CN216847556U - Window chip and sample room for in-situ liquid scanning electron microscope - Google Patents

Window chip and sample room for in-situ liquid scanning electron microscope Download PDF

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Publication number
CN216847556U
CN216847556U CN202122778825.4U CN202122778825U CN216847556U CN 216847556 U CN216847556 U CN 216847556U CN 202122778825 U CN202122778825 U CN 202122778825U CN 216847556 U CN216847556 U CN 216847556U
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window
chip
nano
electron microscope
scanning electron
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谭立怡
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Nantong Li Si Yi Electronics Technology Co ltd
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Shaoxing Lisiyi Instrument Equipment Co ltd
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Abstract

The utility model relates to a window chip and a sample room for an in-situ liquid scanning electron microscope, belonging to the technical field of electron microscopes. According to the utility model, the nano-marker is manufactured on the side, close to the electron beam, of the window film, so that the rapid and effective focusing of the electron beam is facilitated, the observation of the sample in the sample chamber below the window under a relatively ideal focusing condition is realized, and the problem of low definition of an in-situ liquid scanning electron microscope caused by poor focusing is solved.

Description

Window chip and sample room for in-situ liquid scanning electron microscope
Technical Field
The utility model belongs to the technical field of electron microscopes, and relates to a window chip and a sample chamber for an in-situ liquid scanning electron microscope.
Background
The in-situ liquid chamber electron microscope technology breaks through the limitation of the traditional electron microscope, can carry out real-time high-resolution observation on a sealed liquid sample in the vacuum environment of the electron microscope, and has good development prospect. Compared with a transmission electron microscope, the scanning electron microscope has the advantages that the equipment and the test cost are relatively low, the sample space in the electron microscope vacuum chamber is large, and the matching with the in-situ liquid chamber is more favorably realized. However, when the scanning electron microscope is used, more electron beam focusing adjustment is required, a window film has a certain influence on the observed definition of a sample, and particularly when the sample in liquid moves, image change caused by movement and image deterioration caused by poor focusing are not easy to distinguish, so that the difficulty in electron beam focusing operation is possibly increased obviously, and the definition of in-situ liquid scanning electron microscope analysis is influenced by poor focusing.
In the prior art, holes are punched in the window film to expose the liquid, but this method may cause evaporation of the liquid into the vacuum chamber and increase instability of the liquid sample. The four corners of the window film can also be used as reference objects to help the electron beam adjustment to a certain extent, but the four corners of the window film can be far away from the interested sample area, so that the difficulty in retrieving the sample area after the focusing adjustment is increased, and the phenomenon of poor focusing can occur in the process of retrieving the sample. An electrode is also manufactured on one side of the window film close to the liquid, and the window film is used for heating and other functions, but is not suitable for the application of an in-situ liquid scanning electron microscope for assisting the focusing of electron beams.
SUMMERY OF THE UTILITY MODEL
In view of the above, the present invention provides a window chip and a sample chamber for an in-situ liquid scanning electron microscope, so as to solve the problem of low resolution of the in-situ liquid scanning electron microscope due to poor focusing.
In order to achieve the purpose, the utility model provides the following technical scheme:
a window chip for an in-situ liquid scanning electron microscope comprises a chip body with an observation hole in the middle and a window film arranged at the observation hole, wherein a plurality of nano markers are arranged on the upper side of the window film at intervals.
Optionally, the nano-tag has a distinct morphology and/or distribution characteristic.
Optionally, the shape of the nano-tag is a cone and/or a rod.
Optionally, the shape of the nano-tag is spherical and/or hemispherical.
Optionally, the nano-tags are of different particle sizes.
Optionally, the material of the window film is silicon nitride, silicon dioxide, a multilayer coated window or a polymer film.
Optionally, the nano-tag is obtained by photolithography, physical deposition, electron beam induced deposition or focused ion beam processing.
Optionally, the nano-markers are protruding particles on the surface of the window film and/or nano-pits on the surface of the window film.
Optionally, the observation hole is in an inverted cone shape and has a large end and a small end, the window film is disposed at the small end of the observation hole, and the nano-tag is located on one side of the window film facing the chip body.
