CN110186845A - Matrix-oxidation film film substrate bond strength detection method in a kind of oxide alloy material - Google Patents
Matrix-oxidation film film substrate bond strength detection method in a kind of oxide alloy material Download PDFInfo
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- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 83
- 239000000956 alloy Substances 0.000 title claims abstract description 61
- 239000000758 substrate Substances 0.000 title claims abstract description 38
- 238000001514 detection method Methods 0.000 title claims abstract description 23
- 238000012360 testing method Methods 0.000 claims abstract description 67
- 230000003647 oxidation Effects 0.000 claims abstract description 61
- 238000000034 method Methods 0.000 claims description 18
- 230000001419 dependent effect Effects 0.000 claims description 12
- 230000006866 deterioration Effects 0.000 claims description 7
- 208000037656 Respiratory Sounds Diseases 0.000 claims description 4
- 238000005259 measurement Methods 0.000 abstract description 3
- 229910045601 alloy Inorganic materials 0.000 description 29
- 239000000463 material Substances 0.000 description 5
- 238000012546 transfer Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 125000004122 cyclic group Chemical group 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- 229910000967 As alloy Inorganic materials 0.000 description 1
- 229910018487 Ni—Cr Inorganic materials 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910002064 alloy oxide Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 210000004209 hair Anatomy 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N19/00—Investigating materials by mechanical methods
- G01N19/04—Measuring adhesive force between materials, e.g. of sealing tape, of coating
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Abstract
The present invention provides matrix-oxidation film film substrate bond strength detection methods in a kind of oxide alloy material, are related to mechanics parameter detection method.Detection method of the invention has fully considered that oxidation film is in the non-uniform problem of tension test when institute tension stress in oxide alloy material, in the calculating formula of the film substrate bond strength, the crack spacing for stretching sample is introduced, the accuracy of measurement of the film substrate bond strength of final oxide alloy material is improved.
Description
Technical field
The present invention relates to matrix-oxidation film film bases in mechanics parameter detection method more particularly to a kind of oxide alloy material
The detection method of bond strength.
Background technique
Steam generator heat-transfer pipe is one of the critical component in nuclear power unit, current domestic and international steam generator heat-transfer pipe
Material be Fe-Ni-Cr based heat resistant alloy or nickel-base alloy manufacture, due to such alloy have higher creep/breaking strength and
Resistance to high temperature corrosion performance is widely used in manufacture steam generator heat-transfer pipe.Material during one's term of military service, oxidation film will appear brokenly
Phenomena such as splitting, peeling off is unable to effective protection matrix, not can guarantee the long-term safety operation of nuclear power unit.Therefore, it accurately detects
The binding force of heat transfer tubing surface film oxide is the premise of nuclear power unit long-term safety operation.In oxidation film detection field,
There is many institutions conducts related work.Chinese patent " 201610948710.6 ", " 201620768876.5 " are related to oxidation film
The detection of thickness.Chinese patent " 201610901180.X ", " 201220699967.X ", " 201210549515.8 " are related to aoxidizing
Continuity detection of film etc..Chinese patent " 201010600584.8 " provides a kind of hot rolled strip surface film oxide adhesive force inspection
Survey method, complex process and the oxidation film adhesive force detection for being not suitable for nuclear power heat transfer tubing.In addition to this, then independent of oxygen
Change the patent application of binding force of membrane detection.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of matrix in oxide alloy material-oxidation film film base junctions to close by force
The detection method of degree.Detection method provided by the invention is simple, easy to operate, and the accuracy of the film substrate bond strength obtained is high.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides matrix-oxidation film film substrate bond strength detection methods in a kind of oxide alloy material, including
Following steps:
Tensile sample is made in oxide alloy material, measures the elasticity modulus of oxidation film in the tensile sample；
Tension test is carried out to the tensile sample, when oxidation film is fallen off, obtains stretching sample, obtains the drawing
Stretch the dependent variable that sample cracks；
Thickness, the crack spacing for measuring the oxidation film for stretching sample, obtain the oxide alloy material using formula (1)
Matrix-oxidation film film substrate bond strength in material:
Wherein, τ is film substrate bond strength, MPa；δ is the oxide thickness for stretching sample, μm；λ is the crackle for stretching sample
Spacing, μm；E is the elasticity modulus of oxidation film, GPa；εmaxThe dependent variable cracked for tensile sample.
