CN106802260A - A kind of method and system for studying film matrix composite construction mechanical property - Google Patents
A kind of method and system for studying film matrix composite construction mechanical property Download PDFInfo
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- CN106802260A CN106802260A CN201611042256.4A CN201611042256A CN106802260A CN 106802260 A CN106802260 A CN 106802260A CN 201611042256 A CN201611042256 A CN 201611042256A CN 106802260 A CN106802260 A CN 106802260A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/40—Investigating hardness or rebound hardness
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
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Abstract
The present invention relates to engineering material technical field, and in particular to a kind of Nanoindentation studies the method and system of film matrix composite construction mechanical property.The method of the film matrix composite construction mechanical property includes：Anodization, in substrate surface original position, grows oxide-film in real time；Impression treatment, stops polarization and carries out impression treatment to the oxide-film.The anodization processing step and the impression process step alternately n times, N >=2, the elastic modelling quantity and hardness of the film matrix composite construction under the conditions of test different-thickness ratio, modulus and the relation between hardness and the respective modulus of film, matrix and hardness that experiment measurement is obtained are set up using nano impress is theoretical.The system of the test film matrix composite construction mechanical property includes electrochemical assembly and nano impress component, can dramatically expand the Study on Problems scope achieved by nano-hardness tester, and under research electrochemical environment film matrix deformation mechanism new analysis means are provided.
Description
Technical field
The present invention relates to engineering material technical field, and in particular to a kind of Nanoindentation studies film-matrix composite construction
The method and system of mechanical property.
Background technology
Material is the basis of human material's civilization, and the development of material technology supports the development of other new technologies.With section
The development and progress of technology, various new materials are developed rapidly and are widely used in high-tech area.Thin-film material is used as one
New function material is planted, has obtained important in fields such as optics, semi-conductor industry, Computer Storage, medicinal pharmacology, hull cells
Using proposing more strict requirements to its reliability, performance etc..The micromechanics of material are to its macroscopic failures
Mechanism has a major impact, therefore, the sign for carrying out thin-film material micromechanics is extremely necessary.
Nanoindentation may be implemented in the performance test of micrometer/nanometer yardstick, by continuous monitoring and record pressure head pressure
Enter sample and from the load in sample surfaces uninstall process and displacement, the load in one complete loading-unloading loop of analysis-
Displacement data can obtain many mechanical properties of material, such as contact stiffness, creep parameters, elastic work etc..Due to the shadow of matrix
Ring, the mechanical property of direct measurement film is often extremely difficult.The load-displacement obtained using Nanoindentation measurement
Data, are not only response of the film to institute's imposed load, but the response of thin film basal body system, generally it is subject to film and base
The respective elasticity of body, the joint effect of plasticity property.
《Film based on Nano Assay technology/matrix system micro mechanical property is characterized》(Wang Zhenlin,《Material Leader》,
The 5A phases of volume 21 in May, 2007) method that film/matrix system mechanical property is measured based on Nanoindentation is disclosed, lead to
The recurrence for crossing the load-deepness test data to loading can isolate film and matrix from the data of film/matrix system
Mechanical property, the matrix effect produced when excessive for impression is the 1/ of film layer using " 1/10 empirical method ", i.e. depth of cup
10, then measured hardness number is close to true hardness.The thickness of the film that the method is tested is fixed, it is impossible to realized continuous
Change the operation of film thickness, although traditional coating process can change film thickness, but the time is long, high cost, and due to
The limitation of coating film thickness precision, it is impossible to realize truly continuous growth of the film since zero thickness and use nanometer simultaneously
Impression instrument carries out in site measurement load-displacement data, is easily caused the discrete of resulting film-matrix system parameter in test process
Change, and then be possible to miss the turning point of some parameter properties.
The content of the invention
Therefore, the technical problem to be solved in the present invention be overcome film of the prior art cannot zero thickness continuously give birth to
It is long, and mechanical property in test film-matrix composite construction can not realize the defect of film layer growth in real time.
In order to solve the above technical problems, the technical solution adopted by the present invention is as follows：
The present invention provides a kind of method for studying film-matrix composite construction mechanical property, comprises the following steps：
Anodization, in substrate surface original position, grows oxide-film in real time；
Impression treatment, stops polarization and carries out impression treatment to the oxide-film；
Wherein, the anodization processing step and the impression process step alternately n times, different thickness are tested in N >=2
The mechanics parameter of the film-matrix composite construction under the conditions of degree ratio.
