CN109959559A - Detect the method and system that coating material stretches fission - Google Patents
Detect the method and system that coating material stretches fission Download PDFInfo
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- CN109959559A CN109959559A CN201910368710.2A CN201910368710A CN109959559A CN 109959559 A CN109959559 A CN 109959559A CN 201910368710 A CN201910368710 A CN 201910368710A CN 109959559 A CN109959559 A CN 109959559A
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- 230000004992 fission Effects 0.000 title claims description 90
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N3/02—Details
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
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- G—PHYSICS
- 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
- G01N2203/0014—Type of force applied
- G01N2203/0016—Tensile or compressive
- G01N2203/0017—Tensile
-
- G—PHYSICS
- 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
- G01N2203/0058—Kind of property studied
- G01N2203/006—Crack, flaws, fracture or rupture
- G01N2203/0062—Crack or flaws
- G01N2203/0064—Initiation of crack
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- G—PHYSICS
- 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
- G01N2203/0058—Kind of property studied
- G01N2203/006—Crack, flaws, fracture or rupture
- G01N2203/0062—Crack or flaws
- G01N2203/0066—Propagation of crack
-
- G—PHYSICS
- 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
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/026—Specifications of the specimen
- G01N2203/0262—Shape of the specimen
- G01N2203/0278—Thin specimens
- G01N2203/0282—Two dimensional, e.g. tapes, webs, sheets, strips, disks or membranes
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- G—PHYSICS
- 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
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/0641—Indicating or recording means; Sensing means using optical, X-ray, ultraviolet, infrared or similar detectors
- G01N2203/0647—Image analysis
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- G—PHYSICS
- 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
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/067—Parameter measured for estimating the property
- G01N2203/0676—Force, weight, load, energy, speed or acceleration
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- G—PHYSICS
- 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
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/067—Parameter measured for estimating the property
- G01N2203/0682—Spatial dimension, e.g. length, area, angle
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Abstract
Present applicant proposes a kind of method and systems for detecting material damage, wherein, coating material and stretching-machine are placed in the sample bin of scanning electron microscope, and the method for detection coating material damage includes: the scan image for acquiring coating material in stretching or compression process；The scan image is handled by loading by means of digital image correlation method；According to treated, the scan image analyzes the damage variation of the coating material.In situ, the microcosmic lower detection in stretching or compression, the accuracy for improving the observation of material damage mechanism and analyzing may be implemented to coating material in the method and system of the detection material damage of the application.
Description
Technical field
The present invention relates to field of material technology, and the method and detection of fission are stretched more particularly, to a kind of detection coating material
The system that coating material stretches fission.
Background technique
Existing probing into for coating material mechanics properties testing and micromechanism of damage, utilizes universal tensile testing machine mostly
It is carried out under macro-scale, generallys use the tension crack process of the method observation coating of high resolution camera shooting, and combined
The strain variation situation of Digital Image Correlation Method measurement coating front surface.
It needs to make tensile sample matrix under normal conditions, coating material to be tested is then sprayed on basis material, it
Typical spray speckle is carried out to coating material surface afterwards, it is therefore an objective to calculate strain for subsequent digital image correlation method and mark is provided
Point.Tension test is carried out to tensile sample using universal tensile testing machine after being ready to complete, needs to utilize height in experimentation
Resolution camera records drawing process to observe the detailed process of coating cracking, and serialograph, so as to utilize number
The strain variation situation of word DIC Method calculating coating front surface.
By digital picture related algorithm software VIC2D, speckle is calculated in drawing process using digital picture related algorithm
In changing rule, obtain strain stress relation.Thermal barrier coating is broadly divided into 4 ranks to face crack cracking in receiving tensile load
Section: (1) when coating just starts to bear tensile load, irregular variation is presented in strain；(2) with the increase of tensile load, coating
Surface strain is orderly fluctuation status, is similar to sine curve, and maximum strain and minimum strain are respectively wave crest and trough, and wave
Peak and trough are constantly mobile to same direction；(3) when tensile load reaches certain phase, the fraction areal strain of coating is sharply
Increase；(4) when the strain of the coating area sharply increased reaches capacity, i.e., the stress in region reaches ultimate tensile, coating
It is broken.But the thickness of many coating materials is smaller, it is more difficult detailed using high resolution camera under macro-scale
The dehiscence process of thin observation coating material.