Preferably, the detailed process of the tension test are as follows:
It takes two tensile samples spare, rough tension test first is carried out to one of tensile sample, then to other one
A tensile sample carries out accurate tension test, obtains stretching sample；
The rough and careless tension test process are as follows: the tensile sample is subjected to stretching examination with 1~2%/min of rate of extension
It tests, makes the oxide layer deterioration on tensile sample, the deflection for measuring tensile sample at this time is n；
The accurate tension test process are as follows: the tensile sample is subjected to stretching examination with 1~2%/min of rate of extension
It tests, after deflection reaches m；Rate of extension is adjusted to 0.1~0.5%/min and continues tension test, until stretching examination
Oxidation film on sample starts shedding off, and terminates tension test, obtains stretching sample；
The difference of the n-m is 2~3%.
The present invention provides matrix-oxidation film film substrate bond strength detection method, this hairs in a kind of oxide alloy material
Bright detection method fully considered in oxide alloy material oxidation film in the non-uniform problem of tension test when institute tension stress,
In the calculating of the film substrate bond strength, the crack spacing for stretching sample is introduced, final oxide alloy material is improved
The accuracy of measurement of film substrate bond strength.
Further, the present invention optimizes by the process of control tension test and stretches the ginseng such as thickness of sample, crack spacing
Number, further improves the accuracy of film substrate bond strength.
Detailed description of the invention
Fig. 1 is the schematic shapes of tensile sample；
Fig. 2 is the force analysis figure for stretching oxidation film in sample；
Fig. 3 is tensile sample in embodiment 1700Stretching sample stretching pattern；
Fig. 4 is tensile sample in embodiment 1700-5Stretching sample shape appearance figure；
Fig. 5 is tensile sample in embodiment 1700-10Stretching sample shape appearance figure.
Specific embodiment
The present invention provides matrix-oxidation film film substrate bond strength detection methods in a kind of oxide alloy material, including
Following steps:
Tensile sample is made in oxide alloy material, measures the elasticity modulus of oxidation film in the tensile sample；
Tension test is carried out to the tensile sample, when oxidation film is fallen off, obtains stretching sample, obtains the drawing
Stretch the dependent variable that sample cracks；
Thickness, the crack spacing for measuring the oxidation film for stretching sample, obtain the oxide alloy material using formula (1)
Matrix-oxidation film film substrate bond strength in material:
Wherein, τ is film substrate bond strength, MPa；δ is the oxide thickness for stretching sample, μm；λ is the crackle for stretching sample
Spacing, μm；E is the elasticity modulus of oxidation film, GPa；εmaxThe dependent variable cracked for tensile sample.
Tensile sample is made in oxide alloy material by the present invention, measures the elasticity modulus of oxidation film in the tensile sample.
The present invention is not specifically limited the source of the oxide alloy material, using quilt well known to those skilled in the art
The alloy material of oxidation, specifically such as, the pure titanium being oxidized or the Incoloy800H alloy being oxidized.
In the present invention, the elasticity modulus of the oxidation film in the oxide alloy material is preferably greater than the elasticity of alloy substrate
Modulus, this is because: if without binding force between oxidation film and alloy substrate, oxidation film not by stress, oxidation film with
Displacement of the alloy substrate on interface will be different；If be well combined between oxidation film and alloy substrate, oxidation film
It is also identical as displacement of the alloy substrate on interface and strain, but since the elasticity modulus of oxidation film and alloy substrate is different,
Shear stress will be generated on interface, if super to maintain oxidation film-alloy substrate to strain consistent shear stress on interface
The bond strength of peroxide film and alloy substrate, it will unsticking phenomenon occurs.