Optionally, for the first time before the anodization processing step, also including carrying out surface preparation to base material coated surface
Step；The pre-treatment step includes cleaning and/or polishes.
Optionally, not in impression process step described in homogeneous, Indentation position is different, depth of cup is identical.
Optionally, each Indentation position spacing is 10 μm~100 μm.
The system that the present invention also provides a kind of test film-matrix composite construction mechanical property：
Including electrochemical assembly, and the nano impress component for being arranged on the electrochemical assembly vertical direction；It is described to receive
Rice impression component is used for the film of growth carries out impression test in real time in the electrochemical assembly.
Optionally, the electrochemical assembly includes electrolytic bath, is arranged on the negative electrode of cell body bottom and is arranged on groove
Positive electrode in body, the negative electrode is connected to the positive pole that the negative pole of power supply, the positive electrode are connected to the power supply.
Optionally, film base material to be plated is directly stacked on the positive electrode, and surface to be coated is near the cell body opening
Surface, and it is parallel with it；The surface to be coated depth in the electrolytic solution is 3mm~8mm.
Optionally, the nano impress component includes pressure head and the pressure head sensor being attached thereto.
Optionally, the nano impress component also includes the displacement of pressing head control module for controlling depth of cup.
Optionally, the pressure head is Berkvich pressure heads.
Technical solution of the present invention, has the following advantages that：
1. a kind of method for studying film-matrix composite construction mechanical property provided in an embodiment of the present invention, including anodization
Treatment and impression treatment.Carry out indentation test in substrate surface original position, and grow oxide-film in real time, and anodization processing step and
Impression process step alternately n times, N >=2 can guarantee that, with the increase of oxide thickness, thickness ratio is continually changing, Jin Ershi
Existing thickness, than the indentation test under the conditions of consecutive variations, is research impression thickness film-matrix composite construction more caused than change
The research of mechanical properties change provides experimental analysis basis, in combination with nano impress theory analysis, finally sets up film-base
Relation between the mechanical property and film of bluk recombination structure, the respective mechanical property of matrix.
The system that the embodiment of the present invention also provides a kind of test film-matrix composite construction mechanical property, including electrochemistry group
Part and electrochemical assembly vertical direction nano impress component is arranged on, nano impress component to growing in real time in electrochemical assembly
Film carry out impression test, the scientific research of nano-hardness tester experiment porch carries out reality to the film that integrated electrochemical experiment porch is formed
When mechanics parameter collection, be greatly enlarged the Study on Problems scope achieved by Conventional nano impression instrument, and be research electrochemistry
Thin film basal body deformation mechanism provides new analysis means under environment.
2. the method for research film-matrix composite construction mechanical property provided in an embodiment of the present invention, enters to base material coated surface
Row cleaning, polishing pretreatment, then carry out anodization to grow oxide-film, energy on positive electrode directly in stacked electrochemical assembly
Ensure that the property of oxide-film is homogeneous, Stability Analysis of Structures meets the required precision of experiment；Each Indentation position is different, it is to avoid same
The continuous impression in one position causes to change and influence follow-up result on material structure.
3. the method for research film-matrix composite construction mechanical property provided in an embodiment of the present invention, is carrying out indentation test
When, using displacement control mode, it is ensured that depth of cup is consistent；The electrolyte for being used is weak acid, to the solubility degree of base material
It is extremely low, and nano-hardness tester pressure head material is diamond or sapphire, is applicable electrolyte environment.
Brief description of the drawings
In order that present disclosure is more likely to be clearly understood, below according to specific embodiment of the invention and combine
Accompanying drawing, the present invention is further detailed explanation, wherein：
Fig. 1 is the operation stream of the method for realizing the research film-matrix composite construction mechanical property described in the embodiment of the present invention
Journey；
Fig. 2 is that the system section for realizing the test film-matrix composite construction mechanical property described in the embodiment of the present invention is illustrated
Figure.
Reference is expressed as in figure：1- electrochemical assemblies；2- nano impress components；3- microscope carriers；11- electrolytic cells；12- bears
Electrode；13- positive electrodes；14- power supplys；15- film base materials to be plated；16- electrolyte；21- pressure heads；22- pressure head sensors.
Specific embodiment
Technical scheme is clearly and completely described below in conjunction with accompanying drawing, it is clear that described implementation
Example is a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, ordinary skill
All other embodiment that personnel are obtained under the premise of creative work is not made, belongs to the scope of protection of the invention.
