CN108106913A - A kind of method of Al-Si alloys OPS polishing sample preparations for EBSD tests - Google Patents
A kind of method of Al-Si alloys OPS polishing sample preparations for EBSD tests Download PDFInfo
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- CN108106913A CN108106913A CN201711155229.2A CN201711155229A CN108106913A CN 108106913 A CN108106913 A CN 108106913A CN 201711155229 A CN201711155229 A CN 201711155229A CN 108106913 A CN108106913 A CN 108106913A
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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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- 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
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Abstract
A kind of method of Al Si alloys OPS polishing sample preparations for EBSD tests, it is that the Al Si alloy samples after mechanical polishing and ultrasonic cleaning are carried out OPS polishing disks to be polished 5 10Min, then the Al Si alloy samples for needing to carry out EBSD analyses are stuck on the fixture of vibropolish, then be placed on the vibrations polishing machine with 0.06umMicroCloth polishing cloths vibrations polishing 34 it is small when, the amplitude of vibratory finishing machine is transferred to maximum.This method can solve the thickness problem of electrobrightening corrosion remelted layer, material benefit more more economical than polishings such as FIB cutting and polishings, the Surface stress layer of sample in cross section also can be effectively removed simultaneously, strong diffraction pattern is generated during favourable EBSD tests, to carry out the research of microstructure and texture to Al Si alloys.
Description
Technical field
A kind of method of Al-Si alloys OPS polishing sample preparations for EBSD tests, is related to using electron backscatter diffraction point
Analysis technology (EBSD) explores the research of the microstructure and texture etc. of Al-Si alloys after high-current pulsed electron beam is handled.
Background technology
After high-current pulsed electron beam repeatedly bombards sample surfaces, rapid melting and fast rapid hardening occur for Al-Si alloy surfaces
Solid, while also induce crystal grain and generate refinement.With the research to high-current pulsed electron beam crystal grain refinement, refinement mechanism etc.
The problem for needing to further investigate as researcher.At present, EBSD technologies can take into account the research of Fine Texture of Material and texture,
As the very means of weight on material structure and textile analysis technology.But the surface stress generated in sample preparation procedure
Layer so that the problem of we can not obtain effective diffraction pattern, and electrobrightening corrodes remelted layer, the polishings such as FIB cutting and polishings
The problems such as polishing area is smaller and of high cost, OPS polishing technologies are efficiency highests at this time, can reach zero loss to remelted layer,
A kind of means of the best removal surface stress of repeatability.
The present invention proposes a kind of OPS polishing method for making sample of Al-Si alloys for EBSD tests, can be used for using
Sample treatment before the surface microscopic tissue and texture in EBSD technical testing Al-Si alloys section.It can solve electrobrightening corruption
The problem of losing remelted layer, material benefit more more economical than the polishing such as FIB cutting and polishing means, while it also can effectively remove sample table
The stressor layers in face are conducive to generate strong diffraction pattern during EBSD tests, in order to carry out microstructure to Al-Si alloys and knit
The research of structure.
The content of the invention
The object of the present invention is to provide the OPS of Al-Si alloys for EBSD tests a kind of polish method for making sample, can be with
For the sample treatment before EBSD technical testings Al-Si alloy surfaces microstructure and texture.It can effectively remove sample table
The stressor layers in face are conducive to generate strong diffraction pattern during EBSD tests, in order to carry out microstructure to Al-Si alloys and knit
The research of structure.
It is provided by the present invention for it is a kind of for EBSD test Al-Si alloys OPS polishing method for making sample, including with
Lower step：
(1) cold edge is carried out to Al-Si-Mg alloys
By the Al-Si alloy samples for needing to carry out EBSD analyses according to being placed in a plastic lid, dental base acrylic resin powder is subsequently poured into,
Dental base acrylic resin powder is allowed to cover sample, finally pours into solidified water, it is allowed to solidify.
(2) Al-Si alloy mechanicals polish
The Al-Si alloy samples surface for needing progress EBSD analyses or section are mechanically polished, it is right after mechanical polishing
Sample carries out ultrasonic cleaning with acetone.