Frequently with observing interface crackle and face crack to the method that Interface Crack extends be by control universal test
What the load gradual change of machine was realized.Such as prepare the identical multiple thermal barrier coating tensile samples of parameter, the respectively fixation to gradually increase
Tensile load thermal barrier coating sample stops stretching, sample is removed the section of tensile sample when stretching reaches determined load
Metallographic specimen is made, observation is under a scanning electron microscope to determine the crackle form and crackle transition process in drawing process.
But this method can not real time reaction crackle expansion process, and load range selection have certain randomness, lead
It causes resulting crackle discontinuous with tensile load changing rule, the accuracy of crack propagation process may be will affect.In addition it is seeing
It examines in the preparation process of sample, it is lack of standardization due to grinding and polishing, it is likely to result in cracked inside brittle coating, influences result sight
The accuracy examined.
In addition, some materials such as fragile material, elastic deformation stage is very short during stretching, fracture behaviour hair
Life is very rapid, when being tested using large-scale cupping machine, is difficult to capture that coating material is detailed to be broken
Journey.
Summary of the invention
The application aims to solve at least one of the technical problems existing in the prior art.
For this purpose, the application first aspect embodiment proposes a kind of method that detection coating material stretches fission, which is applied
Layer material stretches fission method, may be implemented to carry out in situ, microscopically detecting when stretching coating material, improves material damage
The accuracy for hurting mechanism observation and analysis also can capture coating material particularly with some quick coating materials of fission
Detailed fracture process.
The application second aspect embodiment also proposes a kind of system that detection coating material stretches fission.
To solve the above-mentioned problems, the method that the detection coating material of the application first aspect embodiment stretches fission, applies
Layer material and stretching-machine are placed in the sample bin of scanning electron microscope, which comprises estimate the coating material
Draw stage；The rate of extension of the stretching-machine is adjusted according to the draw stage；The coating material is acquired in drawing process
In scan image；And the scan image is handled by loading by means of digital image correlation method, and according to treated
Scan image analyzes the stretching fission of the coating material.
The method for stretching fission according to the detection coating material of the embodiment of the present application, wherein coating material and stretching-machine are put
It sets in the sample bin of scanning electron microscope, the stretching of coating material or compression process is carried out by scanning electron microscope
Original position is observed in real time, realizes the pattern variation from micro-level observation coating material, also, adjust drawing according to draw stage
Stretch the rate of extension of machine, can be more easier to capture the crack initiation of coating material especially fragile material, extension it is specific
Process, and, carrying out in-situ observation can be to avoid the secondary damage to coating material, so that observed result is more accurate.
In some embodiments, the draw stage includes fission safe period and fissions the generation phase, described according to the drawing
The stage of stretching adjusts the rate of extension of the stretching-machine, comprising: reduces the rate of extension of the stretching-machine in the fission generation phase.
In some embodiments, the draw stage includes fission safe period and fission generation phase, the coating material institute
The elasticity modulus of matrix of samples be greater than default modulus threshold value, the drawing that the stretching-machine is adjusted according to the draw stage
Stretch rate, comprising: control the stretching-machine in the fission safe period and stretch with first rate to the coating material；?
The fission generation phase is controlled the stretching-machine and is stretched with the second rate to the coating material, wherein second speed
Rate is less than the first rate.
In some embodiments, the coating material is sprayed on respectively in two matrix of samples, wherein a matrix of samples
On coating material upper surface as scanning surface, the side of the coating material in another matrix of samples is as scanning surface.From
And the front of coating material and the detailed process of lateral dehiscence can be directly observed under the conditions of microcosmic by scanning electron microscope
And then the damage mechanisms of analysis of material, it is adopted using scan image of the scanning electron microscope to drawing process and compression process
Collection, comprising: the scan image of acquisition material upper surface described in stretching or compression process, and, acquisition is being stretched and is being compressed
The scan image of the coating material side in the process, so as to realize cracking to the front of coating material and side
Journey is observed.
In some embodiments, before the coating material being placed on the coating material placement, the method is also wrapped
It includes: speckle is marked on the scanning surface of the coating material by nano-imprint process.