Embodiment
The present embodiment provides a kind of method for studying film-matrix composite construction mechanical property, as shown in figure 1, its specific step
It is rapid as follows：
S1. surface preparation is carried out to base material coated surface
Metal or alloy base material coated surface is cleaned and/or is polished pretreatment.
Used as one embodiment of the present of invention, in the present embodiment, base material is metal.
S2. anodization
Film base material to be plated is directly stacked on the positive electrode, first time anodization is carried out, surface to be coated is in electrolysis
Depth in liquid is 3mm~8mm, makes surface zero thickness to be coated start continuously to grow layer oxide film, polarization time first time
It is 30s~90s.
Used as one embodiment of the present of invention, in the present embodiment, surface to be coated depth in the electrolytic solution is 3mm, the
Polarization time is 60s.
S3. impression treatment
Stop charging, stop polarization, while carrying out first time impression to oxide-film in diverse location using nano-hardness tester
Treatment.Using displacement control mode, keep each Indentation position difference, depth of cup identical.
N position of selection carries out impression, n >=2；Each Indentation position spacing is 10 μm~100 μm, and depth of cup is
200nm~300nm.Take first time impression and process the hardness of n position and the average value of modulus as the thickness ratio (the i.e. depth of cup
Degree/film thickness) under the conditions of film-matrix composite construction hardness and modulus.
Used as one embodiment of the present of invention, in the present embodiment, n=6, each Indentation position spacing is 20 μm, the depth of cup
It is 200nm to spend.
S4.S2 and S3 alternately n times, N >=2
Impression treatment terminates to carry out second anodization, continues in substrate surface original position, grows oxide-film, oxygen in real time
The thickness for changing film continues to increase.Second polarization time is 30s~90s, stops polarization, in step s3 near n position
1mm2Second impression treatment is carried out in region.Using displacement control mode, control depth of cup is identical.
Anodization and impression treatment alternately n times, obtain the film-matrix composite construction under the conditions of N number of thickness ratio
Hardness and modulus, N >=2.
Used as one embodiment of the present of invention, in the present embodiment, second polarization time is 60s.
As convertible embodiment of the invention, n times polarization is carried out, each polarization time not limited to this can be according to experiment
Needs are adjusted.
As one embodiment of the present of invention, in the present embodiment, N=10.
S5. the relation set up between the hardness and modulus of test and the respective hardness of film, matrix and modulus
Comprehensive N number of thickness than condition lower film-matrix composite construction hardness and modulus, with reference to film in nano impress method-
Matrix composite construction is theoretical, sets up between the hardness and Modulus results and the respective hardness of film, matrix and modulus of test acquisition
Relation.
The system that the present embodiment also provides a kind of test film-matrix composite construction mechanical property, as shown in Fig. 2 including electricity
Chemical component 1, and it is arranged on the nano impress component 2 of the vertical direction of electrochemical assembly 1；Nano impress component is used for electrification
The film for learning growth in real time in component carries out impression test.The system is placed on microscope carrier 3.
Electrochemical assembly includes electrolytic bath 11, is arranged on the negative electrode 12 of cell body bottom and is arranged in cell body
Positive electrode 13, negative electrode is connected to the positive pole that the negative pole of power supply 14, positive electrode are connected to power supply.Film base material to be plated 15 is directly folded
Put on positive electrode 13, and surface to be coated is close to cell body open surfaces, and it is parallel with it, surface to be coated is in electrolyte 16
Depth 3mm~8mm and to be powered.Selection weak acid is used as electrolyte 16, and the dissolution degree for treating coating material 15 is extremely low.
As one embodiment of the present of invention, in the present embodiment, positive electricity extremely copper plate electrode, electrolyte is 0.05M
H2C2O4, depth is 3mm in the electrolytic solution on surface to be coated.
Nano impress component 2 includes pressure head 21 and the pressure head sensor 22 being attached thereto, also including for controlling impression
The displacement of pressing head control module of depth.Wherein, pressure head can be diamond or sapphire, be applicable electrolyte environment.As this hair
Bright one embodiment, in the present embodiment, pressure head material is diamond.
Stop being powered, stop polarization, while not carrying out impression reality to oxide-film in the same time using nano impress component 2
Test, using displacement control mode, keep each Indentation position difference, depth of cup identical；Modulus is recorded using pressure head sensor 2
And hardness data.
Obviously, above-described embodiment is only intended to clearly illustrate example, and not to the restriction of implementation method.It is right
For those of ordinary skill in the art, can also make on the basis of the above description other multi-forms change or
Change.There is no need and unable to be exhaustive to all of implementation method.And the obvious change thus extended out or
Among changing still in the protection domain of the invention.
