CN106290029A - A kind of method utilizing high-temperature nano impression instrument to measure material oxidation speed in real time - Google Patents

A kind of method utilizing high-temperature nano impression instrument to measure material oxidation speed in real time Download PDF

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CN106290029A
CN106290029A CN201610797943.0A CN201610797943A CN106290029A CN 106290029 A CN106290029 A CN 106290029A CN 201610797943 A CN201610797943 A CN 201610797943A CN 106290029 A CN106290029 A CN 106290029A
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CN106290029B (en
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冯雪
李燕
方旭飞
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Tsinghua University
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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
    • 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
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    • G01N2203/0236—Other environments

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Abstract

The invention provides a kind of method utilizing high-temperature nano impression instrument to measure material oxidation speed in real time, comprise the steps:, under target temperature, test specimen is carried out nano-indentation experiment, it is thus achieved that the elastic modulus E of matrix when test specimen is not oxidizeds, test specimen is the real-time elastic modulus E of formed oxide-film matrix time oxidizedr, and oxidized the formed oxide thickness of test specimen reaches the elastic modulus E of oxide-film during preset valuef；According to Es、Ef、Er, real-time depth of cup angle value h be calculated test specimen oxidized time real-time oxide thickness d, and utilize formula be calculated test specimen oxidized time real-time oxidation rate wherein, Δ t is time interval, and Δ d is the changing value of real-time oxide thickness in Δ t time interval.The method achieve the real-time online measuring to test specimen oxidation rate under micron and nanoscale, research material surface oxidation behavior under micro-nano-scale is had great importance.

