CN1193738A - Double-sided oxidation bending measurement technology for oxide film stress change - Google Patents
Double-sided oxidation bending measurement technology for oxide film stress change Download PDFInfo
- Publication number
- CN1193738A CN1193738A CN97100973A CN97100973A CN1193738A CN 1193738 A CN1193738 A CN 1193738A CN 97100973 A CN97100973 A CN 97100973A CN 97100973 A CN97100973 A CN 97100973A CN 1193738 A CN1193738 A CN 1193738A
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- sample
- oxide film
- oxidation
- stress
- sided
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- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 35
- 230000003647 oxidation Effects 0.000 title claims abstract description 31
- 238000005259 measurement Methods 0.000 title claims abstract description 19
- 238000005516 engineering process Methods 0.000 title claims abstract description 14
- 238000005452 bending Methods 0.000 title abstract description 12
- 230000008859 change Effects 0.000 title abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 7
- 238000004364 calculation method Methods 0.000 claims abstract description 6
- 239000000956 alloy Substances 0.000 claims description 23
- 229910045601 alloy Inorganic materials 0.000 claims description 22
- 238000000576 coating method Methods 0.000 claims description 9
- 239000011248 coating agent Substances 0.000 claims description 8
- 238000011160 research Methods 0.000 claims description 6
- 230000000052 comparative effect Effects 0.000 claims description 2
- 239000000523 sample Substances 0.000 description 40
- 229910052761 rare earth metal Inorganic materials 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000005275 alloying Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 3
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 229910052727 yttrium Inorganic materials 0.000 description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 3
- 238000000137 annealing Methods 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 235000013619 trace mineral Nutrition 0.000 description 2
- 239000011573 trace mineral Substances 0.000 description 2
- 229910001005 Ni3Al Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910010038 TiAl Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000003026 anti-oxygenic effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000002513 implantation Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
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- Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
- Sampling And Sample Adjustment (AREA)
- Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
Abstract
A double-sided oxidation bending measurement technology for oxidation die stress change sequentially comprises the steps of sample preparation, high-temperature oxidation bending measurement and stress change calculation, and is characterized in that (1) a sample is in a thin strip shape, two sides of the sample are respectively materials to be compared and researched, the length-width ratio is 6-20, the thickness is 0.2-0.4 mm, and (2) the stress change is calculated by adopting the following formula that ζ 'σ' - ζ σ = EH2D/[3(1－μ)L2]Wherein ζ is the oxide film thickness, σ is the in-oxide film stress, E is the Young's modulus, μ is the Poisson's ratio, L is the length, H is the thickness, and D is the bending deflection, wherein the symbol ' represents the treated sample. The method is simple and has high measurement precision.
Description
The present invention relates to measuring technique, the two-sided oxidation flexural measurement technology of the oxide film stress changes that is applicable to the research of metal material high-temperature oxydation is provided especially.
Add the oxidation susceptibility, particularly rare earth element effect that trace element can improve alloy in the alloy, for understanding its mechanism of action from the mechanics angle, it is an important aspect that quantitative measurment oxide film internal stress changes.At present, but the kinetic measurement of oxide film stress, but contain many mechanical parameters owing to measure the computing formula of institute's foundation, these parameters often are difficult to obtain from document, make stress measurement complicated and measure.In addition, present measuring technique is subjected to the restriction of probe temperature and measuring accuracy again, and when particularly studying trace alloying element to the oxide film stress influence, test error be can not ignore.With the immediate technology of the present invention be the single face oxidation flexural measurement method of oxide film stress; single face oxidation bending method is that the most frequently used method of oxide film stress measurement is carried out in metallic high temperature corrosion field; in film field also widespread use; during the oxide film stress measurement; thin bar-shaped sample needs coating single side to protect, and makes sample one side surface that oxidation not take place fully, and film should be very thin; to the bending of the sample effect that do not exert an influence, the film that meets the demands fully up till now exists hardly.The Young modulus and the Poisson's ratio that comprise material in the Stress calculation formula obtain often more complicated of these parameters fully, and therefore, it is lower that test only limits to oxidizing temperature, and the situation that oxidization time is short is particularly at research Al
2O
3Membrane stress or trace element during to the oxide film stress influence precision lower.
