CN114062076A - Sample preparation method for copper foil crystal analysis - Google Patents
Sample preparation method for copper foil crystal analysis Download PDFInfo
- Publication number
- CN114062076A CN114062076A CN202111298990.8A CN202111298990A CN114062076A CN 114062076 A CN114062076 A CN 114062076A CN 202111298990 A CN202111298990 A CN 202111298990A CN 114062076 A CN114062076 A CN 114062076A
- Authority
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- China
- Prior art keywords
- copper foil
- sample
- crystal
- foil sample
- analysis
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 239000011889 copper foil Substances 0.000 title claims abstract description 75
- 239000013078 crystal Substances 0.000 title claims abstract description 34
- 238000004458 analytical method Methods 0.000 title claims abstract description 20
- 238000005464 sample preparation method Methods 0.000 title claims abstract description 14
- 238000005498 polishing Methods 0.000 claims abstract description 9
- 238000010008 shearing Methods 0.000 claims abstract description 4
- 238000005520 cutting process Methods 0.000 claims description 11
- 238000010884 ion-beam technique Methods 0.000 claims description 11
- 238000007664 blowing Methods 0.000 claims description 4
- 238000005530 etching Methods 0.000 claims description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical class Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 229920000742 Cotton Polymers 0.000 claims description 3
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Substances Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 3
- 229960003280 cupric chloride Drugs 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- -1 saturated ammonium cupric chloride Chemical class 0.000 claims description 3
- 239000000523 sample Substances 0.000 abstract description 50
- 229910052802 copper Inorganic materials 0.000 abstract description 6
- 239000010949 copper Substances 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 238000002050 diffraction method Methods 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052721 tungsten Inorganic materials 0.000 abstract description 3
- 239000010937 tungsten Substances 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 14
- 150000002500 ions Chemical class 0.000 description 8
- 238000011160 research Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000011888 foil Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910000365 copper sulfate Inorganic materials 0.000 description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 238000001887 electron backscatter diffraction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- VUCAVCCCXQVHAN-UHFFFAOYSA-L azane dichlorocopper Chemical class N.Cl[Cu]Cl VUCAVCCCXQVHAN-UHFFFAOYSA-L 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 238000000992 sputter etching Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
Abstract
The invention discloses a sample preparation method for copper foil crystal analysis, which comprises the following steps: s1 shearing a copper foil sample; s2 polishing the surface of the copper foil sample, and S3 corroding the surface of the copper foil sample. The sample preparation method is simple and convenient to operate, copper foil crystal grains can be rapidly etched, the crystal profile of copper can be obviously displayed, the prepared sample can visually analyze the crystal grain size on the surface of the copper foil and observe the growth direction of the crystal grains under a crystal phase microscope, a tungsten filament and other low-end scanning electron microscopes, the crystal grains with different component contrasts can be observed under a back scattering electron probe for element analysis and phase-aware two-dimensional distribution, the microscopic crystal grain size, the crystal lattice orientation, the crystal boundary and the residual stress of the copper foil can be counted under an electron back scattering diffraction analysis technical device, and a foundation is further laid for the microscopic crystal analysis of the copper foil material.
Description
Technical Field
The invention relates to the technical field of copper foil crystal observation and analysis, in particular to a sample preparation method for copper foil crystal analysis.
Background
The copper foil is a key basic raw material for manufacturing Copper Clad Laminate (CCL), Printed Circuit Board (PCB) and lithium battery cathode materials. With the arrival of the 5G information era and the rapid development of new energy automobiles, the electrolytic copper foil industry in China is developed dramatically, which is attributed to the constant research on the principle of electrolytic copper foil by copper foil research personnel. The electrolytic copper foil is prepared by taking a copper material as a main raw material, dissolving the copper material to prepare a copper sulfate electrolytic solution, then carrying out direct current electro-deposition on the copper sulfate electrolytic solution in a special electrolytic device to prepare a foil, carrying out a series of treatments such as surface roughening, anti-oxidation treatment and the like on the foil, and finally carrying out slitting detection on the foil to prepare a finished product. In recent years, based on the recognition of the electrolytic principle, researchers have gradually found that copper foil crystal research is the basis of copper foil process principle research. Therefore, more specialized sample preparation methods for copper foil crystal analysis are urgently needed to be developed.