Description

A kind of method utilizing high-temperature nano impression instrument to measure material oxidation speed in real time
Technical field
The present invention relates to engineering material technical field, be specifically related to one and utilize high-temperature nano impression instrument to measure material in real time The method of oxidation rate.
Background technology
Material is the basis of human material's civilization, and it supports the advance of other every new techniques, space flight and aviation, ocean work The national economy production fields such as journey, life sciences and system engineering are required for all kinds of 26S Proteasome Structure and Function material.Along with science and technology Development and the realization of some extreme condition, various new materials develop rapidly and are widely used in high-tech sector, and this is to making Require stricter by reliability of material, Practical Performance etc..Such as, in space flight and aviation thermal protection field, along with electromotor to High thrust-weight ratio develops, and the design inlet temperature of electromotor improves constantly, and before turbine, inlet temperature is also substantially improved, to engine thermal End pieces high-temperature alloy material is had higher requirement, and researching high-temperature alloy material and heat barrier coat material are in high temperature environments Oxidation mechanism to improve its temperature operating limit, improve engine operating temperature there is earth shaking effect.Therefore, carry out Extremely urgent to the study mechanism of material oxidation behavior under room temperature and high-temperature condition.
Research material high-temperature oxydation can use multiple method at present, measures and oxidation reaction product shape including oxidation kinetics Looks detect.These methods are based on oxidizing process kinetics, by the composition of product and pattern, and metal or alloy base Body material carefully detects, and probes into the essence i.e. oxidation mechanism of oxidizing process.Above-mentioned oxidation kinetics measuring method is by even The continuous weight change weighed in test specimen oxidizing process, or measure oxidation reaction speed by measuring the wear rate of reacting gas Rate；Product Shape measure means then include using scanning electron microscope, x-ray spectrometer or transmission electron microscope Come small shape characteristic or the product composition of analytical reactions product.
But, in current research, lack at micron and Nano grade, material oxidation process (i.e. oxidation rate) to be entered The method of row monitoring in real time, causes the observation of oxidizing process and analyzes the real-time Evolution Data lacking micro-scale.
Summary of the invention
Therefore, the technical problem to be solved in the present invention is to overcome prior art to lack at micron and Nano grade material The defect of the method that oxidation rate is monitored in real time.
To this end, the invention provides a kind of method utilizing high-temperature nano impression instrument to measure material oxidation speed in real time, should Method comprises the steps:
Under target temperature, test specimen is carried out nano-indentation experiment, it is thus achieved that the springform of matrix when described test specimen is not oxidized Amount Es, described test specimen is the real-time elastic modulus E of formed oxide-film-matrix time oxidizedr, and described test specimen oxidized institute shape Oxide thickness is become to reach the elastic modulus E of oxide-film during preset valuef；
According to Es、Ef、Er, real-time depth of cup angle value h be calculated described test specimen oxidized time real-time oxide thickness d, And utilize formulaBe calculated described test specimen oxidized time real-time oxidation rateWherein, Δ t is time interval, Δ d is the changing value of real-time oxide thickness in Δ t time interval.
As preferably, utilize formula 1 and formula 2 be calculated described test specimen oxidized time real-time oxide thickness d, public Formula 1 is:
Wherein, P be described test specimen oxidized time real-time load value, α is the characteristic angle of indenter shape, and h is described test specimen quilt Real-time depth of cup angle value during oxidation；
Formula 2 is:
Wherein, P be described test specimen oxidized time real-time load value, h be described test specimen oxidized time real-time depth of cup angle value,The load obtained for the formula 1 derivation derivative to displacement, α is the characteristic angle of indenter shape, ErReal-time for oxide-film-matrix Elastic modelling quantity；Obtain the load p derivative to displacement h according to formula 1 derivation, carry it into the left end of formula 2, i.e. can get one About Es、Ef、Er, the equation of h, d, and Es、Ef、Er, h be all known, can counter release test specimen oxidized time real-time oxidation Film thickness d.
As preferably, it is thus achieved that Es、ErAnd EfStep include:
Described test specimen is placed in the microscope carrier room of nano-hardness tester, and in described microscope carrier room, is passed through protective gas so that institute State test specimen not oxidized, and described microscope carrier room is risen to described target temperature, more described test specimen is carried out nano-indentation experiment Obtain Es；
The intake or the stopping that reducing described protective gas are passed through described protective gas, so that described surface of test piece starts Oxidized, more described test specimen is carried out nano-indentation experiment acquisition Er；
When oxidized the formed oxide thickness of described test specimen reaches preset value, then the oxide-film of described surface of test piece is entered Row nano-indentation experiment obtains Ef。
As preferably, described protective gas includes argon or nitrogen.
