CN108037319A - A kind of preparation method of nickel chromium triangle alfer transmission electron microscope sample - Google Patents
A kind of preparation method of nickel chromium triangle alfer transmission electron microscope sample Download PDFInfo
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- CN108037319A CN108037319A CN201711191771.3A CN201711191771A CN108037319A CN 108037319 A CN108037319 A CN 108037319A CN 201711191771 A CN201711191771 A CN 201711191771A CN 108037319 A CN108037319 A CN 108037319A
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Abstract
The present invention relates to a kind of preparation method of nickel chromium triangle alfer transmission electron microscope sample, this method includes 1）Cut sample；2）Pre-grinding；3）Section；4）Double sprays are thinned；5）It is cleaned by ultrasonic sample three times；6）Cleaning and etc..Nickel chromium triangle alfer transmission sample prepared by the method using the present invention, the thin area of its sample is larger, and thin area's thickness is uniform, and the transmission electron microscope sample picture of better quality can be obtained under transmission electron microscope.
Description
Technical field
The present invention relates to a kind of preparation method of metal sample, more particularly to a kind of nickel chromium triangle alfer transmission electron microscope sample
Preparation method.
Background technology
Nickel chromium triangle alfer is mainly used for making fine resistive element, and the characteristics of alloy is in normal operating temperatures scope
It is interior that there is high resistivity and very low temperature-coefficient of electrical resistance；And compared with general alloy material, the resistance of the alloy is special
Property have abnormality performance.By more than 1000 DEG C heating, insulation, so quick cooling（Water cooling）To the solution treatment state of room temperature
Under, the resistivity of nickel chromium triangle alfer is relatively low；Then pass through 500 DEG C or so of ageing treatment, its resistivity can raise.It is and general
Alloy material（Such as steel, aluminium alloy）Resistivity under solution treatment state is higher, under resistivity is then understood after ageing treatment
Drop.The anomalous resistance characteristic of nickel chromium triangle alfer is related with the special change of its microstructure, and this microstructure characteristic needs
Will use transmission electron microscope just it is observed that.
Transmission electron microscope is the thin area for utilizing the electron beam with certain energy to pass through sample to be tested（Thickness 100nm
Below）, so as to detect the microscopic informations such as the crystal structure in sample, atomic arrangement state.
The sample of high quality is to obtain excellent transmission electron microscope experimental result and the key link of high-quality photos.
The preparation of transmission sample mainly has two methods of the double spray of electrolysis and ion milling, for nickel chromium triangle alfer, due to itself plus
Work hardening tendency it is larger, during ion milling easily produce processing hardening and distortion of lattice, caused by transmission electron microscope observing
When produce illusion, thus should not use.Meanwhile coarse grains, hardness height, the good corrosion resistance of nickel chromium triangle alfer, it is electrolysed
The difficulty that sample preparation is thinned in double sprays is also larger；Especially it is a lack of the double sprays of effectively electrolysis and formula of liquid and corresponding process conditions is thinned,
As the important restriction factor for exploring nickel chromium triangle alfer microstructure and electric property relation.
The content of the invention
The object of the present invention is to provide a kind of preparation method of nickel chromium triangle alfer transmission electron microscope sample, this method makes sample
Processing hardening and distortion of lattice will not be produced during ion milling, the thin area of sample is larger and thickness is more uniform, can be with
Obtain excellent transmission electron microscope experimental result and high quality picture.
The technical scheme is that：
For the preparation of nickel chromium triangle alfer transmission sample to be thinned, the percent by volume of said preparation each component is：8%~12% high chlorine
Acid, 2%~4% citric acid, 84%~90% absolute ethyl alcohol.
Preferable technical solution is that the percent by volume of the preparation each component is：10% perchloric acid, 3% citric acid, 87%
Absolute ethyl alcohol.
Preferable technical solution is that the percent by volume of the preparation each component is：8% perchloric acid, 2% citric acid, 90% nothing
Water-ethanol.
Preferable technical solution is that the percent by volume of the preparation each component is：11% perchloric acid, 4% citric acid, 85%
Absolute ethyl alcohol.
