CN109668839A - A method of identifying copper sheet crystal boundary and crystal face - Google Patents
A method of identifying copper sheet crystal boundary and crystal face Download PDFInfo
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- CN109668839A CN109668839A CN201710950998.5A CN201710950998A CN109668839A CN 109668839 A CN109668839 A CN 109668839A CN 201710950998 A CN201710950998 A CN 201710950998A CN 109668839 A CN109668839 A CN 109668839A
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- G—PHYSICS
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- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
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Abstract
The invention discloses a kind of simple, efficient, easy methods to distinguish the crystal boundary and (111), (110), (100) three kinds of crystal faces on copper sheet surface.This method is that copper to be identified is carried out to heated oxide in air, and end, which is placed under optical microscopy, to be observed, and judges its grain boundary sites according to the juncture area of different colours, judges its indices of crystallographic plane according to colouring information.Crystal plane oxidation speed order is (100) face > (110) face > (111) face, and it is pale yellow-orange-red-pink colour-white-yellow that crystal face color, which changes over time sequence,.Compared with the analysis of conditional electronic back scattering diffraction, operation of the present invention is easy, saves the time, and accuracy is high, and very low to equipment, space requirement, usual conditions can be completed.
Description
Technical field
The present invention relates to a kind of methods using simple, efficient, easy identification copper sheet surface crystal boundary and crystal face.
Background technique
Copper is a kind of transition metal, one of the metal that the mankind have found earliest.Its ductility is good, and thermal conductivity and electric conductivity are high,
It is widely used in the fields such as electrical, light industry, machine-building, construction industry and national defence industry, is metal indispensable in life.Copper
Belong to face-centered cubic crystal, copper atom is distributed on eight angles of cube and the center in six faces.According to the heap of surface atom
Product mode is different, and the surface of copper can be divided into three kinds of crystal faces, i.e. (111), (110) and (100) face again.Theoretical calculation shows (111)
The surface in face can be minimum, and the surface in (110) face energy highest, therefore among three crystal faces, (110) face activity highest, (111) face
It is the most stable.Such as catalysis reaction and growth high-quality graphene in some applications, the nature difference of different crystal faces can be to knot
Fruit causes very big influence.So detection copper crystal face is to the understanding of the fundamental property of metallic copper and efficiently using most important.
Currently, the method for detection copper sheet crystal face is mainly EBSD technology (Electron back
Scatterdiffraction, EBSD), the attachment as scanning electron microscope (SEM).Its principle is that the electronics accelerated is beaten
Backscattered electron is generated on sample, is captured by Crystal surface structure diffraction by detector, to obtain sample surfaces crystal orientation
Structure.However, instrument subscription price is high, process is cumbersome, and detection, time-consuming for data processing, and therefore, it is necessary to develop a kind of letter
The method of single, efficient detection copper sheet crystal face.
Summary of the invention
The object of the present invention is to provide the methods of a kind of simple, efficient detection copper sheet surface crystal boundary and crystal face.
The method provided by the present invention for identifying copper sheet surface crystal boundary and crystal face, is to carry out copper to be identified in air
Heated oxide, end, which is placed under optical microscopy (OM), to be observed, and judges its crystal boundary according to the juncture area of different colours
Position judges its indices of crystallographic plane according to colouring information.
Wherein, heating temperature section is 150 DEG C -350 DEG C, preferably 200 DEG C -250 DEG C.Heating time regard temperature and
Fixed, temperature is higher, and heating time was shorter, by several seconds to dozens of minutes (such as 20s-30min).Below or above above-mentioned temperature range
Also analog result can be obtained, the difference is that the too low required time of temperature is too long, the excessively high then reaction speed of temperature is too fast, no
Easy to operate and differentiation generates oxide color.It is heated to needing 30min when can distinguish crystal face at 150 DEG C, and is generated at 350 DEG C
Same color differentiation only needs 20s.When heating temperature section is 200 DEG C -250 DEG C, according to heating temperature, time preferred 20s-
85s。
The method also includes: the copper is carried out the step of normal pressure annealing before being identified；The annealing
Heating temperature should be not higher than 1085 DEG C, preferably 1070 DEG C -1080 DEG C；Annealing time maintains 10-60min.
Specific annealing steps are as follows: copper being placed in high temperature process furnances, 100-400sccm inert gas, 50- are passed through
200sccm hydrogen, begins to warm up, and anneal 10-60min when temperature is up to slightly below metallic copper fusing point (1085 DEG C), identical
Under the conditions of be cooled to room temperature after take out.
