CN109406280A - A kind of quantitative detecting method of coating material impression fracture toughness - Google Patents
A kind of quantitative detecting method of coating material impression fracture toughness Download PDFInfo
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- CN109406280A CN109406280A CN201811478755.7A CN201811478755A CN109406280A CN 109406280 A CN109406280 A CN 109406280A CN 201811478755 A CN201811478755 A CN 201811478755A CN 109406280 A CN109406280 A CN 109406280A
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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
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/40—Investigating hardness or rebound hardness
- G01N3/42—Investigating hardness or rebound hardness by performing impressions under a steady load by indentors, e.g. sphere, pyramid
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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
- G01N2203/0019—Compressive
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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
- G01N2203/0067—Fracture or rupture
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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
- G01N2203/0076—Hardness, compressibility or resistance to crushing
- G01N2203/0078—Hardness, compressibility or resistance to crushing using indentation
- G01N2203/008—Residual indentation measurement
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Abstract
The invention discloses a kind of quantitative detecting method of coating material impression fracture toughness, includes the following steps: to apply pressure P 1), using pressure head to coating surface, generate impression and crackle；2) coating surface Indentation Modulus E, identation hardness H and crack length c, are determined；3), Indentation Modulus E, identation hardness H, crack length c and pressure P are substituted intoObtain material impression fracture toughness Kc.The quantitative evaluation method of coating material fracture toughness can be established according to Indentation Cracking feature, and basic data is provided and is supported for the design of coating mechanical property and environmental suitability evaluation.
Description
Technical field
The present invention is to belong to material mechanical performance test and evaluation technical field, specially a kind of coating material impression fracture
The quantitative detecting method of toughness.
Background technique
To meet specific environmental protection and functional requirement in modern chain drive and electronic product, such as solar heat protection, conduction, absolutely
Edge, anti-corrosion, stealthy etc. are coated with laminated coating or thin-film material in a manner of being bonded, deposit, spray etc. on critical component surface,
These coating/substrate material systems may be subjected to high temperature for a long time in use, vibration, temperature such as follow at environment-load joint
Destruction, and coating and base material mechanical property and it is hot in terms of there may be biggish difference, be easy
Biggish stress concentration phenomenon is generated at internal system fault location or more material interfaces, coating failure and failure mode mainly show
For interface debonding, unsticking and spallation etc..Coating preferable for relatively thin and binding performance or thin-film material, can be used for analyzing and surveying
It tries coating layer thickness and characteristic size is very limited, the experimental methods such as traditional stretching, shearing, bubbling are in effective load, interface point
Layer, bond strength evaluation etc. have become no longer to be applicable in there are problems and deficiency；In addition, for simulating Re-Li Lian
The high-temperature testing method of destructive process is closed, although amendment bending method can inhibit brittle coating that the dissipation such as spallation, buckling deformation occurs
Behavior, but the high temperature bearing capacity deficiency for making glue-line used in sample limits the raising of experimental temperature.In comparison, it receives
Rice creasing method is more likely to be appropriate for the mechanical property and fracture toughness of test microsize and flexible coating material, and loads temperature
Degree is not limited substantially by glue-line Applicable temperature range.
The fracture toughness that accurately measure coating material layering or cracking, generally should at least meet two conditions: (1) energy
Enough mechanical models for establishing reasonable reflection coating and peeling off from the substrate or cracking；(2) it accurately can measure and calculate reflection circle
The mechanics parameter of face binding performance.There are mainly two types of viewpoints at present: first is that stress viewpoint, generallys use linear elastic fracture mechanics model
The stress intensity factor on farmland characterizes；Second is that energy needed for unit area when energetics viewpoint, i.e. coating are peeled off from substrate
Size is generally characterized using parameters such as fracture toughness, energy release rates, indicates that material is resisted in the case where containing pre- crackle
The ability that the crackle further expands.Caused by nanometer is pressed into test process for crackle, usual indentation feature size is all
Very small (the following magnitude of micron), and the fracture toughness analytic method based on energetics viewpoint is primarily adapted for use in block materials macroscopic view
The expansion process of size crackle, can continue to use under impression micro-scale is still worth discussion, and impression is split after pressure head unloading
Line does not continue to generally extend.