Preferable technical solution is that the percent by volume of the preparation each component is：12% perchloric acid, 4% citric acid, 84%
Absolute ethyl alcohol
The preparation method of nickel chromium triangle alfer transmission electron microscope sample, there is following steps：
1）Sample is cut, the thickness of sample is cut into≤1mm；
2）Pre-grinding, thickness is polishing to as≤50 μm by sample, and holding surface is bright and clean；
3）Section；
4）Double sprays are thinned, and with any double sprays of preparation electrolysis of claim 1-4, its operating condition is that voltage is 45V~60V,
Temperature is -25 DEG C~-20 DEG C；
5）It is cleaned by ultrasonic sample three times；
6）Taken out after the completion of cleaning, spontaneously dry, obtain nickel chromium triangle alfer transmission electron microscope sample.
Step 2）Polished using label sand paper from low to high, for the last time using the polishing of 800# sand paper.
Step 5）The time of the cleaning is 10 minutes every time.
The perchloric acid concentration is pure to analyze（Concentration is not less than 70%）；Citric acid is pure to analyze（Concentration is not less than
99.5%）.
The percetage by weight of each component of nickel chromium triangle alfer of the present invention is：15%-25%Cr、1%-10%、1%-10%
Fe, surplus Ni.
Nickel chromium triangle alfer of the present invention need to control its thickness≤50 μm since hardness itself is larger, therefore, system
Make to be not easy punching during sample.
The sand paper of different model is selected, the sand paper polishing sample of label, last polishing from low to high should use 800#
Sand paper above, makes the surface of pre-grinding sample without deeper cut, in order to avoid influence the final mass of transmission sample.
The thinned essence of the double sprays of electrolysis is a kind of electrobrightening process, it is necessary to control voltage in 45V~60V, voltage mistake
It is high or too low can all influence final thinned effect.
Perchloric acid is mainly used for electrobrightening nickel chromium triangle alfer surface, metal is gradually dissolved to reach thinned mesh
's；Concentration of the alcohol as solvent control perchloric acid, rationally adjusting the proportioning of perchloric acid and ethanol can control the polishing of alloy fast
Rate, improves the thinned uniformity of double sprays, increases thin area's scope of sample.
Adding the organic acids such as citric acid can cause alloy surface convex portion and recess polishing speed to produce difference, i.e. recess subtracts
Thin slow, convex portion is thinned soon, so as to improve the flatness on surface and the uniformity of thickness of sample.
Temperature is also to influence an important factor for effect is thinned in double sprays, and controlled at -25 DEG C~-20 DEG C, temperature is too high, then
Excessive velocities are thinned, sample is easily perforated, and causes thin area's scope less than normal；The too low speed that is then thinned of temperature is excessively slow, or even can not obtain
To thin area.
The method of the invention and preparation are primarily adapted for use in nickel chromium triangle alfer, and the alloy close to other compositions, which can be done, joins
Examine.
The transmission electron microscope sample prepared using the method for the invention, has the spy that thin area is uniform and area is larger
Point, is suitable for transmission electron microscope observing, and the fine structure such as crystal boundary, twin feature clearly can be observed, and be adapted into
Row monocrystalline electron diffraction analysis, to understand the crystal structure characteristic of alloy.
Brief description of the drawings
Fig. 1 is the transmission electron microscope microsctructural photograph of 1 made sample of the embodiment of the present invention；
Fig. 2 is the transmission electron microscope microsctructural photograph of 2 made sample of the embodiment of the present invention；
Fig. 3 is the transmission electron microscope microsctructural photograph of 3 made sample of the embodiment of the present invention；
Fig. 4 is the transmission electron microscope microsctructural photograph of 4 made sample of the embodiment of the present invention.
Embodiment
Illustrate the preparation process of nickel chromium triangle alfer transmission electron microscope sample of the present invention with embodiment 1-4.
Embodiment 1
1）Sample is cut, nickel chromium triangle alfer sample is switched to thickness 1mm with mechanical cutting method.
2）Pre-grinding, with the polishing sample of label sand paper from low to high, polishes by " 8 " font or vertical direction.Often change once
Sand paper pays attention to all cleaning up sand paper and sample, and most sample is milled to 45 μm or so of thickness, last polishing with sand paper in advance at last
The sand paper of more than 800# should be used to carry out, to ensure that pre-grinding sample surfaces are smooth, no marking, folding line or bending.
3）Section：The disk of a diameter of 3 mm is washed into perforating press, ensures punching edge impulse- free robustness, avoids burr from causing point
Electron beam is blocked in end electric discharge.
4）Prepare double hydrojets：Double spray solution of 10% perchloric acid, 3% citric acid, 87% absolute ethyl alcohol are prepared by volume.