The present invention is not specifically limited the shape of the tensile sample, as long as being able to carry out tension test, specifically
Such as cuboid or tensile sample schematic shapes as shown in Figure 1.The present invention is processed into stretching examination to by oxide alloy material
The method of sample is not specifically limited, using preparation method well known to those skilled in the art.
In a specific embodiment of the present invention, in order to verify the accuracy of detection method, the tensile sample is preferably made by oneself；
The preparation method of the tensile sample is preferred are as follows:
Alloy material is made to the shape of tensile sample, obtains alloy test specimen；
Alloy test specimen progress high-temperature oxydation is prepared into oxidation film, obtains tensile sample.
In the present invention, the alloy substrate is preferably 800H alloy；The ingredient of the 800H alloy is as shown in table 1.
Table 1800H alloying component table
| Ingredient | C | Si | Mn | Ni | Cr | Al | Ti | Fe |
| Mass fraction/wt% | 0.063 | 0.05 | 0.81 | 30.67 | 20.6 | 0.42 | 0.47 | Surplus |
The present invention carries out the temperature and time of high-temperature oxydation to the alloy test specimen and process is not specifically limited, this field
Technical staff is configured according to the actual situation.
The present invention is not specifically limited the test method of the elastic modulus E of oxidation film in the tensile sample, using this
Elasticity modulus test method known to the technical staff of field.
After obtaining tensile sample, the present invention carries out tension test to the tensile sample and obtains when oxidation film is fallen off
To sample is stretched, the dependent variable that the tensile sample cracks is obtained.
In the present invention, the detailed process of the tension test preferably includes following steps:
It takes two tensile samples spare, rough tension test first is carried out to one of tensile sample, then to other one
A tensile sample carries out accurate tension test, obtains stretching sample.
In the present invention, the rough and careless tension test process is preferred are as follows: by the tensile sample with rate of extension 1~2%/
Min carries out tension test, makes the oxide layer deterioration on tensile sample, and the deflection for measuring tensile sample at this time is n；The stretching
Rate is more preferably 1%/min.
In the present invention, the accurate tension test process is preferred are as follows: by the tensile sample with rate of extension 1~2%/
Min carries out tension test, after deflection reaches m；Rate of extension is adjusted to 0.1~0.5%/min to continue to stretch examination
It tests, until the oxidation film on tensile sample starts shedding off, terminates tension test, obtain stretching sample；Further preferably are as follows: by institute
It states tensile sample and tension test is carried out with rate of extension 1%/min, after deflection reaches m；Rate of extension is adjusted to
0.1%/min continues tension test, until the oxidation film on tensile sample starts shedding off, terminates tension test, is drawn
Stretch sample.
In the present invention, the difference of the n-m is preferably 2~3%, and further preferably 3%.
In the present invention, the tension test carries out preferably on universal testing machine；During tension test carries out, lead to
The dependent variable ε that the tensile sample cracks can be obtained in the machine of overstretching testmax。
The present invention can accurately test oxidation film in oxide alloy material by the setting to tension test process
The critical moments being detached from alloy substrate, and then the critical state that oxidation film has just been separated with alloy substrate is obtained, and obtain corresponding
Stretching sample, and then accurately obtain the relevant parameter for stretching oxidation film in sample, such as thickness and crack spacing.
It obtains after stretching sample, the present invention measures thickness, the crack spacing of the oxidation film for stretching sample, utilizes formula
(1) matrix-oxidation film film substrate bond strength in the oxide alloy material is obtained:
Wherein, τ is film substrate bond strength, MPa；δ is the oxide thickness for stretching sample, μm；λ is the crackle for stretching sample
Spacing, μm；E is the elasticity modulus of oxidation film, GPa；εmaxThe dependent variable cracked for tensile sample.
In the present invention, the force analysis figure for stretching oxidation film in sample, as shown in Figure 2.The oxygen according to fig. 2
Change the force analysis figure of film, obtains thickness δ, crack spacing λ that gained stretches oxidation film in sample.
