CN106706639A - Method for measuring full-field real-time oxidation rate by scanning morphology - Google Patents
Method for measuring full-field real-time oxidation rate by scanning morphology Download PDFInfo
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- CN106706639A CN106706639A CN201611179372.0A CN201611179372A CN106706639A CN 106706639 A CN106706639 A CN 106706639A CN 201611179372 A CN201611179372 A CN 201611179372A CN 106706639 A CN106706639 A CN 106706639A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B11/00—Measuring arrangements characterised by the use of optical techniques
- G01B11/02—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness
- G01B11/06—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B11/00—Measuring arrangements characterised by the use of optical techniques
- G01B11/02—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness
- G01B11/06—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material
- G01B11/0616—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material of coating
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
- G01N21/8422—Investigating thin films, e.g. matrix isolation method
Abstract
The invention provides a method for measuring the full-field real-time oxidation rate by scanning morphology. Real-time scanning on the material surface morphology is achieved through an in-situ scanning probe imaging function of a scanning instrument, and then full-field oxidation rate measurement of the material surface in a high-temperature environment is achieved. The method comprises the steps that a marker is prefabricated on the surface of a test piece, then the temperature is increased to a target temperature, the test piece surface morphology including the prefabricated marker is scanned as the initial morphology, and in the process, protective gas is introduced to prevent the prefabricated marker and the portion, under the prefabricated marker, of the test piece surface from being oxidized; introduction of the protective gas is stopped, real-time on-line recording on the test piece surface oxidation morphology is conducted through the in-situ scanning imaging function, the initial morphology and the real-time morphology of the test piece surface before and after oxidation are compared and analyzed, related data is extracted, and the oxidation rate of any portion of the test piece surface is calculated according to the formula. A new method is provided for studying the oxidation behavior of the material in micro-nano scale at different temperatures.
Description
Technical field
The present invention relates to a kind of method by scanning the real-time oxidation rate of the topography measurement whole audience, belong to Experiments of Machanics technology
Field.
Background technology
Material is the important foundation of human material's civilization, and it supports the progress of other every new technologies, space flight and aviation, sea
The national economy production field such as foreign engineering, life science and energy project is required for all kinds of 26S Proteasome Structure and Function materials.With science
The development of technology and the realization of some extreme conditions, various new materials are developed rapidly, and are widely used in new and high technology
Field and some extreme Service Environments, reliability, performance of the material being used for etc. propose more strict requirements.
By taking space flight and aviation thermal protection field as an example, as engine develops to thrust-weight ratio high, the design inlet temperature of engine is constantly carried
Height, inlet temperature is also substantially improved before turbine, and requirement higher is proposed to engine thermal end pieces high-temperature structural material, research
High-temperature structural material and heat barrier coat material oxidation mechanism in high temperature environments are started to improving its temperature operating limit, raising
Machine operating temperature has extremely important effect.Therefore, the mechanism of the oxidation behavior to material under room temperature and high-temperature condition is ground
Study carefully and be extremely necessary.
Current research material high-temperature oxydation can use various methods, including oxidation kinetics measurement and oxidation reaction product shape
Looks are detected.These methods are based on oxidizing process dynamics, by composition and pattern to product, and to metal or alloy
Matrix material carefully detected, probes into the essence i.e. oxidation mechanism of oxidizing process.Above-mentioned oxidation kinetics measuring method includes
By the weight change in consecutive weighings test specimen oxidizing process, or oxidation is measured by measuring the wear rate of reacting gas
Reaction rate；Product Shape measure means then include using SEM, x-ray spectrometer or transmitted electron
Microscope carrys out small shape characteristic or the product composition of analytical reactions product.But in current research, lack in micron
With the method that Nano grade carries out the whole audience, real-time monitoring to material oxidation process, cause the observation of oxidizing process and analysis shortage
The real-time Evolution Data of micro-scale.
