CN112595565A - Preparation method of 2xxx series aluminum alloy transmission electron microscope sample - Google Patents
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- 230000005540 biological transmission Effects 0.000 title claims abstract description 36
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 47
- 239000007788 liquid Substances 0.000 claims abstract description 28
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000007921 spray Substances 0.000 claims abstract description 17
- 239000011159 matrix material Substances 0.000 claims abstract description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 6
- 238000005507 spraying Methods 0.000 claims description 88
- 238000004140 cleaning Methods 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 11
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000011148 porous material Substances 0.000 claims description 6
- 238000002834 transmittance Methods 0.000 claims description 6
- 239000005357 flat glass Substances 0.000 claims description 4
- 230000008033 biological extinction Effects 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 238000005868 electrolysis reaction Methods 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- GBAPRSGLWUEXIR-UHFFFAOYSA-N nitromethanol Chemical compound OC[N+]([O-])=O GBAPRSGLWUEXIR-UHFFFAOYSA-N 0.000 claims description 3
- 238000004080 punching Methods 0.000 claims description 3
- 239000003792 electrolyte Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 7
- 239000007769 metal material Substances 0.000 abstract description 2
- 238000005464 sample preparation method Methods 0.000 abstract description 2
- 229910001250 2024 aluminium alloy Inorganic materials 0.000 description 12
- 150000002500 ions Chemical class 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 230000009977 dual effect Effects 0.000 description 4
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical group OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 4
- 238000003917 TEM image Methods 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 238000007725 thermal activation Methods 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010849 ion bombardment Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000992 sputter etching Methods 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
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- 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
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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
- G01N1/286—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
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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
- G01N1/34—Purifying; Cleaning
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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
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
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Abstract
本发明公开了一种2xxx系铝合金透射电镜样品的制备方法，属于透射电镜样品制备技术领域。该方法通过选择一定浓度的硝酸和甲醇按照1：3的体积比例混合而成的双喷液，控制双喷电压在18～22V之间，双喷温度在5℃～10℃之间在双喷电解减薄仪上对样品进行减薄。合适的双喷液、双喷电压和双喷温度的选择，使样品表面光亮，降低了第二相和基体之间的电位差，有效的避免了筛孔的出现，实现了均匀减薄，可在10～20s达到减薄效果，大大地提高了效率，并且在减薄过程中无应力以及热输入，提供了一种快速可靠的制样方法。利用本发明可以方便简捷地制备出没有筛孔，薄区面积更大的透射样品，对含有粗大第二相的金属材料透射样品制备具有重要的借鉴意义。The invention discloses a preparation method of a 2xxx series aluminum alloy transmission electron microscope sample, and belongs to the technical field of transmission electron microscope sample preparation. The method selects a double-spray liquid mixed with a certain concentration of nitric acid and methanol in a volume ratio of 1:3, controls the double-spray voltage between 18 and 22V, and controls the double-spray temperature between 5°C and 10°C. The samples were thinned on an electrolytic thinning machine. Appropriate selection of double-spray liquid, double-spray voltage and double-spray temperature makes the surface of the sample bright, reduces the potential difference between the second phase and the matrix, effectively avoids the appearance of sieve holes, realizes uniform thinning, and can be The thinning effect is achieved within 10-20s, which greatly improves the efficiency, and there is no stress and heat input during the thinning process, providing a fast and reliable sample preparation method. The invention can conveniently and simply prepare transmission samples without sieve holes and with larger thin area, which has important reference significance for the preparation of transmission samples of metallic materials containing coarse second phases.
Description
Technical Field
The invention relates to the technical field of transmission electron microscope sample preparation, in particular to a preparation method of a 2xxx series aluminum alloy transmission electron microscope sample.
