CN107436258A - Application of the double spray thining methods based on difference between current in transmission electron microscope sample preparation - Google Patents
Application of the double spray thining methods based on difference between current in transmission electron microscope sample preparation Download PDFInfo
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- CN107436258A CN107436258A CN201610361523.8A CN201610361523A CN107436258A CN 107436258 A CN107436258 A CN 107436258A CN 201610361523 A CN201610361523 A CN 201610361523A CN 107436258 A CN107436258 A CN 107436258A
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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 present invention discloses application of the double spray thining methods based on difference between current in transmission electron microscope sample preparation, sample is ground on metallographic fine sandpaper, electrolyte is added in the electrolytic cell that device is thinned in twin-jet electropolishing, electrolytic cell is cooled using liquid nitrogen, the specimen holder equipped with Al-alloy metal sequin is inserted into the middle position of electrolytic cell；Close total power switch, adjust decomposition voltage knob, voltage stabilization is set on earth, a corresponding electric current I1 occur counterclockwise in U1, jet pump knob, jet pump knob is turned clockwise immediately on earth after on earth in rotate counterclockwise, and adjust voltage knob simultaneously, so as to get electric current I2 differ 40-60mA with electric current I1 before, and stable electric current I2 and voltage now, sample is thinned, to alarm sound of perforating.The present invention realizes the central hole of sample, and weakened region is bigger, improves the quality of film sample, and Shi Bao areas thickness is thinner, and thin area is bigger, improves the quality of transmission electron microscope picture.
Description
Technical field
The invention belongs to technical field prepared by transmission electron microscope sample, more particularly, is related to double based on difference between current
Spray application of the thining method in transmission electron microscope sample preparation.
Background technology
The development of new material is maked rapid progress at present, and higher requirement is proposed to sample preparation.The development side of sample preparation
To that should be that preparation time is shorter, penetration of electrons area be bigger, and the thickness in thin area is thinner, and height local is thinned.High-quality thin film
Sample is characterized in：Sample central hole, weakened region is big, and surface is flat, under an optical microscope it can be seen that having around hole more
Layer interference fringe.TEM sample is prepared in electron micrology research work, is played vital effect, is very fine
Technical work.Its importance and workload will typically account for more than half of whole test job, and even more than 90%, to expect
Good TEM results, first have to the film sample prepared, this is also one of key to reap the fruit of one's research.
The content of the invention
The method for preparing TEM sample is thinned it is an object of the invention to overcome the deficiencies of the prior art and provide double sprays, with reality
Existing sample central hole, weakened region is bigger, so as to improve the quality of transmission electron microscope picture.
The technical purpose of the present invention is achieved by following technical proposals：
Application of the double spray thining methods based on difference between current in transmission electron microscope sample preparation, twin-jet electropolishing are thinned device and carried out
The preparation of transmission electron microscope sample, adjust decomposition voltage knob, make voltage stabilization in U1, jet pump knob counterclockwise on earth, now
There is a corresponding electric current I1, turn clockwise jet pump knob immediately on earth after on earth in rotate counterclockwise, and adjust simultaneously
Economize on electricity pressure knob, the electric current I2 for making newly to obtain differ 40-60mA, and stable electric current I2 and voltage now with electric current I1 before,
Sample is thinned, completing sample to alarm sound of perforating prepares.
In the above-mentioned technical solutions, it is 50um-70um sample to be milled into thickness on metallographic fine sandpaper, and metallographic fine sandpaper is
200-500 mesh, sample is added in turn using the metallographic fine sandpaper of 200 mesh, 220 mesh, 320 mesh and 500 mesh when being prepared
Work.
In the above-mentioned technical solutions, electrolyte is added in the electrolytic cell that device is thinned in twin-jet electropolishing, electrolyte has volume hundred
The nitric acid of fraction 30% and the absolute methanol composition of percentage by volume 70%, are cooled using liquid nitrogen to electrolytic cell, be down to-
Between 20-- 30 DEG C.
In the above-mentioned technical solutions, it is 30-50s that whole stabling current I2 and voltage, which carry out the thinned time to sample,.
The present invention provides a kind of process for setting specific electrolytic parameter, starts the difference of both front and back electric current by being electrolysed
Value makes the thinned sample of the double sprays of electrolysis, and weakened region is bigger, improves the quality of film sample, Shi Bao areas thickness is more in central hole
Thin, thin area is bigger, improves the quality of transmission electron microscope picture.
Brief description of the drawings
Fig. 1 is the TEM pictures of aluminum alloy sample prepared by traditional method for making sample.
Fig. 2 is the TEM pictures of the aluminum alloy sample prepared using the inventive method, and that circle marks is Al (Sc, Zr).
Embodiment
Technical scheme is further illustrated with reference to specific embodiment.
Device is thinned up to electromechanical development in science and technology Co., Ltd MTP-1A type magnetically-actuateds twin-jet electropolishing using Shanghai religion to carry out thoroughly
Penetrate the preparation of electron microscopic sample.
Prepared using aluminium alloy as sample, it is 50um- that aluminum alloy sample is milled into thickness on metallographic fine sandpaper
70um, aluminum alloy flake is washed into Φ 3mm sequin with Φ 3mm disks Developing devices, metallographic fine sandpaper is 200-500 mesh, is entered
Row is processed to sample in turn when preparing using the metallographic fine sandpaper of 200 mesh, 220 mesh, 320 mesh and 500 mesh.
