KR20160118852A - Test method of interfacial adhesion - Google Patents

Test method of interfacial adhesion Download PDF

Info

Publication number
KR20160118852A
KR20160118852A KR1020150047661A KR20150047661A KR20160118852A KR 20160118852 A KR20160118852 A KR 20160118852A KR 1020150047661 A KR1020150047661 A KR 1020150047661A KR 20150047661 A KR20150047661 A KR 20150047661A KR 20160118852 A KR20160118852 A KR 20160118852A
Authority
KR
South Korea
Prior art keywords
hardness
bonding force
substrate
thin film
interfacial
Prior art date
Application number
KR1020150047661A
Other languages
Korean (ko)
Other versions
KR101685507B1 (en
Inventor
김종헌
권동일
Original Assignee
(주)프론틱스
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by (주)프론틱스 filed Critical (주)프론틱스
Priority to KR1020150047661A priority Critical patent/KR101685507B1/en
Publication of KR20160118852A publication Critical patent/KR20160118852A/en
Application granted granted Critical
Publication of KR101685507B1 publication Critical patent/KR101685507B1/en

Links

Images

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N19/00Investigating materials by mechanical methods
    • G01N19/04Measuring adhesive force between materials, e.g. of sealing tape, of coating
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N3/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/40Investigating hardness or rebound hardness
    • G01N3/42Investigating hardness or rebound hardness by performing impressions under a steady load by indentors, e.g. sphere, pyramid
    • GPHYSICS
    • G06COMPUTING; CALCULATING OR COUNTING
    • G06FELECTRIC DIGITAL DATA PROCESSING
    • G06F17/00Digital computing or data processing equipment or methods, specially adapted for specific functions
    • G06F17/10Complex mathematical operations
    • G06F17/11Complex mathematical operations for solving equations, e.g. nonlinear equations, general mathematical optimization problems
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/0001Type of application of the stress
    • G01N2203/001Impulsive
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/0014Type of force applied
    • G01N2203/0016Tensile or compressive
    • G01N2203/0019Compressive
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/0058Kind of property studied
    • G01N2203/0076Hardness, compressibility or resistance to crushing
    • G01N2203/0078Hardness, compressibility or resistance to crushing using indentation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/02Details not specific for a particular testing method
    • G01N2203/0202Control of the test
    • G01N2203/0212Theories, calculations

Landscapes

  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Mathematical Physics (AREA)
  • Mathematical Analysis (AREA)
  • Mathematical Optimization (AREA)
  • General Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Chemical & Material Sciences (AREA)
  • Computational Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Theoretical Computer Science (AREA)
  • Pure & Applied Mathematics (AREA)
  • Data Mining & Analysis (AREA)
  • Algebra (AREA)
  • Databases & Information Systems (AREA)
  • Software Systems (AREA)
  • General Engineering & Computer Science (AREA)
  • Operations Research (AREA)
  • Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)

Abstract

The present invention relates to a method of evaluating an interface bonding force.
According to the present invention measuring a maximum indentation load (L max) and the maximum indentation depth (h max) through the interface bonding strength evaluation bangbeopneun indentation test; The maximum indentation load (L max) and the maximum indentation depth (h max) the hardness (H s, H f, H c) calculation expression plastic zone volume (V s, V f) hardness (H s of the substrate by applying a calculation formula ), calculating a hardness (H f), the composite hardness (H c), the plastic region of the substrate volume (V s), the plastic zone volume (V f) of the thin film of the thin film; Comparing the hardness (H s ) of the substrate and the hardness (H f ) of the thin film; Calculating an interfacial parameter (x 3 ) by substituting the hardnesses (H s , H f , H c ) and the plastic zone volumes (V s , V f ) into the interfacial variable (x 3 ) calculating equation; And a step of calculating W adhesion by an interfacial bonding force through a calculation formula of W adhesion by an interface, thereby obtaining a quantitative interfacial bonding force which is not affected by the test conditions.

Description

{Test method of interfacial adhesion}

The present invention relates to a method of evaluating an interface bonding force. More specifically, it is possible to calculate the quantitative interfacial bonding force value independent of the test conditions such as the indentation depth of the indentor in the indentation test, and it can be applied regardless of the material of the substrate and the thin film, And an evaluation method.

In general, it is very important to accurately evaluate the interfacial bonding force between different materials bonded by a coating material, a brazing material, a welding material, a solder material, or the like in thin film and packaging technologies in the development of materials and development of packaging packaging techniques.