Background
The 2xxx series aluminum alloy is widely applied to the fields of rail transit, aerospace and the like due to higher specific strength, specific stiffness, excellent corrosion resistance, processing and forming performance and other comprehensive mechanical properties. With the rapid development and the further deepening of the lightweight concept in the fields of high-speed railways, aerospace and the like in China, the 2xxx series aluminum alloy is more and more widely applied to important equipment in the fields. Although China is a large using country of aluminum alloy, China is not a strong country, a plurality of product specifications and process standards directly imitate the foreign countries, and with the development of the industrialization process, the service environment of 2xxx aluminum alloy is more and more rigorous, higher requirements are provided for the mechanical property of the material, and the macroscopic mechanical property of the material is closely related to the microstructure and the deformation mechanism of the material. The transmission electron microscope is essential in the research and development of materials as a main characterization means for researching the microstructure characteristics and the evolution of the materials, and has important significance for deeply disclosing a potential mechanism behind the macroscopic performance of the materials and improving the application of key aluminum alloy components in the independent research and development and the product updating in China.
The first and most important step in transmission electron microscopy is to obtain a good transmission sample, the preparation of which accounts for more than 90% of the whole transmission experiment workload. At present, the preparation of a 2xxx series aluminum alloy transmission electron microscope sample mainly comprises three methods of ion thinning, double-spraying thinning and double-spraying post-ion thinning. The method can generate interference of external factors such as stress, dislocation and the like, and simultaneously consumes long time, one day or even several days is generally needed for preparing a good transmission sample, while the thickness of the sample prepared by electrolytic double spraying is required to be about 40-50 um, the stress, dislocation and the like can not be introduced by the electrolytic double spraying, the double spraying thinning time is short, and the efficiency is obviously higher than that of ion thinning. Therefore, at present, in order to save time and improve efficiency, electrolysis double spraying is generally adopted. However, since the interface between the second phase in the 2xxx aluminum alloy and the matrix is relatively active and the second phase is in a coarse lath shape, the periphery of the second phase is preferentially corroded in the electrolytic double-spraying process and then is washed away by the double-spraying beam to form a sieve hole, so that a high-quality sample is difficult to obtain. Therefore, it is currently generally adopted to perforate under double-jet and reduce the thickness to a certain thickness and then perform ion thinning, so that the preparation time of the transmission sample can be shortened to several hours, but the success rate of sample preparation is not high, and the area of a thin area is small. Therefore, it is urgent to find a method for preparing a high-quality transmission sample simply and rapidly, which is convenient to operate and does not introduce external interferences such as stress, dislocation and the like.
Disclosure of Invention
Aiming at the problems that the quality of the existing double-spraying thinning preparation sample is poor and the period of the ion thinning preparation sample is long, the invention aims to provide the preparation method of the 2xxx series aluminum alloy transmission electron microscope sample, the method is suitable for the preparation of the 2xxx series aluminum alloy material transmission electron microscope sample containing a large precipitated phase, can avoid the occurrence of sieve pores, prepare the transmission sample with excellent quality, further improve the efficiency and realize simpler and more convenient sample preparation.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a 2xxx series aluminum alloy transmission electron microscope sample comprises the following steps:
(1) mechanically thinning a 2xxx series aluminum alloy sample on metallographic abrasive paper to a thickness of 40-50 um, and punching the mechanically thinned sample through a puncher to obtain a metal wafer with the diameter of 3 mm;
(2) adding double-spraying liquid into an electrolytic bath of the electrolytic double-spraying thinning instrument, and adjusting the flow rate of an injection pump of the electrolytic double-spraying thinning instrument to ensure that the opposite double-spraying liquid sprayed by the double nozzles has certain pressure and is just in contact with and is aligned with the middle of the two nozzles;
(3) adding liquid nitrogen into the electrolytic bath for cooling, and measuring the temperature of the double-spraying liquid in the electrolytic bath by using a thermometer to control the temperature of the double-spraying liquid in the electrolytic bath to be between 5 and 10 ℃;
(4) the method comprises the following steps of (1) installing a metal wafer sample prepared in the step (1) on a sample clamp, inserting the sample clamp into the middle of two nozzles of an electrolysis double-spraying thinning instrument, adjusting the double-spraying voltage to be 18-22V, setting proper light transmittance and then starting double spraying to thin the sample;
(5) and after the sample is subjected to double-spraying perforation to the set light transmittance, the alarm of the double-spraying instrument is sounded, and the sample is taken down and is sequentially washed by water and absolute ethyl alcohol, so that the aluminum alloy transmission electron microscope sample is obtained.