Nano-indentation experiment is a kind of important laboratory facilities for measuring material Micro Mechanical Properties at present.It is by continuous prison
Pressure-measuring head press-in sample and from sample surfaces unload this complete loading-unloading during load-displacement curves, point
Analysis extracts many micromechanics of material, for example：Load-deformation curve, creep, fatigue, storage modulus, loss mould
Amount, fracture toughness, elastic work, plastic work done etc..Can be used for metal, alloy, semiconductor, soft material, thin-film material, biomaterial,
The research of thin film basal body system etc..In the last few years, with the raising and progress of instrument and equipment precision and resolution ratio etc., nanometer pressure
The application temperature of trace technology is also being stepped up, and is capable of achieving the simulation to the extreme service temperature of portion of material.Meanwhile, nano impress
The in-situ scanning probe microscope imaging function of instrument can realize that carrying out real-time online to the evolutionary process of material surface pattern sweeps
Retouch, record the processes such as growth, the evolution of oxide layer, oxidizing process and mechanism for research material in micron and nanoscale are provided
Effective analysis means.
The content of the invention
It is an object of the invention to provide a kind of method by scanning the real-time oxidation rate of the topography measurement whole audience, the method is led to
The in-situ scanning probe microscope imaging function for crossing nano-hardness tester is realized to material surface including complete including prefabricated label
The real time scan of pattern and record, so realize to material in minute yardstick, normal temperature and under high-temperature condition oxidation rate measurement.
The present invention compared with prior art, with advantages below and high-lighting effect：Visited by using the in-situ scanning of nano-hardness tester
The real-time in-situ scanning including the surface topography including prefabricated label to material surface of pin microscope imaging functional realiey, enters
And realize the real-time measurement of full field of oxidation rate to material and structure under micron and nanoscale.The certainty of measurement of instrument
Up to nanoscale, it is possible to achieve assessment of the oxidation initial stage to material and structure oxidation rate, it is also possible to which research material and structure exist
Oxidation behavior under room temperature and high temperature.
The present invention provides a kind of method by scanning the real-time oxidation rate of the topography measurement whole audience, comprises the following steps：
1) after treatment surface of test piece, select region to be studied in surface of test piece and prefabricated label is set, wherein, prefabricated mark
Note thing protrusion surface of test piece, and do not aoxidized under target temperature；
2) under conditions of protective gas is passed through, with scanner under target temperature to including prefabricated label, treat
Survey region carries out real-time in-situ scanning, and initial topographical information in the range of writing scan in interior surface of test piece；
3) stop being passed through protective gas, surface of test piece starts oxidation, to including including prefabricated label, region to be studied
Surface of test piece carry out real-time in-situ scanning, and real-time topographical information in the range of writing scan；
4) the elemental height H of prefabricated label is extracted from initial topographical information0And the area to be studied of surface of test piece
The elemental height h of any point in domain0, the real-time height H of prefabricated label is extracted from real-time topographical information1And it is to be studied
The real-time height h of any point in region1；
5) difference in height using any point in region to be studied in initial topographical information, real-time topographical information obtains first
Height difference, the second height difference is obtained using difference in height of the prefabricated label in initial topographical information, real-time topographical information,
The difference of the first height difference and the second height difference is calculated, the oxide-film real-time thickness d of any in region to be studied is obtained, and
Binding time is spaced, and obtains the real-time oxidation rate w of any point in region to be studied, and then can obtain scanning the real-time oxygen of the whole audience
Change speed,
D=(h1-h0)-(H1-H0) formula 1
Wherein, Δ t is time interval, and Δ d is the change in Δ t time interval internal oxidition film thicknesses.
Preferably, step 1) in the mode for the treatment of surface of test piece be included in surface of test piece and prepare micro-structural, or sanding and polishing.
Preferably, step 1) in prefabricated label be arranged on around region to be studied, region to be studied and pre- must be ensured
Label processed is in sweep limits.
Preferably, the prefabricated label includes steady oxide, and the material not aoxidized under target temperature.
Preferably, step 2) in protective gas include at least one of argon gas, nitrogen gas.
Preferably, step 2), step 3) in scan method include contact mode probe scanning, percussion mode probe scanning
At least one of scan method.
Preferably, scanner includes nano-hardness tester.
Preferably, step 2) in target temperature range for normal temperature to 1000 DEG C.
Preferably, the preparation method of prefabricated label includes at least one of sputtering, photoetching, deposition, plating method.
Brief description of the drawings
Embodiment is described by with reference to accompanying drawings below, features described above of the invention and technological merit will become
More understand and be readily appreciated that.