The object of the present invention is to provide a kind of different materials high temperature oxidation resistance that is applicable to compare, be specially adapted to add in the alloy stress measurement technology of micro-antioxygenic property research, its measuring accuracy is higher, and method is simple.
The invention provides a kind of two-sided oxidation flexural measurement technology of oxidation mould stress changes, comprise specimen preparation successively, the high-temperature oxydation flexural measurement, the stress changes calculation procedure is characterized in that:
(1) sample is thin strip, and the two sides is respectively the material that needs comparative studies, and length breadth ratio is between 6～20, and thickness is 0.2～0.4mm;
(2) following formula is adopted in the calculating of stress changes:
ξ′σ′-ξσ＝EH
2D/[3(1-μ)L
2]
-------oxide thickness of ξ in the formula
σ-------oxide film internal stress
The Young modulus of E--------sample
μ--the Poisson's ratio of-----sample
The length of L--------sample
The thickness of H--------sample
The sag of D--------sample
The treated sample of symbol ' expression wherein.
When being primarily aimed at the alloying component variation, measuring technique of the present invention, wherein mainly refers to alloy after surface treatment to the influence of oxide film internal stress, in well-oxygenated environment, and with not surface treated alloy ratio, the change of the oxide film internal stress that the surface generates.When measuring, a side of sample is through surface treatment (for example, ion injects alloying element, surface-coated rare earth oxide, or the like).During sample oxidation at high temperature, if the oxide film internal stress difference that two sides generate, sample will bend, because common compression chord in the oxide film, sample is to the less lateral bending song of stress, and crooked size characterizes the degree of STRESS VARIATION.The oxide film stress changes can calculate, and analyzes the stress of thin bar-shaped sample, according to the mechanical balance principle, can get system of equations.Draw ξ ' σ '-ξ σ=EH after finding the solution
2D/[3 (1-μ) L
2].
Add the antioxygenic property that trace rare-earth element can significantly improve alloy in the high temperature alloy.According to this result, add rare earth element in the alloy and become the important means of improving the alloy inoxidizability.For Al
2O
3Film forms alloy and Cr below 850 ℃
2O
3Film forms alloy, and it is less to the oxidation kinetics influence of alloy to add trace rare-earth element, and new technology can directly obtain the difference of stress changes, that is, and and Δ σ=EH
2D/[3 (1-μ)-3L
2], because Al
2O
3And Cr
2O
3Be two kinds of most important oxides in the high temperature corrosion field, new technology is of universal significance to a certain extent, aspect high-temperature protection coating, and system for example: the shallow layer/base material of modification/shallow layer, also can measure the oxide film stress changes.General bureau it, the present invention has following advantage:
When (1) adopting the present invention to study because sample does not need coating single side protection, therefore, during the sample oxidation time of temperature and oxidation unrestricted, particularly got rid of the relation with the diaphragm protective value, improved measuring accuracy,
(2) single face oxidation bend specimen needs plated film to protect; the specimen preparation complexity by contrast, utilizes the present invention to reduce this link of coating single side in the specimen preparation (coating technique requires very high); in addition, among the present invention once experiment finished secondary experiment content in the single face oxidation bending method.In a word, use of the new technology and simplified experimentation.
When (3) calculating stress changes among the present invention, only need the mechanics parameter of undressed alloy sample, (mechanical parameter of film is measured very difficultly under the high temperature, has reduced the error of calculation so also to have simplified experimentation.
(4) the sample amount of bow is big in the single face oxidation bending method, and the sample amount of bow is little in the two-sided oxidation bending method, and the sample amount of bow is little, can guarantee the establishment of Stress calculation formula, and feasible less by the crooked stress that discharges itself, and always effect is to make the measuring accuracy raising.
