CN106290029B - A method of material oxidation rate is measured in real time using high-temperature nano impression instrument - Google Patents
A method of material oxidation rate is measured in real time using high-temperature nano impression instrument Download PDFInfo
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- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 82
- 230000003647 oxidation Effects 0.000 title claims abstract description 78
- 239000000463 material Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000012360 testing method Methods 0.000 claims abstract description 96
- 238000007373 indentation Methods 0.000 claims abstract description 24
- 238000002474 experimental method Methods 0.000 claims abstract description 19
- 239000011159 matrix material Substances 0.000 claims abstract description 14
- 239000007789 gas Substances 0.000 claims description 25
- 230000001681 protective effect Effects 0.000 claims description 20
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 230000008859 change Effects 0.000 claims description 6
- 238000006073 displacement reaction Methods 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 238000009795 derivation Methods 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 240000007594 Oryza sativa Species 0.000 claims 1
- 235000007164 Oryza sativa Nutrition 0.000 claims 1
- 235000009566 rice Nutrition 0.000 claims 1
- 238000011160 research Methods 0.000 abstract description 5
- 238000010301 surface-oxidation reaction Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 18
- 230000008569 process Effects 0.000 description 7
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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
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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
- G01N2203/022—Environment of the test
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Abstract
The present invention provides a kind of methods measuring material oxidation rate in real time using high-temperature nano impression instrument, include the following steps：Nano-indentation experiment is carried out to test specimen under target temperature, the elastic modulus E of matrix when acquisition test specimen is not oxidizeds, test specimen forms the real-time elastic modulus E of oxidation film matrix when being aoxidizedrAnd test specimen is formed the elastic modulus E of oxidation film when oxide thickness reaches preset value by oxidationf；According to Es、Ef、Er, real-time depth of cup angle value h is calculated real-time oxide thickness d when test specimen is aoxidized, and utilizes formulaReal-time oxidation rate when test specimen is aoxidized is calculatedWherein, Δ t is time interval, and Δ d is the changing value of the real-time oxide thickness in Δ t time intervals.The method achieve the real-time online measurings of the oxidation rate to test specimen under micron and nanoscale, have great importance for surface oxidation behavior of the research material under micro-nano-scale.
Description
Technical field
The present invention relates to engineering material technical fields, and in particular to a kind of to measure material in real time using high-temperature nano impression instrument
The method of oxidation rate.
Background technology
Material is the basis of human material's civilization, it supports the advance of other every new technologies, space flight and aviation, ocean work
The national economy production field such as journey, life science and system engineering is required for all kinds of structure and function materials.With science and technology
Development and certain extreme conditions realization, various new materials rapidly develop and are widely used in high-tech sector, this is to making
It is stringenter with requirements such as the reliability of material, practical performances.For example, in space flight and aviation thermal protection field, with engine to
High thrust-weight ratio development, the design inlet temperature of engine are continuously improved, and inlet temperature is also substantially improved before turbine, to engine thermal
More stringent requirements are proposed for end pieces high-temperature alloy material, and researching high-temperature alloy material and heat barrier coat material are under high temperature environment
Oxidation mechanism to improve its temperature operating limit, improve engine operating temperature have extremely important effect.Therefore, carry out
It is extremely urgent to the mechanism study of oxidation behavior of the material under room temperature and high-temperature condition.
A variety of methods can be used in research material high-temperature oxydation at present, including oxidation kinetics measures and oxidation reaction product shape
Looks detect.These methods are based on oxidation process dynamics, pass through composition to reaction product and pattern and metal or alloy base
Body material is carefully detected, and the essence i.e. oxidation mechanism of oxidation process is probed into.Above-mentioned oxidation kinetics measurement method passes through company
The continuous weight change weighed in test specimen oxidation process, or measure oxidation reaction speed by measuring the wear rate of reaction gas
Rate；Reaction product Shape measure means include then using scanning electron microscope, x-ray spectrometer or transmission electron microscope
To analyze the small shape characteristic or product composition of reaction product.
However, in current research, lack micron and Nano grade to material oxidation process (i.e. oxidation rate) into
The method that row monitors in real time causes the observation of oxidation process to lack the real-time Evolution Data of micro-scale with analysis.
Invention content
Therefore, the technical problem to be solved in the present invention is that the prior art is overcome to lack in micron and Nano grade to material
The defect for the method that oxidation rate is monitored in real time.
