TEM (Transmission Electron Microscope) carrier network capable of preparing samples in multiple regions

Abstract

The utility model discloses a TEM (Transmission Electron Microscope) carrying net capable of preparing samples in multiple areas, which consists of an inner ring, an outer ring and carrying net areas, the carrying net areas are connected between the inner ring and the outer ring, at least two separation strips are also connected between the inner ring and the outer ring, and the carrying net areas between the inner ring and the outer ring are separated into more than two sample preparation areas; according to the TEM carrier net, the carrier net area is partitioned through the partition strips, so that mutual pollution is avoided during sample preparation, particularly, the TEM carrier net is loaded on a double-inclination sample rod and can rotate in the alpha direction and the beta direction, the crystal zone axis of a sample is parallel to an electron beam, and effective diffraction patterns can be rapidly obtained; the point cannot be achieved by a single-dip single-grid sample rod and a single-dip multi-grid sample rod; and after digital identification is carried out on each sample preparation area, the sample preparation areas can be quickly identified in an electron microscope observation window and cannot be confused, so that the test work can be accurately and quickly carried out, and the TEM test and analysis efficiency of multiple samples is greatly improved.

Description

Technical Field

[0001] The utility model relates to the field of a grid used for transmission electron microscope (TEM) testing (TEM grid for short), in particular to a TEM grid capable of preparing samples in multiple regions. Background Art

[0002] TEM grid is the most commonly used consumable of transmission electron microscope (TEM or EM for short). It is mainly used to reinforce and support samples and to carry the samples under test during TEM observation. TEM grid is in the shape of a disc with a universal diameter of 3mm. Currently, the most common TEM grid is made of copper sheet. Due to its simple processing, suitable hardness and high cost performance, it is widely used. Therefore, "copper grid" is often used to refer to "grid". Figure 1 As shown, the conventional TEM grid consists of an outer ring 102 and a grid area 101 connected to the outer ring 102, and the grid area 101 is a continuous area that can only carry one type of sample.

[0003] At the same time, the TEM grid needs to be loaded on the sample holder before it can be moved to the TEM electron beam area for testing. The sample holder includes a single-tilt sample holder, a double-tilt sample holder, and a similar sample holder that can carry a 3mm grid. The single-tilt sample holder can only be tilted or rotated in one direction, and is divided into a single-tilt single-grid sample holder and a single-tilt multi-grid sample holder. Figure 2 As shown in the figure, the single-tilt single-grid sample holder is a sample holder that can only hold one TEM grid. Figure 3 As shown, the single-tilt multi-grid sample holder is a sample holder that can hold multiple TEM grids. Figure 4 As shown, the double-tilt sample holder can be tilted or rotated in two mutually perpendicular directions, but the double-tilt sample holder can only hold one TEM grid; combined with Figure 5 and Figure 6 As shown, the single-tilt sample holder can only rotate in the α direction, while the double-tilt sample holder can rotate in the α direction or the β direction respectively.

[0004] In TEM testing, it is very necessary to rotate the sample rod, because in crystal sample testing, it is often necessary to adjust the sample angle so that the crystal zone axis of the crystal sample is parallel to the electron beam to obtain an effective diffraction pattern. In a crystal, any group of crystal planes that intersect or are parallel to the same crystal direction line between crystal planes constitute a crystal zone, which is called the crystal zone axis. Figure 7 As shown, the common feature of all crystal planes in the same crystal axis is that the normals of all crystal planes are perpendicular to the crystal axis.

[0005] Combination Figure 8As shown in the figure, when the electron beam passes through the crystal sample, the electron beam and the crystal sample interact coherently to produce a diffraction pattern. The crystal structure of the sample can be known by analyzing the diffraction pattern. An effective diffraction pattern can only be obtained when the electron beam is parallel to the crystal zone axis of the crystal sample. However, in the actual sample preparation process, when the sample is placed on the TEM grid, not all samples' crystal zone axes are parallel to the electron beam. Therefore, it is necessary to rotate the sample on the TEM grid in the α or β direction to make its crystal zone axis parallel to the electron beam, thereby producing an effective diffraction pattern.

