CN110455840A - A kind of sample preparation methods that electrolytic capacitor is analyzed with electronics aluminum foil method to EBSD - Google Patents

A kind of sample preparation methods that electrolytic capacitor is analyzed with electronics aluminum foil method to EBSD Download PDF

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CN110455840A
CN110455840A CN201910666039.XA CN201910666039A CN110455840A CN 110455840 A CN110455840 A CN 110455840A CN 201910666039 A CN201910666039 A CN 201910666039A CN 110455840 A CN110455840 A CN 110455840A
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aluminum foil
ebsd
electrolytic capacitor
sample
analyzed
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汪战胜
陈锦雄
罗向军
汪启桥
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Ruyuan Yao Autonomous County Dongyangguang Formed Foil Co Ltd
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Ruyuan Yao Autonomous County Dongyangguang Formed Foil Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating 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
    • G01N23/20Investigating 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
    • G01N23/20008Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
    • G01N23/2005Preparation of powder samples therefor
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating 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
    • G01N23/20Investigating 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
    • G01N23/203Measuring back scattering
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/05Investigating materials by wave or particle radiation by diffraction, scatter or reflection
    • G01N2223/053Investigating materials by wave or particle radiation by diffraction, scatter or reflection back scatter
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/10Different kinds of radiation or particles
    • G01N2223/102Different kinds of radiation or particles beta or electrons
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/60Specific applications or type of materials
    • G01N2223/646Specific applications or type of materials flaws, defects

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  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
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Abstract

The present invention provides the sample preparation methods that a kind of electrolytic capacitor is analyzed with electronics aluminum foil method to EBSD.Sample preparation methods include the following steps: to sample and inlay;Mechanical polishing;Vibropolish;Electrobrightening;Dissolving resin.Method of the invention can convenient, fast, accurately obtain the sample examination face for meeting EBSD analysis and requiring of high quality, the compliance rate of sample is up to 90~98% or more, detection and analysis suitable for electrolytic capacitor with from electronics aluminum foil method to face crystal grain, it lays a good foundation to carry out research crystal grain orientation, grain boundary features with the association study for corroding long short-bore and etched foil specific volume, provides support to study the relationship of the crystal property of electrolytic capacitor electric aluminum foil and the comprehensive performance of product.

Description

A kind of sample preparation methods that electrolytic capacitor is analyzed with electronics aluminum foil method to EBSD
Technical field
The present invention relates to electric aluminum foils to test and analyze technical field, more particularly, to a kind of electrolytic capacitor electronics The sample preparation methods of aluminium foil normal direction EBSD analysis.
Background technique
Electronic light foil is high-end aluminium foil, is mainly used for the Important Components aluminium electrolutic capacitor of electronics industry.With electronics The rapid development of industry, the performance and integrated level of electronic product are higher and higher, require also increasingly to increase to electronic component, equally For electric aluminum foil, higher requirements are also raised.Electric aluminum foil is in corrosion process, and with the growth of hole, it can encounter sky The matrixes defect such as position, dislocation, impurity and crystal boundary, these defects can significantly affect the growth of hole, cause the holes such as short-bore, side opening Defect reduces the area expanding rate of etched foil, finally influences specific volume, and wherein crystal boundary is to influence its hole to grow most important factor.Electricity The research of sub- aluminium foil normal direction crystal grain is significant to control electric aluminum foil section number of grain boundaries and grain boundary features, passes through different systems The fractograph analysis for spending light foil, can observe directly the section crystal grain and orientation information of sample, to analyze section crystal grain Control mode, it is significant for improving the long short-bore of etched foil, promotion etched foil specific volume, it is the weight of electric aluminum foil technology analysis Want means.