Below by embodiment in detail the present invention is described in detail.
Embodiment 1
Specimen preparation: the alloy of being studied is prepared into (40-60) * (5-10) * (0.2-0.45) mm size, and sample one side ion injects the alloying element of being studied.
Test operation: sample is fixed on the high temperature alloy bar, with platinum filament one thin quartz fibre is tied up on sample one side or directly be hanging on the little sky of sample lower curtate, insert then in the high temperature furnace, and mounting flange, system vacuumizes, and vacuum tightness is 10
-5During torr, begin to heat up, when reaching design temperature, charge into oxidizing gas, utilize reading microscope to observe quartz fibre simultaneously, the deflection of record sample; Judge the influence of rare earth element according to the direction of sample bending, crooked size characterizes the degree of STRESS VARIATION, if ion injects rare earth element the oxidation kinetics of alloy is not influenced, and the change of stress can quantitative Analysis so.Computing formula is: Δ σ=EH
2D/[3 (1-μ) ξ L
2], Δ σ changes for the oxide film internal stress in the formula, and ξ is an oxide thickness, and E, μ, L, H are respectively Young modulus, Poisson's ratio, length, the thickness of sample, and D is the sample sag.
Sample: the casting alloy Co-30Cr-6Al of 53.3 * 7.1 * 0.46mm size, the congruent film that ion sputtering 20 μ m in two sides are thick, sample side ion injects 2 * 10 then
17Y+/cm
2, the voltage when ion injects remains on 80KeV.Sample is heated to 500 ℃ of insulations in a vacuum and carried out stress relief annealing in 10 hours then.
Experiment: when carrying out oxidation experiment in 900 ℃ of air, find the initial oxidation stage, ion injects yttrium makes surfaces A l
2O
3Mould stress increases (2.5GPa); The degree that internal stress is increased reduces, and develops into that finally the film internal stress is reduced, and carries out with oxidation, and stress changes remains on 1-2GPa.
Embodiment 2
Sample: the Ni-15Cr-6Al of 55 * 10 * 0.4mm size, carry out aluminising under 900 ℃ and handle, a side ion of sample injects 1 * 10
17And 1 * 10
16Y+/cm
2, sample is heated to 650 ℃ of insulations in a vacuum and carried out stress relief annealing in 4 hours then.
Experiment: during oxidation, measurement result shows that the rare earth yttrium can reduce growth stress in the oxide film in 1100 ℃ of air, and implantation dosage is big more, and effect is remarkable more, and the yttrium that various dose is injected reduces stress 2 and 7GPa respectively.
Embodiment 3
Specimen preparation: the alloy of being studied is prepared into (40-60) * (5-10) * (0.2-0.45) mm size, and sample one side applies one deck rare earth oxide, and alloy material comprises: Fe-20Cr, Fe-25Cr, Ni20Cr etc.; The rare earth oxide that applies has CeO
2
Test operation: the same.
Embodiment 4
Specimen preparation: the high temperature alloy specimen preparation becomes (40-60) * (5-10) * (0.2-0.45) mm size, adopts different process at the preparation of sample two sides two kinds of different high-temperature protection coatings, the perhaps high-temperature protection coating of different components.For example: high temperature alloy is: In738, Fecralloy, Haynes214, Ni3Al, TiAl etc.
High-temperature protection coating comprises: Co30Cr6Al, Co30Cr6AlY, Ni15Cr6Al, Ni15Cr6AlY, ZrO
2/ Y
2O
3Deng.
Test operation: the same.
Embodiment 5
Specimen preparation: be prepared into (40-60) * (5-10) * (0.2-0.45) mm size substrate, be the variation of the unrelieved stress of the film of research different process preparation. the substrate both sides are coated with the different films of same thickness.
Substrate can be: glass sheet, and pure titanium sheet, the film of research comprises: TiN, SiO
2, Al
2O
3, MCrAlY (M=Fe, Co, Ni) etc.
