CN108796597A - A kind of Al/Ti cold rolling composite plates electrolytic polishing method - Google Patents
A kind of Al/Ti cold rolling composite plates electrolytic polishing method Download PDFInfo
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- CN108796597A CN108796597A CN201810571604.XA CN201810571604A CN108796597A CN 108796597 A CN108796597 A CN 108796597A CN 201810571604 A CN201810571604 A CN 201810571604A CN 108796597 A CN108796597 A CN 108796597A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/16—Polishing
- C25F3/18—Polishing of light metals
- C25F3/20—Polishing of light metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/16—Polishing
- C25F3/22—Polishing of heavy metals
- C25F3/26—Polishing of heavy metals of refractory metals
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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
- G01N1/32—Polishing; Etching
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Abstract
The invention belongs to electrobrightening technical fields, disclose a kind of Al/Ti cold rolling composite plates electrolytic polishing method, after new electrolytic polishing method, sample is clamped with fixture and is put into Si Teer Lectropol-5 electrobrightening instrument, it is 12 to control speed stream, voltage 10-15V, temperature is 2-5 DEG C, time 100-120s, is washed with water after the completion of polishing, with alcohol rinse, cold wind drying；It carries out electron backscatter diffraction (EBSD) and analyzes calibration.Al/Ti cold rolling composite plates surface-brightening such as mirror after electrobrightening, the defects of without apparent corrosion pit, when carrying out EBSD, the Al layers of interface both sides and Ti layer can be carried out at the same time EBSD and demarcate, and calibration rate is very high, reaches 99% or more.
Description
Technical field
The invention belongs to electrobrightening technical field more particularly to a kind of Al/Ti cold rolling composite plates electrolytic polishing methods.
Background technology
Currently, the prior art commonly used in the trade is such：The density of titanium is small, and specific strength is high, and heat-proof corrosion-resistant is good, is very
The good strong alloy material of heat, the reserves very abundant in the earth's crust.The linear expansion coefficient very little of titanium, generates in heating and cooling
The features such as thermal stress is smaller, mechanical performance and good mechanical properties is a kind of excellent structural material, thus space flight and aviation,
The fields such as chemical industry, metallurgy, which are obtained for, to be widely applied.Same metal is not alternately or the metallic multilayer of enhancing metal layer composition is multiple
Condensation material can significantly improve the mechanical property of material.Al/Ti composite materials are existed due to its excellent mechanical property and low-density
There are prodigious potentiality in commercial Application.Since Al ratios Ti is cheap, so economically this composite material has more than single Ti
Attraction.Can be used to produce double metallic composite material with multi-layer structure by cold rolling, due to Ti hexagonal crystallographic texture and
Difference between the face-centered cubic crystal structure of Al may influence the deformation in cold-rolled process and Al-Ti interface microstructures
Variation, therefore study Al-Ti interface microstructures tissue be conducive to analysis cold-rolled process in different metal interface tissue
Change procedure.Electron backscatter diffraction (EBSD) technology has become the microstructural powerful tool of analysis in recent years.
Traditional electrolytic polishing process, bath composition is complicated, and containing harmful substance, environmental pollution is larger.And not
With the two different metal materials of electrobrightening simultaneously, this brings difficulty to the research of Al/Ti composite materials.It is therefore desirable to
A kind of simple at split-phase and neutrality environmental protection Al/Ti composite plate electrobrightening technologies are developed to have a very important significance.
In conclusion problem of the existing technology is：Traditional electrolytic polishing process handles Al/Ti cold rolling composite plates
When, workpiece surface can be caused to shade, be easy to form hot spot and piebald, and brightness is not obvious.It is electron backscattered in progress
It can not be carried out at the same time calibration for Al layers and Ti layers when diffraction (EBSD) is analyzed, seriously affect experiment process.
Solve the difficulty and meaning of above-mentioned technical problem：After new electrolytic polishing method, the Al/Ti after electrobrightening
Cold rolling composite plate surface-brightening such as mirror the defects of without apparent corrosion pit, is analyzed carrying out electron backscatter diffraction (EBSD)
When, the Al layers of interface both sides can be carried out at the same time EBSD calibration with Ti layers, and interface grain structure is high-visible, and calibration rate is very
Height reaches 99% or more.Conventional efficient is greatly improved, the Micro-Structure Analysis of sample is conducive to.
Invention content
In view of the problems of the existing technology, the present invention provides a kind of Al/Ti cold rolling composite plates electrolytic polishing methods.
The invention is realized in this way a kind of electrolytic polishing liquid, which is characterized in that the electrolytic polishing liquid is according to volume ratio
For perchloric acid：Alcohol=1:9.