These interfacial bonding forces have not been quantified because of the experimental and theoretical difficulties in bonding different materials. Accordingly, in the industrial field, a number of methods have been developed and used to obtain interfacial bonding forces through a variety of researches and experiments.

Particularly, the development of interfacial fracture mechanics test method to evaluate the resistance of the interface when fracture mechanics test is applied and crack propagation is introduced into interface is active.

A method of evaluating the interfacial bonding force as the interfacial fracture energy, which is the degree of interfacial resistance against the growth of cracks, using the interfacial fracture mechanics test method will be described with reference to FIGS. 1 and 2. FIG.

The test piece 51 used for obtaining the interface bonding force includes a rod-shaped substrate 53 for evaluating the bonding force and a thin film 55 bonded to one region along the longitudinal direction of the substrate 53. The test piece 51 is divided into a first region I made of only the substrate 53 and a second region II having the thin film 55 attached to the substrate 53. [ In the second region of the specimen 51, a crack is formed between the substrate 53 and the thin film 55 in order to perform a test for obtaining an interfacial bonding force. Such a crack is referred to as a preliminary crack.

In order to measure the bonding force of the specimen 51, a load applying system 60 for applying a load by fixing the specimen 51 is used. The load applying system 60 is used to measure the bonding force of the specimen 51, A load applying section 65 for applying a load to the test piece 51 and a pair of control levers 65 for finely adjusting the position of the test piece 51 in the longitudinal direction, (63).

The process of measuring the interface bonding force of the test piece 51 using the load application system 60 is as follows.

First, the second region II of the test piece 51 is fixed to the specimen fixing portion 61 in a cantilever shape so that a load can be applied to the first region I of the specimen 51. The position of the specimen 51 is finely adjusted by the control lever 63 so that the load point spaced a certain distance from the specimen fixing section 61 is positioned below the load applying section 65 and then the load applying section 65 ) Is lowered to apply a load to the first region (I).

When the load is applied, the displacement of the test piece 51 increases with an increase in the load, and the crack length between the substrate 53 and the thin film 55 rapidly increases. When the variation of the crack length is examined with time, the crack length rapidly increases instantly at the point where the preliminary crack ends and the crack growth starts.

In addition, when the crack length between the substrate 53 and the thin film 55 rapidly increases, the load tends to decrease sharply. Since the crack grows in the opposite direction to the loading point, the moment (force) applied to the cracked point becomes larger as the crack grows.

This is because it can provide a larger driving force for crack growth, and therefore, the applied load tends to be rather reduced.

However, as the displacement of the specimen increases with the increase of the conventional load, the method of evaluating the interfacial bonding force for measuring the length of the cracks between the substrate and the thin film causes cracks between the substrate and the thin film to measure the bonding force, There is a problem that a quantitative interface bonding force can not be obtained since the test method is qualitatively evaluated.

In addition, when the load is applied to the specimen, the influence of the substrate and the thin film is affected by the interfacial bonding force. Therefore, the crack length of the substrate and the thin film increases as the displacement of the specimen increases. There is a problem in that it is difficult to evaluate only the interface bonding force and the interface bonding force can not be evaluated accurately.

In addition, in the case of a specimen having fragile properties, the specimen may be broken before cracks occur between the substrate and the thin film, so that the specimen having fragile properties has a problem in that it can not be evaluated even with a qualitative interfacial bonding force.

In addition, when measuring the crack length of the substrate and the thin film, it is not possible to measure the crack length by the naked eye or the measuring instrument when the specimen of the nanomaterial is measured. Therefore, a measuring instrument capable of measuring the crack length is separately required, The method is complicated and troublesome.

Accordingly, the present invention has been made in view of the above-mentioned background, and it is an object of the present invention to provide a method of evaluating an interfacial bonding force with high accuracy, which is capable of calculating a quantitative interfacial bonding force value independent of test conditions such as indentation depth, The purpose is to provide.

In addition, when the indentation test is performed on the nano material in order to calculate the interfacial bonding force of the nano material, the measurement process is simple and easy measurement is possible, The present invention has an object to provide a method of evaluating an interfacial bonding force capable of evaluating the interfacial bonding force by performing a test.

Further, it is an object of the present invention to provide a method of evaluating an interfacial bonding force that can measure interfacial bonding force without destroying a specimen, and it is not necessary to observe a deformation and a fracture region at an interface, thereby enabling easy and convenient measurement.

Further, the objects of the present invention are not limited thereto, and other objects not mentioned can be clearly understood by those skilled in the art from the following description.