Fig. 1 be the present embodiments relate to the method by scanning the real-time oxidation rate of the topography measurement whole audience experiment stream
Cheng Tu；
Fig. 2 is the selected basic principle schematic diagram of prefabricated marker location；
Fig. 3 a are the schematic diagram of scanning surface of test piece before oxidation；
Fig. 3 b are the initial shape appearance figure of surface of test piece obtained using scanning probe microscopy imaging function；
After Fig. 4 a are to aoxidize, the schematic diagram of surface of test piece is scanned；
After Fig. 4 b are to aoxidize, the surface of test piece pattern in real time in situ obtained using scanning probe microscopy imaging function
Figure；
In figure, the prefabricated labels of 1-；2- scans probe；The initial pattern of 4- surface of test piece；5- oxide-films；6- surface of test piece realities
When pattern.
Specific embodiment
It is of the present invention a kind of by scanning the real-time oxidation rate of the topography measurement whole audience to describe below with reference to the accompanying drawings
Method embodiment.One of ordinary skill in the art will recognize, in feelings without departing from the spirit and scope of the present invention
Under condition, described embodiment can be modified with a variety of modes or its combination.Therefore, accompanying drawing and description are at this
It is illustrative in matter, is not intended to limit the scope of the claims.Additionally, in this manual, accompanying drawing do not press than
Example draws, and identical reference represents identical part.
The signified whole audience refers to the every bit in region to be studied in the present invention, is different to the measurement of single-point and right
The measurement of Zone Full equalization, measurement of full field refers to treat every bit in survey region all to realize measurement.
A kind of experiment flow by scanning the method for the real-time oxidation rate of the topography measurement whole audience that Fig. 1 is provided for the present invention
Figure, its concrete operation step is as follows：
A. binding purpose processes the surface of test specimen 10, and such as preparing oxidation of the micro-structural to study micro-structural thereon drills
Change process, or sanding and polishing is with research material integrated oxidation evolutionary process, and selected region to be studied 102, the region to be studied
102 can be the part surface of the test specimen of the micro-structural or sanding and polishing for preparing, and take up an official post on the surface in test specimen region to be studied and take
One point A, vertical dotted line is the position of point A such as in Fig. 3, Fig. 4, below each step will measurement point location A oxide thickness；
B. prefabricated label 101 is set in surface of test piece.The selected basic principle such as institute of accompanying drawing 2 of prefabricated marker location
Show：Prefabricated label 101 need to be arranged on surface of test piece according to the size of sweep limits, be distributed in around region to be studied, it is ensured that
High-temperature nano impression instrument can be scanned to the surface of test piece comprising prefabricated label in same width scan image, in figure in dotted line i.e.
Be sweep limits, take up an official post on the surface in the region to be studied of test specimen and take a point A, below each step will be with any in region to be studied
Illustrated as a example by the oxide thickness of point location A.Prefabricated label is not aoxidized under target temperature, can select Stable Oxygen
Compound etc..The preparation method of prefabricated label includes sputtering, photoetching, deposition, plating etc. so that prefabricated label protrudes test specimen table
Face；
C. under conditions of protective gas is passed through, test specimen is integrally warming up to target temperature, target temperature range is normal
Temperature to 1000 DEG C, with high-temperature nano impression instrument to being carried out in real time including the surface of test piece including prefabricated label, region to be studied
In-situ scanning, as shown in Figure 3,4, scanning probe is scanned perpendicular to surface of test piece, and the initial shape in the range of writing scan
Looks information, wherein protective gas can be argon gas or nitrogen or other inert gases；
D. stop being passed through protective gas, material surface starts oxidation, to including including prefabricated label, region to be studied
Surface of test piece carry out real-time in-situ scanning, and the real-time topographical information in the range of writing scan, in Fig. 3, Fig. 4,4 is test specimen
The initial pattern in surface, 6 is the real-time pattern of surface of test piece；
E. contrast material aoxidizes forward and backward surface topography, and the initial of prefabricated label is extracted from initial topographical information
Height H0And the elemental height h of surface of test piece location A0, prefabricated label is extracted from the real-time topographical information of surface of test piece
Real-time height H1And the real-time height h of location A1；
F. the difference in height using location A in initial topographical information, real-time topographical information obtains the first height difference, utilizes
Difference in height of the prefabricated label in initial topographical information, real-time topographical information obtains the second height difference, calculates the first height
Difference and the difference of the second height difference, obtain the oxide-film real-time thickness d of location A, and binding time is spaced, and obtains to be studied
The real-time oxidation rate w of any point in region.