Ion milling (Ion Mill) as an Ion beam cutting polishing system fabricated using the tip technology provides reliable, high performance sample preparation capability. Ion Mill bombards the surface of a sample under the action of electric field acceleration after ionization of argon, and physically sputters and bombards the surface of the sample in a momentum transfer mode, so that the surface of the sample is finely polished, and the sample preparation requirements of surface sensitive analysis technologies such as a high-magnification scanning electron microscope and EBSD are met.
Currently, reports on preparation methods of copper foil crystal analysis samples are still few.
Disclosure of Invention
In view of the above technical problems in the related art, the present invention provides a sample preparation method for copper foil crystal analysis, which can overcome the above disadvantages in the prior art.
In order to achieve the technical purpose, the technical scheme of the invention is realized as follows:
a sample preparation method for copper foil crystal analysis comprises the following steps:
s1 clipping a copper foil sample: shearing a copper foil sample according to the size of the sample table;
s2, polishing the surface of the copper foil sample, namely putting the copper foil sample into an ion beam cutting polisher, setting parameters of the ion beam cutting polisher, and polishing the copper foil sample;
s3, corroding the surface of the copper foil sample, namely taking out the polished copper foil sample, dipping a cotton swab in corrosive liquid to wipe the surface of the copper foil sample for 2 seconds, and blowing the copper foil sample dry after flushing with running water.
Further, the size of the copper foil sample cut in S1 is 0.5CM in length and 0.5CM in width.
Further, the parameters of the ion beam cutting polisher set in the step S2 are specifically set as a plane sample, the voltage is 8KV, the ion source deflection angle is 6 degrees, and the time is 60 minutes; then the voltage is switched to 2KV, the deflection angle of the ion source is 2 degrees, and the time is 30 minutes; and finally, switching to a section sample, wherein the voltage is 8KV, the ion source deflection angle is 0 DEG, and the time is 20 minutes.
Further, the etching solution in S3 is a solution prepared from a saturated ammonium cupric chloride solution and a saturated ferric chloride solution.
The invention has the beneficial effects that: the sample preparation method is simple and convenient to operate, copper foil crystal grains can be quickly etched, the crystal outline of copper can be obviously displayed, the prepared sample can visually analyze the crystal grain size on the surface of the copper foil and observe the growth direction of the crystal grains under a crystalline phase microscope, a tungsten filament and other low-end scanning electron microscopes, the crystal grains with different component contrasts can be observed under a back scattering electron probe for element analysis and phase-knowing two-dimensional distribution, the microscopic crystal grain size, the lattice orientation, the crystal boundary and the residual stress of the copper foil can be counted under an electron back scattering diffraction analysis technical device, and a foundation is further laid for the microscopic crystal analysis of the copper foil material.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a graph showing the effects of polishing and etching on a copper foil sample according to a sample preparation method according to an embodiment of the present invention: (1) observation of the crystalline phase of the polished and etched copper foil sample, (2) SEM observation of the polished and etched copper foil sample;
FIG. 2 is a graph showing the effect of a copper foil sample polished according to a sample preparation method of an embodiment of the present invention: (1) BSE observation of the polished copper foil samples, (2) EBSD analysis effect of the polished copper foil samples.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments that can be derived by one of ordinary skill in the art from the embodiments given herein are intended to be within the scope of the present invention.
The sample preparation method for the copper foil crystal analysis comprises the following steps:
s1 clipping a copper foil sample: shearing a copper foil sample according to the size of the sample table;
s2, polishing the surface of the copper foil sample, namely putting the copper foil sample into an ion beam cutting polisher, setting parameters of the ion beam cutting polisher, and polishing the copper foil sample;
s3, corroding the surface of the copper foil sample, namely taking out the polished copper foil sample, dipping a cotton swab in corrosive liquid to wipe the surface of the copper foil sample for 2 seconds, and blowing the copper foil sample dry after flushing with running water.