Claims (10)
1. it is a kind of study film-matrix composite construction mechanical property method, it is characterised in that comprise the following steps：
Anodization, in substrate surface original position, grows oxide-film in real time；
Impression treatment, stops polarization and carries out impression treatment to the oxide-film；
Wherein, the anodization processing step and the impression process step alternately n times, different-thickness ratio is tested in N >=2
Under the conditions of film-matrix composite construction mechanics parameter.
2. a kind of method for studying film-matrix composite construction mechanical property according to claim 1, it is characterised in that the
Once before the anodization processing step, also including carrying out surface preparation to base material coated surface the step of；The pretreatment step
It is rapid to include cleaning and/or polish.
3. it is according to claim 1 and 2 it is a kind of study film-matrix composite construction mechanical property method, it is characterised in that
Not in impression process step described in homogeneous, Indentation position is different, depth of cup is identical.
4. a kind of method of the research film-matrix composite construction mechanical property according to claim any one of 1-3, its feature
It is that each described Indentation position spacing is 10 μm~100 μm.
5. the system of a kind of test film-matrix composite construction mechanical property, it is characterised in that including electrochemical assembly, Yi Jishe
Put the nano impress component in the electrochemical assembly vertical direction；The nano impress component is used for the electrochemical assembly
In in real time growth film carry out impression test.
6. the system of test film according to claim 5-matrix composite construction mechanical property, it is characterised in that the electricity
The positive electrode that chemical component includes electrolytic bath, is arranged on the negative electrode of cell body bottom and is arranged in cell body, the negative electricity
Pole is connected to the positive pole that the negative pole of power supply, the positive electrode are connected to the power supply.
7. the system of test film according to claim 6-matrix composite construction mechanical property, it is characterised in that to be coated
Base material is directly stacked on the positive electrode, and surface to be coated is close to the cell body open surfaces, and parallel with it；It is described to treat
Coated surface depth in the electrolytic solution is 3mm~8mm.
8. the system of the test film according to claim any one of 5-7-matrix composite construction mechanical property, its feature exists
In the nano impress component includes pressure head and the pressure head sensor being attached thereto.
9. the system of test film according to claim 8-matrix composite construction mechanical property, it is characterised in that described to receive
Rice impression component also includes the displacement of pressing head control module for controlling depth of cup.
10. the system of test film according to claim 8 or claim 9-matrix composite construction mechanical property, it is characterised in that institute
Pressure head is stated for Berkvich pressure heads.
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| CN201611042256.4A CN106802260A (en) | 2016-11-22 | 2016-11-22 | A kind of method and system for studying film matrix composite construction mechanical property |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018223760A1 (en) * | 2017-06-09 | 2018-12-13 | 清华大学 | Electrochemical biosensor electrode, sensor and preparation method therefor |
| CN109001064A (en) * | 2018-08-23 | 2018-12-14 | 江苏亨通光导新材料有限公司 | A kind of method of quantitative measurment and evaluation preform polishing effect |
| WO2019015359A1 (en) * | 2017-07-19 | 2019-01-24 | 清华大学 | Gold-film electrode, electrochemical biosensor electrode, sensor, and manufacturing method therefor |
| CN109520828A (en) * | 2018-10-11 | 2019-03-26 | 西北工业大学 | The elasticity modulus test method of film |
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| JPS63117241A (en) * | 1986-11-05 | 1988-05-21 | Hitachi Ltd | Method and apparatus for measuring hardness |
| JPH08159941A (en) * | 1994-12-07 | 1996-06-21 | Natl Res Inst For Metals | Measuring instrument for hardness of minute surface |
| CN102944490A (en) * | 2012-11-29 | 2013-02-27 | 厦门大学 | High-temperature rigidity measuring method based on electrified heating |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018223760A1 (en) * | 2017-06-09 | 2018-12-13 | 清华大学 | Electrochemical biosensor electrode, sensor and preparation method therefor |
| WO2019015359A1 (en) * | 2017-07-19 | 2019-01-24 | 清华大学 | Gold-film electrode, electrochemical biosensor electrode, sensor, and manufacturing method therefor |
| CN109001064A (en) * | 2018-08-23 | 2018-12-14 | 江苏亨通光导新材料有限公司 | A kind of method of quantitative measurment and evaluation preform polishing effect |
| CN109520828A (en) * | 2018-10-11 | 2019-03-26 | 西北工业大学 | The elasticity modulus test method of film |
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