(3) Al-Si alloys are polished using OPS polishing disks
The Al-Si alloy samples surface for needing progress EBSD analyses or section are placed on essence to throw on OPS polishing disks, used
OPS liquid (the thin SiO of o.o5um2Suspension) it is polished 5-10Min.
(4) Al-Si-Mg alloys vibropolish
The Al-Si alloy samples for needing to carry out EBSD analyses are stuck on the fixture of vibropolish, is then placed on and carries
When vibropolish 3-4 is small on the vibrations polishing machine of 0.06umMicroCloth polishing cloths, the amplitude of vibratory finishing machine is transferred to most
Greatly.
(5) Al-Si alloys are carried out unloading sample
The Al-Si alloy samples for needing to carry out EBSD analyses are placed in Heating Furnace, dental base acrylic resin powder is waited to use tweezer after melting
Son is drawn off.
(6) cleaning preservation is carried out to Al-Si alloys
It is carried out ultrasonic cleaning by the alloy after being polished to Al-Si OPS with acetone, then carries out drying preservation.Machinery
The degree of polishing can't see cut after amplifying 500 times with light microscope.
According to the method for the above-mentioned OPS polishing sample preparations for Al-Si alloys, to the Al-Si alloys by vibropolish
EBSD analyses are carried out, since vibropolish effectively eliminates Al-Si alloy samples surface answering due to generations such as mechanical polishings
Power layer, therefore strong diffraction pattern can be obtained, and then obtain the microstructure and texture pattern of Al-Si alloy samples.
Using a kind of method of the OPS polishing sample preparations provided by the present invention for Al-Si alloys for EBSD tests, letter
It is single practical, it can repeat to prepare the Al-Si alloy samples for EBSD microstructures and textile analysis.
1. it must ensure the smooth of sample tested surface after mechanical polishing.Ultrasound is carried out clearly with acetone to sample after mechanical polishing
It washes 5 minutes, pollutes polishing fluid to avoid sample chip remaining after antiscuffing paste or mechanical polishing.
2. the amplitude that vibropolish is polishing machine should tune up maximum, be conducive to remove the stress on surface.
3. the sample prepared will be stored in drying bottle in time, its oxidation is prevented.
Description of the drawings
Fig. 1 is the EBSD Euler diagrams in Al-17.5Si sections after 5 high-current pulsed electron beam processing.
Fig. 2 is the EBSD Euler diagrams in Al-17.5Si sections and crystal boundary figure after 15 high-current pulsed electron beam processing.
Fig. 3 is the EBSD Euler diagrams in Al-17.5Si sections and crystal boundary figure after 25 high-current pulsed electron beam processing.
Fig. 4 is the EBSD Euler diagrams in Al-17.5Si sections and crystal boundary figure after 25 high-current pulsed electron beam processing.
Specific embodiment
Example 1
Cold edge will be carried out by 5 high-current pulsed electron beams treated Al-17.5Si alloy samples section into Ф's 30
Sample.After its solidification, mechanically polished, ultrasonic cleaning is carried out with acetone to sample after mechanical polishing；Then by machine
Sample after tool polishing is thrown in essence is polished 5Min on OPS polishing disks using the OPS liquid of o.o5um, then the processing of 5 subpulses
Al-17.5Si alloy samples afterwards are stuck on the fixture of vibropolish, while are placed on 0.06umMicroCloth polishing cloths
Vibratory finishing machine on vibrations polishing 3 it is small when, the amplitude of vibratory finishing machine is transferred to maximum.Finally by 5 subpulses, treated
Al-17.5Si alloy samples are placed in Heating Furnace, and dental base acrylic resin powder is waited to be drawn off after melting with tweezers, and to Al-Si OPS
It is carried out ultrasonic cleaning by the alloy after polishing with acetone, is then carried out drying preservation and is treated that EBSD is tested.Fig. 1 is 5 high currents
The EBSD Euler diagrams in Al-17.5Si sections after pulsed electron beam processing.
