CN108169262A - A kind of method of Fast Calibration metal crystal face - Google Patents
A kind of method of Fast Calibration metal crystal face Download PDFInfo
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- CN108169262A CN108169262A CN201711384239.3A CN201711384239A CN108169262A CN 108169262 A CN108169262 A CN 108169262A CN 201711384239 A CN201711384239 A CN 201711384239A CN 108169262 A CN108169262 A CN 108169262A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20058—Measuring diffraction of electrons, e.g. low energy electron diffraction [LEED] method or reflection high energy electron diffraction [RHEED] method
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/203—Measuring back scattering
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
- G01N2223/053—Investigating materials by wave or particle radiation by diffraction, scatter or reflection back scatter
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
- G01N2223/056—Investigating materials by wave or particle radiation by diffraction, scatter or reflection diffraction
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
- G01N2223/056—Investigating materials by wave or particle radiation by diffraction, scatter or reflection diffraction
- G01N2223/0565—Investigating materials by wave or particle radiation by diffraction, scatter or reflection diffraction diffraction of electrons, e.g. LEED
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Abstract
The present invention provides a kind of methods of Fast Calibration metal crystal face, the metal is, for example, copper foil, judge crystal face using the thickness of oxide of copper surface formation after high-temperature oxydation and the relationship of color, different crystal faces are due to oxidation rate difference, sull just has different thickness, and contrast (color) thus then has different difference.The difference of different crystal faces optical microphotograph just under can be clearly seen that.Method proposed by the present invention by very shirtsleeve operation, can distinguish different crystal faces under an optical microscope.
Description
Technical field
Method more particularly to a kind of optically Fast Calibration copper the present invention relates to a kind of Fast Calibration metal crystal face
The method of crystal face.
Background technology
Copper is that a kind of usage history is long and widely used metal.It has very excellent heat conduction and conduction property,
Therefore as metal material preferred in power transmission and electronic device applications, especially in the information age of high speed development, copper
Play particularly important role.The crystal plane structure of copper is cubic lattice, and common crystal face has (100), (111), (410) etc.
Deng.Its crystal face is different, can show widely different even a completely different physico-chemical property.The crystal face letter of sample is only understood
Breath, can just continue to study accordingly.Therefore in production application and scientific research, the crystal face for demarcating copper is particularly important
One technical work.
The method of calibration copper crystal face common at present is all based on greatly diffraction method, including：X-ray diffraction method (XRD),
Electron backscatter diffraction method (EBSD) and low-energy electron diffraction method (LEED) etc..These methods all rely on the instrument to involve great expense
Device equipment, sample preparation is complicated for operation, and calibration process is time-consuming, can not realize economy and rapidly crystal face calibration.Therefore, a kind of letter is found
The technology of single Fast Calibration copper crystal face plays particularly important effect in the research and application of copper.
Invention content
The present invention proposes a kind of method of optically Fast Calibration copper crystal face, and described method includes following steps：
(1) metal sample to be measured is positioned in apparatus for baking and carries out heated oxide；
(2) after the completion of metal sample oxidation to be measured, with optics microscope direct observing, you can observe metal-like to be measured
The colouring information that product are shown；
(3) crystal face of metal sample to be measured is determined according to the correspondence between metal crystal face and colouring information.
Preferably, following normalization step is further included before step (1)：
S1：Standard metal specimen with different crystal faces is demarcated with diffraction approach, wherein, the diffraction approach includes X
Ray diffraction method (XRD), electron backscatter diffraction method (EBSD) or low-energy electron diffraction method (LEED)；
S2：Standard metal specimen is positioned in apparatus for baking and carries out heated oxide；
S3：After the completion of standard metal specimen oxidation, with optics microscope direct observing, you can observe with different crystal faces
The different colours information that shows of standard metal specimen；
S4：Establish the correspondence between metal crystal face and colouring information.
Preferably, the apparatus for baking is thermal station, oven or CVD tube furnaces.
Preferably, the temperature of the heated oxide is 100 DEG C~250 DEG C, and the time is 30-90 minutes.
Preferably, the metal sample to be measured is the monocrystalline copper foil with certain crystal face.
Preferably, the standard metal specimen is the monocrystalline copper foil with certain crystal face.
The present invention judges crystal face using the thickness of oxide of copper surface formation after high-temperature oxydation and the relationship of color, no
With crystal face due to oxidation rate difference, sull just has different thickness, and contrast (color) thus then has different
Difference.The difference of different crystal faces optical microphotograph just under can be clearly seen that.Method proposed by the present invention, by very simple
Single operation, can distinguish different crystal faces under an optical microscope.
The advantage of the invention is that：
1. the present invention is a kind of method of optically Fast Calibration copper crystal face；
2. the present invention utilizes common thermal station, oven, CVD tube furnaces etc. to copper foil heated oxide, easy to operate；
3. the present invention can distinguish different crystal faces easily under an optical microscope；
4. all fairly simple, the required instrument (heating units such as oven, light microscope) of operation according to the present invention
It is typical, it is time saving to save trouble.