5）The double spray samples of electrolysis：50V, temperature are adjusted to the double sprays of nickel chromium triangle alfer sample electrolysis, voltage using double spray instrument
Control is at -25 DEG C.Until when photosensor is alarmed, immediately close off power supply and stop double sprays.
6）Cleaning：The thinned sample of double sprays is cleaned by ultrasonic three times with absolute ethyl alcohol, 10 minutes every time.
7）Preserve：The sample that cleaning is completed, which is placed in alcohol, stands 10-20 minutes, then takes out and is placed on filter paper,
After its natural drying after, be positioned in transmission sample box preserve it is stand-by；
The sample is observed under transmission electron microscope, it is seen that its thin area is larger and thickness is more uniform, can shoot clearly microcosmic
Structure photo, is shown in attached drawing 1.
Embodiment 2
1）Sample is cut, nickel chromium triangle alfer sample is switched to thickness 0.8mm with mechanical cutting method.
2）Pre-grinding, with the sand paper polishing sample of label from low to high, polishes by " 8 " font or vertical direction.Often change one
Secondary sand paper pays attention to all cleaning up sand paper and sample, and most sample is milled to 42 μm or so of thickness with sand paper in advance at last, and last beats
Mill should use the sand paper of more than 800# to carry out, to ensure that pre-grinding sample surfaces are smooth, no marking, folding line or bending.
3）Section：The disk of a diameter of 3 mm is washed into perforating press, ensures punching edge impulse- free robustness, avoids burr from causing point
Electron beam is blocked in end electric discharge.
4）Prepare double hydrojets：Double spray solution of 8% perchloric acid, 2% citric acid, 90% absolute ethyl alcohol are prepared by volume.
5）The double spray samples of electrolysis：55V, temperature are adjusted to the double sprays of nickel chromium triangle alfer sample electrolysis, voltage using double spray instrument
Control is at -23 DEG C.Until when photosensor is alarmed, immediately close off power supply and stop double sprays.
6）Cleaning：The thinned sample of double sprays is cleaned by ultrasonic three times with absolute ethyl alcohol, 10 minutes every time.
7）Preserve：The sample that cleaning is completed is placed on standing 10-20 minutes in alcohol, then takes out and is placed on filter paper
On, after its natural drying after, be positioned in transmission sample box preserve it is stand-by.
The sample is observed under transmission electron microscope, it is seen that its thin area is larger and thickness is more uniform, can shoot clearly
Microsctructural photograph, is shown in attached drawing 2.
Embodiment 3：
1）Sample is cut, nickel chromium triangle alfer sample is switched to thickness 0.5mm with mechanical cutting method.
2）Pre-grinding, with the sand paper polishing sample of label from low to high, polishes by " 8 " font or vertical direction.Often change one
Secondary sand paper pays attention to all cleaning up sand paper and sample, and most sample is milled to 40 μm or so of thickness with sand paper in advance at last, and last beats
Mill should use the sand paper of more than 800# to carry out, to ensure that pre-grinding sample surfaces are smooth, no marking, folding line or bending.
3）Section：The disk of a diameter of 3 mm is washed into perforating press, ensures punching edge impulse- free robustness, avoids burr from causing point
Electron beam is blocked in end electric discharge.
4）Prepare double hydrojets：Double spray solution of 11% perchloric acid, 4% citric acid, 85% absolute ethyl alcohol are prepared by volume.
5）The double spray samples of electrolysis：60V, temperature are adjusted to the double sprays of nickel chromium triangle alfer sample electrolysis, voltage using double spray instrument
Control is at -25 DEG C.Until when photosensor is alarmed, immediately close off power supply and stop double sprays.
6）Cleaning：The thinned sample of double sprays is cleaned by ultrasonic three times with absolute ethyl alcohol, 10 minutes every time.
7）Preserve：The sample that cleaning is completed, which is placed in alcohol, stands 10-20 minutes, then takes out and is placed on filter paper,
After its natural drying after, be positioned in transmission sample box preserve it is stand-by.
The sample is observed under transmission electron microscope, it is seen that its thin area is larger and thickness is more uniform, can shoot clearly
Microsctructural photograph, is shown in attached drawing 3.
Embodiment 4
1）Sample is cut, nickel chromium triangle alfer sample is switched to thickness 0.7mm with mechanical cutting method.