[0006] However, the traditional TEM grid is a continuous area that can only carry one type of sample. During the test, the sample needs to be changed frequently, which is time-consuming, labor-intensive and costly. Figure 3 The single-tilt multi-grid sample holder can only rotate in the α direction during testing, but not in the β direction. This limits the operation of adjusting its crystal zone axis when obtaining effective diffraction patterns, making it difficult to improve the TEM testing and analysis efficiency of multiple samples.

[0007] Therefore, the traditional TEM grid needs to be improved. Utility Model Content

[0008] The utility model aims to provide a TEM grid capable of preparing samples in multiple regions, thereby improving the TEM testing and analysis efficiency of multiple samples.

[0009] The technical solution of the utility model is as follows: a TEM grid capable of preparing samples in multiple regions, comprising an inner ring, an outer ring and a grid region, wherein the grid region is connected between the inner ring and the outer ring, and at least two dividing strips are connected between the inner ring and the outer ring, so as to separate the grid region between the inner ring and the outer ring into more than two sample preparation regions.

[0010] The TEM grid capable of preparing samples in multiple regions, wherein: two dividing strips are connected between the inner ring and the outer ring, the two dividing strips are in a straight line passing through the center of the inner ring, and separate the grid region between the inner ring and the outer ring into two sample preparation regions of equal area.

[0011] The TEM grid capable of multi-region sample preparation, wherein: three dividing bars are connected between the inner ring and the outer ring, the three dividing bars are located on different straight lines passing through the center of the inner ring, and the angle between adjacent dividing bars is 120°, dividing the grid area between the inner ring and the outer ring into three sample preparation areas of equal area.

[0012] The TEM grid capable of preparing samples in multiple regions, wherein: four dividing strips are connected between the inner ring and the outer ring, the four dividing strips are arranged in a cross shape on two straight lines passing through the center of the inner ring, and the grid region between the inner ring and the outer ring is divided into four sample preparation regions of equal area.

[0013] The TEM grid capable of multi-region sample preparation, wherein: five dividing strips are connected between the inner ring and the outer ring, the five dividing strips are evenly distributed on different straight lines passing through the center of the inner ring, and the angle between adjacent dividing strips is 72°, dividing the grid area between the inner ring and the outer ring into five sample preparation areas of equal area.

[0014] The TEM grid capable of multi-region sample preparation, wherein: six dividing strips are connected between the inner ring and the outer ring, the six dividing strips are evenly distributed on three straight lines passing through the center of the inner ring, and the angle between adjacent dividing strips is 60°, dividing the grid area between the inner ring and the outer ring into six sample preparation areas of equal area.

[0015] The TEM grid capable of preparing samples in multiple regions, wherein: the separation strip is composed of two parallel connecting lines, and the region between the two connecting lines is a separation strip, which is used to separate different sample preparation regions.

[0016] The TEM grid capable of preparing samples in multiple regions, wherein: the surface of the sample preparation region is coated with a polyvinyl formal film, and the surface of the polyvinyl formal film is sprayed with a carbon support film.

[0017] The TEM grid capable of preparing samples in multiple regions, wherein: the TEM grid is a metal grid and is manufactured by a template etching method.

[0018] The TEM grid capable of preparing samples in multiple regions, wherein: the TEM grid is made of non-metallic material and is manufactured by a 3D printer.

[0019] Compared with the traditional TEM grid, the TEM grid capable of multi-region sample preparation of the utility model has the following beneficial effects: the grid areas are partitioned and zoned by dividing strips, so that mutual contamination will not be caused during sample preparation; in particular, the TEM grid is loaded on a double-tilt sample rod and can be rotated in the α and β directions, so that the crystal band axis of the sample is parallel to the electron beam, so as to quickly obtain an effective diffraction pattern, which cannot be achieved by a single-tilt single-grid sample rod and a single-tilt multi-grid sample rod; and after the sample preparation areas are marked with patterns or numbers, they can be quickly identified in the electron microscope observation window without confusion, so that the test work can be carried out accurately and quickly, greatly improving the TEM test and analysis efficiency of multiple samples. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] The drawings described herein are only for explanation purposes and are not intended to limit the scope of the present invention in any way; the shapes and proportional dimensions of the components in the drawings are only for illustration purposes and are used to help understand the present invention, but are not intended to specifically limit the shapes and proportional dimensions of the components of the present invention; those skilled in the art, under the guidance of the present invention, can select various possible shapes and proportional dimensions to implement the present invention according to specific circumstances.