5. oxidizing temperature according to the present invention and time can be by operator's sets itselfs, as long as ensureing to do a crystal face
With the correlation calibration of color.
Description of the drawings
Fig. 1 (a) is copper (100) crystal face in 120 DEG C of air oxidations 1 hour as a result, Fig. 1 (b) is that the sample is corresponding
LEED。
Fig. 2 (a) is copper (111) crystal face in 120 DEG C of air oxidations 1 hour as a result, Fig. 2 (b) is that the sample is corresponding
LEED。
Fig. 3 (a) is copper (410) crystal face in 120 DEG C of air oxidations 1 hour as a result, Fig. 3 (b) is that the sample is corresponding
LEED。
Specific embodiment
The present invention is described in further details with reference to specific embodiment, the raw material can unless otherwise instructed
It is obtained from open commercial sources.
Embodiment one：A kind of method of optically Fast Calibration copper crystal face, includes the following steps：
(1), by copper sample sample preparation to be measured；
(2), sample to be tested is positioned in oven, heated oxide 30-90 minutes at 100 DEG C~250 DEG C；
(3), after the completion of sample to be tested oxidation, with optics microscope direct observing, you can see what different crystal faces were shown
Different colours；
(4) crystal face of copper sample to be measured is determined according to the correspondence between copper crystal face and colouring information.
Wherein, copper sample can be easily obtained.LEED is done when obtaining copper sample simultaneously to compare.The heating dress
It puts including thermal station, oven, CVD tube furnaces etc..
It, under an optical microscope can be with after the copper foil of different crystal faces is put 100 DEG C in air~250 DEG C heated oxides
It is clearly seen that different colors.
Sample obtained is firstly placed on optical microphotograph Microscopic observation, it can be found that the color of different crystal faces is quite similar, nothing
Method is distinguished, when sample in an oven 120 DEG C of heated oxides after sixty minutes, it can be found that different colors, by color and LEED
Crystal face calibration result compare, so as to obtain different crystal faces this condition oxidation under standard results.Therefore,
Following normalization step is further included before above-mentioned demarcating steps (one)：
1st, by the X-ray diffraction method (XRD) of the copper sample with different crystal faces, electron backscatter diffraction method (EBSD) or low
Energy method of electron diffraction (LEED) is demarcated, and specifically may include the copper sample of the different crystal faces such as copper (100), copper (111), copper (410)
Product；
2nd, after the copper sample for determining each crystal face, barbecue process is carried out to each copper sample with heated oxide；Preferably, institute
The baking process stated carries out in thermal station, oven or CVD tube furnaces, and temperature setting is at 100 DEG C~250 DEG C, time 30-90
Minute；
3rd, to the copper sample optics microscope direct observing of different crystal faces, you can see the difference that different crystal faces are shown
Color；
4th, the correspondence between different colours and crystal face that different crystal faces are shown is established.
Wherein, it can record the correspondence between colouring information and crystal face in minute book to establish correspondence, also may be used
Being recorded in a manner of taking pictures；Preferably, microscope photo is inputted in computer equipment, by taking color equipment can
Check corresponding colouring information, such as RGB information or CMYK information, Lab information.
Wherein, under the conditions of above-mentioned 120 DEG C of air oxidations 1 hour, the corresponding colouring information of copper (100) crystal face is believed with RGB
Breath is expressed as：R values are 240-250, and G values are 100-150, and B values are 30-60；Copper (111) crystal face is corresponding after oxidation
Colouring information is expressed as with RGB information：R values are 245-255, and G values are 200-220, and B values are 150-180；Copper (410)
Corresponding colouring information is expressed as crystal face with RGB information after oxidation：R values are 210-240, and G values are 40-70, and B values are
60-80。
It should be noted that although above example and tests below one to three are copper for example, other metals
The crystal plane direction of paillon can also be measured with same method.
Experiment one：A kind of method of optically Fast Calibration copper crystal face of this experiment is to carry out according to the following steps：
(1), by copper (100) sample sample preparation；
(2), sample is positioned in oven, heated oxide 60 minutes at 120 DEG C；
(3), after the completion of sample oxidation, with optics microscope direct observing, it can be seen that the color that crystal face is shown.
Under this experimental condition, oxygen during heating in air easily aoxidizes copper, generates copper oxide film, optics contrast
It changes, color can observe.
Experiment two：A kind of method of optically Fast Calibration copper crystal face of this experiment is to carry out according to the following steps：
(1), by copper (111) sample sample preparation；
(2), sample is positioned in oven, heated oxide 60 minutes at 120 DEG C；
(3), after the completion of sample oxidation, with optics microscope direct observing, you can see the color that crystal face is shown.
Under this experimental condition, oxygen during heating in air easily aoxidizes copper, generates copper oxide film, optics contrast
It changes, color can observe.
