CN114088496B - Device for preparing transmission electron microscope powder sample - Google Patents
Device for preparing transmission electron microscope powder sample Download PDFInfo
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- CN114088496B CN114088496B CN202111416332.4A CN202111416332A CN114088496B CN 114088496 B CN114088496 B CN 114088496B CN 202111416332 A CN202111416332 A CN 202111416332A CN 114088496 B CN114088496 B CN 114088496B
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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
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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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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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
- G01N23/2005—Preparation of powder samples therefor
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Abstract
The invention discloses a device for preparing a transmission electron microscope powder sample, which comprises a supporting unit and a solvent absorbing unit; a channel is arranged in the supporting unit, one end of the channel is connected with the back surface of the copper net, and the other end of the channel is connected with the solvent absorbing unit; the front surface of the copper net is loaded with powder sample dispersion liquid; the solvent absorption unit is used for generating negative pressure and separating solvent and powder samples in the powder sample dispersion liquid. According to the device disclosed by the invention, the negative pressure generated by the solvent absorption unit is used for separating the solvent from the powder sample in the powder sample dispersion liquid, so that the solvent in the powder sample is rapidly reduced, the solvent content is greatly reduced, the subsequent baking time is shortened, and the efficiency and the success rate of preparing the powder sample are improved. According to the invention, the copper net can be fixed in the vertical direction by means of vacuum suction, and the copper net is fixed in the horizontal direction by means of the limiting top cover, so that the problem of overturning the copper net in the pipetting process is avoided.
Description
Technical Field
The invention discloses a device for preparing a transmission electron microscope powder sample, and belongs to the technical field of sample preparation.
Background
The transmission electron microscope is used for observing the microstructure of the sample by using the electron beam as a light source, and the resolution of the transmission electron microscope can reach 0.1-0.2 nm due to the very short wavelength of the electron beam. In recent years, with the development of spherical aberration correction technology, the spatial resolution of transmission electron microscopy has reached sub-angstrom (50 pm) size. Therefore, the microstructure information of the sample can be easily obtained by using the transmission electron microscope.
The preparation of the transmission electron microscope sample is a long, complex and precise process, and has very strong technical skill. To obtain high quality electron micrographs, it is a very important step to make good samples. The transmission electron microscope samples are mainly divided into three types of powder, film and biology, wherein the powder samples are the most widely related types in the fields of chemistry and materials, and the most huge types in the field of transmission electron microscope analysis. Transmission electron microscope powder sample preparation typically takes the following steps:
(1) Selecting a proper copper net (common carbon film, ultrathin carbon film or micro grid) according to the particle size of the powder sample and shooting requirements;
(2) Taking out the copper net by forceps, putting the film face upwards, and putting the film on filter paper horizontally;
(3) Adding a proper amount of powder and a solvent (ethanol, tertiary butanol or purified water and the like) into a centrifuge tube, performing ultrasonic dispersion for 10-30 min, sucking 30-60 mu L of dispersion liquid by using a pipetting gun, and then dripping the dispersion liquid onto a copper mesh;
(4) And after the solvent in the dispersion liquid is naturally dried (more than 15 min), loading the copper mesh loaded with the powder sample on a sample rod for electron microscope observation.
However, the preparation of the above-mentioned powder sample for transmission electron microscopy has the following problems: the dispersion liquid dropped on the copper net is completely penetrated downwards by gravity, and the penetration time of the dispersion liquid is longer. For some powder samples (such as graphene, molybdenum disulfide and other two-dimensional materials), pure water is required to be used for dispersing, the wettability of the pure water and the copper mesh is extremely poor, when the dispersed liquid drops onto the copper mesh, the dispersed liquid is generally adhered to the copper mesh in an approximately spherical mode, and is difficult to quickly suck by filter paper below the copper mesh, so that drying can be realized only by self volatilization. But the volatilization of the purified water is slower, so that the preparation time of the transmission electron microscope powder sample is longer and the efficiency is lower.
Disclosure of Invention
The purpose of the application is to provide a device for preparing a transmission electron microscope powder sample, so as to solve the technical problem of low efficiency existing in the existing preparation of the transmission electron microscope powder sample.