For this purpose, the present invention provides a kind of method measuring material oxidation rate in real time using high-temperature nano impression instrument, it should
Method includes the following steps：
Under target temperature to test specimen carry out nano-indentation experiment, obtain the test specimen it is not oxidized when matrix springform
Measure Es, the test specimen forms the real-time elastic modulus E of oxidation film-matrix when being aoxidizedrAnd the test specimen is by oxidation institute shape
The elastic modulus E of oxidation film when reaching preset value at oxide thicknessf；
According to Es、Ef、Er, real-time depth of cup angle value h the real-time oxide thickness d when test specimen is aoxidized is calculated,
And utilize formulaThe real-time oxidation rate when test specimen is aoxidized is calculatedWherein, Δ t is time interval,
Δ d is the changing value of the real-time oxide thickness in Δ t time intervals.
Preferably, the real-time oxide thickness d when test specimen is aoxidized is calculated using formula 1 and formula 2, it is public
Formula 1 is：
Wherein, P is real-time load value when the test specimen is aoxidized, and α is the characteristic angle of indenter shape, and h is the test specimen quilt
Real-time depth of cup angle value when oxidation；
Formula 2 is：
Wherein, P is real-time load value when the test specimen is aoxidized, and h is the real-time depth of cup angle value when test specimen is aoxidized,For the load obtained for 1 derivation of formula to the derivative of displacement, α is the characteristic angle of indenter shape, ErFor the real-time of oxidation film-matrix
Elasticity modulus；Derivative of the load p to displacement h is obtained according to 1 derivation of formula, carries it into the left end of formula 2, you can obtain one
About Es、Ef、Er, h, d equation, and Es、Ef、Er, h be all known, you can the anti-real-time oxidation released when test specimen is aoxidized
Film thickness d.
Preferably, obtaining Es、ErAnd EfThe step of include：
The test specimen is placed in the microscope carrier room of nano-hardness tester, and protective gas is passed through so that institute into the microscope carrier room
It is not oxidized to state test specimen, and the microscope carrier room is risen into the target temperature, then nano-indentation experiment is carried out to the test specimen
Obtain Es；
It reduces the intake of the protective gas or stopping is passed through the protective gas, so that the surface of test piece starts
It is aoxidized, then nano-indentation experiment is carried out to the test specimen and obtains Er；
When the test specimen forms oxide thickness by oxidation and reaches preset value, then to the oxidation film of the surface of test piece into
Row nano-indentation experiment obtains Ef。
Preferably, the protective gas includes argon gas or nitrogen.
Preferably, before the test specimen is placed in the microscope carrier room of nano-hardness tester, the surface of test piece is polished to full
The requirement of sufficient nano-indentation experiment.
Preferably, obtaining the springform that the test specimen is formed oxidation film when oxide thickness reaches preset value by oxidation
Measure EfThe step of in, the preset value be dIt is default, the depth of cup of the nano-indentation experiment is h, then dIt is default≥10h。
Preferably, ranging from 20 DEG C to 1200 DEG C of the target temperature.
Technical solution of the present invention has the following advantages that：
The method provided by the invention for measuring material oxidation rate in real time using high-temperature nano impression instrument, passes through nano impress
Instrument measures elastic modulus E of the test specimen under different conditionss、Er、Ef, in conjunction with film-basis mechanism opinion of nano impress, realize to test specimen
The real-time online measuring of oxidation rate under micron and nanoscale, for Surface Oxygen of the research material under micro-nano-scale
Change behavior has great importance.Moreover, because the measurement accuracy of instrument is up to nanoscale, it is thus possible to realize oxidation initial stage pair
The assessment of material oxidation rate, also being capable of oxidation behavior of the research material under room temperature and high temperature.
The method provided by the invention for measuring material oxidation rate in real time using high-temperature nano impression instrument is protected by adjusting
The air velocity of gas controls oxidation rate, finally combines film-basis mechanism opinion of nano impress, oxide layer on test specimen may be implemented
The measurement of the processes and then realization such as growth, evolution to material oxidation rate under minute yardstick, room temperature and high-temperature condition.
Description of the drawings
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art are briefly described, it should be apparent that, in being described below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, other drawings may also be obtained based on these drawings.
Fig. 1 is the method for measuring material oxidation rate in real time using high-temperature nano impression instrument that embodiment of the present invention provides
Flow chart；
Fig. 2 forms the schematic diagram of oxide thickness in oxidation film-matrix when being aoxidized by the test specimen.
In figure：1- matrixes；2- oxidation films；3- indentation test front surface profiles；4- indentation test rear surface profiles；5- pressure heads
Schematic diagram；P- test specimens real-time load value when being aoxidized；Real-time depth of cup angle value when being aoxidized of test specimen described in h-；hcIndentation test
Contact depth；a1Pressure head projects radius with basis material contact zone；a2Pressure head projects radius with oxidation film contact zone.
Specific implementation mode
Clear, complete description is carried out to technical scheme of the present invention below in conjunction with attached drawing.