Summary of the invention
In view of this, it is an object of the invention to propose a kind of quantitative detecting method of coating material impression fracture toughness,
Realize the quantitative assessment to coating material fracture toughness.
Based on a kind of above-mentioned purpose quantitative detecting method of coating material impression fracture toughness provided by the invention, including such as
Lower step: 1), using pressure head to coating surface apply pressure P, generate impression and crackle；2) coating surface Indentation Modulus, is determined
E, identation hardness H and crack length c；3), by Indentation Modulus E, identation hardness H, crack length c and pressure P
It substitutes intoObtain material impression fracture toughness Kc。
Further,ByWithSimultaneous obtains
Out, wherein λr(φ) is a characteristic unrelated with pressure head, ε=λr(φ)(cotα)2/3。
Further, the pressure P is the load of impression.
Further, when use pressure head applies pressure P to coating surface straight down, when generating impression and crackle, pressure head
Vertex of a cone half-angle be α, impression contact characteristic size a, the characteristic size b radially extended, depth of cup d, central facial cleft
Line size h and surface radial cracking length c；The center load that relatively coincide is formed after center/radial cracking sufficiently extends
Penny-shaped crack when, meet relational expression P/h3/2=constant, at this point, corresponding stress strength factor K can be determined by following formula,
That is:
χ indicates a constant, related with pressure head/sample material system；
When crackle system reaches Leveraging Extensions, the stress strength factor K that external applied load generates is equal to fracture toughness Kc, have:
K=Ke+Kr=Kc (2)
K in formulaeIndicate the elastic part of stress intensity factor, KrIndicate Residual stress intensity factors；
During pressure head loads and unloads, formula (2) variation are as follows:
P in formulamIndicate impression maximum load；
In crack propagation, when crack front keeps semi-circular shape, crackle equilibrium radius meets:
Median cracks:
Radial cracking:
Further, it is assumed that the characteristic area that the characteristic radius by expected pressure head contact position is b removes, and obtains one without outer
Add the elastic half-space of stress；The presence of impression can make material remove part generation plastic deformation, contact radius, compression distance
Respectively a and d can absorb impression generation in the case where material volume is constant by the volume expansion in this feature region
Irrecoverable strain, it is assumed that δ V indicates impression volume, and V indicates characteristic area, then configuration strain may be expressed as:
Along one uniformly distributed hydrostatic pressure p of removal portion of external boundary and radial applicationb:
κ indicates bulk modulus in formula, and E and ν respectively indicate the Young's modulus and Poisson's ratio of measured material, wherein E=3 (1-
ν) κ, i.e. identation hardness, may be expressed as:
α in formula0For pressure head geometric constant,
Again the material part of compression is moved back in original hole, and restores the cohesiveness of its contact interface, then allowed
System freely relaxes, in this way, plastic zone will cause to generate outside effective residual load P on crack surfacerIf pbExpand in crackle
It is remained unchanged in exhibition, then Pr=ζ pbb2 (12)
Here, ζ indicates an integral constant, and under conditions of crackle sufficiently extends, i.e. h is much larger than b, PrIt can be reduced to a collection
Midpoint power, when meeting penny-shaped crack form, stress intensity factor caused by residual load be may be expressed as:
Here, f (φ) is the angle function for indicating free surface effect, and for situation involved in this work, formula (1) becomes
For
By formula (10) substitute into formula (12), and with formula (13) and formula (14) simultaneous, can obtain:
For infinitely great isotropism elastic-plastic matrix
Wherein E is Young's modulus, and m ≈ 1/2 can obtain above formula substitution formula (15):
Further, willSubstitution formula (8) can must split sharp critical stress intensity factors
Expression formula, it may be assumed that
Wherein, ε=λr(φ)(cotα)2/3。
Further, the pressure head is Bo Shi (Berkovich) triangular pyramid diamond penetrator.
Further, ε is the geometric corrections factor unrelated with material, it depends on the radial cracking form that impression is formed,
For Bo Shi (Berkovich) triangular pyramid diamond penetrator, ε=1.034.