It obtains the elastic modulus E of oxidation film, stretch oxide thickness δ, the crack spacing λ of sample, tensile sample generation is split
The dependent variable ε of linemaxAfterwards, using formula (1), interfacial shear stress τ can be obtained.
Below with reference to embodiment to matrix-oxidation film film substrate bond strength inspection in oxide alloy material provided by the invention
Survey method is described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
Using 800H alloy as alloy material, according to the schematic diagram of Fig. 1, alloy test specimen is prepared, alloy surface of test piece is polished
Polishing treatment；
It takes series alloy test specimen to take out after 700 DEG C of heat preservations aoxidize 100h, obtains tensile sample700, measurement gained, which stretches, to be tried
Sample700The elastic modulus E of middle oxidation film700For 109GPa；
Take two identical tensile samples700, first by a tensile sample700Tension test is carried out with 1% rate of extension,
Make the oxide layer deterioration on tensile sample, measures tensile sample at this time700Deflection be 12%；Second stretching is tried again
Sample700First with 1% rate of extension carry out tension test, until deflection be 9%, then continued with 0.5% rate of extension
Tension test, until oxidation film starts to peel off, tensile sample at this time700Deflection be 11.3%, terminate tension test, obtain
Stretch sample；And obtain tensile sample700The dependent variable cracked is 0.8%；
The force analysis figure for stretching oxidation film in sample according to Fig.2, measures under scanning electron microscope and stretches sample
Oxidation film with a thickness of 1.5 μm, crack spacing is 3.2 μm.
It is obtained according to formula (1), aoxidizing matrix-oxidation film film substrate bond strength in 800H alloy material is 909MPa；
Fig. 3 is gained tensile sample700The stretching shape appearance figure of the stretching sample of (cyclic oxidation 0 time).
In order to simulate the practical situations of 800H alloy, to obtained tensile sample700Cyclic oxidation is carried out, specifically:
By tensile sample700Continue to be cooled to room temperature in 700 DEG C of progress high-temperature oxydation 30min；Then heat to 700 DEG C of progress high temperature oxygens
Change 30min, and so on ..., obtain cyclic oxidation 5 times and 10 times tensile samples700-5And tensile sample700-10；
According to above-mentioned tension test, gained tensile sample is measured respectively700-5And tensile sample700-10Film base junction close it is strong
Degree, is listed in table 2 respectively.
Fig. 4 and Fig. 5 is respectively tensile sample700-5And tensile sample700-10Stretching sample shape appearance figure.
Embodiment 2
Similar to Example 1, difference is only that the temperature of high-temperature oxydation is 800 DEG C；
In addition, difference also resides in: taking two identical tensile samples800, first by a tensile sample800With 1% drawing
It stretches rate and carries out tension test, make the oxide layer deterioration on sample, the deflection for measuring tensile sample at this time is 10%；Again by
Two tensile samples800Tension test is first carried out with 1% rate of extension, until deflection is 7%, then with 0.5% stretching speed
Rate continues tension test, until oxidation film starts to peel off, the deflection of tensile sample at this time is 9.1%, terminates and stretches
Test obtains stretching sample.
Gained tensile sample800, tensile sample800-5And tensile sample800-10Film substrate bond strength result be listed in table 2.
Embodiment 3
Similar to Example 1, difference is only that the temperature of high-temperature oxydation is 900 DEG C；
In addition, difference also resides in: taking two identical tensile samples900, first by a tensile sample900With 1% drawing
It stretches rate and carries out tension test, make the oxide layer deterioration on tensile sample, the deflection for measuring tensile sample at this time is 8.5%；
Again by second tensile sample900Tension test is first carried out with 1% rate of extension, until deflection is 6%, then with 0.5%
Rate of extension continues tension test, until oxidation film starts to peel off, the deflection of tensile sample at this time is 8.1%, eventually
Only tension test obtains stretching sample；
Gained tensile sample800, tensile sample800-5And tensile sample800-10Film substrate bond strength result be listed in table 2.