As shown in Figure 1, the method provided in this embodiment for measuring material oxidation rate in real time using high-temperature nano impression instrument
Include the following steps：
(a) surface of test piece is polished to the requirement for meeting nano-indentation experiment.The purpose is to improve material surface
Finish, to ensure being smoothed out for step b.
(b) test specimen is placed in the microscope carrier room of nano-hardness tester, and be passed through into the microscope carrier room protective gas with
Keep the test specimen not oxidized, and the microscope carrier room is risen into the target temperature, then nano impress is carried out to the test specimen
Experiment obtains Es。
(c) it reduces the intake of the protective gas or stopping is passed through the protective gas, so that the surface of test piece
Start to be aoxidized, then nano-indentation experiment is carried out to the test specimen and obtains Er。
(d) stop being passed through the protective gas, set the preset value that the test specimen is formed oxide thickness by oxidation, when
Nano-indentation experiment acquisition E is carried out to the oxidation film of the surface of test piece again after reaching preset valuef。
(e) the real-time oxide thickness d when test specimen is aoxidized is calculated using formula 1 and formula 2, formula 1 is：
Wherein, P is real-time load value when the test specimen is aoxidized, and α is the characteristic angle of indenter shape, and h is the test specimen quilt
Real-time depth of cup angle value when oxidation.
Formula 2 is：
Wherein, P is real-time load value when the test specimen is aoxidized, and h is the real-time depth of cup angle value when test specimen is aoxidized,For the load obtained for 1 derivation of formula to the derivative of displacement, α is the characteristic angle of indenter shape, ErFor the reality of oxidation film-matrix
When elasticity modulus.
(f) formula is utilizedThe real-time oxidation rate when test specimen is aoxidized is calculatedWherein, Δ t is
Time interval, Δ d are the changing value of the real-time oxide thickness in Δ t time intervals.
The above method provided in this embodiment controls oxidation rate by adjusting the air velocity of protective gas, finally combines
The film of nano impress-basis mechanism opinion may be implemented the processes such as growth, evolution of oxide layer on test specimen and then realize to material in micro- ruler
The measurement of oxidation rate under degree, room temperature and high-temperature condition.
Above-mentioned formula 1 and formula 2 are obtained based on the nano impress theoretical calculation of film-basal body structure, and calculating process is：
With reference to figure 2, in the conical pressure head that Fig. 2 is provided, 1 is matrix, and 2 be oxidation film；3 be indentation test front surface profile, and 4 be impression
Rear surface profile is tested, 5 be pressure head schematic diagram, and P is real-time load value when test specimen is aoxidized, and h is that the test specimen is real when being aoxidized
When depth of cup angle value, hcIt is a for the contact depth of indentation test1Radius, a are projected for pressure head and basis material contact zone2For pressure
Head projects radius with oxidation film contact zone.
There is following relationship for Fig. 2 conical pressure heads provided：
Introduce a1、a2Geometrical relationship formula have：
It may finally push away：
In above-mentioned formula：D is the real-time oxide thickness when test specimen is aoxidized, and h is that the test specimen is real when being aoxidized
When depth of cup angle value, EsFor the elasticity modulus of test specimen matrix when not oxidized, ErOxygen is formed when being aoxidized by the test specimen
Change the real-time elasticity modulus of film-matrix, P is real-time load value, h when the test specimen is aoxidizedcFor the contact depth of indentation test,
a1Radius, a are projected for pressure head and basis material contact zone2Radius is projected for pressure head and oxidation film contact zone, Δ t is time interval,
Δ d is the changing value of the real-time oxide thickness in Δ t time intervals.
In method provided in this embodiment, protective gas be prevent oxidation occur gas, include but are not limited to argon gas,
Nitrogen etc..Moreover, in step (b), needs to be passed through enough protective gas into microscope carrier room, just the test specimen can be made not by oxygen
Change, certainly, the intake of protective gas is related with the oxidation resistent susceptibility of the model of used nano-hardness tester and test specimen, ability
Field technique personnel are referred to the flow of relevant parameter setting protective gas in the prior art.In in step (c) or (d), due to
It reduces the intake of the protective gas or stopping is passed through the protective gas, so that test specimen is aoxidized.
In method provided in this embodiment, the preset value is to refer to oxidation when to oxidation film progress nano-indentation experiment
The thickness that film has, value can be estimated according to material oxidation performance.Preferably, obtaining the test specimen by oxidation institute shape
The elastic modulus E of oxidation film when reaching preset value at oxide thicknessfThe step of in, the preset value be dIt is default, the nanometer pressure
The depth of cup of trace experiment is h, then dIt is default≥10h.That is, depth of cup selects within the 1/10 of oxide thickness,
What is measured is exactly the elasticity modulus of oxidation film.Why require oxidation a period of time, oxide thickness to reach preset value here, with
The precision of nano-hardness tester is related, for example nano-hardness tester tests accurate range in 30-200nm, it may be necessary to thickness of oxidation film
Degree at least 300nm or more can just do experiment oxygen determination film character.