Having the beneficial effect that for the quantitative detecting method of coating material impression fracture toughness of the present invention need to only determine this test
Under the conditions of coating surface impression E, H value and crack length c, formula (18) can be substituted into and calculate its fracture toughness；
1) experimental methods such as tradition stretching, shearing, bubbling are overcome in the preferable coating of relatively thin and binding performance (or film)
The problem of in terms of fracture characteristics test and quantitative assessment and deficiency, improve coating and carry out fracture under Simulated Service hot environment
A possibility that toughness quantitative assessment；
2) a kind of stress intensity factor analytic method for being suitable for the estimation of coating nano impress fracture toughness is provided, without
Whether the information such as concern coat system crack initiation site, extensions path and extension length meet the expected requirements.
Detailed description of the invention
Fig. 1 is coating surface indentation method schematic diagram described in the specific embodiment of the invention.
Bullet-plasticity configuration when Fig. 2 is full and down described in the specific embodiment of the invention.
Residual plastic load when Fig. 3 is complete unloading described in the specific embodiment of the invention.
Fig. 4 is radial cracking described in the specific embodiment of the invention.
Wherein: 101- Bo Shi (Berkovich) triangular pyramid diamond penetrator
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, and reference
Attached drawing, the present invention is described in more detail.
As shown in Figures 1 to 4, a kind of quantitative detecting method of coating material impression fracture toughness, includes the following steps:
1) pressure P, is applied to coating surface using pressure head, generates impression and crackle；2), determine that coating surface Indentation Modulus E, impression are hard
Spend H and crack length c；3), Indentation Modulus E, identation hardness H, crack length c and pressure P are substituted intoObtain material impression fracture toughness Kc。
ByWithSimultaneous obtains, wherein λr
(φ) is a characteristic unrelated with pressure head, ε=λr(φ)(cotα)2/3。
After preparing coating sample according to actual demand, coating surface development is received using special-purpose nanometer impression test system
Rice micro-indentation test, as shown in Figure 1, and using Bo Shi triangular pyramid diamond penetrator 101 generate indentation crack as research object, to material
Expect impression fracture toughness KcAnalytic formula carry out theory deduction it is as follows:
Fig. 2 schematically illustrates the impression deformation that Bo Shi (Berkovich) triangular pyramid pressure head 101 is formed on coating material surface
And crack pattern, when use pressure head applies pressure P to coating surface straight down, when generating impression and crackle, the vertex of a cone of pressure head
Half-angle is α, impression contact characteristic size a, the characteristic size b radially extended, depth of cup d, median plane crack size h
And surface radial cracking length c；Marshall and Lawn is had found by Germicidal efficacy, when center/radial cracking sufficiently extends
When forming the penny-shaped crack for the center load that relatively coincide later, meet relational expression P/h3/2=constant, at this point, corresponding stress is strong
Degree factor K can be determined by following formula, it may be assumed that
χ indicates a constant, related with pressure head/sample material system；
When crackle system reaches Leveraging Extensions, the stress strength factor K that external applied load generates is equal to fracture toughness Kc, for
Elastic-plastic system shown in Fig. 2, has:
K=Ke+Kr=Kc (2)
K in formulaeIndicate the elastic part of stress intensity factor, KrIndicate Residual stress intensity factors；
During pressure head loads and unloads, formula (2) variation are as follows:
P in formulamIndicate impression maximum load；
In crack propagation, when crack front keeps semi-circular shape, crackle equilibrium radius meets:
Median cracks:
Radial cracking:
Bullet-plastic problems of Fig. 2 can be analyzed to the superposition of elastic problem and residual plastic problem, wherein in elastic situation
Under, KcComponent of elasticity reach its maximum value in maximum load, when unloading, then restores completely；Residual plastic field by pressure head around
The deformation mismatch stress of material generates, KcResidual components reach its maximum value in maximum load, pressure head is kept not after withdrawing from
Become.
In the event of a break, crack propagation process is usually irreversible, only works as hR> hMWhen, formula (7) can table
Show that crack propagation is in energy balance state, for Median cracks,Meeting above-mentioned inequality must be in loading procedure
The middle propagation behavior for inhibiting crackle, this is nearly impossible in actual test；For radial cracking,It is above-mentioned not
Equation can meet automatically.