The invention provides a device for preparing a transmission electron microscope powder sample, which comprises a supporting unit and a solvent absorbing unit;
a channel is arranged in the supporting unit, one end of the channel is connected with the back surface of the copper net, and the other end of the channel is connected with the solvent absorbing unit; the front surface of the copper net is loaded with powder sample dispersion liquid;
the solvent absorption unit is used for generating negative pressure and separating solvent and powder samples in the powder sample dispersion liquid.
Preferably, the support unit comprises a support column and a sample base with a first channel arranged inside, and one end of the first channel is connected with the solvent absorption unit;
the support column set up in on the sample base, the support column is interior axially to be provided with the second passageway of first passageway intercommunication, the one end of second passageway with the back of copper mesh meets.
Preferably, the port of the second channel connected with the copper mesh is funnel-shaped.
Preferably, the device further comprises a limit cap;
a limiting hole is formed in the limiting top cover;
the copper net is arranged in the limiting hole;
the support column penetrates through the limiting hole and is connected with the copper net.
Preferably, the limiting hole is funnel-shaped, and the minimum inner diameter of the limiting hole is equal to the outer diameter of the supporting column.
Preferably, the device further comprises a spacer in the shape of a groove;
the supporting unit is arranged in the cushion block;
the side wall of the cushion block is connected with the limit top cover and used for supporting the limit top cover, so that the top end of the support column is lower than the plane where the maximum diameter of the limit hole is located.
Preferably, the number of the support columns is a plurality.
Preferably, a plurality of support columns are uniformly arranged on the sample base in an array mode.
Preferably, the solvent absorption unit comprises a micro vacuum pump or a syringe.
Preferably, the sample base and the limit top cover are made of polytetrafluoroethylene.
Compared with the prior art, the device for preparing the transmission electron microscope powder sample has the following beneficial effects:
according to the device for preparing the transmission electron microscope powder sample, the negative pressure generated by the solvent absorption unit is used for separating the solvent from the powder sample in the powder sample dispersion liquid, so that the solvent in the powder sample is rapidly reduced, the solvent content is greatly reduced, the subsequent baking time is shortened, and the efficiency and the success rate of preparing the powder sample are improved.
According to the invention, the copper mesh can be fixed in the vertical direction by means of vacuum suction, and the copper mesh is fixed in the horizontal direction by means of the limiting top cover, so that the problem of overturning the copper mesh in the pipetting process is avoided, and the problem of overturning the copper mesh when pure water is used for preparing powder sample dispersion liquid is avoided.
Drawings
FIG. 1 is a schematic diagram of the overall structure of an apparatus for preparing a powder sample for transmission electron microscopy according to an embodiment of the present invention;
FIG. 2 is a top view of a support unit in an apparatus for preparing a powder sample for transmission electron microscopy according to an embodiment of the present invention;
FIG. 3 is a schematic view of section A-A of FIG. 2;
FIG. 4 is a schematic diagram of a micro vacuum pump in an apparatus for preparing a powder sample for transmission electron microscopy according to an embodiment of the present invention;
FIG. 5 is a schematic structural view of an air extraction joint in an apparatus for preparing a powder sample for a transmission electron microscope according to an embodiment of the present invention;
FIG. 6 is a schematic diagram of the structure of an exhaust tube in an apparatus for preparing a powder sample for transmission electron microscopy according to an embodiment of the present invention;
FIG. 7 is a top view of a limit cap in an apparatus for preparing a powder sample for a transmission electron microscope according to an embodiment of the present invention;
FIG. 8 is a schematic view in section B-B of FIG. 7;
FIG. 9 is a front view of a spacer block in an apparatus for preparing a powder sample for a transmission electron microscope according to an embodiment of the present invention;
fig. 10 is a top view of a spacer in an apparatus for preparing a powder sample for a transmission electron microscope according to an embodiment of the present invention.