Currently, there are many existing technologies about crystal grain analysis of electrolytic capacitor electric aluminum foil, wherein spar degree method It is a kind of indirect method for measuring cubic texture in aluminium foil, since the corrosion resistance of cubic texture is good, table after coarse micro-grain sample etch Face is in the matrix of white light tone, by measure white spar body number come indicate cubic texture number, it is anti-corrosion using aluminium foil crystal face Property different principle, the detection of aluminium foil cubic texture is carried out with simple chemical corrosion method, the method is simple, but quantitative accurate Property it is low and need certain experiential basis.Etch pit method is that have the place of dislocation under the conditions of specific etch using test check face Preferential corrosion generates dislocation etch pit, and the texture of crystal is orientated where the shape of dislocation pit will depend on it, is counted by etch pit Can be determined that the texture orientation of crystal where etch pit, the method is simple and can quantify, but the influence factor of quantitative result compared with It is more, such as sampling method and operation technique etc..Electron backscatter diffraction (EBSD) technology is existed based on electron beam in scanning electron microscope The analysis of diffraction Kikuchi band that inclination sample surfaces excites and formed, and then determination crystal structure, orientation and relevant information side Method has important role in the tissue characterization of crystalline material and analysis.In electric aluminum foil material, EBSD is mainly used for taking To analysis, the analysis of micro- textile analysis, crystal boundary, grain size measurement etc., since backscattered electron only occurs in tens, sample surface layer The depth bounds of nanometer, and EBSD technology needs to tilt the viewing surface of sample into 70 degree, and by electron beam in viewing surface It excites and forms diffraction Kikuchi and bring and analyzed, sample viewing surface is required very high, sample preparation procedure difficulty is big.It is existing There is technology CN106504251A to disclose a kind of electric aluminum foil cubic texture detection method of content based on picture processing, the technology In aluminium foil cubic texture content is measured using spar degree method, by the number of pixel shared by the aluminium foil that extracts of statistics with The number of pixel shared by the non-cubic texture extracted obtains content of the cubic texture in aluminium foil, instead of traditional artificial The method of observation determines cubic texture content, and the problem that unresolved dosing accuracy is low.How crystallography side is comprehensively used Method analyzes this technical problem, and there are no refer to that electrolytic capacitor electronics aluminum foil method analyzes to EBSD in existing technology Method.
Summary of the invention
The technical problem to be solved by the present invention is to overcome existing electric aluminum foil crystal grain analysis method dosing accuracy is low, lack It falls into and insufficient, a kind of sample preparation methods that electrolytic capacitor electronics aluminum foil method is analyzed to EBSD is provided.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
A kind of sample preparation methods that electrolytic capacitor is analyzed with electronics aluminum foil method to EBSD, include the following steps:
S1. it samples and inlays: sample being carried out to inlay solidification with epoxy resin;
S2. it mechanically polishes: using SiC waterproof abrasive paper and SiO2Polishing fluid successively polishes sample tested surface;
S3. vibropolish, polishing fluid SiO vibropolish: are carried out using vibropolish instrument2
S4. electrobrightening: perchloric acid, ethyl alcohol and ethylene glycol monobutyl ether mixed liquor are used as polishing fluid and carries out electrolysis throwing Light;
S5. dissolving resin: epoxy resin is inlayed in dissolution, obtains final sample to be tested.
Wherein, fixed for convenience and hold and take, sample of the invention can be taken to cutting box-like size, preferably 30mm* 50mm。
It is washed using water as cleaning agent after mechanically polishing SiC water sand paper polishing in S2.
Electrolytic capacitor electric aluminum foil will often analyze the depth and etched foil ratio of corrosion hole in research and development and production The relationship of appearance, and corroding the depth of hole and electronics foil normal direction crystal grain quantity, grain boundary features, crystal grain defect has close pass System, the signal of EBSD come from specimen surface 10-50nm depth, and the more high effective information collected of specimen surface finish is just more More, style is more clear, can obtain clearly EBSD Kikuchi style using method of the invention.
Sample preparation methods of the invention are easy to operate, realize easily and fast, accurately obtain electrolytic capacitor electricity consumption The sub- comprehensive crystallography information of aluminium foil, analysis corrosion hole depth reason, while being but also widely used for the processing procedure prison of electric aluminum foil Control, Improving The Quality of Products.
It can get the bright and clean pollution-free, non-oxidation layer of specimen surface, without surface stress using sample preparation methods of the invention Sample, it is convenient, fast, accurately obtain high quality meet EBSD analysis require sample examination face.
Preferably, SiC waterproof abrasive paper described in S2 is finished to successively be thrown using 400#, 2000#, 5000#SiC waterproof abrasive paper Light processing, polishing total time are 2~5min, and polishing time length directly affects the removal degree of Micro scratching.
Preferably, SiO described in S22The partial size of polishing fluid is 80~100nm, and polishing time is 5~10min.When polishing Between directly affect the final finish of sample.