In the step (1), 400#, 800#, 1200# and 2000# sandpaper are sequentially adopted to mechanically thin the sample, a smooth and flat glass plate is placed below the sandpaper, the sample is dragged by a rubber to be ground on the sandpaper in an 8-shaped track so as to realize uniform thinning, and the sample is prevented from being uneven and generating extinction stripes under a transmission electron microscope to influence subsequent observation.
In the step (2), the double-spraying liquid is prepared by mixing nitric acid with the concentration of 14-15 mol/L and methanol with the concentration of 24.56-24.68 mol/L according to the weight ratio of 1: 3, the low-proportion and weak-acidity double-spray liquid of the nitromethanol effectively avoids the condition that the surface of a sample is oxidized due to over strong acidity of the electrolyte.
In the step (4), the temperature of the double-spraying process is controlled between 5 ℃ and 10 ℃, and the potential difference between the second phase and the matrix can be reduced in the temperature range, so that uniform thinning is realized, and the area of a thin area is larger.
In the step (4), the current is 180 mA-220 mA in the double-spraying process, and the temperature in the electrolytic cell is controlled to be 5-10 ℃ so as to avoid the occurrence of sieve pores caused by temperature deviation.
In the step (5), the double-spraying thinning time is generally between 10s and 20s, the sample clamp is taken down and then is firstly cleaned in distilled water, then the sample is taken down from the sample clamp and is sequentially cleaned in water and absolute ethyl alcohol cleaning solution in a multi-stage manner, at least three water and absolute ethyl alcohol cleaning solution are respectively placed, the process of immersing and taking out the sample in the cleaning process is circulated for at least 10 times, and the surface tension of the cleaning solution is fully utilized to clean the sample.
The design mechanism and beneficial effects of the invention are as follows
1. The invention improves the traditional double-spraying liquid, determines the range of double-spraying voltage and the range of double-spraying temperature, has higher thinning rate compared with the currently generally adopted method of carrying out double-spraying thinning at lower temperature and then carrying out ion thinning, shortens the period of sample preparation, has simple sample treatment, no stress in the thinning process, does not generate thermal activation, does not introduce other extra interferences such as dislocation and the like, has bright and flat sample surface and large thin area, improves the quality of transmission electron microscope pictures, and is suitable for preparing a large amount of high-quality 2xxx series aluminum alloy metal transmission samples.
2. The traditional double-spraying liquid for preparing the aluminum alloy is perchloric acid alcohol, but the corrosion resistance of the 2xxx aluminum alloy is poor, and the surface of a sample is seriously oxidized by adopting the traditional perchloric acid alcohol. In order to solve the problem, the invention adopts a less corrosive nitromethanol solution, reduces the concentration of double spraying liquid, and adopts nitric acid with volume fraction of 25% and methanol with volume fraction of 75% to form double spraying liquid, thereby better controlling the size of a thin area and eliminating the phenomenon of surface oxidation of a sample.
3. Through experimental trials of performing large-amplitude voltage regulation between 10V and 60V, the most suitable double-spraying voltage of the 2xxx series aluminum alloy is found to be between 18V and 22V, and the surface of the sample is bright. If the voltage is too high, the surface of the sample is blackened, and if the voltage is too low, the surface of the sample is dark and scratches exist. The invention provides a proper double-spraying voltage range, and can realize good double-spraying effect of the 2xxx series aluminum alloy.
4. On the basis of the 2-3 experiments, the surface of the sample still has a sieve hole, the area of the thin area is small, and a high-quality transmission sample is difficult to obtain. The sieve holes appear in the way that the potential difference between the second phase and the matrix is too large to realize uniform thinning, so that the periphery of the second phase is preferentially corroded, and the second phase is washed away under the action of the double-jet flow, so that the sieve holes appear. The double spraying temperature is adjusted between minus 50 ℃ and 25 ℃, and a great deal of experiments show that for 2xxx series aluminum alloy, the potential difference between the second phase and the matrix can be reduced by increasing the double spraying temperature, the mesh number of the sample is reduced along with the increase of the double spraying temperature, but the surface of the sample is oxidized due to the overhigh temperature. When the temperature is controlled between 5 ℃ and 10 ℃ in the double-spraying process, uniform thinning can be realized, the sample basically has no sieve pores, the yield is improved, and good double-spraying effect can be obtained.
