CN107436309A - The method for preparing TEM sample is thinned in double sprays - Google Patents
The method for preparing TEM sample is thinned in double sprays Download PDFInfo
- Publication number
- CN107436309A CN107436309A CN201610361525.7A CN201610361525A CN107436309A CN 107436309 A CN107436309 A CN 107436309A CN 201610361525 A CN201610361525 A CN 201610361525A CN 107436309 A CN107436309 A CN 107436309A
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Classifications
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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
- G01N23/22—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 measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
-
- 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
-
- 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
-
- 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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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The present invention discloses double sprays and the method for preparing TEM sample is thinned, and it is 50um 70um that sample is milled into thickness 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, relates to the use of double sprays and preparation is thinned
The method of sample.
Background technology
The development of new material is maked rapid progress at present, and higher requirement is proposed to sample preparation.The developing direction of sample preparation
Should be that preparation time is shorter, penetration of electrons area is bigger, and the thickness in thin area is thinner, and height local is thinned.High quality is thin
Membrane sample is characterized in：Sample central hole, weakened region is big, and surface is flat, under an optical microscope it can be seen that hole week
It is with multi-coated interference striped.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, even more than
90%, the TEM results to have expected, the film sample prepared is first had to, this is also the pass to reap the fruit of one's research
One of key.
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：
The method for preparing TEM sample is thinned in double sprays, carries out as steps described below：
Step 1, it is 50um-70um sample to be milled into thickness on metallographic fine sandpaper；
Step 2, 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 the jet pump jet velocity of device is thinned in regulation twin-jet electropolishing, so that double
The opposite electrolyte that nozzle projects is in contact；
Step 3, electrolytic cell is cooled using liquid nitrogen, be 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；
Step 4, total power switch is closed, decomposition voltage knob is adjusted, makes voltage stabilization in U1, jet pump knob inverse time
On earth, now there is a corresponding electric current I1 in pin, is turned clockwise immediately after on earth jet pump knob in rotate counterclockwise
On earth, voltage knob and is adjusted simultaneously, the electric current I2 for making newly to obtain differs 40-60mA with electric current I1 before, and stably
Electric current I2 and voltage now, sample is thinned, and to alarm sound of perforating, immediately closes off general supply.
In the above-mentioned technical solutions, in step 1, metallographic fine sandpaper is 200-500 mesh, when being prepared using 200 mesh,
The metallographic fine sandpaper of 220 mesh, 320 mesh and 500 mesh is processed to sample in turn.
In the above-mentioned technical solutions, in step 2, the opposite electrolyte that twin-jet nozzle projects is in contact, and among two nozzles
Form the electrolyte disc of a diameter of 5-8mm millimeter.
In the above-mentioned technical solutions, in step 4, whole stabling current I2 and voltage carry out the thinned time to sample and are
30—50s。
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
Making the thinned sample of the double sprays of electrolysis, weakened region is bigger, improves the quality of film sample, Shi Bao areas thickness in central hole
Thinner, 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 be transmitted
The preparation of electron microscopic sample.
Prepared using aluminium alloy as sample, aluminum alloy sample is milled into thickness on metallographic fine sandpaper is
Aluminum alloy flake, Φ 3mm sequin is washed into Φ 3mm disks Developing devices by 50um-70um, and metallographic fine sandpaper is
200-500 mesh, using the metallographic fine sandpaper of 200 mesh, 220 mesh, 320 mesh and 500 mesh in turn to sample when being prepared
It is processed.
300ml electrolyte is added 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%, nitric acid is purchased from Chemical Reagent Factory No.5, Tianjin City, mass percent
65-68%, absolute methanol is purchased from Tianjin recovery fine chemistry industry research institute, and 99.5%.Adjust the spray that device is thinned in twin-jet electropolishing
Pump jet velocity is penetrated, so that the opposite electrolyte that twin-jet nozzle projects is in contact, formation one is a diameter of among two nozzles
The electrolyte disc of 5-8mm millimeters.Electrolytic cell is cooled using liquid nitrogen, is down between-20-- 30 DEG C, will be equipped with
The specimen holder of Al-alloy metal sequin is inserted into the middle position of electrolytic cell.
Close general supply " POWER " switch, regulation decomposition voltage " DC POWER " knobs, make voltage stabilization in 60V,
Counterclockwise on earth, now there is a corresponding electric current I1 in jet pump " PUMP " knob, rotate counterclockwise on earth after immediately
Jet pump " PUMP " knob turn clockwise on earth, and adjust polishing voltage simultaneously " DC POWER " knobs, to make newly to obtain
Electric current I2 differ 40-60mA with electric current I1 before, and stable electric current I2 and polishing voltage now is carried out to sample
It is thinned, to alarm sound of perforating, immediately closes off general supply " POWER ", take out sample clamp rapidly, be placed on absolute alcohol
In cleaned, it is 30-50s that whole stabling current I2 and polishing voltage, which carry out the thinned time to sample,.