A sample chamber comprises a box body, wherein a window is arranged on the upper portion of the box body, a window chip is arranged at the position of the window, a bottom chip is arranged at the position, corresponding to the window, of the bottom of the inner side of the box body so as to place a liquid sample, the window chip is applied to the window chip, and one side, provided with a nano marker, faces upwards.
The utility model has the beneficial effects that: the nano-marker is manufactured on one side of the window film close to the electron beam, so that the rapid and effective focusing of the electron beam is facilitated, the sample in the sample chamber below the window is observed under an ideal focusing condition, and the problem of low definition of an in-situ liquid scanning electron microscope caused by poor focusing is solved.
Additional advantages, objects, and features of the utility model will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the utility model. The objectives and other advantages of the utility model may be realized and attained by the means of the instrumentalities and combinations particularly pointed out hereinafter.
Drawings
For the purposes of promoting a better understanding of the objects, aspects and advantages of the utility model, reference will now be made to the following detailed description taken in conjunction with the accompanying drawings in which:
FIG. 1 is a schematic view of a window chip for an in-situ liquid scanning electron microscope;
FIG. 2 is a schematic diagram of the structure of a sample chamber;
FIG. 3 is a schematic view of a chip holder.
Reference numerals: an electron beam 1, a window chip 2, a window film 3, a sample 4, a cone-shaped marker 5, a box body 6, a bottom chip 7, a rod-shaped marker 8, a series size marker 9, a clamping block 10, a set screw 11 and a clamping groove 12.
Detailed Description
The following embodiments of the present invention are provided by way of specific examples, and other advantages and effects of the present invention will be readily apparent to those skilled in the art from the disclosure herein. The utility model is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention. It should be noted that the drawings provided in the following embodiments are only for illustrating the basic idea of the present invention in a schematic way, and the features in the following embodiments and examples may be combined with each other without conflict.
Wherein the showings are for the purpose of illustration only and not for the purpose of limiting the utility model, shown in the drawings are schematic representations and not in the form of actual drawings; to better illustrate the embodiments of the present invention, some parts of the drawings may be omitted, enlarged or reduced, and do not represent the size of an actual product; it will be understood by those skilled in the art that certain well-known structures in the drawings and descriptions thereof may be omitted.
The same or similar reference numerals in the drawings of the embodiments of the present invention correspond to the same or similar components; in the description of the present invention, it should be understood that if there is an orientation or positional relationship indicated by the terms "upper", "lower", "left", "right", "front", "rear", etc., based on the orientation or positional relationship shown in the drawings, it is only for convenience of description and simplification of description, but it is not intended to indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore the terms describing the positional relationship in the drawings are only used for illustrative purposes and are not to be construed as limiting the present invention, and the specific meaning of the terms described above will be understood by those skilled in the art according to the specific circumstances.
Referring to fig. 1 to 2, a window chip for an in-situ liquid scanning electron microscope includes a chip body with an observation hole in the middle and a window film 3 disposed at the observation hole, wherein a plurality of nano markers are disposed at intervals on the upper side of the window film 3.
Optionally, the nano-tag has a distinct morphology and/or distribution characteristic.
Optionally, the shape of the nano-tag is a cone and/or a rod.
Optionally, the shape of the nano-tag is nano-spherical and/or hemispherical.
Optionally, the nanomarkets differ in particle size.
Optionally, the material of the window film 3 is silicon nitride, silicon dioxide, a multi-layer plated window or a polymer film.
Alternatively, the nano-tag is obtained by a method of photolithography, physical deposition, electron beam induced deposition or focused ion beam processing.
Optionally, the nano-tag is a protruding particle on the surface of the window film and/or a nano-pit on the surface of the window film.
Optionally, the observation hole is in an inverted cone shape and has a large end and a small end, the window film 3 is disposed at the small end of the observation hole, and the nano-tag is located on a side of the window film 3 facing the chip body.
A sample chamber comprises a box body 6, wherein a window is arranged on the upper portion of the box body 6, a window chip 2 is arranged at the window, a bottom chip 7 is arranged at the position, corresponding to the window, of the bottom of the inner side of the box body 6 so as to place a liquid sample 4, the window chip 2 is applied to the window chip, and one side, provided with a nano marker, faces upwards.
Examples