The dimensions of the copper foil sample cut in S1 described above were 0.5CM in length and 0.5CM in width.
The parameters of the ion beam cutting polisher set in the above S2 are specifically set as a plane sample, voltage 8KV, ion source deflection angle 6 °, time 60 minutes; then the voltage is switched to 2KV, the deflection angle of the ion source is 2 degrees, and the time is 30 minutes; and finally, switching to a section sample, wherein the voltage is 8KV, the ion source deflection angle is 0 DEG, and the time is 20 minutes.
The etching solution in S3 is a solution prepared from a saturated ammonium cupric chloride solution and a saturated ferric chloride solution.
In order to facilitate understanding of the above-described technical aspects of the present invention, the above-described technical aspects of the present invention will be described in detail below in terms of specific usage.
When the copper foil sample is used specifically, a copper foil sample is firstly sheared, the surface of the copper foil sample is polished by an ion beam cutting polisher, then the surface of the copper foil sample is corroded for 2 seconds by a solution prepared from a saturated ammonium copper chloride solution and a saturated ferric chloride solution, the copper foil sample is dried by blowing after running water washing, then the copper foil sample is observed and measured under a crystal phase microscope, and further observed and analyzed under a scanning electron microscope according to analysis requirements.
In summary, as shown in fig. 1-2, with the aid of the above technical solutions of the present invention, the operation is simple and convenient, copper foil grains can be rapidly etched, so that the crystal profile of copper can be clearly shown, the prepared sample can visually analyze the grain size and the grain growth direction on the surface of the copper foil under a crystal phase microscope, a tungsten filament and other low-end scanning electron microscopes, can observe grains with different component contrast for element analysis and phase-aware two-dimensional distribution under a backscattered electron probe, and can count the microscopic grain size, lattice orientation, grain boundary and residual stress of the copper foil under an electron backscattered diffraction analysis technical device, thereby further laying a foundation for the analysis of the microscopic crystals of the copper foil material.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (4)
1. A sample preparation method for copper foil crystal analysis is characterized by comprising the following steps:
s1 clipping a copper foil sample: shearing a copper foil sample according to the size of the sample table;
s2, polishing the surface of the copper foil sample, namely putting the copper foil sample into an ion beam cutting polisher, setting parameters of the ion beam cutting polisher, and polishing the copper foil sample;
s3, corroding the surface of the copper foil sample, namely taking out the polished copper foil sample, dipping a cotton swab in corrosive liquid to wipe the surface of the copper foil sample for 2 seconds, and blowing the copper foil sample dry after flushing with running water.
2. The method for preparing a sample according to claim 1, wherein the size of the copper foil sample cut in S1 is 0.5CM in length and 0.5CM in width.
3. The sample preparation method according to claim 1, wherein the parameters of the ion beam cutting polisher set in S2 are specifically set as a planar sample, voltage 8KV, ion source deflection angle 6 degrees, time 60 minutes; then the voltage is switched to 2KV, the deflection angle of the ion source is 2 degrees, and the time is 30 minutes; and finally, switching to a section sample, wherein the voltage is 8KV, the ion source deflection angle is 0 DEG, and the time is 20 minutes.
4. The method according to claim 1, wherein the etching solution in S3 is a solution prepared from a saturated ammonium cupric chloride solution and a saturated ferric chloride solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111298990.8A CN114062076A (en) | 2021-11-04 | 2021-11-04 | Sample preparation method for copper foil crystal analysis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111298990.8A CN114062076A (en) | 2021-11-04 | 2021-11-04 | Sample preparation method for copper foil crystal analysis |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114062076A true CN114062076A (en) | 2022-02-18 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111298990.8A Pending CN114062076A (en) | 2021-11-04 | 2021-11-04 | Sample preparation method for copper foil crystal analysis |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115728194A (en) * | 2022-11-21 | 2023-03-03 | 山东大学 | Method for detecting crystal grain morphology of copper foil section |
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- 2021-11-04 CN CN202111298990.8A patent/CN114062076A/en active Pending
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115728194A (en) * | 2022-11-21 | 2023-03-03 | 山东大学 | Method for detecting crystal grain morphology of copper foil section |
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