According to the invention, the step of measuring the maximum indentation load (L max) and the maximum indentation depth (h max) over the indentation test; The maximum indentation load (L max) and the maximum indentation depth (h max) the hardness (H s, H f, H c) calculation expression plastic zone volume (V s, V f) hardness (H s of the substrate by applying a calculation formula ), calculating a hardness (H f), the composite hardness (H c), the plastic region of the substrate volume (V s), the plastic zone volume (V f) of the thin film of the thin film; Comparing the hardness (H s ) of the substrate and the hardness (H f ) of the thin film; Calculating an interfacial parameter (x 3 ) by substituting the hardnesses (H s , H f , H c ) and the plastic zone volumes (V s , V f ) into the interfacial variable (x 3 ) calculating equation; And calculating the work (W) by the interfacial bonding force through a one-dimensional (W) calculation formula based on the interface can be provided.

According to the present invention, it is possible to calculate a quantitative interfacial bonding force value which is independent of the test conditions such as the indentation depth of the indenting member in the indentation test, and has no influence of the substrate and the thin film, so that the accuracy is high.

In addition, when the indentation test is performed on the nano material in order to calculate the interfacial bonding force of the nano material, the measurement process is simple and easy measurement is possible, Test can be performed to evaluate the interfacial bonding force, so that the range of application is wide and it is easy to measure.

Also, the interface bonding force can be measured without destroying the specimen, and there is no need to observe the deformation and the fracture region at the interface, so that an easy and convenient measurement is possible.

1 is a side view showing a state where a test piece is fixed to a conventional interface fracture tester;
2 is a plan view of a conventional interface fracture tester;
3 is a view showing an indentation testing machine according to the present invention;
4 is a block diagram schematically showing a method of evaluating an interfacial bonding force according to the present invention;
5 is a block diagram showing a detailed method of evaluating an interfacial bonding force according to the present invention;
FIG. 6 is a schematic view showing a stress field under pressure particles due to indentation in an indentation test according to the present invention; FIG.
FIG. 7 is a graph showing a load-displacement curve showing the indentation load according to the displacement of the indentor pressing the specimen according to the present invention; FIG.
8 is a schematic view showing a stress field under the pressure particle in the case where the hardness of the substrate is smaller than the hardness of the thin film in the present invention; And
9 is a schematic view showing a stress field under the pressure grains in the case where the hardness of the thin film is smaller than the hardness of the substrate in the present invention.

Hereinafter, some embodiments of the present invention will be described in detail with reference to exemplary drawings. It should be noted that, in adding reference numerals to the constituent elements of the drawings, the same constituent elements are denoted by the same reference symbols as possible even if they are shown in different drawings. In the following description of the present invention, a detailed description of known functions and configurations incorporated herein will be omitted when it may make the subject matter of the present invention rather unclear.

In describing the components of the present invention, the terms first, second, A, B, (a), (b), and the like can be used. These terms are intended to distinguish the constituent elements from other constituent elements, and the terms do not limit the nature, order or order of the constituent elements. When a component is described as being "connected", "coupled", or "connected" to another component, the component may be directly connected to or connected to the other component, It should be understood that an element may be "connected," "coupled," or "connected."

FIG. 3 is a view showing an indentation testing machine according to the present invention, FIG. 4 is a block diagram showing a method of evaluating an interfacial bonding force according to the present invention, FIG. 5 is a block diagram FIG. 6 is a schematic view showing a stress field under the pressure particle due to the indentation in the indentation test according to the present invention, and FIG. 7 is a graph showing a load-displacement curve showing the indentation load according to the displacement, Fig. 8 is a schematic view showing a stress field under the pressure grains in the case where the hardness of the substrate is smaller than the hardness of the thin film in the present invention, and Fig. 9 is a schematic view showing the pressure when the hardness of the thin film is smaller than the hardness of the substrate Is a schematic view showing the stress field under the particle.

As shown in these drawings, the method for evaluating an interfacial bonding force according to the present invention includes the steps of measuring a maximum indentation load L max and a maximum indentation depth h max through an indentation test S410 and a maximum indentation load L max ) and the maximum indentation depth (h max), the hardness (H s, H f, H c) calculation expression plastic zone volume (V s, V f) hardness of the substrate by applying the calculation formula (H s), hardness of the thin film ( H f), the composite hardness (H c), the plastic zone by volume of the substrate (V s), and the step (S420) for calculating a firing zone volume (V f) of the thin film, the hardness of the substrate (H s) and the hardness of the thin film (H f) a comparing step (S430) and, respectively, the hardness (H s, H f, H c) and a plastic zone volume to (V s, V f) of the surface parameters (x 3) surface by applying a calculation formula and a variable (x 3) step (S450) for calculating a phase work (W) by (S440) through the interface bonding force between the work (W) calculated according to the equation and for calculating the surface.