5. In the invention, the mechanical thinning of the sample is sequentially carried out by adopting 400#, 800#, 1200# and 2000# sandpaper, a smooth and flat glass plate is placed under the sandpaper, and the sample is dragged by a rubber to grind on the sandpaper in an 8-shaped track so as to realize uniform thinning, so that the sample is prevented from being uneven to generate extinction stripes to influence subsequent observation.
6. In the invention, the temperature in the electrolytic cell is strictly controlled to be between 5 and 10 ℃ in the double-spraying process, the over-high or over-low temperature is avoided, the current in the double-spraying process is about 180 to 220mA, and the large double-spraying current can realize the quick thinning.
7. In the invention, the double-spraying thinning time is generally 10-20 s, the sample is taken down from the sample clamp and sequentially subjected to multistage cleaning in water and absolute ethyl alcohol cleaning solution, the water and absolute ethyl alcohol cleaning solution are respectively placed at least three times, the process of immersing and taking out the sample is circulated for at least 10 times during cleaning, and the surface tension of the cleaning solution is fully utilized to clean the sample.
Drawings
Fig. 1 is a 2024 aluminum alloy sample prepared by a conventional dual spray process.
Fig. 2 is a 2024 aluminum alloy sample prepared by ion milling after double spraying.
FIG. 3 is a 2024 aluminum alloy sample prepared using the dual spray process of the present invention.
FIG. 4 is a TEM image of a second phase of a 2024 aluminum alloy sample prepared by the dual spray process of the present invention.
FIG. 5 is a TEM image of the dislocation configuration of a 2024 aluminum alloy sample prepared by the dual spray process of the present invention.
Detailed Description
The present invention will be described in more detail with reference to examples. In the example, a sample of 2024 aluminum alloy over-aged at 180 ℃ for 120h is taken as an example, and a transmission sample is prepared by the following specific steps:
step 1: mechanically thinning a sample to a thickness of 40-50 um from the upper part to the lower part of a metal sheet with a thickness of 500um by using a spark wire cutting machine and sequentially adopting 400#, 800#, 1200# and 2000# abrasive paper, placing a smooth and flat glass plate under the abrasive paper in the sample grinding process, dragging the sample to grind on the abrasive paper in an 8-shaped track by using a rubber, and punching the mechanically thinned sample by using a puncher to obtain a metal wafer with a diameter of 3 mm;
step 2: the example used a Tenupol-5 model electrolytic double spray instrument from the struers corporation for a double spray experiment. Nitric acid with the concentration of 14-15 mol/L and methanol with the concentration of 24.56-24.68 mol/L are mixed in an electrolytic tank of a double-spraying thinning instrument according to the ratio of 1: 3, mixing the two solutions in a volume ratio to form double-spraying liquid, and adjusting the flow rate of an injection pump of the double-spraying electrolytic thinning instrument to ensure that the opposite double-spraying liquid sprayed by the double nozzles has certain pressure and is just in contact with and is aligned with the middle of the two nozzles;
and step 3: adding liquid nitrogen into the electrolytic tank for cooling, and measuring the temperature of the double-spray liquid in the electrolytic tank by using a thermometer to control the temperature in the electrolytic tank to be between 5 and 10 ℃;
and 4, step 4: placing a 2024 aluminum alloy sample with the diameter of 3mm on a double-spraying sample clamp, inserting the sample into a double-spraying instrument, adjusting the double-spraying voltage to be about 20V, setting the light transmittance to be 180, and then starting double spraying to thin the sample;
and 5: the double-spraying thinning time is generally 10-20 s, the alarm of a light transmittance double-spraying instrument is sounded when a sample is subjected to double-spraying perforation, the sample clamp is taken down and then is firstly cleaned in distilled water, then the sample is taken down from the sample clamp and is sequentially cleaned in water and absolute ethyl alcohol cleaning liquid in a multistage manner, 5 water and absolute ethyl alcohol cleaning liquid are respectively placed, the process of immersing and taking out the sample during cleaning is at least circulated for 10 times, and the sample is cleaned by fully utilizing the surface tension of the cleaning liquid so as to obtain the sample with a clean and bright surface.