300ml electrolyte is added in the electrolytic cell that device is thinned in twin-jet electropolishing, electrolyte has the nitre of percentage by volume 30%
Acid and the absolute methanol of percentage by volume 70% form, and nitric acid is purchased from Chemical Reagent Factory No.5, Tianjin City, and mass percent 65-
68%, absolute methanol is purchased from Tianjin recovery fine chemistry industry research institute, and 99.5%.Adjust the jet pump spray that device is thinned in twin-jet electropolishing
Firing rate degree, so that the opposite electrolyte that twin-jet nozzle projects is in contact, a diameter of 5-8mm millimeter is formed among two nozzles
Electrolyte disc.Electrolytic cell is cooled using liquid nitrogen, is down between-20-- 30 DEG C, Al-alloy metal roundlet will be housed
The specimen holder of piece is inserted into the middle position of electrolytic cell.
General supply " POWER " switch is closed, regulation decomposition voltage " DC POWER " knobs, makes voltage stabilization in 60V, injection
Counterclockwise on earth, now there is a corresponding electric current I1 in pump " PUMP " knob, rotate counterclockwise after on earth it is clockwise immediately
Rotary jet pump " PUMP " knob on earth, and adjust simultaneously polishing voltage " DC POWER " knobs, make the electric current I2 that newly obtains with
Electric current I1 differs 40-60mA, and stable electric current I2 and polishing voltage now before, sample is thinned, to perforation alarm
The sound, general supply " POWER " is immediately closed off, sample clamp is taken out rapidly, is placed in absolute alcohol and is cleaned, it is whole steady
Determine electric current I2 and polishing voltage to carry out the thinned time to sample be 30-50s.
The sample of preparation is characterized using transmission electron microscope, and prepares sample with tradition and is contrasted, skill of the invention
Art scheme effectively makes sample central hole is thinned, and thin area is big, the transmission picture for better quality of breaking forth, substantially can be direct from figure
Aluminium alloy particle is observed, picture quality of its picture quality apparently higher than conventional method sample preparation.
It should be noted that according to the solution of the present invention, different samples are changed, it is only necessary to control thickness of sample and twice electricity
Difference between stream, it is possible to conveniently and efficiently realize sample preparation, and obtain the picture of high quality.
Exemplary description has been done to the present invention above, it should explanation, in the situation for the core for not departing from the present invention
Under, any simple deformation, modification or other skilled in the art can not spend the equivalent substitution of creative work equal
Fall into protection scope of the present invention.
Claims (4)
1. application of the double spray thining methods based on difference between current in transmission electron microscope sample preparation, it is characterised in that twin-jet electropolishing
The preparation that device carries out transmission electron microscope sample is thinned, adjusts decomposition voltage knob, making voltage stabilization, jet pump knob is counterclockwise in U1
On earth, now there is a corresponding electric current I1, jet pump knob turned clockwise immediately on earth after on earth in rotate counterclockwise,
And voltage knob is adjusted simultaneously, the electric current I2 for making newly to obtain differs 40-60mA, and stable electric current now with electric current I1 before
I2 and voltage, sample is thinned, and completing sample to alarm sound of perforating prepares.
2. application of the double spray thining methods according to claim 1 based on difference between current in transmission electron microscope sample preparation,
Characterized in that, it is 50um-70um that sample is milled into thickness on metallographic fine sandpaper, metallographic fine sandpaper is 200-500 mesh, is entered
Row is processed to sample in turn when preparing using the metallographic fine sandpaper of 200 mesh, 220 mesh, 320 mesh and 500 mesh.
3. application of the double spray thining methods according to claim 1 based on difference between current in transmission electron microscope sample preparation,
Characterized in that, adding electrolyte in the electrolytic cell that device is thinned in twin-jet electropolishing, electrolyte has the nitric acid of percentage by volume 30%
Formed with the absolute methanol of percentage by volume 70%, electrolytic cell is cooled using liquid nitrogen, is down between-20-- 30 DEG C.
4. application of the double spray thining methods according to claim 1 based on difference between current in transmission electron microscope sample preparation,
Characterized in that, it is 30-50s that whole stabling current I2 and voltage, which carry out the thinned time to sample,.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610361523.8A CN107436258A (en) | 2016-05-26 | 2016-05-26 | Application of the double spray thining methods based on difference between current in transmission electron microscope sample preparation |
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| CN201610361523.8A CN107436258A (en) | 2016-05-26 | 2016-05-26 | Application of the double spray thining methods based on difference between current in transmission electron microscope sample preparation |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111650227A (en) * | 2020-06-23 | 2020-09-11 | 广西大学 | Sample preparation method of transmission electron microscope in-situ heating chip of bulk metal sample |
| CN112595565A (en) * | 2020-11-27 | 2021-04-02 | 中国科学院金属研究所 | Preparation method of 2xxx series aluminum alloy transmission electron microscope sample |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111650227A (en) * | 2020-06-23 | 2020-09-11 | 广西大学 | Sample preparation method of transmission electron microscope in-situ heating chip of bulk metal sample |
| CN112595565A (en) * | 2020-11-27 | 2021-04-02 | 中国科学院金属研究所 | Preparation method of 2xxx series aluminum alloy transmission electron microscope sample |
| CN112595565B (en) * | 2020-11-27 | 2022-06-21 | 中国科学院金属研究所 | Preparation method of 2xxx series aluminum alloy transmission electron microscope sample |
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Application publication date: 20171205 |