To solve the above-mentioned problems, the system that the detection coating of the application second aspect embodiment stretches fission, comprising: draw
Machine is stretched, for affiliated coating material to be stretched or compressed to coating material applied force；Scanning electron microscope, affiliated coating material
It is placed on the stretching-machine in the sample bin of the scanning electron microscope, the scanning electron microscope is described for acquiring
Scan image of the coating material in stretching or compression process；Processing unit, for estimating the draw stage of the coating material,
Adjust the rate of extension of the stretching-machine according to the draw stage, and by loading by means of digital image correlation method to the scan image into
Row processing, according to treated, the scan image analyzes the damage variation of the coating material.
The system for stretching fission according to the detection coating material of the embodiment of the present application, wherein coating material and stretching-machine are put
It sets in the sample bin of scanning electron microscope, it can stretching or compression process to coating material by scanning electron microscope
It carries out original position, observe in real time, realize the pattern variation from micro-level observation coating material, also, according to draw stage tune
The rate of extension for saving stretching-machine can be more easier to capture the crack initiation of coating material especially fragile material, extension
Detailed process, and, carrying out in-situ observation can be to avoid the secondary damage to coating material, so that observed result is more accurate.
In some embodiments, the draw stage includes fission safe period and fission generation phase, and the processing unit exists
It is specifically used for when adjusting the rate of extension of the stretching-machine according to the draw stage, reduces the drawing in the fission generation phase
Stretch the rate of extension of machine.
In some embodiments, the draw stage includes fission safe period and fission generation phase, the coating material institute
The elasticity modulus of matrix of samples be greater than default modulus threshold value, described in the processing unit is being adjusted according to the draw stage
It is specifically used for when the rate of extension of stretching-machine, controls the stretching-machine in the fission safe period with first rate to the coating
Material is stretched, and, the stretching-machine is controlled in the fission generation phase, and the coating material is carried out with the second rate
It stretches, wherein second rate is less than the first rate.
In some embodiments, the coating material is coated in respectively in two matrix of samples, wherein in a matrix of samples
Coating material upper surface as scanning surface, the side of the coating material in another matrix of samples is as scanning surface；It is described
Scanning electron microscope is specifically used in scan image, acquires the scanning of coating material upper surface during Compression and Expansion
Image, and, acquire the scan image of the coating material side during stretching.To which scanning electron microscopy can be passed through
Mirror Electronic Speculum directly observes the damage in the front of coating material and the detailed process of lateral dehiscence and then analysis of material under the conditions of microcosmic
Hurt mechanism.
In some embodiments, the system also includes labelling apparatus, the labelling apparatus is used for by the coating material
Material is placed on before the sample bin, marks speckle on the scanning surface of the coating material by nano-imprint process.
Additional aspect and advantage of the invention will be set forth in part in the description, and will partially become from the following description
Obviously, or practice through the invention is recognized.
Detailed description of the invention
Above-mentioned and/or additional aspect of the invention and advantage will become from the description of the embodiment in conjunction with the following figures
Obviously and it is readily appreciated that, in which:
Fig. 1 is the flow chart that the method for fission is stretched according to the detection coating material of one embodiment of the application；
(a)-(e) in Fig. 2 is the fissuring rate process according to the coating material of one embodiment of the application
Scan image schematic diagram；
Fig. 3 is the block diagram that the system of fission is stretched according to the detection coating material of one embodiment of the application；
Fig. 4 is the block diagram of the system of detection coating material stretching fission according to another embodiment of the invention.
Appended drawing reference:
Detect the system 100 that coating material stretches fission；
Stretching-machine 10, scanning electron microscope 20, processing unit 30, labelling apparatus 40.
Specific embodiment
The embodiment of the present invention is described below in detail, the embodiment being described with reference to the drawings is exemplary, and is retouched in detail below
State the embodiment of the present invention.
Below with reference to the accompanying drawings 1 and 2 descriptions stretch fission according to the detection coating material of the application first aspect embodiment
Method.
Wherein, in embodiments herein, coating material and stretching-machine are placed on to the sample of scanning electron microscope
In storehouse, stretching-machine is for being stretched or being compressed to coating material, and it is possible to design the sample that can be placed in electron microscope
Stretching-machine in storehouse, thus, compared to the stretching-machine of usually used macro-size, the stretching-machine that the application uses is smaller
Type.So by scanning electron microscope can stretching to the coating material in sample bin or compression process carry out it is in situ, real
When observe and scan image, also, carry out in-situ observation, can be split to avoid internal caused by grinding and polishing when observation sample preparation
Line avoids secondary damage.