Another object of the present invention is to provide a kind of polishing method using the electrolytic polishing liquid, the polishing methods
Including：Sample is clamped with fixture and is put into Si Teer Lectropol-5 electrobrightening instrument, it is 12 to control speed stream, voltage 10-
15V, temperature are 2-5 DEG C, time 100-120s, are washed with water after the completion of polishing, with alcohol rinse, cold wind drying；It carries out
EBSD is demarcated.
Another object of the present invention is to provide a kind of Al/Ti cold rolling composite plates using the electrolytic polishing liquid to be electrolysed throwing
Light method, the Al/Ti cold rolling composite plates electrolytic polishing method include the following steps：
Al/Ti composite plates after cold rolling are cut into 20x 15x 2mm small size samples by step 1；
Step 2 clamps Al/Ti samples with fixture, and according to 400#, 800#, 1200#, 1600#, 2000# sand paper is beaten successively
Mill, each sand paper are polishing to surface-brightening and ensure that sample surfaces are smooth；
Sample after polishing is steeped into acetone 5min oil removings, is washed, then cleaned with alcohol, cold wind by step 3
Drying；
Step 4 is mechanically polished sample, alcohol is clear successively using 0.5 μm and 0.25 μm of diamond polishing cream
Wash rear cold wind drying；
Step 5, perchloric acid：Alcohol=1:(when electrobrightening, perchloric acid excessive concentration causes 9 configuration electrolytic polishing liquids
Sample surfaces corrode overweight nigrescence；Concentration is too low, and the cut that sample surfaces grinding introduces fails to eliminate, and there are stressor layers)；
Sample is clamped with fixture and is put into Si Teer Lectropol-5 electrobrightening instrument by step 6, is controlled fast stream and is
12, voltage 10-15V, temperature are 2-5 DEG C, time 100-120s, are cleaned with a large amount of water after the completion of polishing, cold with alcohol rinse
Wind is dry；
Step 7 carries out EBSD calibration.
In conclusion advantages of the present invention and good effect are：After new electrolytic polishing method, after electrobrightening
Al/Ti cold rolling composite plates surface-brightening such as mirror the defects of without apparent corrosion pit, is carrying out electron backscatter diffraction (EBSD)
When analysis, compared with traditional polishing method, the Al layers of interface both sides can be carried out at the same time EBSD calibration with Ti layers, and interface is brilliant
Kernel structure is high-visible, and calibration rate is very high, reaches 99% or more.Conventional efficient is greatly improved, the micro- of sample is conducive to
See structural analysis.
Description of the drawings
Fig. 1 is Al/Ti cold rolling composite plates electrolytic polishing method flow chart provided in an embodiment of the present invention.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
As shown in Figure 1, Al/Ti cold rolling composite plates electrolytic polishing method provided in an embodiment of the present invention includes the following steps：
S101：Al/Ti composite plates after cold rolling are cut into 20x 15x 2mm small size samples；
S102：Al/Ti samples are clamped with fixture, according to 400#, 800#, 1200#, 1600#, 2000# sand paper is polished successively,
Each sand paper is polishing to surface-brightening and ensures that sample surfaces are smooth；
S103：Sample after polishing is steeped into acetone 5min oil removings, is then washed, then cleaned with alcohol, it is cold
Wind is dry；
S104：Using 0.5 μm and 0.25 μm of diamond polishing cream, sample is mechanically polished successively, alcohol washes
Cold wind dries up afterwards；
S105：Perchloric acid：Alcohol=1:9 (volume ratios) configure electrolytic polishing liquid；
S106：Sample is clamped with fixture and is put into Si Teer Lectropol-5 electrobrightening instrument, it is 12 to control speed stream,
Voltage 10-15V, temperature are 2-5 DEG C, time 100-120s, are cleaned immediately with a large amount of water after the completion of polishing, with alcohol rinse,
Cold wind dries up；
S107：Carry out EBSD calibration.
Prove part (specific embodiment/experiment/emulation /)
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (3)
1. a kind of electrolytic polishing liquid, which is characterized in that the electrolytic polishing liquid is perchloric acid according to volume ratio：Alcohol=1:9.
2. a kind of polishing method using electrolytic polishing liquid described in claim 1, which is characterized in that the polishing method includes：
Sample is clamped with fixture and is put into Si Teer Lectropol-5 electrobrightening instrument, it is 12, voltage 10-15V, temperature to control speed stream
Degree is 2-5 DEG C, time 100-120s, is washed with water after the completion of polishing, with alcohol rinse, cold wind drying；Carry out EBSD calibration.
