CN108107064A - It is a kind of be used to prepare annealing after aluminum-steel composite board interface EBSD test method - Google Patents
It is a kind of be used to prepare annealing after aluminum-steel composite board interface EBSD test method Download PDFInfo
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- CN108107064A CN108107064A CN201711337784.7A CN201711337784A CN108107064A CN 108107064 A CN108107064 A CN 108107064A CN 201711337784 A CN201711337784 A CN 201711337784A CN 108107064 A CN108107064 A CN 108107064A
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- electrobrightening
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/203—Measuring back scattering
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
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- 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
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- 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
- G01N2001/2866—Grinding or homogeneising
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Abstract
The present invention for it is a kind of be used to prepare annealing after aluminum-steel composite board interface EBSD test method.This method comprises the following steps：The section of aluminum-steel composite board carries out electrobrightening after mechanical lapping and mechanical polishing, wherein：Cathode material is stainless steel, and anode is the sample that upper step obtains, voltage：17~20V, electric current：0.2~0.5A, ice-water bath, polishing time are 20 30S；Wherein, the composition of electrolyte includes hydrochloric acid, methanol and potassium hyperchlorate, adds absolute methanol 90g, 3 5g potassium hyperchlorates in every 10mL hydrochloric acid；It after last sample is rinsed with water, then is placed in ethyl alcohol and is cleaned, then drying preserves, and obtains compound board interface to be measured.This method step is simple, easily operated, and Surface stress layer is can remove during essence is thrown, and helps to study the development law of interface intermetallic compound.
Description
Technical field
The present invention relates to Analysis of Metallic Materials technical fields, and in particular to one kind is spread out for aluminum-steel composite board to be electron backscattered
Penetrate the preparation method of analysis electron backscatter diffraction (EBSD) test sample.
Background technology
Aluminum-steel composite board is using cold rolling, and then annealing makes steel layer and aluminium layer realize strong metallurgical combines one on interface
Kind new material, not only has many advantages, such as that aluminium density is small, conductivity is high, also the intensity with steel is high, is widely used in
The fields such as automobile, aviation, power station.But intermetallic compound may be formed at aluminum steel interface during subsequent anneal, more than certain
Thickness can then reduce the bond strength at interface.Therefore, aluminum-steel composite board prepares microstructure and performance during processing and heat treatment
Between relation become researcher research emphasis.
In order to effectively exploring aluminum-steel composite board in the development law of heat treatment process Interface Microstructure and texture, it is necessary to
Electron backscatter diffraction EBSD analyses are carried out to composite plate.Electron backscatter diffraction (EBSD) technology is based on electricity in scanning electron microscope
Beamlet in the analysis of diffraction Kikuchi band for tilting sample surfaces and exciting and being formed, the data collected can drawing diagram, crystal grain take
Xiang Tu, pole figure and inverse pole figure etc..The electrobrightening of mild steel is to use cathode material as copper sheet, polishing fluid for HCLO4 and
CH3CH2OH mixed solutions；The electrobrightening of fine aluminium and aluminium alloy is to use cathode material as nickel plate or steel, polishing fluid HF
Aqueous acid electrolyte.During traditional EBSD preparation method of sample is used, since the larger and HF of steel aluminium polishing fluid difference is sour
It is dangerous and volatile, it is difficult to be processed by shot blasting by existing polishing agent to aluminum steel composite material, EBSD tests can not be carried out,
It can not observe that aluminum-steel composite board prepares the changing rule of processing and heat treatment process median surface microstructure and texture；Work as use
HClO4When being electrolysed the aluminum-steel composite board in interlayer simultaneously with CH3CH2OH for electrolyte, then existing can not be by interlayer electricity
The deficiencies of solution polishing is drawn.It is rotten caused by technological parameter is unstable also, when conventional electrolytic methods prepare EBSD samples
Etch pit often occurs, and has a significant impact to the generation tool of diffraction pattern.