Fig. 1 is according to the flow chart of the method for the detection coating material damage of one embodiment of the application, such as Fig. 1 institute
Show, the method that the detection coating material of the embodiment of the present application stretches fission includes step S1, step S2, step S3, step S4.
Step S1 estimates the draw stage of coating material.
Specifically, during stretching, strain occurs that the different stages can be divided into coating material, such as there are no generations
The initial stage of cracking tendency, the germinating cracked stage and the stage of producing fracture etc. can generate according to crackle
Different phase setting draws high the time, and when stretching to coating material, which stage can have been estimated based on stretching time, or
Person is judged based on the realtime graphic that scanning electron microscope acquires in which draw stage.
In some embodiments, draw stage may include fission safe period and fission generation phase, and fission safe period is for example
Initial stage, the germinating stage and the stage of producing fracture that the fission generation phase for example cracks.
Step S2 adjusts the rate of extension of stretching-machine according to draw stage.
Specifically, it for some coating materials, especially fragile material such as ceramic material, strains during stretching
Stage is very short, and fracture behaviour generation is very rapid, is difficult to capture the careful fracture process of coating material, thus, in this Shen
In embodiment please, fragile material in a disguised form is delayed to generate the time of fission by adjusting the rate of extension of stretching-machine, more
Convenient for detecting its detailed process being broken.
In some embodiments, in order to be more conducive to detect the fission process of coating material, subtract in the fission generation phase
The rate of extension of small stretching-machine.For example, the rate of extension adjustable extent of stretching-machine is in 0.036mm/min-1mm/min range
It is interior, by slow down rate of extension, it can be achieved that coating material such as brittle ceramic coating " delay " Tensile Fracture Process, so as to
To realize that observation coating material slowly cracks to the detailed process for disconnecting peeling.
In further embodiments, the elasticity modulus of the matrix of samples where coating material is greater than default modulus threshold value, i.e.,
The elasticity modulus of matrix of samples is bigger, is unlikely to deform, then controls stretching-machine in fission safe period with first rate to coating material
Material is stretched；Coating material is stretched with the second rate in fission generation phase control stretching-machine, wherein the second rate is small
In first rate.For example, in fission safe period control stretching-machine with the stretching speed of 0.8,0.6,0.4,0.2 or 0.1 (mm/min)
Rate stretches coating material, when that will crack, reduce stretching-machine rate of extension for example control stretching-machine with
0.08, the rate of extension of 0.06,0.04 or 0.03 (mm/min) stretches coating material, is equivalent to and has elongated coating material
Material generates the process of fission, so as to more easily capture the detailed fission process of coating material, is conducive to subsequent stretching
The analysis and deduction for mechanism of fissioning.
Step S3 acquires scan image of the coating material in stretching or compression process.
Specifically, scanning electron microscope is scanned the scanning surface of coating material to obtain scan image, scanning electricity
Sub- microscope continuously shot images or can carry out overall process video recording in the detection process, and scan image is transferred at image
Manage device such as computer system.
Step S4 is handled scan image by loading by means of digital image correlation method, and scan image divides according to treated
Analyse the stretching fission of coating material.
Specifically, after processing unit receives scan image, scan image is handled by loading by means of digital image correlation method,
Wherein, loading by means of digital image correlation method is a kind of image measuring method using computer vision technique, for measuring the whole audience of object
Or the deformation or strain of part.The basic principle is that carrying out grid dividing to the region to be measured of body surface before deforming, pass through
Natural or made speckle in the digital picture collected of comparison deformation front and back, according to correlation function predetermined into
Row calculates, and then obtains the deflection or strained situation of body surface.So by loading by means of digital image correlation method to scan image into
Row processing, can obtain the germinating and situation of change that coating material is fissioned in stretching or compression process.
After handling by loading by means of digital image correlation method scan image, the strain size on coating material surface can be obtained
And its change procedure, it can the detailed process for clearly capturing coating material face checking, the position including crack initiation,
The path of crack propagation and speed etc., it is thus possible to the damage variation for being more clear, accurately observing and analyzing coating material.