The indentation tester is shown in FIG. 3, in which a specimen 350 having a thin film bonded onto a substrate of a press-in testing machine 300 is placed on or fixed on a surface plate 330, and then the pressure particle 310 presses the specimen 350 Is a mechanical property evaluation test method capable of measuring not only the hardness and the elastic modulus but also the strength and residual stress of the specimen by the reaction of the specimen 350 with respect to the applied force.

In the present invention, as the pressure particle 310 presses the test piece 350 gradually through the indentation test using the indentation testing device 300, the pressure particle 310 presses the test piece 350 with a depth and a load value, And the hardness and complex hardness of the thin film and the volume value of the substrate and the thin film are calculated to calculate the interfacial bonding force.

4, the interfacial bonding force evaluating method of the present invention will be sequentially described. First, the maximum indentation load and the maximum indentation depth of the specimen are measured (S410) by the indentation test of the indentation tester, and the measured maximum indentation load and the maximum indentation depth The hardness of the substrate, the hardness of the thin film, the complex hardness, the volume of the fired region of the substrate, and the volume of the fired region of the thin film are calculated (S420) by substituting the hardness of the substrate and the volume of the fired region.

After comparing the hardness of the substrate with the hardness of the thin film (S430), the interface parameters are calculated (S440) according to the case where the hardness of the substrate is smaller than the hardness of the thin film and the hardness of the thin film is smaller than the hardness of the substrate (S450).

6 shows an expanding cavity model (ECM) showing the stress field under the pressure particles due to the indenters for pressing the specimen, and assumes that the hemispherical calcination zone is constrained in a linear form according to the indentation test do.

That is, as the indentor presses the specimen, a semi-spherical core is generated in the lower portion of the indentation to transmit the pressing force of the indentor corresponding to the contact radius of the indentor. Then, The extended pore model is generated mathematically to show that the core and the plastic zone appear as a hemispherical linear shape.

It is also possible to know the radius of the sintered area by the indentation test of various materials by irradiating the stress field under the sub-particles over the entire sintered region from the core to the radius of the sintering zone with the hemispherical core having the radius of contact of the indenter Let's do it.

Figure pat00001

here,

Figure pat00002
Is the radius of the core (
Figure pat00003
),
Figure pat00004
Quot; means the half-angle of indentation of the indenter,
Figure pat00005
The elastic modulus,
Figure pat00006
Means the yield strength.

The radius of the plastic region of the substrate and the thin film can be calculated by Equation (1), and the plastic region volume of the substrate and the thin film is calculated by substituting the plastic region radius of the substrate and the thin film into the plastic region volume calculating equation of the substrate and the thin film. The equation is expressed by the following equation.

Figure pat00007

Figure pat00008

Equation (2) is a firing region volume calculating equation of the substrate, and the firing region volume of the substrate is a value obtained by subtracting the volume by the thickness of the thin film from the hemisphere volume formed by the radius of the firing region of the substrate.

Equation (3) is a firing region volume calculation formula of the thin film, and the volume of the firing region of the thin film becomes a volume value of the hemispherical volume consisting of the firing region radius of the thin film.

In addition, the hardness of the substrate, the hardness and the hardness of the thin film are the values obtained by dividing the maximum indentation load by the contact area. The maximum indentation load can be measured from the indentation tester, and the contact area is determined by considering the shape of the indentor And is calculated by the actual contact depth, and the calculation formula is expressed by the following equation.

The composite hardness is the hardness of the specimen bonded to the substrate and the composite hardness is calculated by measuring the maximum indentation depth and the maximum indentation load when the indentor presses the specimen at a depth greater than a certain depth during the indentation test do.

That is, in the indentation test, when the indentor pushes the specimen, the influence of the interface and the substrate occurs when the indentation depth of the indentor is more than 10% of the thickness of the thin film. Therefore, the maximum indentation load value in the indentation test is 10 %, The depth to be measured on the pressure particle at that time becomes the maximum indentation depth value.

Figure pat00009

Figure pat00010

Equation 4 is a hardness calculating formula,

Figure pat00011
Refers to the contact area, and the maximum indentation load is measured on each substrate, thin film, and substrate, and the contact area is calculated. Subsequently, the hardness and complex hardness values of the substrate and the thin film are substituted .