Process: after sample is finished, take out, observe sample bending direction and degree, judge that respectively two survey stress intensity and the relative difference in the film.
Claims (4)
1. the two-sided oxidation flexural measurement technology of an oxidation mould stress changes comprises specimen preparation successively, the high-temperature oxydation flexural measurement, and the stress changes calculation procedure is characterized in that:
(1) sample is thin strip, and the two sides is respectively the material that needs comparative studies, and length breadth ratio is between 6～20, and thickness is 0.2～0.4mm;
(2) following formula is adopted in the calculating of stress changes:
ξ′σ′-ξσ＝EH
2D/[3(1-μ)L
2]
-------oxide thickness of ξ in the formula
σ-------oxide film internal stress
The Young modulus of E--------sample
μ--the Poisson's ratio of-----sample
The length of L--------sample
The thickness of H--------sample
The sag of D--------sample
The treated sample of symbol ' expression wherein.
2. by the two-sided oxidation flexural measurement technology of the described oxide film stress changes of claim 1, it is characterized in that: as required research material order Al
2O
3Film forms alloy, perhaps Cr below 850 ℃
2O
3When film formed alloy, stress changes difference computing formula was:
Δσ＝EH
2D/[3(1-μ)-3L
2]
3. by claim 1, the two-sided oxidation flexural measurement technology of 2 described oxide film stress changes is characterized in that: the method that the preparation of two-sided sample can adopt ion to inject.
4. press claim 1, the two-sided oxidation flexural measurement technology of 2 described oxide film stress changes, it is characterized in that: the preparation of two-sided sample can be adopted the method for applying coating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 97100973 CN1091253C (en) | 1997-03-17 | 1997-03-17 | Bending measurement method for stress change of oxide film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 97100973 CN1091253C (en) | 1997-03-17 | 1997-03-17 | Bending measurement method for stress change of oxide film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1193738A true CN1193738A (en) | 1998-09-23 |
| CN1091253C CN1091253C (en) | 2002-09-18 |
Family
ID=5165444
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 97100973 Expired - Fee Related CN1091253C (en) | 1997-03-17 | 1997-03-17 | Bending measurement method for stress change of oxide film |
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|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100527804C (en) * | 2004-10-11 | 2009-08-12 | 汤姆森特许公司 | Display device with cathode ray tube and corresponding fixing system |
| CN105699209A (en) * | 2016-03-31 | 2016-06-22 | 青岛理工大学 | Oxide film stress testing method and device based on wedge-shaped high-temperature alloy sheet |
| CN103954641B (en) * | 2013-12-09 | 2016-10-05 | 青岛理工大学 | High-temperature alloy oxide film in-situ dynamic real-time stress testing method |
| CN109813613A (en) * | 2019-03-18 | 2019-05-28 | 清华大学 | The detection method of material bending performance |
-
1997
- 1997-03-17 CN CN 97100973 patent/CN1091253C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100527804C (en) * | 2004-10-11 | 2009-08-12 | 汤姆森特许公司 | Display device with cathode ray tube and corresponding fixing system |
| CN103954641B (en) * | 2013-12-09 | 2016-10-05 | 青岛理工大学 | High-temperature alloy oxide film in-situ dynamic real-time stress testing method |
| CN105699209A (en) * | 2016-03-31 | 2016-06-22 | 青岛理工大学 | Oxide film stress testing method and device based on wedge-shaped high-temperature alloy sheet |
| CN105699209B (en) * | 2016-03-31 | 2018-05-04 | 青岛理工大学 | Oxide film stress testing method and device based on wedge-shaped high-temperature alloy sheet |
| CN109813613A (en) * | 2019-03-18 | 2019-05-28 | 清华大学 | The detection method of material bending performance |
| CN109813613B (en) * | 2019-03-18 | 2020-11-10 | 清华大学 | Method for detecting bending performance of material |
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| Publication number | Publication date |
|---|---|
| CN1091253C (en) | 2002-09-18 |
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