List of parts and reference numerals:
0. a cushion block; 0-1, side walls; 1. a sample base; 1-1, a first channel; 1-2, a first threaded interface; 1-3, supporting columns; 1-4, a second channel; 1-5, a first port; 2. an air extraction joint; 2-1, a second threaded interface; 2-2, a pagoda interface; 3. a limit top cover; 3-1, limiting holes; 3-2, a second port; 4. an exhaust pipe; 5. a micro vacuum pump; 5-1, an air pipe joint; 5-2, adjusting a knob; 5-3, a switch.
Detailed Description
In the following description, for purposes of explanation and not limitation, specific details are set forth such as the particular system architecture, techniques, etc., in order to provide a thorough understanding of the embodiments of the present invention. It will be apparent, however, to one skilled in the art that the present invention may be practiced in other embodiments that depart from these specific details. In other instances, detailed descriptions of well-known systems, devices, circuits, and methods are omitted so as not to obscure the description of the present invention with unnecessary detail.
As shown in fig. 1, the apparatus for preparing a powder sample for a transmission electron microscope according to an embodiment of the present invention includes a support unit and a solvent absorption unit;
wherein a channel is arranged in the supporting unit, one end of the channel is connected with the back surface of the copper net, and the other end of the channel is connected with the solvent absorbing unit; the front side (film side) of the copper mesh is loaded with powder sample dispersion liquid;
the solvent absorption unit is used for generating negative pressure and separating solvent and powder samples in the powder sample dispersion liquid. The solvent absorbing unit may be a micro vacuum pump 5 or a syringe, which is not limited in the embodiment of the present invention, so long as a negative pressure can be generated. When the miniature vacuum pump 5 is adopted, the diaphragm of the miniature vacuum pump 5 is made of EPDM material, so that the pumping speed of the miniature vacuum pump can be easily adjusted according to the suction force of the copper mesh, and the damage of the copper mesh is avoided.
According to the embodiment of the invention, the negative pressure generated by the solvent absorption unit is used for separating the solvent from the powder sample in the powder sample dispersion liquid, so that the solvent in the powder sample is rapidly reduced, the solvent content is greatly reduced, the subsequent baking time is shortened, and the efficiency and the success rate of preparing the powder sample are improved.
Further, the structure of the supporting unit in the embodiment of the invention is shown in fig. 2 and 3, and the supporting unit comprises a supporting column 1-3 and a sample base 1 provided with a first channel 1-1 inside, wherein one end of the first channel 1-1 is provided with a first threaded interface 1-2, one end of the air extraction joint 2 is provided with a second threaded interface 2-1, and the first threaded interface 1-2 and the second threaded interface 2-1 are matched, so that the connection between the first channel 1-1 and the air extraction joint 2 is realized. The other end of the air extraction joint 2 is a pagoda joint 2-2, the air extraction joint 2 is connected with one end of an air extraction pipe 4 through the pagoda joint 2-2, and the other end of the air extraction pipe 4 is connected with a solvent absorption unit. When the solvent absorption unit is a micro vacuum pump 5, the structure of the micro vacuum pump 5 is shown in fig. 4, and the micro vacuum pump comprises an air pipe joint 5-1 for connecting an air suction pipe 4, an adjusting knob 5-2 for adjusting the suction force and a switch 5-3; the connection mode of the air extraction joint 2 and the first channel 1-1 can also be plug connection. The structure of the suction connector 2 is shown in fig. 5, and the structure of the suction pipe 4 is shown in fig. 6.
The support column 1-3 is arranged on the sample base 1, a second channel 1-4 communicated with the first channel 1-1 is axially arranged in the support column 1-3, and one end of the second channel 1-4 is connected with the back surface of the copper net.
The number of the support columns 1-3 in the embodiment of the invention can be one or more, when the number of the support columns is more than one, the support columns 1-3 can be uniformly or non-uniformly arranged on the sample base 1, preferably, the support columns 1-3 are uniformly arranged on the sample base 1 in an array mode, and the arrangement can reduce the preparation difficulty of a preparation process.
The supporting unit of the embodiment of the invention consists of the supporting columns 1-3 and the sample base 1, and the structure can realize the simultaneous operation of a plurality of supporting columns 1-3 and prepare powder samples with high flux.