The effects of the sample prepared by the method and the sample prepared by the traditional process parameters are respectively observed by a metallographic microscope, as shown in figure 1, the sample is a 2024 aluminum alloy sample prepared by the traditional double-spraying process parameters, the double-spraying process parameters are 18V in voltage, the double-spraying temperature is-30 ℃ to-20 ℃, the double-spraying current is 70mA to 90mA, the double-spraying time is 1 to 2min, the double-spraying effect is poor, a large number of sieve pores exist on the surface of the sample, and the thin area of the sample is small. As shown in FIG. 2, in the 2024 aluminum alloy sample prepared by ion thinning after double spraying, because the potential around the second phase is higher during double spraying and is preferentially corroded, a plurality of thin areas with smaller areas exist on the sample, and under the action of ion bombardment, a large number of holes are simultaneously formed on the surface of the sample, and the holes are combined to form larger holes, so that the sample is basically free of the thin areas, and the quality is poorer. As shown in fig. 3, compared with the sample prepared by the conventional double-spraying method, the 2024 aluminum alloy sample prepared by the double-spraying process of the present invention has a clean and flat surface and only one large hole, and when the prepared sample is observed by a transmission electron microscope, the thin area of the sample is large and the quality of the sample is good. As shown in FIG. 4, a TEM picture of a second phase taken by an undeformed sample of 2024 aluminum alloy prepared by the double-spray process of the invention can clearly see the morphology of the second phase, no dislocation and other additional artifacts are introduced during the sample preparation process, and the prepared TEM sample has high quality. FIG. 5 shows a dislocation configuration TEM image of a sample after the 2024 aluminum alloy prepared by the double-spray process is deformed, wherein no additional dislocation is introduced in the sample preparation process, the dislocation configuration is clear and visible, and the prepared TEM sample has high quality. Therefore, the TEM sample with good effect can be very conveniently and quickly prepared by adopting the method, and the TEM picture with high quality can be obtained.
In the preparation process of a transmission electron microscope sample, nitric acid with the concentration of 14-15 mol/L and methanol with the concentration of 24.56-24.68 mol/L are selected according to the ratio of 1: 3, controlling the double-spraying voltage to be 18-22V, and thinning the sample on a double-spraying electrolytic thinning instrument at the double-spraying temperature of 5-10 ℃. The proper selection of the double-spraying liquid, the double-spraying voltage and the double-spraying temperature ensures that the surface of a sample is bright, the potential difference between a second phase and a matrix is reduced, the occurrence of sieve pores is effectively avoided, the uniform thinning is realized, the thinning effect can be achieved within 10-20 s, the double-spraying time is shortened, and the efficiency is greatly improved. Compared with other complex processes such as ion thinning after double spraying, the invention has high thinning rate, greatly saves the time and cost of experiments, particularly introduces false images and great errors to the observation of tissues seriously affected by thermal activation, deformation and the like of GP regions, dislocations and the like, has no stress and heat input in the thinning process, provides a rapid and reliable sample preparation method, and has important reference significance for the preparation of metal material transmission samples containing thick second phases.