As preferably, before described test specimen is placed in the microscope carrier room of nano-hardness tester, described surface of test piece is polished to full The requirement of foot nano-indentation experiment.
As preferably, it is thus achieved that oxidized the formed oxide thickness of described test specimen reaches the springform of oxide-film during preset value Amount EfStep in, described preset value is dPreset, the depth of cup of described nano-indentation experiment is h, then dPreset≥10h。
As preferably, described target temperature is in the range of 20 DEG C to 1200 DEG C.
Technical solution of the present invention, has the advantage that
What the present invention provided utilizes the method that high-temperature nano impression instrument measures material oxidation speed in real time, passes through nano impress Test specimen elastic modulus E under different conditions measured by instruments、Er、Ef, the film-base in conjunction with nano impress is theoretical, it is achieved that to test specimen The real-time online measuring of the oxidation rate under micron and nanoscale, for research material Surface Oxygen under micro-nano-scale Change behavior has great importance.It is additionally, since the certainty of measurement of instrument up to nanoscale, it is thus possible to realize the oxidation initial stage pair The assessment of material oxidation speed, it is also possible to research material oxidation behavior under room temperature and high temperature.
What the present invention provided utilizes the method that high-temperature nano impression instrument measures material oxidation speed in real time, is protected by regulation The air velocity of gas controls oxidation rate, and the film-base finally combining nano impress is theoretical, it is possible to achieve oxide layer on test specimen The processes such as growth, evolution and then realization are to material measurement of oxidation rate under minute yardstick, room temperature and high-temperature condition.
Accompanying drawing explanation
In order to be illustrated more clearly that the specific embodiment of the invention or technical scheme of the prior art, below will be to specifically In embodiment or description of the prior art, the required accompanying drawing used is briefly described, it should be apparent that, in describing below Accompanying drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not paying creative work Put, it is also possible to obtain other accompanying drawing according to these accompanying drawings.
The method utilizing high-temperature nano impression instrument to measure material oxidation speed in real time that Fig. 1 provides for embodiment of the present invention Flow chart；
Fig. 2 is described test specimen schematic diagram of oxide thickness in formed oxide-film-matrix time oxidized.
In figure: 1-matrix；2-oxide-film；3-indentation test front surface profile；4-indentation test rear surface profile；5-pressure head Schematic diagram；P-test specimen is real-time load value time oxidized；Real-time depth of cup angle value when test specimen is oxidized described in h-；hc-indentation test The contact degree of depth；a1-pressure head projects radius with matrix material contact area；a2-pressure head projects radius with oxide-film contact area.
Detailed description of the invention
Below in conjunction with accompanying drawing, technical scheme is carried out clear, complete description.
As it is shown in figure 1, the method utilizing high-temperature nano impression instrument to measure material oxidation speed in real time that the present embodiment provides Comprise the following steps:
A described surface of test piece is polished to meet the requirement of nano-indentation experiment by ().Its objective is to improve material surface Fineness, to ensure being smoothed out of step b.
B described test specimen is placed in the microscope carrier room of nano-hardness tester by (), and be passed through in described microscope carrier room protective gas with Make described test specimen not oxidized, and described microscope carrier room is risen to described target temperature, more described test specimen is carried out nano impress Experiment obtains Es。
C () reduces the intake of described protective gas or stopping is passed through described protective gas, so that described surface of test piece Start oxidized, more described test specimen is carried out nano-indentation experiment acquisition Er。
D () stops being passed through described protective gas, set the preset value of oxidized the formed oxide thickness of described test specimen, when After reaching preset value, oxide-film to described surface of test piece carries out nano-indentation experiment and obtains E againf。
(e) utilize formula 1 and formula 2 be calculated described test specimen oxidized time real-time oxide thickness d, formula 1 is:
Wherein, P be described test specimen oxidized time real-time load value, α is the characteristic angle of indenter shape, and h is described test specimen quilt Real-time depth of cup angle value during oxidation.
Formula 2 is:
Wherein, P be described test specimen oxidized time real-time load value, h be described test specimen oxidized time real-time depth of cup angle value,The load obtained for the formula 1 derivation derivative to displacement, α is the characteristic angle of indenter shape, ErReality for oxide-film-matrix Time elastic modelling quantity.
F () utilizes formulaBe calculated described test specimen oxidized time real-time oxidation rateWherein, Δ t is Time interval, Δ d is the changing value of real-time oxide thickness in Δ t time interval.
The said method that the present embodiment provides controls oxidation rate by the air velocity of regulation protective gas, finally combines The film of nano impress-base is theoretical, it is possible to achieve the process such as the growth of oxide layer, evolution and then realize material at micro-chi on test specimen The measurement of oxidation rate under degree, room temperature and high-temperature condition.