The copper also needs to carry out it into electrochemistry throwing in ethyl alcohol/Phosphoric Acid polishing fluid before carrying out normal pressure annealing
Light.
The concrete composition of the polishing fluid are as follows: deionized water (mL), phosphoric acid (mL), ethyl alcohol (mL), isopropanol (mL) and urine
Plain (g) is matched in the ratio of 250:125:125:25:4；The condition of the electrochemical polish are as follows: holding voltage is 5V, electricity
Stream is 2A, polishing time 3min.
Argon gas, nitrogen etc. may be selected in the inert gas.
The copper can be fine copper either with copper alloy as main component, material etc..
The shape of the copper can be copper sheet, copper foil, copper sheet, copper billet etc., and preferably relatively thin sample, the thickness of sample the thick, heats
Time is longer.
The present invention uses heated oxide, fast, at low cost because of this method simplicity, unrestricted, heats to the copper
The mode of oxidation is also not necessarily limited to thermal station heating, other heating means such as laser heating etc., and all mode of oxidizing are suitable for
Such invention.
With the increase of heating time, copper sheet oxide on surface color can generate regular variation, color change direction are as follows:
Pale yellow-orange-red-pink colour-white-yellow.But it is not limited solely to a kind of color, should be a color interval, very
To the combination of available two kinds of colors.But it will appear other colors after heating time is too long, it is increasingly complex because generating
Substance such as copper carbonate.
Identical crystal face is identical in same time color, and different crystal faces are different in same time color, but can be with the time
Growth is changed according to above-mentioned color change direction.
Different crystal faces generate different colours to the copper under heating, mainly due to the oxide layer upper surface of different-thickness and
Caused by interference of the lower surface to light.X-ray diffraction analysis show it is such under the conditions of, the oxide of copper Surface Creation is oxidation
Copper (CuO).Since the reactivity of three kinds of crystal faces (111) of copper, (110), (100) is different, cause to generate oxygen in same time
The thickness of compound is different, and the color shown after interfering light is different, with the increase of thickness, color occurrence law
Variation.Three kinds of crystal plane oxidation speed speed sequence is (100) face > (110) face > (111) face.What this method can symbolize
Crystal face is (111), (110), (100) three kinds of crystal faces.Copper also contains other high-order crystal faces, does not do statement and depth in this invention
Study carefully.
It compares according to EBSD result, the present invention can symbolize all crystal faces and crystal boundary completely, and accuracy is close
100%.The two compare it can be concluded that, in three kinds of crystal faces, (100) face oxidation rate is most fast, be initially completed color cycle, and
(111) face is most slow.
Therefore the present invention will heat 1-2min at characterized copper in air 200 DEG C, light is placed under the microscope, according to above-mentioned
Color change rule, the most fast person of color change are (100) face, and changing most slow person is (111) face, and person placed in the middle is (110) face.
Detailed description of the invention
Fig. 1 is the optical microscope photograph of copper foil surface after 1055 DEG C of annealing 1 hour, should be apparent that surface in figure
Upper various linear crystal boundaries.
Fig. 2 is in embodiment 1 at 200 DEG C, the optical microscope photograph of the copper foil after aoxidizing under the conditions of 90s.
Fig. 3 be the sample optical microscope that is obtained in embodiment 1 by oxidizing process with by electron backscatter diffraction table
The comparison figure for the spectrogram obtained.As seen from the figure, new detection technique is consistent with traditional technology (EBSD) result height.
Fig. 4 is electron backscatter diffraction analytical standard spectrogram in embodiment 1.
Fig. 5 is the X-ray photoelectron spectroscopic analysis figure of copper foil after aoxidizing in embodiment 1.
Fig. 6 is in embodiment 2 at 150 DEG C, the optical microscope photograph of the copper foil after aoxidizing under the conditions of 30min.
Fig. 7 is in embodiment 3 at 250 DEG C, the optical microscope photograph of the copper foil after aoxidizing under the conditions of 25s.
Fig. 8 is to be divided by the sample optical microscope that oxidizing process obtains with by electron backscatter diffraction in embodiment 3
Analyse the comparison figure of obtained spectrogram.
Fig. 9 is in embodiment 4 at 300 DEG C, the optical microscope photograph of the copper foil after aoxidizing under the conditions of 20s.