Preferably, SiO described in S32The partial size of polishing fluid is 50~80nm, and the time is 150~180min.
It is highly preferred that SiO described in S32The partial size of polishing fluid is 50~70nm.It such as can be 50nm, 60nm, 70nm Or 80nm.
Preferably, the volume ratio of perchloric acid, ethyl alcohol and ethylene glycol monobutyl ether is 8:1~1.5:1~1.5 in S4.
0.05~0.5A/cm of current density of electrobrightening described in S42, voltage 30V, 5~15S of time.
It is highly preferred that 0.15~0.45A/cm of current density of electrobrightening described in S42, the time is 10~15S.Such as It can be 0.15A/cm2、0.25A/cm2、0.35A/cm2Or 0.45A/cm2
The purpose of electrobrightening is removal specimen surface oxide layer, and the parameter selections such as current density, voltage, time are improper then It causes removal to be not thorough or excessively degrade, influences the clarity of the final style of sample.
Wherein, the polishing time of S3 vibropolish of the invention and S4 electrobrightening is especially heavy to specimen surface finish It wanting, inventor stumbles under suitable polishing process of the invention, and surface smoothness is high, and the effective information of acquisition is more, The chrysanthemum sample of formation is apparent.
Preferably, the solvent of dissolved epoxy described in S5 is analysis pure acetone, dissolution time 5-10h.
It is highly preferred that dissolution time described in S5 is 10h.
It is more highly concentrated and contaminant free to analyze pure acetone concentration, can shorten dissolution time, time acetone solution time is short then cannot Thoroughly by solidified resin dissolution, required sample can not be obtained, time length can then reduce efficiency.
Compared with prior art, the beneficial effects of the present invention are:
The present invention provides the preparation methods that a kind of electrolytic capacitor is analyzed with electronics aluminum foil method to EBSD, can conveniently, fastly The sample examination face for meeting EBSD analysis and requiring that is prompt, accurately obtaining high quality, the compliance rate of sample up to 90~98% or more, Detection and analysis suitable for electrolytic capacitor with from electronics aluminum foil method to face crystal grain, for carry out research crystal grain orientation, grain boundary features with The association study for corroding long short-bore and etched foil specific volume is laid a good foundation, for the crystal spy for studying electrolytic capacitor electric aluminum foil The relationship of property and the comprehensive performance of product provides support.
Detailed description of the invention
Fig. 1 is the distribution of orientations figure and crystal boundary figure of sample EBSD analysis prepared by embodiment 1.
Fig. 2 is the distribution of orientations figure and crystal boundary figure of sample EBSD analysis prepared by embodiment 2.
Fig. 3 is the distribution of orientations figure and crystal boundary figure of sample EBSD analysis prepared by embodiment 3.
Specific embodiment
The present invention is further illustrated With reference to embodiment, but embodiment the present invention is not done it is any The restriction of form.Unless otherwise indicated, source chemicals used in the embodiment of the present invention are the source chemicals routinely bought.
Embodiment 1
A kind of electrolytic capacitor, to EBSD analysis method, is included the following steps: with electronics aluminum foil method
S1. it samples and inlays: sample being cut into 30mm*50mm with paper knife, carried out inlaying solidification with epoxy resin;
S2. it mechanically polishes: successively being polished with 400#, 2000#, 5000#SiC waterproof abrasive paper, polishing time 3min, used Water as cleaning agent, after with partial size be 100nmSiO2Polishing fluid polishes sample tested surface, polishing time 5min;
S3. vibropolish: vibropolish is carried out using vibropolish instrument, polishing fluid is that partial size is 80nmSiO2Polishing fluid, Time is 150min;
S4. electrobrightening: ethyl alcohol: perchloric acid: hexylene glycol monobutyl ether=8:1:1 polishing fluid, current density is used 0.15A/cm2, voltage 30V, time 5S;
S5.EBSD analysis: inlaying resin with the acetone solution for analyzing pure grade, and time 8h obtains final sample to be tested, Sample to be tested is placed in Electronic Speculum and obtains Kikuchi style using EBSD analysis system.
The normal direction distribution of orientations figure of the present embodiment EBSD analysis electrolytic capacitor electric aluminum foil is shown in Fig. 1, the calibration of sample Rate works well up to 94% or more.