Above-mentioned formula 1 and formula 2 are nano impress Theoretical Calculation based on film-basal body structure and obtain, and its calculating process is: With reference in the conical pressure head that Fig. 2, Fig. 2 provide, 1 is matrix, and 2 is oxide-film；3 is indentation test front surface profile, and 4 is impression Experiment rear surface profile, 5 be pressure head schematic diagram, P be test specimen oxidized time real-time load value, h be described test specimen oxidized time reality Time depth of cup angle value, hcFor the contact degree of depth of indentation test, for a1Radius, a is projected with matrix material contact area for pressure head2For pressure Head projects radius with oxide-film contact area.
The conical pressure head provided for Fig. 2 has a relationship below:
h = ∫ 0 1 f ′ ( x ) d x 1 - x 2 = ∫ 0 1 a 2 t a n α d x 1 - x 2 = ∫ 0 π 2 a 2 t a n α cos t d t 1 - sin 2 t = π 2 a 2 t a n α
P = E s ha 2 ( cosh - 1 ( a 2 a 1 ) ( a 2 a 1 ) 2 + 1 - 1 - ( a 1 a 2 ) 2 ) + E f ha 2 ( - cosh - 1 ( a 2 a 1 ) ( a 2 a 1 ) 2 + 1 - ( a 1 a 2 ) 2 )
S = d P d h = d P / da 2 d h / da 2
E r = S 2 a 2
Introduce a1、a2Geometrical relationship formula have:
π 2 ( a 2 - a 1 ) t a n α = d
May finally push away:
P = 2 E s h 2 π tan α ( cosh - 1 ( h h - d ) ( h h - d ) 2 + 1 - 1 - ( h - d h ) 2 ) + 2 E f h 2 π tan α ( - cosh - 1 ( h h - d ) ( h h - d ) 2 + 1 - ( h - d h ) 2 ) d P d h = π tan α 4 h E r .
In above-mentioned formula: d be described test specimen oxidized time real-time oxide thickness, h be described test specimen oxidized time real Time depth of cup angle value, EsFor described the test specimen elastic modelling quantity of matrix, E time not oxidizedrBy described test specimen oxidized time formed oxygen Change film-matrix real-time elastic modelling quantity, P be described test specimen oxidized time real-time load value, hcFor the contact degree of depth of indentation test, a1Radius, a is projected with matrix material contact area for pressure head2Projecting radius for pressure head with oxide-film contact area, Δ t is time interval, Δ d is the changing value of real-time oxide thickness in Δ t time interval.
The present embodiment provide method in, protective gas be anti-oxidation occur gas, include but are not limited to argon, Nitrogen etc..And, in step (b), need in microscope carrier room, be passed through enough protective gas, described test specimen just can be made not by oxygen Changing, certainly, the intake of protective gas is relevant with the oxidation resistent susceptibility of the model of used nano-hardness tester and test specimen, ability Field technique personnel are referred to relevant parameter in prior art and set the flow of protective gas.In step (c) or (d), due to The intake or the stopping that reducing described protective gas are passed through described protective gas, and then make test specimen oxidized.
In the method that the present embodiment provides, described preset value refers to carry out oxide-film oxidation during nano-indentation experiment The thickness that film has, its value can be estimated according to material oxidation performance.As preferably, it is thus achieved that described test specimen oxidized institute shape Oxide thickness is become to reach the elastic modulus E of oxide-film during preset valuefStep in, described preset value is dPreset, described nanometer pressure The depth of cup of trace experiment is h, then dPreset≥10h.It is to say, depth of cup selects within the 1/10 of oxide thickness, Record is exactly the elastic modelling quantity of oxide-film.The most why requiring to aoxidize a period of time, oxide thickness reaches preset value, with The precision of nano-hardness tester is relevant, such as nano-hardness tester test accurately range at 30-200nm, it may be necessary to thickness of oxidation film Spend at least more than 300nm and just can do experiment survey oxide-film character.
In said method, nano-hardness tester can monitor continuously pressure head press-in sample and when sample surfaces unloads the load of pressure head Lotus and displacement, the load-displacement data obtained in a complete loading-unloading loop can be used for a lot of 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, the soft or detection analysis of hard material, including optical thin film, microelectronics Plated film, protectiveness is thin etc.；Matrix can be soft or hard material, including metal, alloy, quasiconductor, glass, mineral with have Machine material etc..
And, in the range of very high temperature can be born in the microscope carrier room of nano-hardness tester.It is to say, what the present embodiment provided Method can carry out nano indentation test in different temperatures scope to test specimen, and the size of its temperature range depends on utilized nanometer pressure The performance of trace instrument.At present, the microscope carrier room in nano-hardness tester common on market can withstand up to 1200 DEG C, the most now goes up State the scope of target temperature described in method up to 20 DEG C to 1200 DEG C.
Need it is further noted that control the test specimen state of oxidation mode with the type of nano-hardness tester relevant.Except What the present embodiment provided utilizes protective gas to outside the mode controlling the test specimen state of oxidation, and those skilled in the art can also use In prior art, alternate manner controls the test specimen state of oxidation.
For the present invention provide method for, step (a) it is not necessary to.When test specimen itself has met nanometer pressure The requirement of trace experiment, the most negligible step (a).
Obviously, above-described embodiment is only for clearly demonstrating example, and not restriction to embodiment.Right For those of ordinary skill in the field, can also make on the basis of the above description other multi-form change or Variation.Here without also cannot all of embodiment be given exhaustive.And the obvious change thus extended out or Change among still in the protection domain of the invention.