Figure 10 is that the optical microscopy of copper foil shines after shooting oxidation in different time under conditions of 150 DEG C in embodiment 5
Piece.
Figure 11 is that the optical microscopy of copper foil shines after shooting oxidation in different time under conditions of 200 DEG C in embodiment 6
Piece.
Figure 12 is that the optical microscopy of copper foil shines after shooting oxidation in different time under conditions of 250 DEG C in embodiment 7
Piece.
Specific embodiment
Method of the invention is illustrated below by specific embodiment, but the present invention is not limited thereto, it is all at this
Any modifications, equivalent replacements, and improvements etc. done within the spirit and principle of invention, should be included in protection model of the invention
Within enclosing.
Experimental method described in following embodiments is unless otherwise specified conventional method；The reagent and material, such as
Without specified otherwise, commercially obtain.
Below in conjunction with attached drawing, the present invention will be described in detail:
The first step, the processing of copper:
The sample copper (copper foil, copper sheet etc.) for being intended to characterization carries out electrochemical polish 3min (its in ethyl alcohol/Phosphoric Acid
In, the concrete composition of polishing fluid are as follows: deionized water (mL), phosphoric acid (mL), ethyl alcohol (mL), isopropanol (mL) are pressed with urea (g)
The ratio of 250:125:125:25:4 is matched；The condition of the electrochemical polish are as follows: holding voltage be 5V, electric current 2A,
Polishing time is 3min.), cleaning drying is placed in high temperature process furnances, is passed through 100-400sccm inert gas (such as argon gas, nitrogen
Gas etc.), 50-200sccm hydrogen, begin to warm up.The copper annealing 10- when temperature is up to slightly below metallic copper fusing point (1085 DEG C)
60min takes out after being cooled to room temperature under the same conditions.Fig. 1 is the optical microscope photograph on copper sheet surface after annealing.In Fig. 1,
Some copper surfaces crystal boundary can be observed under an optical microscope by taking out under room temperature after annealing, and copper sheet surface is in nothing at this time
Color/white, and each crystal face is without color distinction.Further heating can make more crystal boundaries and crystal face show.
Second step heats thermal station, and copper is placed in thermal station by temperature between 150 DEG C -350 DEG C, heats 10s-30min
Copper is removed afterwards.Close thermal station.
Copper after heating is placed under optical microscopy and observes by third step, according to pale yellow-orange-red-powder
Color-white-yellow sequence, the most fast person of color change are (100) face, are secondly (110) face, are finally (111) face.
Embodiment 1, oxidizing process detect copper sheet crystal face
The first step, by the copper foil (purity 99.9%) of 100 μ m-thicks in polishing fluid (ingredient is phosphoric acid, ethyl alcohol, isopropanol)
Electrochemical polish 3min, deionized water cleaning, N2Drying.
The copper foil is placed on the middle part for being placed in clean quartz ampoule in quartz substrate, quartz ampoule is put by second step
In high temperature process furnances, so that the middle part of quartz ampoule is located at the central area of tube furnace, the argon of 200sccm is then passed through in quartz ampoule
The hydrogen of gas and 100sccm, starting tube furnace are begun to warm up, and temperature reaches 1075 DEG C of after annealing 10min.Closing tube furnace makes it
It is cooled to room temperature.
Thermal station temperature is risen to 200 DEG C by third step, and copper foil is placed on it, and 90s is heated in air, removes copper foil and cold
But room temperature is arrived.Close thermal station.
Gained copper foil is placed in optical microphotograph under the microscope by the 4th step, and gained photo is as shown in Figure 2.It can be seen from figure
Examine, presented in figure it is orange-yellow, light color it is orange and light yellow.Orange-yellow face is the most fast face of reaction speed, i.e. (100) face.Together
Reason, the orange face of light color are (110) face, and light yellow face is (111) face.
5th step, in order to verify the authenticity of acquired results, by sample carry out electron backscatter diffraction characterization, and with oxidation
Crystal face information obtained by method is compared, and acquired results are as shown in Figure 3.Fig. 4 is electron backscatter diffraction analytical standard spectrogram.In electricity
In sub- back scattering diffraction analysis, blue series represent (111) face, and green system represents (110) face, and red colour system represents (110) face.From
Fig. 3 can be seen that electron backscatter diffraction and analyze (100) face symbolized, reaction speed is most fast in corresponding oxidizing process one
Face, i.e. (100) face；And electron backscatter diffraction analyzes (111) face symbolized, reaction speed is most slow in corresponding oxidizing process
On one side, i.e. (111) face.Therefore, distinguish that the obtained result of copper sheet crystal face is accurate, true, reliable using oxidizing process.In addition, electric
The crystal boundary oxidizing process of the copper foil surface symbolized in the analysis of sub- back scattering diffraction can all observe, indicate oxidizing process for
Crystal boundary characterization precision is very high, almost up to 100%.