Table 2 aoxidizes matrix-oxidation film film substrate bond strength in 800H alloy material
From table 2 it can be seen that the oxidation cycle number of 800H alloy at different temperatures is more, it is outer needed for oxide film breakdown
Power is smaller, this has important meaning to the service life of prediction alloy oxide film.In the process, temperature is higher, cyclic oxidation number
More, oxidation film is lower with matrix alloy interface bond strength, is more easy to appear peeling phenomenon under the conditions of external force.It is this simultaneously
Phenomenon matches with the pattern for the stretching sample that Fig. 3~5 are shown.
From Examples 1 to 3 as can be seen that detection method provided by the invention obtains film substrate bond strength and stretches sample
Shape appearance figure matches, and matches with practical theory, illustrates that detection method of the invention is feasible.
Embodiment 4
It takes the oxidation 800H alloy material after using 700 DEG C of oxidation 500h as oxide alloy material, obtains tensile sample；
The elasticity modulus for measuring oxidation film in tensile sample is 97GPa；
It takes two tensile samples spare, a tensile sample is first subjected to tension test with 1% rate of extension, makes to stretch
Oxide layer deterioration on sample, the deflection for measuring tensile sample at this time is 10%；Second tensile sample is first drawn with 1% again
Stretch rate carry out tension test, until deflection be 7.5%, tension test is then continued with 0.5% rate of extension, directly
Start to peel off to oxidation film, the deflection of tensile sample is 9.1% at this time, terminates tension test, obtains stretching sample；And it obtains
The dependent variable that tensile sample cracks is 0.8%；
Oxidation film force analysis figure in stretching sample according to Fig.2, measures the oxygen for stretching sample under scanning electron microscope
Change film with a thickness of 2.1 μm, crack spacing is 4.5 μm.
It is 805MPa according to the binding force that formula (1) obtains alloy substrate-oxidation membrane material film base.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (2)
1. matrix-oxidation film film substrate bond strength detection method in a kind of oxide alloy material, which is characterized in that including following
Step:
Tensile sample is made in oxide alloy material, measures the elasticity modulus of oxidation film in the tensile sample；
Tension test is carried out to the tensile sample, when oxidation film is fallen off, obtains stretching sample, obtains the stretching examination
The dependent variable that sample cracks；
Thickness, the crack spacing for measuring the oxidation film for stretching sample, are obtained in the oxide alloy material using formula (1)
Matrix-oxidation film film substrate bond strength:
Wherein, τ is film substrate bond strength, MPa；δ is the oxide thickness for stretching sample, μm；λ be stretch sample crackle between
Away from, μm；E is the elasticity modulus of oxidation film, GPa；εmaxThe dependent variable cracked for tensile sample.
2. detection method according to claim 1, which is characterized in that the detailed process of the tension test are as follows:
It takes two tensile samples spare, rough tension test first is carried out to one of tensile sample, then to another drawing
It stretches sample and carries out accurate tension test, obtain stretching sample；
The rough and careless tension test process are as follows: the tensile sample is subjected to tension test with 1~2%/min of rate of extension, is made
Oxide layer deterioration on tensile sample, the deflection for measuring tensile sample at this time is n；
The accurate tension test process are as follows: the tensile sample is subjected to tension test with 1~2%/min of rate of extension, when
After deflection reaches m；Rate of extension is adjusted to 0.1~0.5%/min and continues tension test, until on tensile sample
Oxidation film starts shedding off, and terminates tension test, obtains stretching sample；
The difference of the n-m is 2~3%.
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| CN201910608295.3A CN110186845B (en) | 2019-07-08 | Method for detecting bonding strength of matrix-oxide film matrix in oxidized alloy material |
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| CN201910608295.3A CN110186845B (en) | 2019-07-08 | Method for detecting bonding strength of matrix-oxide film matrix in oxidized alloy material |
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