The Chinese patent of 105628474 A of Publication No. CN discloses a kind of aluminum steel by after grinding and buffing and answers
Condensation material is electrolysed aluminum side using hydrofluoric acid aqueous solution, reuses nital and the composite sample after electrolysis is wiped clearly
Washing the method for 30-60s makes the grain structure of aluminum steel composite material both sides show simultaneously.This kind of method is divided into two steps, step
Cumbersome, hydrofluoric acid is dangerous and volatile in electrolyte, and cannot effectively eliminate the stressor layers of sample surfaces, what aluminum steel interface was formed
Interlayer, which also fails to calibrate, to be come.
The content of the invention
It is insufficient present in current techniques the purpose of the present invention is being directed to, it is compound to provide aluminum steel after one kind is used to prepare annealing
The method of board interface EBSD tests.The electrolyte that this method is formed using potassium hyperchlorate, hydrochloric acid and methanol, by appropriate technique
The selection of parameter can go out matrix steel and coating aluminium by electrobrightening simultaneously, and most important is that can go out metallic intermediate layer with electrobrightening
Between compound layer.And this method step is simple, and it is easily operated, Surface stress layer is can remove during essence is thrown, helps to study
The development law of intermetallic compound.
The technical solution adopted by the present invention is as follows：
It is a kind of be used to prepare annealing after aluminum-steel composite board interface EBSD test method, comprise the following steps：
1) prepared by sample
The mild steel combined after mill-annealed and pure aluminium clad sheet are cut, then by the section of aluminum-steel composite board downward
It is placed in mounting press and carries out edge sample；
2) mechanical lapping
The section of sample is ground successively with the sand paper of 400#, 800#, 1000#, 1500# and 2000#；
3) mechanically polish：Section obtained above is subjected to rough polishing first with the diamond spraying polishing agent that granularity is 1.5
Polishing, polishing disk rotating speed 450-600r/min, polishing time are 2~3min；Then it is 0.3 aluminum oxide suspension to use granularity again
(concentration 20%) carries out essence polishing, rotating speed 60-100r/min, and polishing time is 1~2min；Sample is taken out again, is used
Acetone is cleaned by ultrasonic；
4) electrobrightening
Sample after mechanical lapping is polished carries out electrobrightening, and the technical parameter of electrobrightening is：Cathode material is not
Become rusty steel, the sample that anode obtains for upper step, voltage：17~20V, electric current：0.2~0.5A, ice-water bath, polishing time 20-
30S；Wherein, the composition of electrolyte includes hydrochloric acid, methanol and potassium hyperchlorate, adds absolute methanol 90g, 3-5g high in every 10mL hydrochloric acid
Potassium chlorate；
5) ethyl alcohol cleans
It after sample after electrobrightening is rinsed with water, then is placed in ethyl alcohol and is cleaned, then drying preserves, and is treated
Survey compound board interface.
The hydrochloric acid is that mass fraction concentration is 37%.
The beneficial effects of the invention are as follows：
1) present invention passes through mechanical grinding grinding and polishing using potassium hyperchlorate, hydrochloric acid, the mixed liquor of methanol as electrolytic polishing liquid
Light, electrobrightening handle sample interface, and the stressor layers of sample surfaces can be effectively removed after rough polishing and essence throwing, are conducive to
EBSD generates strong diffraction pattern when testing, in order to carry out preparing the interlayer generated after processing and heat treatment to aluminum-steel composite board
Microstructure and texture research and analysis；
2) present invention have many advantages, such as it is fairly simple, conveniently, effect it is relatively good and relatively safe and applicable in low-carbon
Steel, fine aluminium composite material interface EBSD test, efficiently solve composite material interface EBSD observation during sample prepare
It is difficult.