Embodiment 2
A kind of electrolytic capacitor, to EBSD analysis method, is included the following steps: with electronics aluminum foil method
S1. it samples and inlays: sample being cut into 30mm*50mm with paper knife, carried out inlaying solidification with epoxy resin;
S2. it mechanically polishes: successively being polished with 400#, 2000#, 5000#SiC waterproof abrasive paper, polishing time 3min, used Water as cleaning agent, after with partial size be 100nmSiO2Polishing fluid polishes sample tested surface, polishing time 8min;
S3. vibropolish: vibropolish is carried out using vibropolish instrument, polishing fluid is that partial size is 70nmSiO2Polishing fluid, Time is 150min;
S4. electrobrightening: ethyl alcohol: perchloric acid: hexylene glycol monobutyl ether=8:1:1 polishing fluid, current density is used 0.25A/cm2, voltage 30V, time 8S;
S5.EBSD analysis: inlaying resin with the acetone solution for analyzing pure grade, and time 8h obtains final sample to be tested, Sample to be tested is placed in Electronic Speculum and obtains Kikuchi style using EBSD analysis system.
The normal direction distribution of orientations figure of the present embodiment EBSD analysis electrolytic capacitor electric aluminum foil is shown in Fig. 2, the calibration of sample Rate works well up to 95% or more.
Embodiment 3
A kind of electrolytic capacitor, to EBSD analysis method, is included the following steps: with electronics aluminum foil method
S1. it samples and inlays: sample being cut into 30mm*50mm with paper knife, carried out inlaying solidification with epoxy resin;
S2. it mechanically polishes: successively being polished with 400#, 2000#, 5000#SiC waterproof abrasive paper, polishing time 5min, used Water as cleaning agent, after with partial size be 100nmSiO2Polishing fluid polishes sample tested surface, polishing time 10min;
S3. vibropolish: vibropolish is carried out using vibropolish instrument, polishing fluid is that partial size is 60nmSiO2Polishing fluid, Time is 180min;
S4. electrobrightening: ethyl alcohol: perchloric acid: hexylene glycol monobutyl ether=8:1:1 polishing fluid, current density is used 0.35A/cm2, voltage 30V, time 8S;
S5.EBSD analysis: inlaying resin with the acetone solution of the pure grade of analysis, time 10h, obtains final to be tested Sample to be tested is placed in Electronic Speculum and obtains Kikuchi style using EBSD analysis system by sample.
The normal direction distribution of orientations figure of the present embodiment EBSD analysis electrolytic capacitor electric aluminum foil is shown in Fig. 3, the calibration of sample Rate works well up to 98% or more.
Embodiment 4
A kind of electrolytic capacitor, to EBSD analysis method, is included the following steps: with electronics aluminum foil method
S1. it samples and inlays: sample being cut into 30mm*50mm with paper knife, carried out inlaying solidification with epoxy resin;
S2. it mechanically polishes: successively being polished with 400#, 2000#, 5000#SiC waterproof abrasive paper, polishing time 5min, used Water as cleaning agent, after with partial size be 80nmSiO2Polishing fluid polishes sample tested surface, polishing time 10min;
S3. vibropolish: vibropolish is carried out using vibropolish instrument, polishing fluid is that partial size is 60nmSiO2Polishing fluid, Time is 180min;
S4. electrobrightening: ethyl alcohol: perchloric acid: hexylene glycol monobutyl ether=8:1:1 polishing fluid, current density is used 0.35A/cm2, voltage 30V, time 8S;
S5.EBSD analysis: inlaying resin with the acetone solution of the pure grade of analysis, time 10h, obtains final to be tested Sample to be tested is placed in Electronic Speculum and obtains Kikuchi style using EBSD analysis system by sample.
The normal direction distribution of orientations figure of the present embodiment EBSD analysis electrolytic capacitor electric aluminum foil is shown in Fig. 3, the calibration of sample Rate works well up to 96% or more.