Namely use formula d=(h1-h0)-(H1-H0) calculate location A real-time oxide thickness d, in real time oxidation speed
Rate can useIt is calculated, and then can obtain the real-time oxidation rate of whole audience optional position, you can obtains scanning the whole audience
Real-time oxidation rate.
Wherein, d is oxide-film real-time thickness, H0It is the elemental height of prefabricated label, h0It is the elemental height of location A, H1
It is the real-time height of prefabricated label, h1It is the real-time height of location A, Δ t is time interval, and Δ d is in Δ t time intervals
The change of oxide thickness.
The formula proving of real-time oxide thickness d is as follows：
Fig. 3 a are that oxidation is preceding to be scanned including the test specimen including prefabricated label, region to be studied using high-temperature nano impression instrument
The schematic diagram on surface, Fig. 3 b are including prefabricated mark using the scanning probe microscopy imaging function acquisition of high-temperature nano impression instrument
Note thing is in the interior initial pattern of surface of test piece.
With reference to Fig. 3, to being obtained before oxidation including the initial pattern of surface of test piece including prefabricated label by simple
Data processing, it is zero elevation to select prefabricated label bottom, and the height in this coordinate system is represented with subscript ' m '.Then initial pattern
The elemental height coordinate of prefabricated label in coordinate system(be on the occasion of), location A is initial in initial pattern coordinate system
Height coordinate(can be on the occasion of also can be negative value).
After Fig. 4 a are to aoxidize, the schematic diagram including the surface of test piece including prefabricated label is scanned；Fig. 4 b are generation
After oxidation, the shape in real time in situ of the surface of test piece including prefabricated label is included using the acquisition of scanning probe microscopy imaging function
Looks.
As shown in fig. 4 a, wherein the part as oxide layer 5 represented with hatching.With reference to Fig. 4, to the bag obtained after oxidation
Prefabricated label is included in the interior real-time pattern of surface of test piece by simple data processing, the bottom of now prefabricated label is selected
It is zero elevation, the height in this coordinate system is represented with subscript ' n '.Then in real-time pattern coordinate system prefabricated label real-time height
Coordinate(can be on the occasion of also can be negative value), the real-time height coordinate of location A in real-time pattern coordinate system(can
It is on the occasion of also being negative value).
Surface of test piece start oxidation after, it is prefabricated mark object area below surface of test piece due to prefabricated marking thing covering not
Aoxidize, prefabricated label is not also aoxidized in itself.The elemental height coordinate of known label prefabricated before oxidation isThe real-time height coordinate of prefabricated label is after oxidationTherefore in real-time pattern coordinate system, zero before oxidation is flat
The coordinate in face is：
Therefore, in real-time pattern coordinate system, the coordinate of the elemental height of location A meets formula 3 before oxidation：
Further derive, can obtain in real-time pattern coordinate system, the coordinate of the elemental height of location A is before oxidation：
Therefore the real-time oxide thickness of whole audience location A is：
In above-mentioned formula：D is oxide-film real-time thickness, H0It is the elemental height of prefabricated label, h0It is initial for location A
Highly, H1It is the real-time height of prefabricated label, h1It is the real-time height of location A,It is prefabricated mark in initial pattern coordinate system
Remember the elemental height coordinate of thing,It is the elemental height coordinate of location A in initial pattern coordinate system,It is real-time pattern coordinate
The real-time height coordinate of prefabricated label in system,It is the real-time height coordinate of location A in real-time pattern coordinate system,For real-time
The coordinate of zero plane before being aoxidized in pattern coordinate system,It is location A elemental height before being aoxidized in real-time pattern coordinate system
Coordinate.
Evolution of the present invention using the in-situ scanning probe microscope imaging function of nano-hardness tester to material surface pattern
Process carries out real-time online scanning, records growth, the evolutionary process of oxide layer, and the real-time thickness of oxide-film is obtained using formula
Degree, and then obtain the real-time oxidation rate of whole audience optional position.The present invention is micro- using the in-situ scanning probe of nano-hardness tester
Mirror imaging function realizes the real-time in-situ scanning including the surface topography including prefabricated label to material surface, and then realizes
The real-time online measuring of the oxidation rate to material and structure under micron and nanoscale.The certainty of measurement of instrument is reachable to be received
Meter level, it is possible to achieve oxidation assessment of the initial stage to material and structure oxidation rate, it is also possible to research material and structure in room temperature and
Oxidation behavior under high temperature.