The utility model provides an original position liquid sample room for scanning electron microscope, as shown in fig. 1 ~ 2, including the sealed box body 6 of window is seted up on upper portion, window department is equipped with window chip 2, the inboard bottom of box body 6 corresponds the position of window and is equipped with bottom chip 7 in order to place liquid sample 4, window chip 2 includes that the middle part is seted up the chip body that is the observation hole of back taper and corresponds observation hole position and set up window film 3 on the chip body downside, the side interval sets up a plurality of nanometer markers on window film 3.
The nano marker can be a conical marker 5 or a rod-shaped marker 8, electron beam focusing can be performed on the nano marker by using a traditional scanning electron microscope focusing adjusting means, the electron beam 1 is emitted to the window film 3 through the window, and the sample 4 in liquid below the film can be better observed by performing photographic analysis after the focusing adjustment is completed, so that image blurring caused by unfocused electron beam 1 is avoided.
The nano-tag in this embodiment is on the liquid side above the window rather than below the window, which avoids the difficulty of focusing operations where the image is not as clear as the particles above the window across the window. The nano-tag density cannot be too great and a blank window film 3 needs to be left for viewing the sample 4 under the film. The nano-tag should also have an obvious morphology or distribution characteristic, which facilitates distinguishing the nano-tag from the sample 4 particles in the liquid, and the distinct morphology characteristic also facilitates better judgment of focusing conditions during focusing operations, thereby achieving ideal focusing. The nano-tag minimum feature size cannot be too large or it cannot serve to help fine-tune the image to achieve good focusing of the electron beam 1. The ideal nano-tag minimum feature size should be no greater than 100 nanometers. The morphological features of the cone-shaped markers 5 and the rod-shaped markers 8 in this embodiment are very sharp, and the spherical nano-markers may not be as easily distinguishable from the particles in the liquid to some extent according to the specific sample condition. By arranging the marking particles in order, the marking particles can be conveniently identified. The spherical or hemispherical nano-markers with different sizes are orderly arranged to form the series of size markers 9, and the large nano-markers can be used for finding the nano-markers first and then the small nano-markers can be used for realizing ideal focusing. The nano-markers can be raised particles, nano-pits on the surface of the film, or a combination of the above ways.
The preparation method of the nano-label comprises photoetching, electron beam induced deposition, focused ion beam processing and the like; the diluted nanoparticle solution can also be dropped onto the window where the liquid is allowed to dry and the nanoparticle label particles are deposited. The material of the window film 3 includes silicon nitride, silicon dioxide, a multi-layer coated window, a polymer film, and the like.
Since the window film 3 of the window chip 2 is very thin, if one side of the window chip 2 is directly fixed on the surface of the base for carrying out marking particle deposition or marking pit etching, the film is easily damaged due to the contact between the film and the surface of the base. In addition, the upper surface and the lower surface of the chip are required to be turned over before and after the nano marker is prepared in the chip using process, the total size of the chip is very small, so that the chip is easy to slip and damage due to the fact that the chip is not firmly clamped when the chip is clamped by tweezers in the reverse operation, and the chip is very fragile and cannot be clamped by too much force. The present application thus also provides a chip holder to address this problem.
As shown in fig. 3, a chip clamp includes clamping blocks 10 disposed oppositely, clamping grooves 12 are disposed on opposite sides of the clamping blocks 10, clamping slits communicated with the clamping grooves 12 are disposed in the middle of the clamping blocks 10 adjacent to the clamping grooves 12, and locking mechanisms are disposed at positions of the clamping blocks corresponding to the clamping slits and include two sets of locking set screws 11 with opposite locking directions. The use method of the chip clamp comprises the following steps: placing the window chip 2 in the clamping groove 12 of the clamp, so that the part of the observation hole is away from the underlying support base, and the window film 3 is prevented from being damaged by contact with the surface of the base; and then the set screw 11 is locked to turn the window chip 2 and the clamp together, so that the difficulty of directly clamping the chip by tweezers to perform turning operation is avoided. The clamp is fixed by two sets of fastening screws 11 in opposite directions, so that when the chip is turned over together with the clamp in the clamp, the fastening and detaching sequence of the fastening screws 11 is changed, and the difficulty that the fastening screws 11 are loosened from the lower part of the clamp to open the clamp after turning can be avoided.
Finally, the above embodiments are only intended to illustrate the technical solutions of the present invention and not to limit the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions, and all of them should be covered by the claims of the present invention.