In short, in the stretching of micro-level in-situ observation coating material or compression process, it can be with synchronous recording displacement/load
Lotus signal so as to realize the analysis to coating material mechanical property, and can record coating material under micro-nano-scale
The change procedure of material, so as to infer micromechanism of damage of the coating material in stretching or compression process
The method for stretching fission according to the detection coating material of the embodiment of the present application, wherein coating material and stretching-machine are put
It sets in the sample bin of scanning electron microscope, the stretching of coating material or compression process is carried out by scanning electron microscope
Original position is observed in real time, realizes the pattern variation from micro-level observation coating material, also, adjust drawing according to draw stage
Stretch the rate of extension of machine, can be more easier to capture the crack initiation of coating material especially fragile material, extension it is specific
Process, and, carrying out in-situ observation can be to avoid the secondary damage to coating material, so that observed result is more accurate.
Further, many coating materials are prepared by the methods of plasma spraying or physical vapour deposition (PVD)
, due to the particularity of spraying method, the coating thickness of coating material may be subjected to limitation, such as certain ceramic coating materials
Spraying prepare thickness generally within the scope of tens microns to several millimeters.Due to the limitation of coating material thickness, in reality
The situation of change that coating material front surface can only be often observed in observation process, can not observe coating material side and material
The variation that inside occurs.
In order to solve the problems, such as to propose further above, in the embodiment of the present application, coating material is sprayed on two respectively
In matrix of samples, wherein the upper surface of the coating material in a matrix of samples is as scanning surface, in another matrix of samples
The side of coating material is as scanning surface.It, both can be with when acquiring scan image of the coating material in stretching or compression process
The scan image in stretching or compression process coating material upper surface is acquired, can also acquire and be applied in stretching or compression process
The scan image of layer material side, even if being limited by thickness, also may be implemented to its side shape particularly with brittle coating material
Looks variation is observed.To which surface, the boundary of coating material can be directly observed under the conditions of microcosmic by scanning electron microscope
The crack initiation and propagation situation in face, and then can more correctly infer the damage mechanisms of coating material.
Wherein, in embodiment, matrix of samples is removably disposed on stretching-machine, and the drawing to coating material may be implemented
It stretches or compresses, space can also be saved in sample bin.Specifically, stretching-machine may include driving gear unit, control and letter
Number detection unit and clamping unit etc. spray upper coating material, and clamping and fixation in the matrix of samples of two different structures
Onto stretching-machine.It is of course also possible to the bracket for individually having fixture is arranged, matrix of samples can clamping on the bracket, and lead to
Overstretching machine is stretched or is compressed to matrix of samples, and then realizes the stretching or compression to coating material.And in order to enable
Stretching-machine can be placed at sample bin, and compared to the stretching-machine that macroscopic view observation uses, small-sized stretching-machine is can be used in the application.
Besides, the strain measurement for carrying out loading by means of digital image correlation method under a scanning electron microscope, exactly uses scanning electron
Microscope replaces generic digital camera, using the microcosmic digital picture in scanning electron microscope subject deformation process, by
In scanning electron microscope shooting image amplification factor usually more than hundred times, in order to enable scanning electron microscope shoot image it is clear
The speckle for telling body surface, in the embodiment of the present application, by nano-imprint process such as electron beam lithography or
Grain self-assembling technique come when marking speckle on the scanning surface of coating material, that is, being handled as loading by means of digital image correlation method to
Measured zone, and then scan image is handled using loading by means of digital image correlation method to obtain the strain on coating material surface and side
Size and its change procedure, the micromechanism of damage of reasoning coating material.
For example, coating material to be observed is chosen tensile sample basis material according to coating material attribute and is made
Standby two kinds of tensile sample matrixes of different shapes, then spray coating material to be observed in matrix of samples, and sample preparation is completed
The label of speckle is carried out on the surface to be observed of coating using nanometer embossing afterwards, wherein just face to be observed includes coating material
Front surface and side；It is ready after two matrix of samples are mounted on stretching-machine, and to entire compact tensile machine into
Sample bin is sent into scanning electron microscope after row dust removal process.Sample bin side has chip to contact with scanning electron microscope
Connection is, it can be achieved that control of the computer system to compact tensile machine；Rate of extension, tensile load etc. are set on the computer systems
Then parameter adjusts the camera lens of scanning electron microscope to suitable amplification factor, to the defocused ginseng found in region to be observed
Examination point, that is, speckle.It is then turned on scanning electron microscope kinescope recording function, can be started to coating material during stretching
Its front surface and side are observed, and the rate of extension of stretching-machine is adjusted during stretching, and can suspend stretching at any time
Then machine carries out high magnification numbe photographing operation using scanning electron microscope, scan image is as shown in Fig. 2, so as to realize
Coating material is observed in stretching or compression process from its front surface and side respectively, to painting in stretching or compression process
Layer material carries out multi-faceted observation, facilitates position, the direction of finding crack initiation, convenient for observing the expansion process of crackle, such as
In Fig. 2 shown in (a)-(e), the micromechanism of damage of coating material is preferably inferred.