Therefore, Median cracks reach its maximum length during loading, and radial cracking then continues extension until completely
Unloading, the research object of this part work are the radial cracking after impression, therefore, when calculating its fracture toughness, component of elasticity
Influence it is negligible.In this way, formula (2) becomes:
Next, need to only determine χrIt can obtain KcAnalytical expression.For the indentation surface after unloading, such as Fig. 2 institute
Show, and in particular to following analytical procedure:
1) assume that the characteristic radius by expected pressure head contact position is that the characteristic area of b removes, obtain one without applied stress
Elastic half-space；
2) presence of impression can make material remove part generate plastic deformation, contact radius, compression distance be respectively a and
D can absorb irrecoverable the answering of impression generation in the case where material volume is constant by the volume expansion in this feature region
Become, it is assumed that δ V indicates impression volume, and V indicates characteristic area, then configuration strain may be expressed as:
3) for by material removal be partially elastically restored to its primitive character radius b, can along remove portion of external boundary and
It is radial to apply a uniformly distributed hydrostatic pressure
pb:
κ indicates bulk modulus in formula, and E and ν respectively indicate the Young's modulus and Poisson's ratio of measured material, wherein E=3 (1-
ν) κ, here, pbThe pressure p being different from pressure heada, i.e. identation hardness may be expressed as:
α in formula0For pressure head geometric constant,
4) material part of compression is moved back in original hole again, and restores the cohesiveness of its contact interface, then
System is allowed freely to relax, in this way, plastic zone will cause to generate outside effective residual load P on crack surfacerIf pbIn crackle
It is remained unchanged in extension, then PrSize can be by pbHorizontal component along the zone crack Line Integral obtain, i.e.,
Pr=ζ pbb2 (12)
Here, ζ indicates an integral constant,
Under conditions of crackle sufficiently extends, i.e. h is much larger than b, PrIt can be reduced to a centrostigma power, when meeting penny-shaped crack
When form, stress intensity factor caused by residual load be may be expressed as:
Here, f (φ) is the angle function for indicating free surface effect,
For situation involved in this work, formula (1) becomes:
By formula (10) substitute into formula (12), and with formula (13) and formula (14) simultaneous, can obtain:
For infinitely great isotropism elastic-plastic matrix, had according to the theory analysis of Lawn:
Wherein E is Young's modulus, and m ≈ 1/2 can obtain above formula substitution formula (15):
Here, λr(φ) is a characteristic unrelated with pressure head/sample system.
It willSubstitution formula (8) can must split the expression formula of sharp critical stress intensity factors,
That is:
Wherein, ε=λr(φ)(cotα)2/3, ε is the geometric corrections factor unrelated with material here, it depends on impression shape
At radial cracking form, for 101 triangular pyramid diamond penetrator of Bo Shi (Berkovich), ε=1.034.
It so only need to determine coating surface impression E, H value and crack length c under this test condition, formula can be substituted into
(18) its fracture toughness is calculated.Coating surface Indentation Modulus and hardness can be obtained by analytical Calculation or access reference books, be split
Line characteristic length is determined by impression microscopic appearance.
For the preferable coating of relatively thin and binding performance (or film) material, the impression Evaluation of Fracture Toughness method of foundation can have
Effect solves traditional means of experiment, and there are problems and deficiency in terms of effective load, interface debonding, bond strength；Root
The characteristics of according to coating (or film) material nano impression test, has developed from stress intensity factor angle and has been suitable for quantitative assessment painting
The analytic method of layer surface impression fracture toughness.
It is disconnected in the preferable coating of relatively thin and binding performance (or film) to overcome the experimental methods such as tradition stretching, shearing, bubbling
The problem of splitting in terms of characteristic test and quantitative assessment with it is insufficient, improve coating carries out under Simulated Service hot environment be broken it is tough
A possibility that property quantitative assessment；Provide a kind of stress intensity factor parsing for being suitable for the estimation of coating nano impress fracture toughness
Whether method meets the expected requirements without information such as concern coat system crack initiation site, extensions path and extension lengths.