Equation (5) is a contact area calculating formula,

Figure pat00012
Is the actual contact depth of the indentor. When the indentation tester applies a load to the specimen, the specimen undergoes elastic deformation, and the actual contact depth is the value obtained by subtracting the elastic deformation depth from the maximum indentation depth.

That is, the actual contact depth, which is the contact depth of the actual specimen, is obtained by subtracting the elastic bending depth, which is the elastic deformation around the contact point, at the maximum indentation depth measured by the indentation tester, and the elastic bending depth is calculated by the elastic bending depth calculating equation And the elastic bending depth calculation equation is expressed by the following equation.

Figure pat00013

Equation (6) is an elastic bending depth calculating equation,

Figure pat00014
Means the depth of elastic bending due to the elastic deformation of the material,
Figure pat00015
Is the stiffness, which means the slope at the maximum indentation depth of the load removal curve in the load-displacement curve shown in FIG. 7,
Figure pat00016
Is a correction constant and is determined according to the shape of the indentor. For example, when the indentor is an angular indentation of a square-pyramidal type,
Figure pat00017
The value is 0.75.

That is, the contact area can be calculated by substituting the actual contact depth, which is a value obtained by subtracting the elastic bending depth calculated in the equation (6) from the maximum indentation depth, in the equation (5), and the value obtained by dividing the maximum indentation load by the contact area And the hardness value and the composite hardness value of the thin film.

A method of obtaining the interface bonding force through the volume value and the hardness value will be described later.

That is, in order to obtain the interfacial bonding force, it is possible to obtain a quantitative interfacial bonding force by dividing the work by the interface and then dividing it by the volume affected by the interface, which will be described in detail below.

In the indentation test, in the indentation test in the case where there is an additional work due to the interface, the total work due to the abrasive particles is the sum of work done by the substrate and work done by the thin film and interface, The work of the interface can be obtained by subtracting the total work of the indenter in the case where there is no additional work due to the interface in the indentation test.

The total work of the indenter in the case where there is no additional work due to the interface is expressed by Equation (7), and the total work of the indenter in the case of additional work by the interface is expressed by Equation (8).

Figure pat00018

here,

Figure pat00019
Means the total work of the indenter if there is no additional work by the interface,
Figure pat00020
Quot; means work by the substrate,
Figure pat00021
Means work by thin film.

Figure pat00022

here,

Figure pat00023
Means the total work of the indentation tester in case of additional work due to the interface,
Figure pat00024
Means work by an interface.

Also, the work generated in the indentation test can be used as a value obtained by expanding the hardness evaluation equation, dividing the work required for plastic deformation by the plastic deformation volume, and expressed as Equation (9) below.

Figure pat00025

here,

Figure pat00026
Quot; means hardness,
Figure pat00027
Means the load,
Figure pat00028
Means the area,
Figure pat00029
The term "plastic deformation"
Figure pat00030
Means the plastic deformation volume.

Substituting equation (9) into equation (7) and equation (8) results in equations (10) and (11).

Figure pat00031

Figure pat00032

In addition, when the thin film is bonded to the substrate, the firing region of the substrate or the thin film, which is expanded when the sample is pressed due to the interfacial bonding force, is constrained by the interfacial bonding force, and the hardness of the bonded substrate and thin film is relatively weak The plastic deformation is constrained by the material having a high hardness.

Accordingly, when the hardness of the substrate is smaller than the hardness of the thin film, as shown in Fig. 8, the firing region volume of the substrate is limited by the interface bonding force, and assuming that the deformation of the firing region volume in the hemispherical shape is linearly limited The plastic zone volume value of the substrate whose deformation is limited by the interfacial bonding force is calculated by multiplying the interfacial parameter which is a dimensionless parameter for correcting the plastic zone volume of the substrate.

That is, the volume of the plastic zone of the substrate is represented by the product of the interface variables as the deformation is restricted by the interface bonding force, and the sum of the plastic zone volume of the substrate and the plastic zone volume of the thin film, do.

Figure pat00033

Figure pat00034
Means the sum of the volume of the sintering region of the substrate and the volume of the sintering region of the thin film,
Figure pat00035
Quot; refers to the volume of the firing region of the substrate,
Figure pat00036
Means the volume of the plastic zone of the thin film,
Figure pat00037
Is an interfacial variable.

Using these interface variables, Equation (11) can be re-expressed as Equation (11).

Figure pat00038

The interfacial parameter values can be calculated from the hardness and complex hardness of the substrate and the thin film, and the volume of the firing region of the substrate and the thin film as shown in the following equation.

