CN108169262B - Method for rapidly calibrating metal crystal face - Google Patents
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- CN108169262B CN108169262B CN201711384239.3A CN201711384239A CN108169262B CN 108169262 B CN108169262 B CN 108169262B CN 201711384239 A CN201711384239 A CN 201711384239A CN 108169262 B CN108169262 B CN 108169262B
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- 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
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- 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
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
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- G01N2223/056—Investigating materials by wave or particle radiation by diffraction, scatter or reflection diffraction
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- 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 invention provides a method for rapidly calibrating a crystal face of a metal, wherein the metal is copper foil, the crystal face is judged by utilizing the relation between the thickness and the color of an oxide formed on the surface of the copper after high-temperature oxidation, and due to different oxidation rates of different crystal faces, an oxide film has different thicknesses, so that the contrast (color) is different. The difference of different crystal planes can be clearly seen under optical microscopy. The method provided by the invention can distinguish different crystal faces under an optical microscope through very simple operation.
Description
Technical Field
The invention relates to a method for quickly calibrating a metal crystal face, in particular to a method for quickly calibrating a copper crystal face by an optical method.
Background
Copper is a metal that has a long history of use and is widely used. It has very excellent heat and electrical conductive properties, and thus becomes a preferred metal material for power transmission and electronic device applications, and particularly, copper plays an extremely important role in the information age of rapid development. The crystal plane structure of copper is cubic, and the common crystal planes are (100), (111), (410) and the like. The crystal planes of the crystal grains are different, and show greatly different or completely different physicochemical properties. Only if the crystal face information of the sample is clear, the corresponding research can be continued. Therefore, in production application and scientific research, the calibration of the crystal face of copper is an especially important technical work.
Most of the current common methods for calibrating copper crystal faces are based on diffraction methods, and comprise the following steps: x-ray diffraction (XRD), Electron Back Scattering Diffraction (EBSD), and Low Energy Electron Diffraction (LEED), among others. These methods all rely on expensive instruments and equipment, are complex in sample preparation operation, time-consuming in calibration process, and cannot realize economical and rapid crystal face calibration. Therefore, finding a technology for simply and rapidly calibrating the copper crystal face plays an extremely important role in the research and application of copper.
Disclosure of Invention
The invention provides a method for rapidly calibrating a copper crystal face by an optical method, which comprises the following steps:
firstly, placing a metal sample to be detected in a baking device for heating and oxidizing;
after the metal sample to be detected is oxidized, directly observing the metal sample by using an optical microscope, and observing the color information expressed by the metal sample to be detected;
and (III) determining the crystal face of the metal sample to be detected according to the corresponding relation between the metal crystal face and the color information.
Preferably, the following standardization step is further included before the step (one):
s1: calibrating a standard metal sample with different crystal faces by using a diffraction method, wherein the diffraction method comprises an X-ray diffraction method (XRD), an electron back scattering diffraction method (EBSD) or a low-energy electron diffraction method (LEED);
s2: placing a standard metal sample in a baking device for heating and oxidizing;
s3: after the standard metal sample is oxidized, the standard metal sample is directly observed by an optical microscope, and then different color information shown by the standard metal sample with different crystal faces can be observed;
s4: and establishing a corresponding relation between the metal crystal face and the color information.
Preferably, the baking apparatus is a hot plate, an oven or a CVD tube furnace.
Preferably, the temperature of the heating oxidation is 100-250 ℃, and the time is 30-90 minutes.
Preferably, the metal sample to be measured is a single crystal copper foil with a certain crystal face.
Preferably, the standard metal sample is a single crystal copper foil having a certain crystal face.
The invention judges the crystal face by using the relation between the thickness and the color of the oxide formed on the surface of the copper after high-temperature oxidation, and the oxide film has different thicknesses and thus different contrasts (colors) due to different oxidation rates of different crystal faces. The difference of different crystal planes can be clearly seen under optical microscopy. The method provided by the invention can distinguish different crystal faces under an optical microscope through very simple operation.