Experiment three：A kind of method of optically Fast Calibration copper crystal face of this experiment is to carry out according to the following steps：
(1), by copper (410) sample sample preparation；
(2), sample is positioned in oven, heated oxide 60 minutes at 120 DEG C；
(3), after the completion of sample oxidation, with optics microscope direct observing, you can see the color that crystal face is shown.
Under this experimental condition, oxygen during heating in air easily aoxidizes copper, generates copper oxide film, optics contrast
It changes, color can observe.
As can be seen that the copper on different crystal faces can obtain not after peroxidating in above-mentioned experiment one to the method for experiment three
Same color can be used for advantageously demarcating crystal face rapidly.
Claims (6)
- A kind of 1. method of Fast Calibration metal crystal face, which is characterized in that described method includes following steps：(1) metal sample to be measured is positioned in apparatus for baking and carries out heated oxide；(2) after the completion of metal sample oxidation to be measured, with optics microscope direct observing, you can observe metal sample table to be measured The colouring information revealed；(3) crystal face of metal sample to be measured is determined according to the correspondence between metal crystal face and colouring information.
- 2. according to the method described in claim 1, it is characterized in that, following normalization step is further included before step (1)：S1：Standard metal specimen with different crystal faces is demarcated with diffraction approach, wherein, the diffraction approach includes X ray Diffraction approach (XRD), electron backscatter diffraction method (EBSD) or low-energy electron diffraction method (LEED)；S2：Standard metal specimen is positioned in apparatus for baking and carries out heated oxide；S3：After the completion of standard metal specimen oxidation, with optics microscope direct observing, you can observe the mark with different crystal faces The different colours information that metalloid sample is shown；S4：Establish the correspondence between metal crystal face and colouring information.
- 3. method according to claim 1 or 2, which is characterized in that the apparatus for baking is thermal station, oven or CVD tubular types Stove.
- 4. method according to claim 1 or 2, which is characterized in that the temperature of the heated oxide is 100 DEG C~250 DEG C, Time is 30-90 minutes.
- 5. according to the method described in claim 1, it is characterized in that, the metal sample to be measured is the copper with certain crystal face Foil.
- 6. according to the method described in claim 2, it is characterized in that, the standard metal specimen is the copper with certain crystal face Foil.
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| CN201711384239.3A CN108169262B (en) | 2017-12-20 | 2017-12-20 | Method for rapidly calibrating metal crystal face |
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| CN201711384239.3A CN108169262B (en) | 2017-12-20 | 2017-12-20 | Method for rapidly calibrating metal crystal face |
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| CN108169262B CN108169262B (en) | 2020-06-02 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113092463A (en) * | 2019-12-23 | 2021-07-09 | 北京大学 | Method for detecting two-dimensional material grain boundary |
Citations (5)
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|---|---|---|---|---|
| CN101659004A (en) * | 2009-09-11 | 2010-03-03 | 四川大学 | Orientation method of copper single crystal |
| CN101949810A (en) * | 2010-08-12 | 2011-01-19 | 中国石油天然气集团公司 | Method for identifying and assessing needle-like ferrite pipe line steel tissues |
| CN102364323A (en) * | 2011-10-18 | 2012-02-29 | 广东电网公司电力科学研究院 | Display method of tempered martensitic steel carbide colour metallography and electrothermal metallographic chromogenic device special for display method |
| CN102721715A (en) * | 2012-06-07 | 2012-10-10 | 山西太钢不锈钢股份有限公司 | Dual-phase stainless steel crystalline grain structure display method |
| CN109668839A (en) * | 2017-10-13 | 2019-04-23 | 中国科学院化学研究所 | A method of identifying copper sheet crystal boundary and crystal face |
-
2017
- 2017-12-20 CN CN201711384239.3A patent/CN108169262B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101659004A (en) * | 2009-09-11 | 2010-03-03 | 四川大学 | Orientation method of copper single crystal |
| CN101949810A (en) * | 2010-08-12 | 2011-01-19 | 中国石油天然气集团公司 | Method for identifying and assessing needle-like ferrite pipe line steel tissues |
| CN102364323A (en) * | 2011-10-18 | 2012-02-29 | 广东电网公司电力科学研究院 | Display method of tempered martensitic steel carbide colour metallography and electrothermal metallographic chromogenic device special for display method |
| CN102721715A (en) * | 2012-06-07 | 2012-10-10 | 山西太钢不锈钢股份有限公司 | Dual-phase stainless steel crystalline grain structure display method |
| CN109668839A (en) * | 2017-10-13 | 2019-04-23 | 中国科学院化学研究所 | A method of identifying copper sheet crystal boundary and crystal face |
Non-Patent Citations (1)
| Title |
|---|
| 高婕 等: "晶格取向对铜氧化失效的影响", 《2009年全国电子电镀及表面处理学术交流会论文集》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113092463A (en) * | 2019-12-23 | 2021-07-09 | 北京大学 | Method for detecting two-dimensional material grain boundary |
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