Figure pat00039

In the case where there is an additional work due to the interface, in the case where there is no additional work due to the interface in Equation 13, which is the total work function of the indentation tester, subtraction of Equation 10, which is the total work function of the indentation tester, do.

Figure pat00040

As a result, equation (15), which is a day-to-day calculation by the interface, is derived.

Also, the interface bonding force per unit area can be calculated by dividing the work done by the interface by the volume of the substrate whose deformation is limited by the interface bonding force. The unit is [N / m 2 ], and the interfacial bonding force per unit area Which is a constant value, irrespective of the test conditions of the test piece.

Figure pat00041

here

Figure pat00042
Refers to the interfacial bonding force per unit area.

Since the interfacial bonding force per unit area is a quantitative interfacial bonding force value, it is easy to evaluate the interfacial bonding force and it is not complicated and it can be applied irrespective of the material of the specimen. It is possible to obtain an accurate interface bonding force value.

Therefore, if the maximum indentation depth and the maximum indentation load are measured through the indentation test, the total work of the indentation tester can be calculated according to the depth at which the indentor presses the substrate and the thin film according to expression (15) The interface bonding force per unit area can be calculated regardless of the maximum indentation depth, which is the depth at which the substrate and the thin film are pressed, and the test condition.

However, this is the interfacial bonding force per unit area in the case where the hardness of the substrate is smaller than the hardness of the thin film and the deformation of the firing region of the substrate is limited by the interfacial bonding force.

On the other hand, when the hardness of the thin film is smaller than the hardness of the substrate, as shown in FIG. 9, the volume of the plastic zone of the thin film is limited by the interface bonding force and the deformation of the hemispherical plastic zone is linearly limited. The plastic zone volume of the thin film, whose deformation is limited by the interfacial bonding force, is calculated by multiplying the interfacial parameter, which is a dimensionless variable that corrects the plastic zone volume of the plastic zone.

That is, the plastic region volume of the thin film is represented by the product of the interfacial variables as the deformation is limited due to the interface bonding force, and the sum of the plastic region volume of the substrate and the plastic region volume of the thin film, .

Figure pat00043

Using these interface variables, Equation (11) can be re-expressed as Equation (11).

Figure pat00044

The interfacial variables in Equation (18) can be expressed as the following equation.

Figure pat00045

In the case where there is no additional work due to the interface, in the case where there is no additional work due to the interface in Equation 18, which is the total work function of the indentation tester, subtraction of Equation 10, which is the total work function of the indentation tester, do.

Figure pat00046

As a result, Equation 20, which is a day-to-day calculation based on the interface, is derived.

In addition, the interface bonding force per unit area can be calculated by dividing the interface work by the volume of the thin film whose deformation is limited by the interface bonding force. The unit is [N / m 2 ], and the interfacial bonding force per unit area Which is a constant value, irrespective of the test conditions of the test piece.

Figure pat00047

Since the interfacial bonding force per unit area is a quantitative interfacial bonding force value, it is easy to evaluate the interfacial bonding force and it is not complicated and it can be applied irrespective of the material of the specimen. It is possible to obtain an accurate interface bonding force value.

5, the maximum indentation load and the maximum indentation depth are measured (S410) in the indentation tester to calculate the hardness, hardness, hardness, composite hardness, substrate volume, And the calculated hardness of the substrate and the thin film is compared (S430).

Since the deformation of the fired region volume is limited by the interfacial bonding force between the substrate and the thin film, the interfacial parameter is calculated (S440), and the interfacial parameter is calculated (S440) ) And calculating the work by the interface (S450) are different depending on each case.

In addition, by calculating the work by the interface (S450) and dividing it by the deformed volume in which the deformation of the plastic zone volume is limited by the interface joining force in each case, the quantitative interface joining force value So that the measurement is facilitated and accurate measurement can be performed.

According to the embodiments of the present invention having such a shape and structure, it is possible to calculate a quantitative interfacial bonding force value which is independent of the test conditions such as the indentation depth of the indentation in the indentation test and has no influence of the substrate and the thin film, have.

In addition, when the indentation test is performed on the nano material in order to calculate the interfacial bonding force of the nano material, the measurement process is simple and easy measurement is possible, Test can be performed to evaluate the interfacial bonding force, so that the range of application is wide and it is easy to measure.

Also, the interface bonding force can be measured without destroying the specimen, and there is no need to observe the deformation and the fracture region at the interface, so that an easy and convenient measurement is possible.