Claims (9)

1. The utility model provides an in situ liquid is window chip for scanning electron microscope, includes that the chip body of viewing aperture and the window film of setting in viewing aperture department are seted up at the middle part, its characterized in that: the upper side of the window film is the side close to the electron beam, and a plurality of nano markers are arranged at intervals on the side.
2. The window chip for an in-situ liquid scanning electron microscope according to claim 1, wherein: the shape of the nano-label is cone-shaped and/or rod-shaped.
3. The window chip for an in-situ liquid scanning electron microscope according to claim 1, wherein: the shape of the nano-tag is spherical and/or semispherical.
4. The window chip for an in-situ liquid scanning electron microscope according to claim 1, wherein: the nano-tags have different particle sizes.
5. The window chip for an in-situ liquid scanning electron microscope according to claim 1, wherein: the window film is made of silicon nitride, silicon dioxide, a multilayer coating film window or a polymer film.
6. The window chip for an in-situ liquid scanning electron microscope according to claim 1, wherein: the nano-tag is obtained by photoetching, physical deposition, electron beam induced deposition or focused ion beam processing.
7. The window chip for an in-situ liquid scanning electron microscope according to claim 1, wherein: the nano-markers are particles protruding from the surface of the window film and/or nano-pits in the surface of the window film.
8. The window chip for an in-situ liquid scanning electron microscope according to claim 1, wherein: the observation hole is the back taper, has main aspects and tip, and the window film sets up the tip at the observation hole, and nanometer mark thing is located window film and is faced chip body one side.
9. The utility model provides a sample room, is equipped with the box body of window including upper portion, and window department is equipped with the window chip, and the inboard bottom of box body corresponds the position of window and is equipped with bottom chip in order to place liquid sample, its characterized in that: the window chip is applied to the window chip as claimed in any one of claims 1 to 8, and the side provided with the nano-markers faces upwards.
CN202122778825.4U 2021-11-11 2021-11-11 Window chip and sample room for in-situ liquid scanning electron microscope Active CN216847556U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202122778825.4U CN216847556U (en) 2021-11-11 2021-11-11 Window chip and sample room for in-situ liquid scanning electron microscope

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202122778825.4U CN216847556U (en) 2021-11-11 2021-11-11 Window chip and sample room for in-situ liquid scanning electron microscope

Publications (1)

Publication Number Publication Date
CN216847556U true CN216847556U (en) 2022-06-28

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN202122778825.4U Active CN216847556U (en) 2021-11-11 2021-11-11 Window chip and sample room for in-situ liquid scanning electron microscope

Country Status (1)

Country Link
CN (1) CN216847556U (en)

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Effective date of registration: 20220804

Address after: 226001 auxiliary building of Qixiu community, xinchengqiao street, Chongchuan District, Nantong City, Jiangsu Province

Patentee after: NANTONG LI SI YI ELECTRONICS TECHNOLOGY Co.,Ltd.

Address before: 312000 room 601-602, block B, Kechuang building, No. 586, West Ring Road, Keqiao Economic Development Zone, Keqiao District, Shaoxing City, Zhejiang Province

Patentee before: Shaoxing lisiyi Instrument Equipment Co.,Ltd.

TR01 Transfer of patent right