Example 2
Cold edge will be carried out by 15 high-current pulsed electron beams treated Al-17.5Si alloy samples section into Ф's 30
Sample.After its solidification, mechanically polished, ultrasonic cleaning is carried out with acetone to sample after mechanical polishing；Then by machine
Sample after tool polishing is thrown in essence is polished 8Min on OPS polishing disks using the OPS liquid of o.o5um, then the processing of 15 subpulses
Al-17.5Si alloy samples afterwards are stuck on the fixture of vibropolish, while are placed on 0.06umMicroCloth polishing cloths
Vibratory finishing machine on vibrations polishing 2 it is small when, the amplitude of vibratory finishing machine is transferred to maximum.Finally by 15 subpulses, treated
Al-17.5Si alloy samples are placed in Heating Furnace, and dental base acrylic resin powder is waited to be drawn off after melting with tweezers, and to Al-Si OPS
It is carried out ultrasonic cleaning by the alloy after polishing with acetone, is then carried out drying preservation and is treated that EBSD is tested.Fig. 2 (a) and (b) are
The EBSD Euler diagrams in Al-17.5Si sections and crystal boundary figure after 15 high-current pulsed electron beam processing.
Example 3
Cold edge will be carried out by 25 high-current pulsed electron beams treated Al-17.5Si alloy samples section into Ф's 30
Sample.After its solidification, mechanically polished, ultrasonic cleaning is carried out with acetone to sample after mechanical polishing；Then by machine
Sample after tool polishing is thrown in essence is polished 10Min on OPS polishing disks using the OPS liquid of o.o5um, then at 25 subpulses
Al-17.5Si alloy samples after reason are stuck on the fixture of vibropolish, while are placed on and are polished with 0.06umMicroCloth
When vibropolish 3 is small on the vibrations polishing machine of cloth, the amplitude of vibratory finishing machine is transferred to maximum.It finally will be after the processing of 25 subpulses
Al-17.5Si alloy samples be placed in Heating Furnace, dental base acrylic resin powder is waited to be drawn off after melting with tweezers, and to Al-Si
It is carried out ultrasonic cleaning by the alloy after OPS polishings with acetone, is then carried out drying preservation and is treated that EBSD is tested.Fig. 3) (a) and
(b) it is the EBSD Euler diagrams in Al-17.5Si sections and crystal boundary figure after 25 high-current pulsed electron beam processing.
Example 4
100 high-current pulsed electron beams treated Al-17.5Si alloy samples section will be passed through and carry out cold edge into Ф 30
Sample.After its solidification, mechanically polished, ultrasonic cleaning is carried out with acetone to sample after mechanical polishing；Then will
Sample after mechanical polishing is thrown in essence is polished 10Min on OPS polishing disks using the OPS liquid of o.o5um, then 100 subpulses
Treated, and Al-17.5Si alloy samples are stuck on the fixture of vibropolish, while are placed on and are thrown with 0.06umMicroCloth
When vibrations polishing 3 is small on the vibrations polishing machine of light cloth, the amplitude of vibrations polishing machine is transferred to maximum.It finally will be at 100 subpulses
Al-17.5Si alloy samples after reason are placed in Heating Furnace, and dental base acrylic resin powder is waited to be drawn off after melting with tweezers, and to Al-
It is carried out ultrasonic cleaning by the alloy after Si OPS polishings with acetone, is then carried out drying preservation and is treated that EBSD is tested.Fig. 4 (a)
With) (b) be the EBSD Euler diagrams in Al-17.5Si sections and crystal boundary figure after the processing of 100 high-current pulsed electron beams.