The preferred embodiments of the present invention are the foregoing is only, is not intended to limit the invention, for those skilled in the art
For member, the present invention can have various modifications and variations.All any modifications within the spirit and principles in the present invention, made,
Equivalent, improvement etc., should be included within the scope of the present invention.
Claims (9)
1. a kind of method by scanning the real-time oxidation rate of the topography measurement whole audience, it is characterised in that comprise the following steps：
1) after treatment surface of test piece, select region to be studied in surface of test piece and prefabricated label is set, wherein, prefabricated label
Protrusion surface of test piece, and do not aoxidized under target temperature；
2) under conditions of protective gas is passed through, with scanner under target temperature to including prefabricated label, to be studied
Region carries out real-time in-situ scanning, and initial topographical information in the range of writing scan in interior surface of test piece；
3) stop being passed through protective gas, surface of test piece starts oxidation, to including the examination including prefabricated label, region to be studied
Part surface carries out real-time in-situ scanning, and real-time topographical information in the range of writing scan；
4) the elemental height H of prefabricated label is extracted from initial topographical information0And appoint in the region to be studied of surface of test piece
The elemental height h of a bit0, the real-time height H of prefabricated label is extracted from real-time topographical information1And in region to be studied
The real-time height h of any point1；
5) difference in height using any point in region to be studied in initial topographical information, real-time topographical information obtains the first height
Difference, the second height difference is obtained using difference in height of the prefabricated label in initial topographical information, real-time topographical information, is calculated
First height difference and the difference of the second height difference, obtain the oxide-film real-time thickness d of any in region to be studied, and combine
Time interval, obtains the real-time oxidation rate w of any point in region to be studied, and then can obtain scanning the real-time oxidation speed of the whole audience
Rate,
D=(h1-h0)-(H1-H0) formula 1
Wherein, Δ t is time interval, and Δ d is the change in Δ t time interval internal oxidition film thicknesses.
2., according to a kind of method by scanning the real-time oxidation rate of the topography measurement whole audience described in claim 1, its feature exists
In：Step 1) in the mode for the treatment of surface of test piece be included in surface of test piece and prepare micro-structural, or sanding and polishing.
3., according to a kind of method by scanning the real-time oxidation rate of the topography measurement whole audience described in claim 1, its feature exists
In：Step 1) in prefabricated label be arranged on around region to be studied, must ensure that region to be studied and prefabricated label are located
In in sweep limits.
4., according to a kind of method by scanning the real-time oxidation rate of the topography measurement whole audience described in claim 1, its feature exists
In：The prefabricated label includes steady oxide, and the material not aoxidized under target temperature.
5., according to a kind of method by scanning the real-time oxidation rate of the topography measurement whole audience described in claim 1, its feature exists
In：Step 2) in protective gas include at least one of argon gas, nitrogen gas.
6., according to a kind of method by scanning the real-time oxidation rate of the topography measurement whole audience described in claim 1, its feature exists
In：Step 2), step 3) in scan method include that at least one of contact mode probe scanning, percussion mode probe scanning are swept
Retouch method.
7., according to a kind of method by scanning the real-time oxidation rate of the topography measurement whole audience described in claim 1, its feature exists
In：Scanner includes nano-hardness tester.
8., according to a kind of method by scanning the real-time oxidation rate of the topography measurement whole audience described in claim 1, its feature exists
In：Step 2) in target temperature range for normal temperature to 1000 DEG C.
9. according to a kind of method by scanning the real-time oxidation rate of the topography measurement whole audience described in claim 1 or 3, its feature
It is：The preparation method of prefabricated label includes at least one of sputtering, photoetching, deposition, plating method.
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| CN108519177A (en) * | 2018-05-16 | 2018-09-11 | 清华大学 | A kind of method and device measuring oxidation film internal stress by prefabricated marker |
| CN109029279A (en) * | 2018-07-23 | 2018-12-18 | 清华大学 | Deformation measurement method and device |
| CN109297420A (en) * | 2018-11-26 | 2019-02-01 | 瓦房店轴承集团国家轴承工程技术研究中心有限公司 | The detection method of bearing roller surface melanism film film thickness |
| CN114689644A (en) * | 2022-03-29 | 2022-07-01 | 清华大学 | High-temperature environment parameter measuring method and device |
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| CN114689644A (en) * | 2022-03-29 | 2022-07-01 | 清华大学 | High-temperature environment parameter measuring method and device |
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