 5, etc.
And S122, determining the initial unloading rigidity of the film corresponding to each pressure head according to the relationship curve of the indentation load and the indentation depth of the film corresponding to each pressure head.
As shown in fig. 5, according to the unloading curve L of the film corresponding to the ith indenteri2To determine the initial unload stiffness of the film corresponding to the ith indenter. The initial unload stiffness is the unload curve Li2At indentation load FiIs a maximum value FimaxThe slope of time. Wherein the initial unload stiffness may be calculated by the following equation:
Figure BDA0001825215270000061
wherein S isiAn initial unload stiffness for the film corresponding to the ith indenter; fimaxThe maximum indentation load of the film corresponding to the ith indenter; h isimaxThe maximum indentation depth of the film corresponding to the ith indenter; h isicFor the unloading curve Li2Is the indentation depth at the intersection of the tangent line of (a) and the transverse axis, which tangent line crosses the unloading curve Li2Up corresponds to himaxPoint (2) of (c).
And S123, obtaining the elastic modulus of the film corresponding to each pressure head according to the initial unloading rigidity of the film corresponding to each pressure head and the area of the pressure joint surface of each pressure head.
Specifically, the initial unload stiffness and the area of the pressure head-film crimping surface are substituted into a preset formula to obtain the elastic modulus, wherein the preset formula is as follows:
Figure BDA0001825215270000062
wherein E isiModulus of elasticity, S, of the film corresponding to the ith indenteriInitial unload stiffness, M, for film corresponding to ith indenteriThe area of the crimping surface of the ith indenter. Taking an indenter having a cylindrical shape as an example, the pressing surface of the indenter and the thin film is the bottom surface of the indenter, and the predetermined formula can be converted into:
Figure BDA0001825215270000063
wherein R isiIs the radius of the bottom surface of the ith ram.
In step S13, the area of the pressure contact surface and the reference elastic modulus are fitted to obtain a fitting function of the area of the pressure contact surface and the elastic modulus.
In one embodiment, the area of the crimping surface is used as an independent variable, the reference elastic modulus is used as a dependent variable, an exponential decay model is selected as a function to be fitted, and a least square method is used for fitting to determine a constant in the function to be fitted, so that the fitting function is obtained. The exponential decay model may be a logarithmic function, and of course, other functions may be used, and this disclosure is not further described herein. In another embodiment, the fitting function is obtained by fitting the area of the pressure contact surface as an independent variable and the reference elastic modulus as a dependent variable by the least square method.
In step S14, the elastic modulus when the area of the pressure contact surface is zero is determined as the target elastic modulus from the fitting function.
The area of the pressure contact surface in the fitting function is set to 0, and the target elastic modulus is obtained.
In other embodiments of the present disclosure, after obtaining the reference elastic modulus of the film at each indenter, a curve fitting may be performed on the area of the crimping surface and the reference elastic modulus, and the elastic modulus at the time when the area of the crimping surface is 0 may be extrapolated from the obtained curve. Taking a pressure head with a cylindrical shape as an example, the bottom surface of the pressure head is a pressure contact surface, and the area of the pressure contact surface is proportional to the radius of the bottom surface of the pressure head. As shown in FIG. 6, it is possible to curve-fit the radius R of the bottom surface of the indenter and the reference elastic modulus, and extrapolate the elastic modulus E to the case where the radius R of the bottom surface of the indenter is 0 from the obtained curve as the target elastic modulus E*。
Other embodiments of the disclosure will be apparent to those skilled in the art from consideration of the specification and practice of the disclosure. This application is intended to cover any variations, uses, or adaptations of the disclosure following, in general, the principles of the disclosure and including such departures from the present disclosure as come within known or customary practice within the art. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the disclosure being indicated by the following claims.

Claims (5)

1. A method for measuring the elastic modulus of a film, comprising:
providing a test piece, wherein the test piece comprises a base body and a thin film, and the thin film covers the surface of the base body;
providing a plurality of indenters, and performing an indentation test on the film by using each indenter to obtain an elastic modulus of the film corresponding to each indenter and serve as a reference elastic modulus, wherein the area of a crimping surface on each indenter for contacting with the film is different;
fitting the area of the crimping surface and the reference elastic modulus to obtain a fitting function of the area of the crimping surface and the elastic modulus;
determining the elastic modulus when the area of the crimping surface is zero as a target elastic modulus according to the fitting function;
wherein, the indentation test of the film by using each indenter to obtain the elastic modulus of the film corresponding to each indenter comprises the following steps:
applying an indentation load to the film by using each pressure head to obtain a relation curve between the indentation load and the indentation depth of the film corresponding to each pressure head, wherein the indentation load applied to the film by each pressure head is increased within a first preset time and is decreased within a second preset time, and the first preset time is equal to the second preset time;
determining the initial unloading rigidity of the film corresponding to each pressure head according to the curve of the film corresponding to the indentation load and the indentation depth of each pressure head;
obtaining the elastic modulus of the film corresponding to each pressure head according to the initial unloading rigidity of the film corresponding to each pressure head and the area of the pressure joint surface of each pressure head;
the pressure head is of a cylindrical structure, and the crimping surface is the bottom surface of the pressure head.
2. The method for testing the elastic modulus of a thin film according to claim 1, wherein fitting the area of the crimping surface and the reference elastic modulus to obtain a fitting function of the area of the crimping surface and the elastic modulus comprises:
and fitting by using a least square method by using the area of the crimping surface as an independent variable and the reference elastic modulus as a dependent variable to obtain the fitting function.
3. The method for testing the elastic modulus of the film according to claim 1, wherein obtaining the elastic modulus of the film corresponding to each indenter based on the initial unloading stiffness of the film corresponding to each indenter and the area of the crimping surface of each indenter comprises:
substituting the initial unloading rigidity and the area of the crimping surface into a preset formula to obtain the elastic modulus, wherein the preset formula is as follows:
Figure FDA0003389196180000021
wherein S isiFor the initial unload stiffness, M, of the film corresponding to the ith indenteriThe area of the pressure contact surface of the ith pressure head, EiThe modulus of elasticity of the film corresponding to the ith indenter.
4. The method for testing elastic modulus of a film according to claim 1, wherein the first predetermined time and the second predetermined time are both 1 s.
5. The method for testing elastic modulus of a film according to claim 4, wherein the test piece has a cubic structure, and one tenth of the edge length of the test piece is greater than or equal to the radius of the bottom surface of the indenter.
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