6th step carries out X-ray photoelectricity to the copper foil after oxidation to determine copper foil surface oxide composition generated
Sub- energy spectrum analysis.Acquired results are as shown in Figure 5.In figure, the absorption peak positioned at the two sides Cu2p1 is that the exclusive shake of copper oxide swashs companion
Peak, thus may determine that, generated oxide is copper oxide (CuO) on copper foil.
Embodiment 2, oxidizing process detect copper sheet crystal face
Operating method is substantially the same as embodiment 1, difference are as follows: and thermal station temperature is changed to 150 DEG C, and heating time is changed to 30min,
Subsequent process is the same as embodiment 1.Gained optical microscope photograph is Fig. 6.Copper foil degree of oxidation with it is more identical in embodiment 1,
And three kinds of colors can be distinguished, i.e., orange-yellow, light color is orange and light yellow.Similarly, orange-yellow face is (100) face, light color
Orange face is (110) face, and light yellow face is (111) face.
Embodiment 3, oxidizing process detect copper sheet crystal face
Operating method is substantially the same as embodiment 1, difference are as follows: and thermal station temperature is changed to 250 DEG C, and heating time is changed to 25s, with
Process afterwards is the same as embodiment 1.Gained optical microscope photograph is Fig. 7, and figure is Fig. 8 compared with electron backscatter diffraction analysis.?
In the shorter time, copper foil degree of oxidation is relatively deep compared with embodiment 1, has red appearance.Red face and orange-yellow face are
(100) face, the orange face of light color are (110) face, and light yellow face is (111) face.
Embodiment 4, oxidizing process detect copper sheet crystal face
Operating method is substantially the same as embodiment 1, difference are as follows: and thermal station temperature is changed to 300 DEG C, and heating time is changed to 20s, with
Process afterwards is the same as embodiment 1.Gained optical microscope photograph is Fig. 9.Within the shorter time, copper foil degree of oxidation it is most fast one
Face has passed past pink colour section and white is presented.Degree of oxidation has been leaped to next stage compared with embodiment 1, that is, has been occurred in figure
White face, red face, orange-yellow face and light yellow face.White face and red face are (100) face, and orange-yellow face is (110) face, shallowly
Yellow face is (111) face.
Embodiment 5, oxidizing process detect copper sheet crystal face
Thermal station is warming up to 150 DEG C later with embodiment 1 by the first and second step, and the copper foil after annealing is placed on thermal station and is added
Heat.Optical microphotograph sem observation is carried out to copper foil when 10min, 20min, 30min, acquired results are as shown in Figure 10.By scheming
It is found that at this temperature, oxidation rate is very slow, copper foil surface color change trend is smaller for middle observation.However, at longer one
In, the oxidation rate of three kinds of crystal faces abides by above-mentioned rule, i.e. (100) face > (110) face > (111) face.
Embodiment 6, oxidizing process detect copper sheet crystal face
Operating method is substantially the same as embodiment 5, difference are as follows: thermal station temperature is changed to 200 DEG C, and respectively at 85s,
175s, 275s, 455s, 1055s, 1895s carry out optical microphotograph sem observation to it, and acquired results are as shown in figure 11.By Tu Zhongguan
It examines it is found that at this temperature, oxidation rate becomes faster, transformation of the color to next color can be completed in tens seconds.It is identical
, within the longer time, the oxidation rate of three kinds of crystal faces abides by above-mentioned rule, i.e., (100) face > (110) face >
(111) face.
Embodiment 7, oxidizing process detect copper sheet crystal face
Operating method is substantially the same as embodiment 5, difference are as follows: thermal station temperature is changed to 250 DEG C, and respectively at 25s,
40s, 55s, 75s, 90s, 135s, 170s, 260s carry out optical microphotograph sem observation to it, and acquired results are as shown in figure 12.By scheming
Middle observation is it is found that at this temperature, quickly, transformation of the color to next color can be completed in oxidation rate in more than ten seconds.