To further increase the absorption range of the solvent, the first port 1-5 of the second channel 1-4 connected with the copper mesh is configured to be funnel-shaped in the embodiment of the present invention.
Under normal conditions, the copper mesh is small in weight, the copper mesh can turn over and enter into the liquid drops in the process of dispersing the liquid drops from the powder sample to the copper mesh, so that the uniformity of the load of the powder sample particles is affected, the powder particles are adhered to the back surface of the copper mesh, and part of particles which are not firmly adhered fall into a lens cone in the process of observing the sample, so that an electron microscope is easily polluted.
In order to solve the above problems, the device for preparing a powder sample of a transmission electron microscope according to the embodiment of the present invention further includes a limit cap 3, the structure of which is shown in fig. 7 and 8; a limiting hole 3-1 is arranged on the limiting top cover 3; the copper net is arranged in the limiting hole 3-1; the supporting column 1-3 penetrates into the limiting hole 3-1 and is connected with the copper net.
The limiting hole 3-1 in the embodiment of the invention can limit the lateral displacement of the copper net; the negative pressure generated by the solvent absorption unit can enable the copper net to be tightly attached to the support columns 1-3, so that the longitudinal displacement of the copper net is limited; under the condition that the transverse displacement and the longitudinal displacement are limited, the overturning of the copper mesh can be avoided, and the uniformity of the particle load of the powder sample is ensured.
In order to facilitate the dispersion liquid to be dropped on the copper mesh and the copper mesh to be taken out, the second port 3-2 where the maximum diameter of the limiting hole 3-1 is located in the embodiment of the invention is shaped like a funnel, the minimum inner diameter of the limiting hole 3-1 is equal to the outer diameter of the supporting column 1-3, and the diameter of the copper mesh is larger than or equal to the minimum inner diameter of the limiting hole 3-1 and smaller than the maximum inner diameter of the limiting hole 3-1.
Further, the device for preparing the powder sample of the transmission electron microscope of the embodiment of the invention further comprises a cushion block 0 in a groove shape, and the structure of the cushion block 0 is shown in fig. 9 and 10; the supporting unit is arranged in the cushion block 0; the side wall 0-1 of the cushion block 0 is connected with the limit top cover 3 and is used for supporting the limit top cover 3, so that the top end of the support column 1-3 is lower than the plane where the maximum diameter of the limit hole 3-1 is located.
When the copper net is used, the top end of the supporting column 1-3 is 0.2-0.5 mm lower than the bottom end of the funnel-shaped groove of the limiting hole 3-1 (namely the bottom end of the second port 3-2), the copper net is easy to put on the sample supporting column 1-3 because the limiting hole 3-1 is the funnel-shaped groove, and after the copper net is attached to the top end of the sample supporting column 1-3, the copper net just falls in the limiting hole 3-1, and the limiting hole 3-1 can ensure that the copper net cannot transversely move. When the copper net is required to be taken out, only the cushion block 0 needs to be removed, at the moment, the limit top cover 3 is unsupported and can be directly attached to the sample base 1, the top end of the support column 1-3 is close to the plane where the maximum diameter of the limit hole 3-1 is located or penetrates out of the limit hole 3-1, so that the copper net is ejected out, and the copper net is completely exposed at the upper end of the limit top cover 3, so that the subsequent baking and taking are facilitated.
The material of the sample base 1 and the limit top cover 3 in the embodiment of the invention is plastic or metal, for example, polytetrafluoroethylene, polypropylene, polycarbonate, aluminum, copper, iron and the like. Because polytetrafluoroethylene has the advantages of high temperature resistance, corrosion resistance, weather resistance, no adhesion and the like, the polytetrafluoroethylene is suitable for preparing powder dispersion liquid samples with any properties, and is particularly easy to clean, and the material of the sample base 1 and the limit top cover 3 in the embodiment of the invention is preferably polytetrafluoroethylene.
In the embodiment of the invention, the solvent absorption unit is taken as a micro vacuum pump 5 as an example, and the using method of the device is described as follows:
(1) The suction connector 2 is screwed into the screw thread provided in the first channel 1-1 of the sample holder 1 and the sample holder 1 is placed in the recess of the spacer block 0.