In the above method, the load of pressure head when nano-hardness tester can continuously monitor pressure head indentation sample and be unloaded from sample surfaces
Lotus and displacement, the load-displacement data obtained in a complete loading-unloading circuit can be used for many of analysis of material
Mechanical property, such as contact stiffness, creep, elastic work, plastic work done, fracture toughness, load-deformation curve, fatigue, storage modulus
And loss modulus etc..It is applicable to organic or inorganic, soft or hard material detection and analysis, including optical thin film, microelectronics
Plated film, protectiveness are thin etc.；Matrix can be soft or hard material, including metal, alloy, semiconductor, glass, mineral and have
Machine material etc..
Moreover, the microscope carrier room of nano-hardness tester can be born within the scope of very high temperature.That is, provided in this embodiment
Method can carry out nano indentation test in different temperatures range to test specimen, and the size of temperature range depends on utilized nanometer pressure
The performance of trace instrument.Currently, the microscope carrier room in common nano-hardness tester can withstand up to 1200 DEG C in the market, thus at this time on
The range of target temperature described in method is stated up to 20 DEG C to 1200 DEG C.
It should be further noted that the mode of the control test specimen state of oxidation is related with the type of nano-hardness tester.In addition to
It is provided in this embodiment by protective gas come control the test specimen state of oxidation in the way of outside, those skilled in the art can also use
Other manner controls the test specimen state of oxidation in the prior art.
For method provided by the invention, step (a) it is not necessary to.When test specimen itself has met nanometer pressure
The requirement of trace experiment, you can ignore step (a).
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (6)
1. a kind of method measuring material oxidation rate in real time using high-temperature nano impression instrument, which is characterized in that this method includes
Following steps：
Under target temperature to test specimen carry out nano-indentation experiment, obtain the test specimen it is not oxidized when matrix elastic modulus Es,
The test specimen forms the real-time elastic modulus E of oxidation film-matrix when being aoxidizedrAnd the test specimen forms oxygen by oxidation
Change the elastic modulus E of oxidation film when film thickness reaches preset valuef；
According to Es、Ef、Er, real-time depth of cup angle value h the real-time oxide thickness d when test specimen is aoxidized, and profit is calculated
Use formulaThe real-time oxidation rate when test specimen is aoxidized is calculatedWherein, △ t are time interval, and △ d are
The changing value of real-time oxide thickness in △ t time intervals；
Wherein, the real-time oxide thickness d when test specimen is aoxidized is calculated using formula 1 and formula 2, formula 1 is：
Wherein, P is real-time load value when the test specimen is aoxidized, and α is the characteristic angle of indenter shape, and h is that the test specimen is aoxidized
When real-time depth of cup angle value；
Formula 2 is：
Wherein, P is real-time load value when the test specimen is aoxidized, and h is the real-time depth of cup angle value when test specimen is aoxidized,For
For the load obtained according to 1 derivation of formula to the derivative of displacement, α is the characteristic angle of indenter shape, ErFor the real-time of oxidation film-matrix
Elasticity modulus.
2. according to the method described in claim 1, it is characterized in that, obtaining Es、ErAnd EfThe step of include：
The test specimen is placed in the microscope carrier room of nano-hardness tester, and protective gas is passed through so that the examination into the microscope carrier room
Part is not oxidized, and the microscope carrier room is risen to the target temperature, then carries out nano-indentation experiment acquisition to the test specimen
Es；
It reduces the intake of the protective gas or stopping is passed through the protective gas, so that the surface of test piece starts by oxygen
Change, then nano-indentation experiment is carried out to the test specimen and obtains Er；
When the test specimen forms oxide thickness by oxidation and reaches preset value, then the oxidation film of the surface of test piece is received
Rice indentation test obtains Ef。
3. according to the method described in claim 2, it is characterized in that, the protective gas includes argon gas or nitrogen.
4. according to the method described in claim 2, it is characterized in that, by the test specimen be placed in nano-hardness tester microscope carrier room it
Before, the surface of test piece is polished to the requirement for meeting nano-indentation experiment.
5. method according to claim 1 to 4, which is characterized in that obtain the test specimen and formed by oxidation
The elastic modulus E of oxidation film when oxide thickness reaches preset valuefThe step of in, the preset value be dIt is default, the real-time impression
Depth value is h, then dIt is default≥10h。
6. method according to claim 1 to 4, which is characterized in that ranging from 20 DEG C of the target temperature
To 1200 DEG C.
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