2）Pre-grinding, with the sand paper polishing sample of label from low to high, polishes by " 8 " font or vertical direction.Often change one
Secondary sand paper pays attention to all cleaning up sand paper and sample, and most sample is milled to 35 μm or so of thickness with sand paper in advance at last, and last beats
Mill should use the sand paper of more than 800# to carry out, to ensure that pre-grinding sample surfaces are smooth, no marking, folding line or bending.
3）Section：The disk of a diameter of 3 mm is washed into perforating press, ensures punching edge impulse- free robustness, avoids burr from causing point
Electron beam is blocked in end electric discharge.
4）Prepare double hydrojets：Double spray solution of 12% perchloric acid, 4% citric acid, 84% absolute ethyl alcohol are prepared by volume.
5）The double spray samples of electrolysis：45V, temperature are adjusted to the double sprays of nickel chromium triangle alfer sample electrolysis, voltage using double spray instrument
Control is at -20 DEG C.Until when photosensor is alarmed, immediately close off power supply and stop double sprays.
6）Cleaning：The thinned sample of double sprays is cleaned by ultrasonic three times with absolute ethyl alcohol, 10 minutes every time.
7）Preserve：The sample that cleaning is completed, which is placed in alcohol, stands a period of time, then takes out and is placed on filter paper, treats
Its spontaneously dry after, be positioned in transmission sample box preserve it is stand-by.
The sample is observed under transmission electron microscope, it is seen that its thin area is larger and thickness is more uniform, can shoot clearly
Microsctructural photograph, is shown in attached drawing 4.
Claims (8)
- A kind of 1. preparation for being used to nickel chromium triangle alfer transmission electron microscope sample be thinned, it is characterised in that the body of said preparation each component Accumulating percentage is：8%~12% perchloric acid, 2%~4% citric acid, 84%~90% absolute ethyl alcohol.
- 2. preparation according to claim 1, it is characterised in that the percent by volume of the preparation each component is：10% high chlorine Acid, 3% citric acid, 87% absolute ethyl alcohol.
- 3. preparation according to claim 1, it is characterised in that the percent by volume of the preparation each component is：8% high chlorine Acid, 2% citric acid, 90% absolute ethyl alcohol.
- 4. preparation according to claim 1, it is characterised in that the percent by volume of the preparation each component is：11% high chlorine Acid, 4% citric acid, 85% absolute ethyl alcohol.
- 5. preparation according to claim 1, it is characterised in that the percent by volume of the preparation each component is：12% high chlorine Acid, 4% citric acid, 84% absolute ethyl alcohol.
- 6. the preparation method of nickel chromium triangle alfer transmission electron microscope sample, it is characterised in that have following steps：1）Sample is cut, the thickness of sample is cut into≤1mm；2）Pre-grinding, thickness is polishing to as≤50 μm by sample, and holding surface is bright and clean；3）Section；4）Double sprays are thinned, and with any double sprays of preparation electrolysis of claim 1-4, its operating condition is that voltage is 45V~60V, Temperature is -25 DEG C~-20 DEG C；5）It is cleaned by ultrasonic sample three times；6）Taken out after the completion of cleaning, spontaneously dry, obtain nickel chromium triangle alfer transmission electron microscope sample.
- 7. preparation method according to claim 6, it is characterised in that：Step 2）Beaten using the sand paper of label from low to high Mill, for the last time using the polishing of 800# sand paper.
- 8. preparation method according to claim 6, it is characterised in that：Step 5）The time of the cleaning is 10 points every time Clock.
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| CN201711191771.3A CN108037319B (en) | 2017-11-24 | 2017-11-24 | Preparation method of nickel-chromium-aluminum-iron alloy transmission electron microscope sample |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108802076A (en) * | 2018-06-12 | 2018-11-13 | 黄淮学院 | A kind of electrolytic polishing method preparing pure titanium or titanium alloy EBSD samples |
| 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 |
| CN114486959A (en) * | 2022-02-14 | 2022-05-13 | 广东工业大学 | Method for preparing eutectic high-entropy alloy TEM sample |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108802076A (en) * | 2018-06-12 | 2018-11-13 | 黄淮学院 | A kind of electrolytic polishing method preparing pure titanium or titanium alloy EBSD samples |
| 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 |
| CN114486959A (en) * | 2022-02-14 | 2022-05-13 | 广东工业大学 | Method for preparing eutectic high-entropy alloy TEM sample |
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