(2) One end of the air extraction pipe 4 is inserted into the pagoda interface of the air extraction joint 2, and the other end is inserted into the air extraction joint 2 of the micro vacuum pump 5.
(3) The limiting top cover 3 is buckled on the sample base 1, so that the supporting columns 1-3 on the sample base 1 are inserted into the limiting holes 3-1 of the limiting top cover 3, and the lower surface of the limiting top cover 3 is contacted with the side wall 0-1 of the cushion block 0.
(4) And starting the micro vacuum pump 5, placing the copper mesh in the limiting hole 3-1 of the limiting top cover 3, and adjusting the micro vacuum pump 5 according to the suction force of the copper mesh to enable the copper mesh to be tightly attached to the supporting column 1-3.
(5) And dispersing and dripping the powder sample on the front surface of the copper mesh by using a liquid-transferring gun, sucking the solvent in the powder sample dispersion liquid into the second channels 1-4 in the supporting columns 1-3 from the front surface of the copper mesh through the copper mesh under the action of suction force, and attaching the powder sample particles on the front surface of the copper mesh.
(6) After all copper nets or part of copper nets in the limiting holes 3-1 are dripped with dispersion liquid, the micro vacuum pump 5 is turned off, and the cushion block 0 under the sample base 1 is taken down, so that the copper nets on the supporting columns 1-3 of the sample base 1 are ejected out from the limiting holes 3-1 of the limiting top cover 3.
(7) And (3) placing the whole device under a baking lamp for baking for 3-15 min, and taking down the copper mesh loaded with the powder sample from the base support column 1-3 for transmission electron microscope observation after baking.
(8) And (3) using a tap water flushing device, cleaning residues in the channel, and preparing the sample again after drying.
The device provided by the embodiment of the invention is of a split structure, and is convenient to assemble, disassemble and clean. When the device is used, after the powder sample dispersion liquid is dripped on the copper mesh, the dispersion liquid can be quickly sucked into the channel under the action of suction force, only powder sample particles are attached to the copper mesh, a very small amount of dispersion liquid is remained on the copper mesh, and the drying time of the dispersion liquid, especially the pure water dispersion liquid with poor volatility, can be greatly shortened.
The device can realize high success rate and high flux preparation of powder samples.
The foregoing description is only a few examples of the present application and is not intended to limit the present application in any way, and although the present application is disclosed in the preferred examples, it is not intended to limit the present application, and any person skilled in the art may make some changes or modifications to the disclosed technology without departing from the scope of the technical solution of the present application, and the technical solution is equivalent to the equivalent embodiments.
Claims (10)
1. The device for preparing the transmission electron microscope powder sample is characterized by comprising a supporting unit, a limiting top cover and a solvent absorbing unit;
a channel is arranged in the supporting unit, one end of the channel is connected with the back surface of the copper net, and the other end of the channel is connected with the solvent absorbing unit; the front surface of the copper net is loaded with powder sample dispersion liquid;
a limiting hole is formed in the limiting top cover; the copper net is arranged in the limiting hole; the solvent absorption unit is used for generating negative pressure and separating solvent and powder samples in the powder sample dispersion liquid.
2. The device according to claim 1, wherein the support unit comprises a support column and a sample base having a first channel disposed therein, one end of the first channel being connected to the solvent absorbing unit;
the support column set up in on the sample base, the support column is interior axially to be provided with the second passageway of first passageway intercommunication, the one end of second passageway with the back of copper mesh meets.
3. The device of claim 2, wherein the port of the second channel that interfaces with the copper mesh is funnel-shaped.
4. A device according to claim 2 or claim 3, wherein the support post penetrates into the aperture to interface with the copper mesh.
5. The device of claim 4, wherein the limiting aperture is funnel-shaped in shape, and a minimum inner diameter of the limiting aperture is equal to an outer diameter of the support post.
6. The device of claim 4, further comprising a spacer having a groove shape;
the supporting unit is arranged in the cushion block;
the side wall of the cushion block is connected with the limit top cover and used for supporting the limit top cover, so that the top end of the support column is lower than the plane where the maximum diameter of the limit hole is located.