While the present invention has been described in connection with what is presently considered to be the most practical and preferred embodiments, it is to be understood that the invention is not limited to the disclosed embodiments. That is, within the scope of the present invention, all of the components may be selectively coupled to one or more of them.

The foregoing description is merely illustrative of the technical idea of the present invention, and various changes and modifications may be made by those skilled in the art without departing from the essential characteristics of the present invention. Therefore, the embodiments disclosed in the present invention are intended to illustrate rather than limit the scope of the present invention, and the scope of the technical idea of the present invention is not limited by these embodiments. The scope of protection of the present invention should be construed according to the following claims, and all technical ideas within the scope of equivalents should be construed as falling within the scope of the present invention.

Claims (12)

Measuring a maximum indentation load (L max ) and a maximum indentation depth (h max ) through an indentation test;
The maximum indentation load (L max) and the maximum indentation depth (h max) the hardness (H s, H f, H c) calculation expression plastic zone volume (V s, V f) hardness of the substrate by applying the calculation formula (H s), calculating a hardness (H f), the composite hardness (H c), the plastic zone volume (V s), the plastic zone volume (V f) of the thin film of the substrate of the thin film;
Comparing the hardness (H s ) of the substrate with the hardness (H f ) of the thin film;
Calculating an interfacial parameter x 3 by substituting each of the hardnesses (H s , H f , H c ) and the volumes (V s , V f ) into an interfacial variable (x 3 ) calculation expression; And
Interfacial bonding strength evaluation method including the step of using the calculation formula work (W adhesion) by the interface calculating the work (W adhesion) due to the interfacial bonding strength.
The method according to claim 1,
When the hardness (H s ) of the substrate is smaller than the hardness (H f ) of the thin film,
The plastic zone volume V s of the substrate is linearly limited by the interface bonding force and the plastic zone volume V s * of the substrate whose deformation is limited by the interface bonding force is multiplied by the interface variable x 3
Figure pat00048
). ≪ / RTI >
3. The method of claim 2,
The W adhesion calculation formula based on the interfacial bonding force,
Figure pat00049
. ≪ / RTI >
The method of claim 3,
(W adhesion ) by the interface bonding force is divided by the firing area volume (V s * ) of the substrate whose deformation is limited by the interface bonding force to calculate the interfacial bonding force per unit area (F adhesion ) .
3. The method of claim 2,
The interfacial variable calculating equation is:
Figure pat00050
. ≪ / RTI >
The method according to claim 1,
When the hardness (H f ) of the thin film is smaller than the hardness (H s ) of the substrate,
The firing area volume (V f ) of the thin film is linearly limited by the interface bonding force and the strain is limited by the interface bonding force. The plastic area volume (V f * ) of the thin film is multiplied by the interface variable (x 3 )
Figure pat00051
) ≪ / RTI >
The method according to claim 6,
The W adhesion calculation formula based on the interfacial bonding force
Figure pat00052
. ≪ / RTI >
8. The method of claim 7,
Wherein an adhesion force per unit area (F adhesion ) is calculated by dividing W adhesion by the interfacial bonding force by a firing area volume (V f * ) of a thin film whose deformation is limited by the interfacial bonding force .
The method according to claim 6,
The interfacial variable calculating equation is:
Figure pat00053
. ≪ / RTI >
The method according to claim 1,
The hardness (H s , H f , H c )
Figure pat00054
, And the contact area (A c ) is calculated by substituting the maximum indentation load (L max ) and the maximum indentation depth (h max ) into the contact area (A c ) calculation formula.
11. The method of claim 10,
The contact area (A c )
Figure pat00055
, And the actual contact depth (h c ) is at the maximum indentation depth (h max )
Figure pat00056
Is a depth value obtained by subtracting the elastic bending depth (h d ) calculated by the elastic bending depth (h d ).
here,
Figure pat00057
Is a correction constant,
S is the slope at the maximum depth of the load removal curve.
The method according to claim 1,
The volume (V s ) calculation equation of the substrate
Figure pat00058
, And the calculation formula of the volume (V f ) of the thin film is
Figure pat00059
ego,
The radius (C s , C f ) of each substrate and film
Figure pat00060
And calculating the interfacial bonding force.
here,
Figure pat00061
The press-fitting half-angle of the indenter,
Figure pat00062
The elastic modulus,
Figure pat00063
Yield strength.
KR1020150047661A 2015-04-03 2015-04-03 Test method of interfacial adhesion KR101685507B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
KR1020150047661A KR101685507B1 (en) 2015-04-03 2015-04-03 Test method of interfacial adhesion