3. a kind of Al/Ti cold rolling composite plate electrolytic polishing methods using electrolytic polishing liquid described in claim 1, feature exists
In the Al/Ti cold rolling composite plates electrolytic polishing method includes the following steps：
Al/Ti composite plates after cold rolling are cut into 20x15x2mm small size samples by step 1；
Step 2 clamps Al/Ti samples with fixture, and according to 400#, 800#, 1200#, 1600#, 2000# sand paper is polished successively, often
Kind sand paper is polishing to surface-brightening and ensures that sample surfaces are smooth；
Sample after polishing is steeped into acetone 5min oil removings, is washed, then cleaned with alcohol by step 3, cold wind drying；
Step 4 is mechanically polished sample, using 0.5 μm and 0.25 μm of diamond polishing cream after alcohol washes successively
Cold wind dries up；
Step 5, perchloric acid：Alcohol=1:9 configuration electrolytic polishing liquids；
Sample is clamped with fixture and is put into Si Teer Lectropol-5 electrobrightening instrument by step 6, and it is 12 to control speed stream, electricity
It is 2-5 DEG C, time 100-120s to press 10-15V, temperature, is cleaned with a large amount of water after the completion of polishing, and with alcohol rinse, cold wind is blown
It is dry；
Step 7 carries out EBSD calibration.
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| CN201810571604.XA CN108796597A (en) | 2018-06-06 | 2018-06-06 | A kind of Al/Ti cold rolling composite plates electrolytic polishing method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109991254A (en) * | 2019-04-29 | 2019-07-09 | 福建工程学院 | A kind of preparation method of pure iron EBSD sample |
| CN110044939A (en) * | 2019-04-22 | 2019-07-23 | 广东省材料与加工研究所 | A kind of steel/iron double metal composite sample preparation method for EBSD test |
| CN110528059A (en) * | 2019-09-23 | 2019-12-03 | 青海大学 | 8 line aluminium alloy electrolytic polishing liquids of one kind and its preparation and polishing method |
| CN110632104A (en) * | 2019-08-22 | 2019-12-31 | 江苏理工学院 | Electrolytic polishing method for pure titanium and titanium alloy EBSD samples |
| CN110724999A (en) * | 2019-10-23 | 2020-01-24 | 沈阳航空航天大学 | Electrolyte for CoCrNi multi-principal-element alloy with high Cr content and corrosion process |
| CN111595876A (en) * | 2020-06-02 | 2020-08-28 | 全球能源互联网研究院有限公司 | Electrolytic clamp and method for preparing EBSD sample of metal sheet |
| CN113295724A (en) * | 2021-05-19 | 2021-08-24 | 上海大学 | Sample for analysis and characterization of electron back scattering diffraction after alloy corrosion and preparation method thereof |
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| CN103226074A (en) * | 2013-03-15 | 2013-07-31 | 北京工业大学 | Cu-Ni alloy electro-polishing method used for EBSD test |
| CN107402150A (en) * | 2017-07-24 | 2017-11-28 | 东北大学 | A kind of electrobrightening preparation method of titanium aluminium base alloy EBSD sample for analysis |
| CN107460534A (en) * | 2017-09-05 | 2017-12-12 | 宝鸡市同业精密科技有限责任公司 | The electrochemical polish liquid and polishing method of a kind of titanium or titanium alloy |
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| CN103226074A (en) * | 2013-03-15 | 2013-07-31 | 北京工业大学 | Cu-Ni alloy electro-polishing method used for EBSD test |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110044939A (en) * | 2019-04-22 | 2019-07-23 | 广东省材料与加工研究所 | A kind of steel/iron double metal composite sample preparation method for EBSD test |
| CN110044939B (en) * | 2019-04-22 | 2021-11-23 | 广东省材料与加工研究所 | Preparation method of steel/iron bimetal composite material sample for EBSD test |
| CN109991254A (en) * | 2019-04-29 | 2019-07-09 | 福建工程学院 | A kind of preparation method of pure iron EBSD sample |
| CN110632104A (en) * | 2019-08-22 | 2019-12-31 | 江苏理工学院 | Electrolytic polishing method for pure titanium and titanium alloy EBSD samples |
| CN110528059A (en) * | 2019-09-23 | 2019-12-03 | 青海大学 | 8 line aluminium alloy electrolytic polishing liquids of one kind and its preparation and polishing method |
| CN110724999A (en) * | 2019-10-23 | 2020-01-24 | 沈阳航空航天大学 | Electrolyte for CoCrNi multi-principal-element alloy with high Cr content and corrosion process |
| CN110724999B (en) * | 2019-10-23 | 2021-09-28 | 沈阳航空航天大学 | Electrolyte for CoCrNi multi-principal-element alloy with high Cr content and corrosion process |
| CN111595876A (en) * | 2020-06-02 | 2020-08-28 | 全球能源互联网研究院有限公司 | Electrolytic clamp and method for preparing EBSD sample of metal sheet |
| CN113295724A (en) * | 2021-05-19 | 2021-08-24 | 上海大学 | Sample for analysis and characterization of electron back scattering diffraction after alloy corrosion and preparation method thereof |
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Application publication date: 20181113 |
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