Embodiment 5
A kind of electrolytic capacitor, to EBSD analysis method, is included the following steps: with electronics aluminum foil method
S1. it samples and inlays: sample being cut into 30mm*50mm with paper knife, carried out inlaying solidification with epoxy resin;
S2. it mechanically polishes: successively being polished with 400#, 2000#, 5000#SiC waterproof abrasive paper, polishing time 5min, used Water as cleaning agent, after with partial size be 100nmSiO2Polishing fluid polishes sample tested surface, polishing time 10min;
S3. vibropolish: vibropolish is carried out using vibropolish instrument, polishing fluid is that partial size is 50nmSiO2Polishing fluid, Time is 180min;
S4. electrobrightening: ethyl alcohol: perchloric acid: hexylene glycol monobutyl ether=8:1:1 polishing fluid, current density is used 0.35A/cm2, voltage 30V, time 8S;
S5.EBSD analysis: inlaying resin with the acetone solution of the pure grade of analysis, time 10h, obtains final to be tested Sample to be tested is placed in Electronic Speculum and obtains Kikuchi style using EBSD analysis system by sample.
The normal direction distribution of orientations figure of the present embodiment EBSD analysis electrolytic capacitor electric aluminum foil is shown in Fig. 3, the calibration of sample Rate works well up to 97% or more.
Embodiment 6
A kind of electrolytic capacitor, to EBSD analysis method, is included the following steps: with electronics aluminum foil method
S1. it samples and inlays: sample being cut into 30mm*50mm with paper knife, carried out inlaying solidification with epoxy resin;
S2. it mechanically polishes: successively being polished with 400#, 2000#, 5000#SiC waterproof abrasive paper, polishing time 5min, used Water as cleaning agent, after with partial size be 100nmSiO2Polishing fluid polishes sample tested surface, polishing time 10min;
S3. vibropolish: vibropolish is carried out using vibropolish instrument, polishing fluid is that partial size is 80nmSiO2Polishing fluid, Time is 180min;
S4. electrobrightening: ethyl alcohol: perchloric acid: hexylene glycol monobutyl ether=8:1.5:1.5 polishing fluid, current density is used 0.5A/cm2, voltage 30V, time 8S;
S5.EBSD analysis: inlaying resin with the acetone solution of the pure grade of analysis, time 10h, obtains final to be tested Sample to be tested is placed in Electronic Speculum and obtains Kikuchi style using EBSD analysis system by sample.
The normal direction distribution of orientations figure of the present embodiment EBSD analysis electrolytic capacitor electric aluminum foil is shown in Fig. 3, the calibration of sample Rate works well up to 90% or more.
Embodiment 7
A kind of electrolytic capacitor, to EBSD analysis method, is included the following steps: with electronics aluminum foil method
S1. it samples and inlays: sample being cut into 30mm*50mm with paper knife, carried out inlaying solidification with epoxy resin;
S2. it mechanically polishes: successively being polished with 400#, 2000#, 5000#SiC waterproof abrasive paper, polishing time 5min, used Water as cleaning agent, after with partial size be 100nmSiO2Polishing fluid polishes sample tested surface, polishing time 10min;
S3. vibropolish: vibropolish is carried out using vibropolish instrument, polishing fluid is that partial size is 80nmSiO2Polishing fluid, Time is 180min;
S4. electrobrightening: ethyl alcohol: perchloric acid: hexylene glycol monobutyl ether=8:1:1 polishing fluid, current density is used 0.05A/cm2, voltage 30V, time 8S;
S5.EBSD analysis: inlaying resin with the acetone solution of the pure grade of analysis, time 10h, obtains final to be tested Sample to be tested is placed in Electronic Speculum and obtains Kikuchi style using EBSD analysis system by sample.
The normal direction distribution of orientations figure of the present embodiment EBSD analysis electrolytic capacitor electric aluminum foil is shown in Fig. 3, the calibration of sample Rate works well up to 91% or more.
Embodiment 8
A kind of electrolytic capacitor, to EBSD analysis method, is included the following steps: with electronics aluminum foil method
S1. it samples and inlays: sample being cut into 30mm*50mm with paper knife, carried out inlaying solidification with epoxy resin;
S2. it mechanically polishes: successively being polished with 400#, 2000#, 5000#SiC waterproof abrasive paper, polishing time 5min, used Water as cleaning agent, after with partial size be 100nmSiO2Polishing fluid polishes sample tested surface, polishing time 10min;
S3. vibropolish: vibropolish is carried out using vibropolish instrument, polishing fluid is that partial size is 80nmSiO2Polishing fluid, Time is 180min;
S4. electrobrightening: ethyl alcohol: perchloric acid: hexylene glycol monobutyl ether=8:1.5:1.5 polishing fluid, current density is used 0.45A/cm2, voltage 30V, time 8S;
S5.EBSD analysis: inlaying resin with the acetone solution of the pure grade of analysis, time 10h, obtains final to be tested Sample to be tested is placed in Electronic Speculum and obtains Kikuchi style using EBSD analysis system by sample.