The embodiment of the present invention be intended to cover fall into all such replacements within the broad range of appended claims,
Modifications and variations.Therefore, all within the spirits and principles of the present invention, any omission, modification, equivalent replacement, the improvement made
Deng should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of quantitative detecting method of coating material impression fracture toughness, characterized by the following steps:
1) pressure, is applied to coating surface using pressure head and generates pressure P, impression and crackle；
2) coating surface Indentation Modulus E, identation hardness H and crack length c, are determined；
3), Indentation Modulus E, identation hardness H, crack length c and pressure P are substituted intoObtain material
Impression fracture toughness Kc。
2. a kind of quantitative detecting method of coating material impression fracture toughness according to claim 1, which is characterized in that institute
State material impression fracture toughnessByWithIt calculates
Out, wherein λr(φ) is a characteristic unrelated with pressure head, ε=λr(φ)(cotα)2/3。
3. a kind of quantitative detecting method of coating material impression fracture toughness according to claim 1, which is characterized in that institute
State the load that pressure is impression.
4. a kind of quantitative detecting method of coating material impression fracture toughness according to claim 1, which is characterized in that when
When applying pressure generation pressure P, impression and crackle to coating surface straight down using pressure head, the vertex of a cone half-angle of pressure head is α, pressure
Trace contact characteristic size a, the characteristic size b radially extended, depth of cup d, median plane crack size h and surface diameter
To crack length c；When forming the penny-shaped crack for the center load that relatively coincide after center/radial cracking sufficiently extends, meet
Relational expression P/h3/2=constant, at this point, corresponding stress strength factor K can be determined by following formula, it may be assumed that
χ indicates a constant, related with pressure head/sample material system；
When crackle system reaches Leveraging Extensions, the stress strength factor K that external applied load generates is equal to fracture toughness Kc, have:
K=Ke+Kr=Kc (2)
K in formulaeIndicate the elastic part of stress intensity factor, KrIndicate Residual stress intensity factors；
During pressure head loads and unloads, formula (2) variation are as follows:
P in formulamIndicate impression maximum load；
In crack propagation, when crack front keeps semi-circular shape, crackle equilibrium radius meets:
Median cracks:
Radial cracking:
5. a kind of quantitative detecting method of coating material impression fracture toughness according to claim 4, which is characterized in that false
If the characteristic area that the characteristic radius by expected pressure head contact position is b removes, an elastic half-space without applied stress is obtained；
The presence of impression can make material remove part generation plastic deformation, and contact radius, compression distance are respectively a and d, in material bodies
In the case that product is constant, the irrecoverable strain of impression generation can be absorbed by the volume expansion in this feature region, it is assumed that δ V
Indicate impression volume, V indicates characteristic area, then configuration strain may be expressed as:
Along one uniformly distributed hydrostatic pressure p of removal portion of external boundary and radial applicationb:
κ indicates bulk modulus in formula, and E and ν respectively indicate the Young's modulus and Poisson's ratio of measured material, wherein E=3 (1- ν) κ,
That is identation hardness may be expressed as:
α in formula0For pressure head geometric constant,
Again the material part of compression is moved back in original hole, and restores the cohesiveness of its contact interface, then allow system
It freely relaxes, in this way, plastic zone will cause to generate outside effective residual load P on crack surfacerIf pbIn crack propagation
It remains unchanged, then Pr=ζ pbb2(12)
Here, ζ indicates an integral constant, and under conditions of crackle sufficiently extends, i.e. h is much larger than b, PrIt can be reduced to a centrostigma
Power, when meeting penny-shaped crack form, stress intensity factor caused by residual load be may be expressed as:
Here, f (φ) is the angle function for indicating free surface effect, and for situation involved in this work, formula (1) becomes
By formula (10) substitute into formula (12), and with formula (13) and formula (14) simultaneous, can obtain:
For infinitely great isotropism elastic-plastic matrix
Wherein E is Young's modulus, and m ≈ 1/2 can obtain above formula substitution formula (15):
6. a kind of quantitative detecting method of coating material impression fracture toughness according to claim 5, which is characterized in that willSubstitution formula (8) can must split the expression formula of sharp critical stress intensity factors, it may be assumed that
Wherein, ε=λr(φ)(cotα)2/3。
7. a kind of quantitative detecting method of coating material impression fracture toughness according to claim 1, which is characterized in that institute
Stating pressure head is Bo Shi Berkovich triangular pyramid diamond penetrator.
8. a kind of quantitative detecting method of coating material impression fracture toughness according to claim 7, which is characterized in that ε
For the geometric corrections factor unrelated with material, it depends on the radial cracking form that impression is formed, for Bo Shi Berkovich tri-
Pyramid diamond penetrator, ε=1.034.
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