Claims (1)
1. a kind of OPS method for making sample of Al-Si alloys for EBSD tests, comprises the following steps：
(1) cold edge is carried out to Al-Si-Mg alloys
The Al-Si alloy samples for needing to carry out EBSD analyses are placed in a plastic lid, are subsequently poured into dental base acrylic resin powder, allow dental base acrylic resin powder
Sample is covered, finally pours into solidified water, it is allowed to solidify；
(2) Al-Si alloy mechanicals are polished
The Al-Si alloy samples surface for needing progress EBSD analyses or section are mechanically polished, to sample after mechanical polishing
Ultrasonic cleaning is carried out with acetone；
(3) Al-Si alloys are polished using OPS polishing disks
The Al-Si alloy samples surface for needing progress EBSD analyses or section are placed on essence to throw on OPS polishing disks, use o.o5um
OPS liquid be polished 5-10Min；
(4) to Al-Si-Mg alloy vibropolish
The Al-Si alloy samples for needing to carry out EBSD analyses are stuck on the fixture of vibropolish, is then placed on and carries
When vibrations polishing 3-4 is small on the vibratory finishing machine of 0.06umMicroCloth polishing cloths, the amplitude of vibratory finishing machine is transferred to most
Greatly；
(5) Al-Si alloys are carried out unloading sample and cleaning preserves
The Al-Si alloy samples for needing to carry out EBSD analyses are placed in Heating Furnace, wait dental base acrylic resin powder will with tweezers after melting
It takes out, it then is carried out ultrasonic cleaning with acetone, finally carries out drying preservation.
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| CN201711155229.2A CN108106913A (en) | 2017-11-20 | 2017-11-20 | A kind of method of Al-Si alloys OPS polishing sample preparations for EBSD tests |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109030148A (en) * | 2018-07-27 | 2018-12-18 | 中南大学 | A kind of preparation method of iron(-)base powder EBSD detection sample |
| CN110455840A (en) * | 2019-07-23 | 2019-11-15 | 乳源瑶族自治县东阳光化成箔有限公司 | A kind of sample preparation methods that electrolytic capacitor is analyzed with electronics aluminum foil method to EBSD |
| CN110618149A (en) * | 2019-10-17 | 2019-12-27 | 江苏理工学院 | Preparation method of magnesium alloy EBSD sample |
| CN111982640A (en) * | 2019-05-22 | 2020-11-24 | 国标（北京）检验认证有限公司 | Preparation method for additive manufacturing of aluminum-silicon alloy for EBSD test |
| CN112461874A (en) * | 2020-11-18 | 2021-03-09 | 成都先进金属材料产业技术研究院有限公司 | Method for preparing titanium alloy EBSD samples in batches |
| CN112985956A (en) * | 2021-02-06 | 2021-06-18 | 贵研铂业股份有限公司 | Method for preparing chemical vapor deposition-state rhenium EBSD sample |
| CN118067757A (en) * | 2024-03-13 | 2024-05-24 | 广西大学 | Preparation method of Sn-Bi-based solder alloy EBSD sample |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109030148A (en) * | 2018-07-27 | 2018-12-18 | 中南大学 | A kind of preparation method of iron(-)base powder EBSD detection sample |
| CN111982640A (en) * | 2019-05-22 | 2020-11-24 | 国标（北京）检验认证有限公司 | Preparation method for additive manufacturing of aluminum-silicon alloy for EBSD test |
| CN110455840A (en) * | 2019-07-23 | 2019-11-15 | 乳源瑶族自治县东阳光化成箔有限公司 | A kind of sample preparation methods that electrolytic capacitor is analyzed with electronics aluminum foil method to EBSD |
| CN110618149A (en) * | 2019-10-17 | 2019-12-27 | 江苏理工学院 | Preparation method of magnesium alloy EBSD sample |
| CN112461874A (en) * | 2020-11-18 | 2021-03-09 | 成都先进金属材料产业技术研究院有限公司 | Method for preparing titanium alloy EBSD samples in batches |
| CN112985956A (en) * | 2021-02-06 | 2021-06-18 | 贵研铂业股份有限公司 | Method for preparing chemical vapor deposition-state rhenium EBSD sample |
| CN118067757A (en) * | 2024-03-13 | 2024-05-24 | 广西大学 | Preparation method of Sn-Bi-based solder alloy EBSD sample |
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