The normal direction distribution of orientations figure of the present embodiment EBSD analysis electrolytic capacitor electric aluminum foil is shown in Fig. 3, the calibration of sample Rate works well up to 97% or more.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description To make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all this Made any modifications, equivalent replacements, and improvements etc., should be included in the claims in the present invention within the spirit and principle of invention Protection scope within.

Claims (10)

1. the sample preparation methods that a kind of electrolytic capacitor is analyzed with electronics aluminum foil method to EBSD, which is characterized in that including as follows Step:
S1. it samples and inlays: sample being carried out to inlay solidification with epoxy resin;
S2. it mechanically polishes: using SiC waterproof abrasive paper and SiO2Polishing fluid successively polishes sample tested surface;
S3. vibropolish, polishing fluid SiO vibropolish: are carried out using vibropolish instrument2
S4. electrobrightening: perchloric acid, ethyl alcohol and ethylene glycol monobutyl ether mixed liquor is used to carry out electrobrightening as polishing fluid;
S5. dissolving resin: epoxy resin is inlayed in dissolution, obtains final sample to be tested.
2. the sample preparation methods that electrolytic capacitor as described in claim 1 is analyzed with electronics aluminum foil method to EBSD, feature exist In SiC waterproof abrasive paper described in S2 is finished to successively be processed by shot blasting using 400#, 2000#, 5000#SiC waterproof abrasive paper, polishing Total time is 2~5min.
3. the sample preparation methods that electrolytic capacitor as claimed in claim 2 is analyzed with electronics aluminum foil method to EBSD, feature exist In SiO described in S22The partial size of polishing fluid is 80~100nm, and polishing time is 5~10min.
4. the sample preparation methods that electrolytic capacitor as described in claim 1 is analyzed with electronics aluminum foil method to EBSD, feature exist In SiO described in S32The partial size of polishing fluid is 50~80nm, and the time is 150~180min.
5. electrolytic capacitor as claimed in claim 4 is with electronics aluminum foil method to EBSD analysis method, which is characterized in that described in S3 SiO2The partial size of polishing fluid is 50~70nm.
6. the sample preparation methods that electrolytic capacitor as described in claim 1 is analyzed with electronics aluminum foil method to EBSD, feature exist In the volume ratio of perchloric acid, ethyl alcohol and ethylene glycol monobutyl ether is 8:1~1.5:1~1.5 in S4.
7. the sample preparation methods that electrolytic capacitor as claimed in claim 6 is analyzed with electronics aluminum foil method to EBSD, feature exist In 0.05~0.5A/cm of current density of electrobrightening described in S42, voltage 30V, 5~15S of time.
8. the sample preparation methods that electrolytic capacitor as claimed in claim 7 is analyzed with electronics aluminum foil method to EBSD, feature exist In 0.15~0.45A/cm of current density of electrobrightening described in S42, the time is 5~8S.
9. the sample preparation side that the electrolytic capacitor as described in claim 1~8 any one is analyzed with electronics aluminum foil method to EBSD Method, which is characterized in that the solvent of dissolved epoxy described in S5 is analysis pure acetone, dissolution time 5-10h.
10. the sample preparation methods that the electrolytic capacitor as described in claim 9 any one is analyzed with electronics aluminum foil method to EBSD, It is characterized in that, dissolution time described in S5 is 10h.
CN201910666039.XA 2019-07-23 2019-07-23 A kind of sample preparation methods that electrolytic capacitor is analyzed with electronics aluminum foil method to EBSD Pending CN110455840A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111650024A (en) * 2020-05-27 2020-09-11 西安泰力松新材料股份有限公司 Tinned copper wire/strip metallographic etchant and metallographic structure sample preparation method
CN111929337A (en) * 2020-06-17 2020-11-13 宁波锦越新材料有限公司 EBSD sample preparation method of Al-Zn-Mg-Cu alloy and EBSD sample
CN113866200A (en) * 2021-09-29 2021-12-31 广西容创新材料产业研究院有限公司 Preparation method of segregation-method high-purity aluminum EBSD sample

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