Description of the drawings
Fig. 1 is mild steel and pure aluminium clad sheet annealed state crystal grain phasor prepared by the embodiment of the present invention 1；
Fig. 2 is mild steel and pure aluminium clad sheet annealed state crystal grain orientation maps prepared by the embodiment of the present invention 1；
Fig. 3 is mild steel and pure aluminium clad sheet annealed state crystal grain phasor prepared by the embodiment of the present invention 2；
Fig. 4 is mild steel and pure aluminium clad sheet annealed state crystal grain orientation maps prepared by the embodiment of the present invention 2.
Specific embodiment
Technical scheme is illustrated with reference to embodiment.
Embodiment 1：
The present invention provides a kind of preparation method for aluminum-steel composite board interface electron backscatter diffraction analysis test sample,
Include the following steps：
1) prepared by sample
By mild steel and pure aluminium clad sheet cut into size be respectively thickness, width and length be respectively 1.6mm, 5mm,
8mm, then by aluminum-steel composite board (composite plate is combined one block of plate after mill-annealed) section i.e. 1.6mm*8mm
It is placed face down in mounting press and carries out edge sample, aluminum-steel composite board electron backscatter diffraction analysis original sample is obtained, convenient for EBSD
The acquisition of data during observation obtains the EBSD testing results of high quality；
2) mechanical lapping
The sample of preparation is subjected to grinding for different passage (400#, 800#, 1000#, 1500# and 2000#), (wherein, slightly
Sand paper 400#, 800# milling time are 3min, and 1500#, 2000# milling time are 2min.Following embodiment is same) pay attention to grinding when
It changes one of sand paper and replaces 90 degree and be ground.The smooth of surface is centainly paid attention to during mechanical lapping, is pressed lightly on, avoids generating platform
Rank.
3) mechanically polish
Rough polishing, polishing disk rotating speed 450-600r/ are carried out first with the diamond spraying polishing agent that granularity is 1.5 microns
Min, polishing time 2min, it is desirable that the smooth no marking of any surface finish.Granularity is 0.3 micron of aluminum oxide suspension when essence is thrown
(mass percentage concentration 20%) carries out essence and throws polishing, rotating speed 60-100r/min.Polishing time is 1min, after essence is thrown
Style is taken out, and is cleaned by ultrasonic 3min with acetone, and the essence that can obtain surface without residual stress throws sample.
4) electrobrightening
Sample after mechanical lapping is polished carries out electrobrightening, and the technical parameter of electrobrightening is：Cathode material is not
Become rusty steel, (anode is sample specimens) voltage：17V, electric current：0.2A, ice-water bath, the composition of electrolytic polishing liquid is potassium hyperchlorate, salt
Acid and methanol, wherein, potassium hyperchlorate solid 3g is weighed, measures hydrochloric acid (mass fraction 37%, density 1.19g/cm3)
10ml, absolute methanol 90g；After hydrochloric acid and methanol are sufficiently mixed, potassium hyperchlorate is dissolved in mixed liquor and obtains electrolyte.Polishing
Time is 20S.
5) ethyl alcohol cleans
Sample after electrobrightening quickly with clear water is rinsed and is cleaned with being placed in ethyl alcohol, and dries up preservation.
The phasor of EBSD sample for analysis is as shown in Figure 1, substantially there is four distributed mutuallies obtained by the present embodiment in figure.In scanning electricity
Two layers of the centre that cannot be distinguished completely under mirror FeAl3And Fe2Al5, must clearly display at this time, as arrow direction indicates.
For crystal grain orientation maps as shown in Fig. 2, crystal boundary is apparent as seen from Figure 2, intermetallic compounds layer grain contours are clear, can meet orientation
Requirement is calculated, it is with obvious effects, and Fe is disclosed in figure2Al5It is mutually column crystal, and its crystal grain orientation can explicitly indicate that.It consequently facilitating will
Crystal structure and orientation information is corresponding with microstructure morphology is studied.