The sample of preparation is characterized using transmission electron microscope, and prepares sample with tradition and is contrasted, technology of the invention
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 straight from figure
Connect and observe aluminium alloy particle, 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 case where not departing from the core of the present invention,
Any simple deformation, modification or other skilled in the art can not spend the equivalent substitution of creative work to fall
Enter protection scope of the present invention.
Claims (4)
1. the method for preparing TEM sample is thinned in pair spray, it is characterised in that carries out as steps described below：
Step 1, it is 50um-70um sample to be milled into thickness on metallographic fine sandpaper；
Step 2, 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 the jet pump jet velocity of device is thinned in regulation twin-jet electropolishing, so that double
The opposite electrolyte that nozzle projects is in contact；
Step 3, electrolytic cell is cooled using liquid nitrogen, be 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；
Step 4, total power switch is closed, decomposition voltage knob is adjusted, makes voltage stabilization in U1, jet pump knob inverse time
On earth, now there is a corresponding electric current I1 in pin, is turned clockwise immediately after on earth jet pump knob in rotate counterclockwise
On earth, voltage knob and is adjusted simultaneously, the electric current I2 for making newly to obtain differs 40-60mA with electric current I1 before, and stably
Electric current I2 and voltage now, sample is thinned, and to alarm sound of perforating, immediately closes off general supply.
2. the method for preparing TEM sample is thinned in double sprays according to claim 1, it is characterised in that in step 1,
Metallographic fine sandpaper is 200-500 mesh, and metallographic when being prepared using 200 mesh, 220 mesh, 320 mesh and 500 mesh is thin
Sand paper is processed to sample in turn.
3. the method for preparing TEM sample is thinned in double sprays according to claim 1, it is characterised in that in step 2,
The opposite electrolyte that twin-jet nozzle projects is in contact, and the electrolysis of a diameter of 5-8mm millimeter is formed among two nozzles
Liquid disk.
4. the method for preparing TEM sample is thinned in double sprays according to claim 1, it is characterised in that in step 4,
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 |
|---|---|---|---|
| CN201610361525.7A CN107436309A (en) | 2016-05-26 | 2016-05-26 | The method for preparing TEM sample is thinned in double sprays |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610361525.7A CN107436309A (en) | 2016-05-26 | 2016-05-26 | The method for preparing TEM sample is thinned in double sprays |
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| CN107436309A true CN107436309A (en) | 2017-12-05 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610361525.7A Pending CN107436309A (en) | 2016-05-26 | 2016-05-26 | The method for preparing TEM sample is thinned in double sprays |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113419085A (en) * | 2021-07-19 | 2021-09-21 | 广东省科学院工业分析检测中心 | Preparation method of tungsten alloy transmission electron microscope sample |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1584543A (en) * | 2004-06-04 | 2005-02-23 | 北京科技大学 | Comfortable sample double spray electrolytically thinning instrument for transmission electronic microscopy |
| CN1696334A (en) * | 2004-05-12 | 2005-11-16 | 中国科学院金属研究所 | Method for preparing film specimen in use for transmission electron microscope |
| CN101532161A (en) * | 2009-03-17 | 2009-09-16 | 北京科技大学 | Constant temperature transmission electron microscope sample double-boost electrolysis thinner |
| CN103335872A (en) * | 2013-06-04 | 2013-10-02 | 首钢总公司 | Method for preparing transmission electron microscope thin film sample of longitudinal section of filament by electrolysis double-spray method |
-
2016
- 2016-05-26 CN CN201610361525.7A patent/CN107436309A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1696334A (en) * | 2004-05-12 | 2005-11-16 | 中国科学院金属研究所 | Method for preparing film specimen in use for transmission electron microscope |
| CN1584543A (en) * | 2004-06-04 | 2005-02-23 | 北京科技大学 | Comfortable sample double spray electrolytically thinning instrument for transmission electronic microscopy |
| CN101532161A (en) * | 2009-03-17 | 2009-09-16 | 北京科技大学 | Constant temperature transmission electron microscope sample double-boost electrolysis thinner |
| CN103335872A (en) * | 2013-06-04 | 2013-10-02 | 首钢总公司 | Method for preparing transmission electron microscope thin film sample of longitudinal section of filament by electrolysis double-spray method |
Non-Patent Citations (6)
| Title |
|---|
| 吴杏芳 等: "《电子显微分析使用方法》", 31 October 1998 * |
| 尤富强: "用双喷减薄仪制备金属材料表面电镜薄膜", 《上海钢研》 * |
| 李树堂: "《金属X射线衍射与电子显微分析技术》", 30 November 1980 * |
| 潘春旭 等: "《材料物理与化学实验教程》", 30 September 2008 * |
| 闫时建 等: "自制双喷电解减薄装置的设计使用", 《分析测试学报》 * |
| 马淑波: "透射电子显微镜样品制备技术（一）薄膜样品制备技术", 《物理测试》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113419085A (en) * | 2021-07-19 | 2021-09-21 | 广东省科学院工业分析检测中心 | Preparation method of tungsten alloy transmission electron microscope sample |
| CN113419085B (en) * | 2021-07-19 | 2022-12-13 | 广东省科学院工业分析检测中心 | Preparation method of tungsten alloy transmission electron microscope sample |
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Application publication date: 20171205 |
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