In short, the method for the detection coating material damage of the embodiment of the present application, by scanning electron microscope from micro-
The tension crack process for observing coating material on scale is seen, coating material can be showed more fully hereinafter under the conditions of extension test
Damage and dehiscence process, also, using scanning electron microscope high magnification numbe observe coating material localized micro tissue regions, be
Infer the mechanism and crack propagation path provides basis and stretching-machine and coating material is directly put that coating material crackle generates
Set in sample bin, thus can carry out in situ, image scanning in real time, avoid secondary damage and be more conducive to understand apply
Damage situation of change of the layer material in stretching or compression process, also, during stretching, it is adjusted and is stretched according to draw stage
The rate of extension of machine in a disguised form extends the time that coating material generates fission, is easy to capture coating material especially brittleness material
The detailed fission process of material；And the matrix of samples of both designs different structure, coating material are sprayed on different examinations respectively
On sample matrix, front surface and side of the speckle in coating material are marked respectively, using as scanning surface, to stretch or compressed
Cheng, can be from the variation of the stress of multiple azimuthal observation coating materials, it can observe the surface and interface of coating material
Crack initiation and propagation situation and interior change situation, convenient for more accurately inferring coating material micromechanism of damage.
The system for stretching fission according to the detection coating material of the application second aspect embodiment is described with reference to the accompanying drawings.
Fig. 3 is the block diagram that the system of fission is stretched according to the detection coating material of one embodiment of the application, such as Fig. 3 institute
Show, the system 100 of the detection coating material damage of the embodiment of the present application includes stretching-machine 10, scanning electron microscope 20, processing
Device 30.
Wherein, stretching-machine 10 is used for coating material applied force to stretch or compress coating material；Coating material and stretching
Machine 10 is placed in the sample bin of scanning electron microscope 20, scanning electron microscope 20 for acquire coating material stretch or
Scan image in compression process；Processing unit 30 is used to estimate the draw stage of the coating material, according to the stretching rank
Section adjusts the rate of extension of the stretching-machine, and is handled by loading by means of digital image correlation method scan image, after processing
Scan image analysis coating material damage variation.
Specifically, scanning electron microscope 20 may include power supply and control system, electron-optical system, signal collection at
As system, sample bin, vacuum chamber etc..After coating material prepares, stretching-machine 10 and coating material are placed on sample bin, and will
Sample bin is put into vacuum chamber, and power supply and control system, electron-optical system, signal collection imaging system and sample bin are all located at very
In empty room.When being observed, vacuum need to be extracted to vacuum chamber by vacuum pump system, and control stretching-machine 10 to coating material
It is stretched or is compressed, the rate of extension of stretching-machine 10 can be adjusted based on different draw stages during stretching, and lead to
It crosses electron-optical system and the acquisition of signal collection imaging system stretches or the scan image of compression process coating material, and then locate
The reason such as computer system of device 30 handles scan image, and then can analyze coating according to treated scan image
The micromechanism of damage of material.
The system 100 of fission is stretched according to the detection coating material of the embodiment of the present application, wherein coating material and stretching-machine
10 are placed in the sample bin of scanning electron microscope 20, by scanning electron microscope 20 can stretching to coating material or
Compression process carries out original position, observes in real time, realizes the pattern variation from micro-level observation coating material, also, according to drawing
The rate of extension of stage adjusting stretching-machine is stretched, the crackle that can be more easier to capture coating material especially fragile material is sprouted
Raw, extension detailed process, and, carrying out in-situ observation can be to avoid the secondary damage to coating material, so that observed result
It is more accurate.
In some embodiments, draw stage may include fission safe period and fission generation phase, and fission safe period is for example
Initial stage, the germinating stage and the stage of producing fracture that the fission generation phase for example cracks.In order to be more conducive to detect
To the fission process of coating material, reduce the rate of extension of stretching-machine in the fission generation phase.For example, the rate of extension of stretching-machine can
Adjustable range is within the scope of 0.036mm/min-1mm/min, by slowing down rate of extension, it can be achieved that coating material such as brittleness is made pottery
" delay " Tensile Fracture Process of porcelain coating, so as to realize that observation coating material slowly cracks to the detailed mistake for disconnecting peeling
Journey.