Bath composition is potassium hyperchlorate, hydrochloric acid and methanol in the present invention, this electrolyte contains perchloric acid sylvite, on a small quantity
Acid, therefore polishing process will not need different time because of different layers and cause excessive erosion, damage sample.During electrobrightening, need
Ensure that sample has the good stability for contacting, ensureing electric current and temperature with fixture, ice water mixing is placed in electrolytic cell periphery
Object is controlled into trip temperature, prevents temperature is excessively high from causing danger.The electrolyte standing time prepared is unsuitable long, does not exceed generally
2 days.Sample after polishing is put into ethyl alcohol and is cleaned multiple times, to remove the polishing fluid of surface residual, ensure specimen surface cleaning,
Totally.Sample after polished and cleaned carries out EBSD structure observations.
Embodiment 2：
The present invention provides a kind of preparation side for aluminum steel composite material interface electron backscatter diffraction analysis test sample
Method includes the following steps：
1) prepared by sample
It is respectively the rectangular of 1.6mm, 5mm, 8mm that mild steel and pure aluminium clad sheet material are cut into thickness, width and length
Shape sample, then using inlay sample powder carry out edge sample obtain aluminum-steel composite board electron backscatter diffraction analysis original sample so that
EBSD facilitates data acquisition so as to obtain the EBSD testing results of high quality when observing；
2) mechanical lapping
The sample of preparation is subjected to grinding for different passage (400#, 800#, 1000#, 1500# and 2000#), (wherein, slightly
Sand paper 400#, 800# milling time are 3min, and 1500#, 2000# milling time are 2min.Following embodiment is same) pay attention to grinding when
It changes one of sand paper and replaces 90 degree and be ground.The smooth of surface is centainly paid attention to during mechanical lapping, is pressed lightly on, avoids generating platform
Rank.
3) mechanically polish
Rough polishing, polishing disk rotating speed 450-600r/ are carried out first with the diamond spraying polishing agent that granularity is 1.5 microns
Min, polishing time 2min, it is desirable that the smooth no marking of any surface finish.Granularity is 0.3 micron of aluminum oxide suspension when essence is thrown
(mass percentage concentration 20%) is polished, rotating speed 60-100r/min.Polishing time is 1min, the style after essence is thrown
It takes out, is cleaned by ultrasonic 3min with acetone, the essence that can obtain surface without residual stress throws sample.
3) electrobrightening
Sample after mechanical lapping is polished carries out electrobrightening, and the technical parameter of electrobrightening is：Cathode material is not
Become rusty steel, (anode is sample) voltage：20V, electric current：0.5A, ice-water bath, the composition of electrolytic polishing liquid is potassium hyperchlorate, hydrochloric acid and
Methanol, wherein, potassium hyperchlorate solid 5g is weighed, measures hydrochloric acid (mass fraction 37%, density 1.19g/cm3) 10ml, nothing
Water methanol 90g；After hydrochloric acid and methanol are sufficiently mixed, potassium hyperchlorate is dissolved in mixed liquor and obtains electrolyte.Polishing time is
30S。
4) ethyl alcohol cleans
Sample after electrobrightening is placed in ethyl alcohol and is cleaned, and dries up preservation.
The phasor of EBSD sample for analysis is as shown in figure 3, substantially there is four distributed mutuallies obtained by the present embodiment in figure.In scanning electricity
Two layers of the centre that cannot be distinguished completely under mirror FeAl3And Fe2Al5, must clearly display at this time, as arrow direction indicates.
For crystal grain orientation maps as shown in figure 4, crystal boundary is apparent as seen from Figure 4, intermetallic compounds layer grain contours are clear, can meet orientation
Requirement is calculated, it is with obvious effects, and Fe is disclosed in figure2Al5It is mutually column crystal, and its crystal grain orientation can explicitly indicate that.It consequently facilitating will
Crystal structure and orientation information is corresponding with microstructure morphology is studied.