Claims (7)

1. one kind utilizes the method that material oxidation speed measured in real time by high-temperature nano impression instrument, it is characterised in that the method includes Following steps:
Under target temperature, test specimen is carried out nano-indentation experiment, it is thus achieved that the elastic modulus E of matrix when described test specimen is not oxidizeds, Described test specimen is the real-time elastic modulus E of formed oxide-film-matrix time oxidizedr, and oxidized the formed oxygen of described test specimen Change film thickness and reach the elastic modulus E of oxide-film during preset valuef；
According to Es、Ef、Er, real-time depth of cup angle value h be calculated described test specimen oxidized time real-time oxide thickness d, and profit Use formulaBe calculated described test specimen oxidized time real-time oxidation rateWherein, Δ t is time interval, and Δ d is The changing value of real-time oxide thickness in Δ t time interval.
Method the most according to claim 1, it is characterised in that utilize formula 1 and formula 2 to be calculated described test specimen by oxygen Real-time oxide thickness d during change, formula 1 is:
Wherein, P be described test specimen oxidized time real-time load value, α is the characteristic angle of indenter shape, and h is that described test specimen is oxidized Time real-time depth of cup angle value；
Formula 2 is:
Wherein, P be described test specimen oxidized time real-time load value, h be described test specimen oxidized time real-time depth of cup angle value,For The load obtained according to the formula 1 derivation derivative to displacement, α is the characteristic angle of indenter shape, ErReal-time for oxide-film-matrix Elastic modelling quantity.
Method the most according to claim 1, it is characterised in that obtain Es、ErAnd EfStep include:
Described test specimen is placed in the microscope carrier room of nano-hardness tester, and in described microscope carrier room, is passed through protective gas so that described examination Part is not oxidized, and described microscope carrier room is risen to described target temperature, more described test specimen is carried out nano-indentation experiment acquisition Es；
The intake or the stopping that reducing described protective gas are passed through described protective gas, so that described surface of test piece starts by oxygen Change, more described test specimen is carried out nano-indentation experiment acquisition Er；
When oxidized the formed oxide thickness of described test specimen reaches preset value, then the oxide-film of described surface of test piece is received Rice indentation test obtains Ef。
Method the most according to claim 3, it is characterised in that described protective gas includes argon or nitrogen.
Method the most according to claim 3, it is characterised in that described test specimen is placed in nano-hardness tester microscope carrier room it Before, described surface of test piece is polished to meet the requirement of nano-indentation experiment.
Method the most according to any one of claim 1 to 5, it is characterised in that obtain that described test specimen is oxidized to be formed Oxide thickness reaches the elastic modulus E of oxide-film during preset valuefStep in, described preset value is dPreset, described nano impress The depth of cup of experiment is h, then dPreset≥10h。
Method the most according to any one of claim 1 to 5, it is characterised in that described target temperature is in the range of 20 DEG C To 1200 DEG C.
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CN107506522A (en) * 2017-07-14 2017-12-22 天津大学 The computational methods of shallow nano impress modulus of elasticity based on molecular dynamics simulation
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CN109029279A (en) * 2018-07-23 2018-12-18 清华大学 Deformation measurement method and device
CN109029279B (en) * 2018-07-23 2020-01-10 清华大学 Deformation measuring method and device
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CN109176161A (en) * 2018-10-18 2019-01-11 中国人民解放军国防科技大学 High-surface-quality processing method for aluminum alloy reflector
CN114689644A (en) * 2022-03-29 2022-07-01 清华大学 High-temperature environment parameter measuring method and device

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