7. The device of claim 2 or 6, wherein the number of support columns is a plurality.
8. The apparatus of claim 7, wherein a plurality of the support columns are disposed uniformly in an array on the sample base.
9. The apparatus of claim 1, wherein the solvent absorption unit comprises a micro vacuum pump or a syringe.
10. The device of claim 4, wherein the sample base and the limit cap are made of polytetrafluoroethylene.
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| JP3696774B2 (en) * | 2000-06-12 | 2005-09-21 | 株式会社巴川製紙所 | Method for producing powder monolayer film laminate |
| JP2005326211A (en) * | 2004-05-13 | 2005-11-24 | Bridgestone Corp | Sample preparation method |
| JP2007047053A (en) * | 2005-08-11 | 2007-02-22 | Sumitomo Metal Mining Co Ltd | Method for preparing sample for transmission electron microscope observation |
| CN101361981A (en) * | 2008-08-25 | 2009-02-11 | 青岛大学 | Preparation method of nano material suitable for infrared-light targeted therapy of cancer |
| JP5435549B2 (en) * | 2009-04-22 | 2014-03-05 | 国立大学法人信州大学 | Electrical conductor and method for forming the same |
| CN101798058B (en) * | 2010-03-12 | 2013-06-19 | 厦门大学 | Method for modifying surface heterogeneous medium of silica-based nanowire |
| CN102200497A (en) * | 2010-03-24 | 2011-09-28 | 国家纳米技术与工程研究院 | Method for preparing powdered test sample for transmission electron microscope |
| CN102419277B (en) * | 2011-08-16 | 2015-01-28 | 中国检验检疫科学研究院 | Identification detection method of nano titanium dioxide in sun-screening cosmetic |
| CN102507285A (en) * | 2011-11-14 | 2012-06-20 | 上海大学 | Preparation method of transmission electron microscope sample for detecting second phase particles in alloy |
| CN102706709A (en) * | 2012-06-08 | 2012-10-03 | 武汉钢铁(集团)公司 | Method for preparing transmission electron microscope sample of rust layer powder test sample |
| CN102735509B (en) * | 2012-06-20 | 2014-04-02 | 大连大学 | Preparation method of transmission electron microscope observation sample of magnetic liquid in magnetic field |
| EP2755226B1 (en) * | 2013-01-15 | 2016-06-29 | Fei Company | Sample carrier for an electron microscope |
| CN103525404B (en) * | 2013-10-12 | 2015-11-18 | 苏州大学 | A kind of fluorescent sensor array based on conjugated polymer and application thereof |
| CN104634737A (en) * | 2013-11-15 | 2015-05-20 | 中国科学院生物物理研究所 | Manual ultralow-temperature sample stage for iPALM (interferometric photoactivated localization microscopy) microscope |
| CN104897454B (en) * | 2015-06-30 | 2018-02-23 | 东南大学 | A kind of preparation method of Nano-Scaled Carbide transmission electron microscope extraction replica sample |
| CN105669045B (en) * | 2016-01-11 | 2018-04-24 | 广东工业大学 | A kind of Cu2ZnSnS4The preparation method and applications of/graphene composite semiconductor films |
| CN106405822A (en) * | 2016-10-08 | 2017-02-15 | 华南师范大学 | Flexible electrowetting display substrate, preparation method thereof and electrowetting display device |
| CN108332989B (en) * | 2018-02-27 | 2020-12-29 | 江南大学 | Method for analyzing high-starch-content cereal grains and observing internal structure |
| CN109254025B (en) * | 2018-11-02 | 2023-09-22 | 内蒙古工业大学 | Device and method for sticking annular carrier net to transmission electron microscope sample |
| CN209372724U (en) * | 2018-12-28 | 2019-09-10 | 重庆大学 | The complementary type loading net used in transmission electron microscope |
| CN111693555B (en) * | 2020-06-18 | 2021-08-10 | 中国科学院地球化学研究所 | Method for in-situ preparation of TEM (transmission electron microscope) sample of nano-scale particles in complex-structure sample |
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