The invention has the advantages that:
1. the invention relates to a method for quickly calibrating a copper crystal face by an optical method;
2. the copper foil is heated and oxidized by utilizing a common heating table, an oven, a CVD tube furnace and the like, so that the operation is simple and convenient;
3. the invention can easily distinguish different crystal faces under an optical microscope;
4. the operation of the invention is simple, the required instruments (heating devices such as ovens, optical microscopes) are common, and the time and the trouble are saved.
5. The oxidation temperature and time can be set by an operator, and only the comparison and calibration of the crystal face and the color are ensured.
Drawings
FIG. 1(a) shows the results of air oxidation of the copper (100) crystal plane at 120 ℃ for 1 hour, and FIG. 1(b) shows the corresponding LEED for this sample.
FIG. 2(a) shows the results of air oxidation of the copper (111) crystal plane at 120 ℃ for 1 hour, and FIG. 2(b) shows the corresponding LEED for this sample.
FIG. 3(a) shows the results of air oxidation of the copper (410) crystal plane at 120 ℃ for 1 hour, and FIG. 3(b) shows the corresponding LEED for this sample.
Detailed Description
The present invention is further described in detail below with reference to specific examples, which are commercially available from the public unless otherwise specified.
The first embodiment is as follows: a method for quickly calibrating a copper crystal face by an optical method comprises the following steps:
preparing a copper sample to be detected;
secondly, placing the sample to be detected in an oven, and heating and oxidizing for 30-90 minutes at 100-250 ℃;
after the sample to be detected is oxidized, directly observing the sample by using an optical microscope to see different colors expressed by different crystal faces;
and (IV) determining the crystal face of the copper sample to be detected according to the corresponding relation between the copper crystal face and the color information.
Among them, copper samples can be easily obtained. The copper samples were also left for LEED for comparison. The heating device comprises a heating table, an oven, a CVD tube furnace and the like.
After the copper foils with different crystal faces are placed in the air and heated and oxidized at 100-250 ℃, different colors can be obviously seen under an optical microscope.
The prepared sample is firstly placed under an optical microscope for observation, the colors of different crystal faces are very similar and can not be distinguished, when the sample is heated and oxidized for 60 minutes at 120 ℃ in an oven, different colors can be found, and the colors are compared with the calibration result of the crystal face of the LEED, so that the standard result of different crystal faces under the condition of oxidation is obtained. Therefore, the temperature of the molten metal is controlled,
before the calibration step (one), the following standardization steps are included:
1. calibrating copper samples with different crystal faces by an X-ray diffraction method (XRD), an electron back scattering diffraction method (EBSD) or a low energy electron diffraction method (LEED), wherein the copper samples can specifically comprise copper (100), copper (111), copper (410) and other copper samples with different crystal faces;
2. after determining the copper sample of each crystal face, roasting each copper sample to be heated and oxidized; preferably, the baking process is carried out in a hot table, an oven or a CVD tube furnace, the temperature is set to be 100-250 ℃, and the time is 30-90 minutes;
3. directly observing copper samples with different crystal faces by using an optical microscope to see different colors shown by the different crystal faces;
4. and establishing the corresponding relation between different colors expressed by different crystal faces and the crystal faces.
The establishment of the corresponding relation can be the corresponding relation between the recorded color information and the crystal face, and can also be recorded in a photographing mode; preferably, the photomicrograph is entered into the computer device and the corresponding color information, for example RGB information, or CMYK information, Lab information, is viewable by the color-taking device.
Wherein, under the condition of air oxidation at 120 ℃ for 1 hour, the color information corresponding to the crystal face of copper (100) is represented by RGB information: r is 240-250, G is 100-150, and B is 30-60; the color information corresponding to the copper (111) crystal face after oxidation is expressed as RGB information: r is 245-255, G is 200-220, and B is 150-180; the color information corresponding to the copper (410) crystal face after oxidation is expressed in terms of RGB information: r is 210-240, G is 40-70, and B is 60-80.