In further embodiments, matrix of samples elasticity modulus of materials selected by certain coating materials is larger, it is more difficult to become
Shape, if all being stretched for the overall process of detection with slower rate of extension, detection process will become tediously long, and
For the fission safe period before coating material cracking, the needs for the observation that is not delayed are therefore, biggish for certain elasticity modulus
Matrix, can correspond to fission safe period and different rates of extension is arranged in the generation phase of fissioning, thus, it is possible to improve stretching detection
Efficiency.Specifically, the elasticity modulus of the matrix of samples where coating material is greater than default modulus threshold value, and presetting modulus threshold value can
To be set according to experiment statistics, coating material is stretched with first rate in fission safe period control stretching-machine；It is fissioning
Generation phase control stretching-machine stretches coating material with the second rate, wherein the second rate is less than first rate.For example,
Fission safe period control stretching-machine with the rate of extension of 0.8,0.6,0.4,0.2 or 0.1 (mm/min) come to coating material into
Row stretches, when that will crack, reduce stretching-machine rate of extension for example control stretching-machine with 0.08,0.06,0.04 or
The rate of extension of 0.03 (mm/min) is equivalent to stretch to coating material and has elongated the mistake that coating material generates fission
Journey, so as to more easily capture the detailed fission process of coating material, conducive to the subsequent analysis for stretching fission mechanism
And deduction.
Further, due to the limitation of coating material thickness, coating material can only be often observed during actual observation
The situation of change for expecting front surface can not observe the variation of coating material side and material internal generation.Thus, the application's
In embodiment, coating material is sprayed on respectively in two matrix of samples, wherein the upper table of the coating material in a matrix of samples
Face is as scanning surface, and the side of the coating material in another matrix of samples is as scanning surface.Scanning electron microscope 20 is being swept
Tracing as when be specifically used for, acquire stretching or compression process coating material upper surface scan image, and, acquisition drawing
It stretches or the scan image of compression process coating material side.Thus can be by scanning electron microscope 20 under the conditions of microcosmic
The surface of coating material, the crack initiation and propagation situation at interface are directly observed, and then can more correctly infer coating material
Damage mechanisms.
In embodiment, matrix of samples is removably disposed on stretching-machine, may be implemented stretching to coating material or
Compression, can also save space in sample bin.It is of course also possible to which the bracket for individually having fixture is arranged, matrix of samples can
Clamping is stretched or is compressed to matrix of samples on the bracket, and through stretching-machine, and then realizes the stretching to coating material
Or compression.
Besides, for the speckle that the image for enabling scanning electron microscope to shoot clearly tells body surface, the application
In embodiment, as shown in figure 4, the system 100 that the detection coating material of the embodiment of the present application damages further includes labelling apparatus 40, mark
Remember that device 40 is used for before coating material is placed on sample bin, by nano-imprint process such as electron beam lithography or
Particles self assemble technology marks speckle on the scanning surface of coating material, that is, when as loading by means of digital image correlation method processing
Region to be measured, and then processing unit 30 handles scan image using loading by means of digital image correlation method to obtain coating material surface
With the strain size and its change procedure of side, the micromechanism of damage of reasoning coating material.
In short, the embodiment of the present application detection coating material damage system 100, using scanning electron microscope 20 from
The tension crack process of coating material is observed on micro-scale, and observes coating material using the high magnification numbe of scanning electron microscope 20
Expect localized micro tissue regions, and adjust the rate of extension of stretching-machine during stretching, capture material can be more easier and existed
Damage and dehiscence process under the conditions of stretching or compression verification, to understand the mechanism and crackle expansion of coating material crackle generation
Path is opened up, and marks front surface and the side of coating material by nano-imprint process, so as to multi-faceted observation coating material
The strain variation situation of material provides more accurate data for damage mechanism analysis and supports, provides damage mechanism analysis result
Accuracy.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " illustrative examples ",
The description of " example ", " specific example " or " some examples " etc. means specific features described in conjunction with this embodiment or example, knot
Structure, material or feature are included at least one embodiment or example of the invention.In the present specification, to above-mentioned term
Schematic representation may not refer to the same embodiment or example.