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
KR1020150047661A KR101685507B1 (en) 2015-04-03 2015-04-03 Test method of interfacial adhesion

Publications (2)

Publication Number Publication Date
KR20160118852A true KR20160118852A (en) 2016-10-12
KR101685507B1 KR101685507B1 (en) 2016-12-13

Family

ID=57173796

Family Applications (1)

Application Number Title Priority Date Filing Date
KR1020150047661A KR101685507B1 (en) 2015-04-03 2015-04-03 Test method of interfacial adhesion

Country Status (1)

Country Link
KR (1) KR101685507B1 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20190043338A (en) * 2017-10-18 2019-04-26 서울대학교산학협력단 Method for Measuring the Hardness using The Continuous Indentation Method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100404659B1 (en) * 2001-05-10 2003-11-07 권동일 Specimen and test method of interfacial adhensive strength
KR20040103208A (en) * 2003-05-31 2004-12-08 한국기계연구원 Method for measuring thin film properties using indenter
KR101258073B1 (en) * 2011-04-27 2013-04-30 한국표준과학연구원 Interfacial delaminating apparatus by introducing a substrate through-thickness crack
KR101309046B1 (en) * 2012-04-27 2013-09-16 한국표준과학연구원 Measuring method for interfacial adhesion strength of film

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100404659B1 (en) * 2001-05-10 2003-11-07 권동일 Specimen and test method of interfacial adhensive strength
KR20040103208A (en) * 2003-05-31 2004-12-08 한국기계연구원 Method for measuring thin film properties using indenter
KR101258073B1 (en) * 2011-04-27 2013-04-30 한국표준과학연구원 Interfacial delaminating apparatus by introducing a substrate through-thickness crack
KR101309046B1 (en) * 2012-04-27 2013-09-16 한국표준과학연구원 Measuring method for interfacial adhesion strength of film

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20190043338A (en) * 2017-10-18 2019-04-26 서울대학교산학협력단 Method for Measuring the Hardness using The Continuous Indentation Method

Also Published As

Publication number Publication date
KR101685507B1 (en) 2016-12-13

Similar Documents

Publication Publication Date Title
Shen et al. Measurement of JR curves using single-specimen technique on clamped SE (T) specimens
EP3754331A1 (en) Method and system for analysing a test piece using a vibrational response signal
KR101707492B1 (en) Evaluating Method Of The Fracture Toughness Using Instrumented indentation testing
CN108414379B (en) Method for extracting metal elastoplasticity parameters through in-situ press-in test
KR101407405B1 (en) Yield strength and Tensile strength Calculation Method of strain-hardening metal using Instrumented Spherical Indentation Technique
Kren et al. Determination of the physic and mechanical characteristics of isotropic pyrolitic graphite by dynamic indentation method
WO2017017409A1 (en) Method for measuring the mechanical properties of materials using depth sensing indentation
Choi et al. Evaluation of nonequibiaxial residual stress using Knoop indenter
EP3165896A1 (en) Device and method for a non-destructive measurement of mechanical properties
KR101685507B1 (en) Test method of interfacial adhesion
RU2382349C2 (en) Method of test of welded blank (versions)
Giuffre et al. Numerical and experimental investigation of ice adhesion using the blister test
JP5865100B2 (en) Defect inspection apparatus and inspection method
MORI et al. Influence of steel static strength on fatigue strength of web-gusset welded joints with UIT
JP6543019B2 (en) Evaluation method of corrosion fatigue life of steel
KR101631747B1 (en) Measuring apparatus and method of elastic modulus for diagnosing material damages
JP2007057325A (en) Remaining lifetime prediction method
Marzi Innovations in fracture testing of structural adhesive bonds
RU2665500C1 (en) Method for determining glass transition temperature
KR100982462B1 (en) Calibration method for rounded shape indenter by using effective radius
CN113029826A (en) Method for determining fracture performance of metal material by using pre-notched small punch test sample
RU2532234C1 (en) Method to measure mechanical properties of material under conditions of confined pressure (versions)
KR20160055630A (en) Apparatus for safety assessement of glass materials and evaluation method thereof
Kim et al. Quantitative characterization of mechanical properties using instrumented indentation
Wang et al. Nanoindentation characteristics of clamped freestanding Cu membranes

Legal Events

Date Code Title Description
A201 Request for examination
E902 Notification of reason for refusal
E701 Decision to grant or registration of patent right
GRNT Written decision to grant
FPAY Annual fee payment

Payment date: 20191024

Year of fee payment: 4