Claims (6)
1. A preparation method of a 2xxx series aluminum alloy transmission electron microscope sample is characterized by comprising the following steps: the method comprises the following steps:
(1) mechanically thinning a 2xxx series aluminum alloy sample on metallographic abrasive paper to a thickness of 40-50 um, and punching the mechanically thinned sample through a puncher to obtain a metal wafer with the diameter of 3 mm;
(2) adding double-spraying liquid into an electrolytic bath of the electrolytic double-spraying thinning instrument, and adjusting the flow rate of an injection pump of the electrolytic double-spraying thinning instrument to ensure that the opposite double-spraying liquid sprayed by the double nozzles has certain pressure and is just in contact with and is aligned with the middle of the two nozzles;
(3) adding liquid nitrogen into the electrolytic bath for cooling, and measuring the temperature of the double-spraying liquid in the electrolytic bath by using a thermometer to control the temperature of the double-spraying liquid in the electrolytic bath to be between 5 and 10 ℃;
(4) the method comprises the following steps of (1) installing a metal wafer sample prepared in the step (1) on a sample clamp, inserting the sample clamp into the middle of two nozzles of an electrolysis double-spraying thinning instrument, adjusting the double-spraying voltage to be 18-22V, setting proper light transmittance and then starting double spraying to thin the sample;
(5) and after the sample is subjected to double-spraying perforation to the set light transmittance, the alarm of the double-spraying instrument is sounded, and the sample is taken down and is sequentially washed by water and absolute ethyl alcohol, so that the aluminum alloy transmission electron microscope sample is obtained.
2. The method for preparing a 2xxx series aluminum alloy transmission electron microscope sample as claimed in claim 1, wherein: in the step (1), 400#, 800#, 1200# and 2000# sandpaper are sequentially adopted to mechanically thin the sample, a smooth and flat glass plate is placed below the sandpaper, the sample is dragged by a rubber to be ground on the sandpaper in an 8-shaped track so as to realize uniform thinning, and the sample is prevented from being uneven and generating extinction stripes under a transmission electron microscope to influence subsequent observation.
3. The method for preparing a 2xxx series aluminum alloy transmission electron microscope sample as claimed in claim 1, wherein: in the step (2), the double-spraying liquid is prepared by mixing nitric acid with the concentration of 14-15 mol/L and methanol with the concentration of 24.56-24.68 mol/L according to the weight ratio of 1: 3, the low-proportion and weak-acidity double-spray liquid of the nitromethanol effectively avoids the condition that the surface of a sample is oxidized due to over strong acidity of the electrolyte.
4. The method for preparing a 2xxx series aluminum alloy transmission electron microscope sample as claimed in claim 1, wherein: in the step (4), the temperature of the double-spraying process is controlled between 5 ℃ and 10 ℃, and the potential difference between the second phase and the matrix can be reduced in the temperature range, so that uniform thinning is realized, and the area of a thin area is larger.
5. The method for preparing a 2xxx series aluminum alloy transmission electron microscope sample as claimed in claim 1, wherein: in the step (4), the current is 180 mA-220 mA in the double-spraying process, and the temperature in the electrolytic cell is controlled to be 5-10 ℃ so as to avoid the occurrence of sieve pores caused by temperature deviation.
6. The method for preparing a 2xxx series aluminum alloy transmission electron microscope sample as claimed in claim 1, wherein: in the step (5), the double-spraying thinning time is generally between 10s and 20s, the sample clamp is taken down and then is firstly cleaned in distilled water, then the sample is taken down from the sample clamp and is sequentially cleaned in water and absolute ethyl alcohol cleaning solution in a multi-stage manner, at least three water and absolute ethyl alcohol cleaning solution are respectively placed, the process of immersing and taking out the sample in the cleaning process is circulated for at least 10 times, and the surface tension of the cleaning solution is fully utilized to clean the sample.
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| CN202011353844.6A CN112595565B (en) | 2020-11-27 | 2020-11-27 | A kind of preparation method of 2xxx series aluminum alloy transmission electron microscope sample |
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| CN114486959A (en) * | 2022-02-14 | 2022-05-13 | 广东工业大学 | A method for preparing eutectic high-entropy alloy TEM samples |
| CN115824745A (en) * | 2022-12-07 | 2023-03-21 | 航鑫材料科技有限公司 | Method for efficiently preparing aluminum alloy transmission electron microscope sample |
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| CN114486959A (en) * | 2022-02-14 | 2022-05-13 | 广东工业大学 | A method for preparing eutectic high-entropy alloy TEM samples |
| CN115824745A (en) * | 2022-12-07 | 2023-03-21 | 航鑫材料科技有限公司 | Method for efficiently preparing aluminum alloy transmission electron microscope sample |
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