Embodiment 3：
Other steps are identical with above-described embodiment 1, and difference is by KClO in electrolyte4It weighs as 7g, then cannot
Aluminum steel both sides and intermetallic compounds layer electrobrightening are drawn.The also non-electrobrightening of intermetallic compounds layer comes out, and both sides
Aluminum steel it is burnt, cause local excessive erosion, can not obtain a result.
Unaccomplished matter of the present invention is known technology.
Claims (2)
1. it is a kind of be used to prepare annealing after aluminum-steel composite board interface EBSD test method, it is characterized in that this method include it is following
Step：
1) prepared by sample
The mild steel combined after mill-annealed and pure aluminium clad sheet are cut, are then placed face down on cutting for aluminum-steel composite board
Edge sample is carried out in mounting press；
2) mechanical lapping
The section of sample is ground successively with the sand paper of 400#, 800#, 1000#, 1500# and 2000#；
3）Mechanical polishing：Section obtained above is subjected to rough polishing polishing first with the diamond spraying polishing agent that granularity is 1.5,
Polishing disk rotating speed is 450-600r/min, and polishing time is 2 ~ 3min；Then it is 0.3 aluminum oxide suspension to use granularity again（Concentration
For 20%）Essence polishing, rotating speed 60-100r/min are carried out, polishing time is 1 ~ 2min；Sample is taken out again, with acetone ultrasound
Cleaning；
4）Electrobrightening
Sample after mechanical lapping is polished carries out electrobrightening, and the technical parameter of electrobrightening is：Cathode material is stainless steel,
The sample that anode obtains for upper step, voltage：17~20V, electric current：0.2~0.5A, ice-water bath, polishing time 20-30S；Its
In, the composition of electrolyte includes hydrochloric acid, methanol and potassium hyperchlorate, adds absolute methanol 90g, 3-5g perchloric acid in every 10mL hydrochloric acid
Potassium；
5) ethyl alcohol cleans
It after sample after electrobrightening is rinsed with water, then is placed in ethyl alcohol and is cleaned, then drying preserves, and obtains to be measured multiple
Plywood interface.
2. the method that aluminum-steel composite board interface EBSD after annealing is tested is used to prepare as described in claim 1, it is characterized in that institute
The hydrochloric acid stated is that mass fraction concentration is 37%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109270096A (en) * | 2018-08-21 | 2019-01-25 | 钢铁研究总院 | A kind of EBSD method for making sample |
| CN109839393A (en) * | 2019-03-22 | 2019-06-04 | 南京理工大学 | Slicker solder and its composite material or its alloy electron backscatter diffraction sample preparation technique |
| CN111735836A (en) * | 2020-06-29 | 2020-10-02 | 中国科学院金属研究所 | Preparation method of ultra-pure high-chromium ferrite stainless steel EBSD sample |
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| CN106501052A (en) * | 2016-12-26 | 2017-03-15 | 国家电网公司 | A kind of preparation method for analyzing test sample for copper aluminum composite material EBSD |
| CN106814026A (en) * | 2015-12-02 | 2017-06-09 | 鞍钢股份有限公司 | A kind of clad plate corrosion resisting property method for rapidly testing |
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| CN101506325A (en) * | 2006-08-30 | 2009-08-12 | 卡伯特微电子公司 | Compositions and methods for cmp of semiconductor materials |
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| CN109270096A (en) * | 2018-08-21 | 2019-01-25 | 钢铁研究总院 | A kind of EBSD method for making sample |
| CN109839393A (en) * | 2019-03-22 | 2019-06-04 | 南京理工大学 | Slicker solder and its composite material or its alloy electron backscatter diffraction sample preparation technique |
| CN111735836A (en) * | 2020-06-29 | 2020-10-02 | 中国科学院金属研究所 | Preparation method of ultra-pure high-chromium ferrite stainless steel EBSD sample |
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Application publication date: 20180601 |