Although an embodiment of the present invention has been shown and described, it will be understood by those skilled in the art that: not
A variety of change, modification, replacement and modification can be carried out to these embodiments in the case where being detached from the principle of the present invention and objective, this
The range of invention is defined by the claims and their equivalents.
Claims (10)
1. a kind of method that detection coating material stretches fission, which is characterized in that coating material and stretching-machine are placed on scanning electricity
In the microscopical sample bin of son, which comprises
Estimate the draw stage of the coating material；
The rate of extension of the stretching-machine is adjusted according to the draw stage；
Acquire the scan image of the coating material during stretching；And
The scan image is handled by loading by means of digital image correlation method, and the scan image analyzes institute according to treated
State the stretching fission of coating material.
2. the method that detection coating material according to claim 1 stretches fission, which is characterized in that the draw stage packet
Include fission safe period and fission generation phase, the rate of extension that the stretching-machine is adjusted according to the draw stage, comprising:
The fission generation phase reduces the rate of extension of the stretching-machine.
3. the method that detection coating material according to claim 1 stretches fission, which is characterized in that the draw stage packet
Fission safe period and fission generation phase are included, the elasticity modulus of the matrix of samples where the coating material is greater than default modulus threshold
Value, the rate of extension that the stretching-machine is adjusted according to the draw stage, comprising:
The stretching-machine is controlled in the fission safe period to stretch the coating material with first rate；
It controls the stretching-machine in the fission generation phase to stretch the coating material with the second rate, wherein described
Second rate is less than the first rate.
4. the method that detection coating material according to claim 1 stretches fission, which is characterized in that the coating material point
Be not sprayed in two matrix of samples, wherein the upper surface of the coating material in a matrix of samples as scanning surface, another
The side of coating material in matrix of samples is as scanning surface, the scanning figure of the acquisition coating material during stretching
Picture, comprising:
The scan image of the coating material upper surface described in stretching or compression process is acquired, and, acquisition is during stretching
The scan image of the coating material side.
5. the method that detection coating material according to claim 1 stretches fission, which is characterized in that by the coating material
Material is placed on before the sample bin, the method also includes:
Speckle is marked on the scanning surface of the coating material by nano-imprint process.
6. a kind of system that detection coating material stretches fission, which is characterized in that the system comprises:
Stretching-machine, for stretching the coating material to coating material applied force；
Scanning electron microscope, the coating material and the stretching-machine are placed on the sample bin of the scanning electron microscope
In, the scanning electron microscope is for acquiring scan image of the coating material in stretching or compression process；
Processing unit adjusts the stretching-machine according to the draw stage for estimating the draw stage of the coating material
Rate of extension, and the scan image is handled by loading by means of digital image correlation method, the scan image according to treated
Analyze the stretching fission of the coating material.
7. the system that detection coating material according to claim 6 stretches fission, which is characterized in that the draw stage packet
Fission safe period and fission generation phase are included, the processing unit is in the stretching speed for adjusting the stretching-machine according to the draw stage
It is specifically used for when rate, reduces the rate of extension of the stretching-machine in the fission generation phase.
8. the system that detection coating material according to claim 6 stretches fission, which is characterized in that the draw stage packet
Fission safe period and fission generation phase are included, the elasticity modulus of the matrix of samples where the coating material is greater than default modulus threshold
Value, the processing unit are specifically used for when adjusting the rate of extension of the stretching-machine according to the draw stage, split described
Become the safe period control stretching-machine to stretch the coating material with first rate, and, in the fission generation phase
It controls the stretching-machine to stretch the coating material with the second rate, wherein second rate is less than described first
Rate.
9. the system that detection coating material according to claim 6 stretches fission, which is characterized in that
The coating material is sprayed on respectively in two matrix of samples, wherein the upper table of the coating material in a matrix of samples
Face is as scanning surface, and the side of the coating material in another matrix of samples is as scanning surface；
The scanning electron microscope is specifically used in scan image, acquires the coating material upper surface during stretching
Scan image, and, the scan image of the acquisition coating material side during stretching.
10. the system that detection coating material according to claim 6 stretches fission, which is characterized in that the system is also wrapped
Labelling apparatus is included, the labelling apparatus is used for before the coating material is placed on the sample bin, passes through nano impression
Technique marks speckle on the scanning surface of the coating material.
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