In the above examples and the following experiments one to three, although copper was used as an example, the crystal plane directions of other metal foils were measured by the same method.
Test one: the method for rapidly calibrating the copper crystal face by an optical method in the test is carried out according to the following steps:
preparing a copper (100) sample;
secondly, placing the sample in an oven, and heating and oxidizing the sample for 60 minutes at 120 ℃;
and (III) directly observing the sample by using an optical microscope after the sample is oxidized, and observing the color shown by the crystal face.
Under the test condition, the oxygen in the air is easy to oxidize the copper during heating, a copper oxide film is generated, the optical contrast is changed, and the color can be observed.
And (2) test II: the method for rapidly calibrating the copper crystal face by an optical method in the test is carried out according to the following steps:
preparing a copper (111) sample;
secondly, placing the sample in an oven, and heating and oxidizing the sample for 60 minutes at 120 ℃;
and thirdly, directly observing the sample by using an optical microscope after the sample is oxidized, and then observing the color shown by the crystal face.
Under the test condition, the oxygen in the air is easy to oxidize the copper during heating, a copper oxide film is generated, the optical contrast is changed, and the color can be observed.
And (3) test III: the method for rapidly calibrating the copper crystal face by an optical method in the test is carried out according to the following steps:
preparing a copper (410) sample;
secondly, placing the sample in an oven, and heating and oxidizing the sample for 60 minutes at 120 ℃;
and thirdly, directly observing the sample by using an optical microscope after the sample is oxidized, and then observing the color shown by the crystal face.
Under the test condition, the oxygen in the air is easy to oxidize the copper during heating, a copper oxide film is generated, the optical contrast is changed, and the color can be observed.
In the above-mentioned methods from the first test to the third test, it can be seen that the copper on different crystal faces can be oxidized to obtain different colors, which can be used to quickly and conveniently mark the crystal faces.
Claims (2)
1. A method for rapidly calibrating a metal crystal face is characterized by comprising the following steps:
placing a metal sample to be detected in a baking device, and heating and oxidizing in the air, wherein the heating and oxidizing temperature is 120 ℃, and the heating and oxidizing time is 1 hour; the metal sample to be detected is a single crystal copper foil with a certain crystal face;
after the metal sample to be detected is oxidized, directly observing the metal sample by using an optical microscope, and observing the color information expressed by the metal sample to be detected;
thirdly, determining the crystal face of the metal sample to be detected according to the corresponding relation between the metal crystal face and the color information;
wherein, before the step (one), the following standardization steps are also included:
s1: calibrating a standard metal sample with different crystal faces by using a diffraction method, wherein the diffraction method comprises an X-ray diffraction method, an electron back scattering diffraction method or a low-energy electron diffraction method; the standard metal sample is a single crystal copper foil with a certain crystal face;
s2: placing a standard metal sample in a baking device for heating and oxidizing;
s3: after the standard metal sample is oxidized, the standard metal sample is directly observed by an optical microscope, and then different color information shown by the standard metal sample with different crystal faces can be observed;
s4: inputting the microscope picture into computer equipment, checking corresponding color information through color taking equipment, and establishing a corresponding relation between a metal crystal face and the color information, wherein the color information is RGB information; the color information corresponding to the copper (100) crystal plane is expressed as RGB information: r is 240-250, G is 100-150, and B is 30-60; the color information corresponding to the copper (111) crystal face after oxidation is expressed as RGB information: r is 245-255, G is 200-220, and B is 150-180; the color information corresponding to the copper (410) crystal face after oxidation is expressed in terms of RGB information: r is 210-240, G is 40-70, and B is 60-80.
2. The method of claim 1, wherein the baking apparatus is a hot plate, an oven, or a CVD tube furnace.
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| CN108169262B true CN108169262B (en) | 2020-06-02 |
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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 |
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- 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 |
|---|
| 晶格取向对铜氧化失效的影响;高婕 等;《2009年全国电子电镀及表面处理学术交流会论文集》;20091231;章节2、3.4、3.5及图6 * |
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