Identical, within the longer time, the oxidation rate of three kinds of crystal faces abides by above-mentioned rule, i.e., (100) face > (110) face >
(111) face.
Claims (10)
1. a kind of method for identifying copper surface crystal boundary and crystal face, is that copper to be identified is carried out to heated oxide in air, terminate
It is placed under optical microscopy and is observed, its grain boundary sites is judged according to the juncture area of different colours, according to colouring information
Judge its indices of crystallographic plane.
2. according to the method described in claim 1, it is characterized by: the temperature of the heating be 150 DEG C -350 DEG C, preferably 200
℃-250℃。
3. according to the method described in claim 2, it is characterized by: the time of the heating depending on temperature, temperature it is higher plus
The hot time was shorter, by several seconds to dozens of minutes, preferably 20s-30min.
4. method according to claim 1-3, it is characterised in that: the method also includes: the copper is carrying out
The step of normal pressure annealing is carried out before identification；The heating temperature of the annealing should be not higher than 1085 DEG C, preferably 1070 DEG C-
1080℃；Annealing time maintains 10-60min.
5. according to the method described in claim 4, it is characterized by: carrying out the specific steps of normal pressure annealing to copper are as follows:
Copper is placed in high temperature process furnances, 100-400sccm inert gas, 50-200sccm hydrogen is passed through, begins to warm up, work as temperature
The 10-60min that anneals when reaching the heating temperature is spent, is taken out after being cooled to room temperature under the same conditions.
6. method according to claim 4 or 5, it is characterised in that: the method also includes: the copper is moved back in progress normal pressure
The step of it is carried out to electrochemical polish in ethyl alcohol/Phosphoric Acid polishing fluid before fire.
7. method according to claim 1-6, it is characterised in that: the copper is that fine copper is either main with copper
Alloy, the material of ingredient；
The shape of the copper is copper sheet, copper foil, copper sheet or copper billet.
8. method according to any one of claims 1-7, it is characterised in that: with the increase of heating time, copper surface
Oxide color can generate regular variation, color change direction are as follows: pale yellow-orange-red-pink colour-white-yellow；
Identical crystal face is identical in same time color, and different crystal faces are different in same time color, but can increase with heating time
It is changed according to the color change direction.
9. method according to claim 1 to 8, it is characterised in that: the indices of crystallographic plane that can be identified are
(111), (110), (100) three kinds of crystal faces.
10. according to the method described in claim 9, it is characterized by: three kinds of crystal plane oxidation speed speed sequence is (100)
Face > (110) face > (111) face.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108169262A (en) * | 2017-12-20 | 2018-06-15 | 北京大学 | A kind of method of Fast Calibration metal crystal face |
| CN110057849A (en) * | 2019-05-29 | 2019-07-26 | 广东省材料与加工研究所 | A kind of composite material and preparation method and application for EBSD test |
| CN113092463A (en) * | 2019-12-23 | 2021-07-09 | 北京大学 | Method for detecting two-dimensional material grain boundary |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106011710A (en) * | 2016-06-06 | 2016-10-12 | 重庆理工大学 | Processing method for obtaining high-proportion special grain boundary from tin bronze |
-
2017
- 2017-10-13 CN CN201710950998.5A patent/CN109668839A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106011710A (en) * | 2016-06-06 | 2016-10-12 | 重庆理工大学 | Processing method for obtaining high-proportion special grain boundary from tin bronze |
Non-Patent Citations (4)
| Title |
|---|
| 朱锦艳 等: "有色合金彩色金相技术的研究与应用", 《太原重型机械学院学报》 * |
| 李炳 等: "单晶铜线材的表面氧化研究", 《西安工业大学学报》 * |
| 马连仲 等: "彩色金相法及其应用", 《国外金属热处理》 * |
| 高捷 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 (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108169262A (en) * | 2017-12-20 | 2018-06-15 | 北京大学 | A kind of method of Fast Calibration metal crystal face |
| CN108169262B (en) * | 2017-12-20 | 2020-06-02 | 北京大学 | Method for rapidly calibrating metal crystal face |
| CN110057849A (en) * | 2019-05-29 | 2019-07-26 | 广东省材料与加工研究所 | A kind of composite material and preparation method and application for EBSD test |
| CN113092463A (en) * | 2019-12-23 | 2021-07-09 | 北京大学 | Method for detecting two-dimensional material grain boundary |
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