[0021] Figure 1 This is a schematic diagram of the planar enlarged structure of a traditional TEM grid;

[0022] Figure 2 It is a schematic diagram of the structure of a single-inclined single-loaded mesh sample rod in the prior art;

[0023] Figure 3 It is a schematic diagram of the structure of a single-tilt multi-loaded mesh sample rod in the prior art;

[0024] Figure 4 It is a schematic diagram of the double-tilt sample rod structure in the prior art;

[0025] Figure 5 It is a schematic diagram of the rotation of the TEM grid along the α direction in the prior art;

[0026] Figure 6 It is a schematic diagram of the rotation of the TEM grid along the β direction in the prior art;

[0027] Figure 7 Schematic diagram of the spatial relationship between the crystal zone plane and the crystal zone axis in the prior art;

[0028] Figure 8 Schematic diagram of the diffraction pattern principle in the prior art;

[0029] Fig. 9 It is a schematic diagram of the planar structure of the TEM grid capable of preparing samples in multiple regions according to the utility model;

[0030] Fig.10 It is a schematic diagram of the structure of the TEM grid capable of preparing samples in four regions according to the utility model;

[0031] Fig.11 It is a schematic structural diagram of a TEM grid coated with a Fanghua film and capable of preparing samples in four regions according to the utility model;

[0032] Fig.12 The utility model is a structural schematic diagram of a TEM grid coated with a Fanghua film and a sprayed carbon support film and capable of preparing samples in four regions.

[0033] The reference numerals in the figure are summarized as follows: outer ring 102 (of conventional TEM grid), grid area 101 (of conventional TEM grid), grid area 201 (of TEM grid of the present invention), outer ring 202 (of TEM grid of the present invention), inner ring 203 (of TEM grid of the present invention), separator 204, Fanghua film 205, and carbon support film 206. DETAILED DESCRIPTION

[0034] The specific implementation manner and examples of the present invention will be described in detail below in conjunction with the accompanying drawings. The described specific examples are only used to explain the present invention and are not used to limit the specific implementation manner of the present invention.

[0035] like Fig. 9 As shown, the TEM grid capable of preparing samples in multiple regions of the present invention comprises an inner ring 203, an outer ring 202 and a grid region 201, wherein the grid region 201 is connected between the inner ring 203 and the outer ring 202, and two, three, four, five or six dividing strips 204 are further connected between the inner ring 203 and the outer ring 202, so as to separate the grid region 201 between the inner ring 203 and the outer ring 202 into two, three, four, five or six sample preparation regions, respectively. Fig. 9 As shown in A, B, C, D, and E.

[0036] In other words, the TEM grid capable of preparing samples in multiple regions of the present invention is composed of three parts: the grid region 201 , the outer ring 202 and the inner ring 203 . The three parts are continuous except for the separation region, and the separation region is the separation strip 204 .

[0037] Specifically, Fig. 9 As shown in E, six dividing bars 204 are connected between the inner ring 203 and the outer ring 202. The six dividing bars 204 are evenly distributed on three straight lines passing through the center of the inner ring 203, and the angle between adjacent dividing bars 204 is 60°, dividing the grid area 201 between the inner ring 203 and the outer ring 202 into six sample preparation areas of equal area.

[0038] Similar, such as Fig. 9 As shown in D, five dividing bars 204 are connected between the inner ring 203 and the outer ring 202. The five dividing bars 204 are evenly distributed on different straight lines passing through the center of the inner ring 203, and the angle between adjacent dividing bars 204 is 72°, dividing the grid area 201 between the inner ring 203 and the outer ring 202 into five sample preparation areas of equal area.

[0039] Similar, such as Fig. 9As shown in C, four dividing bars 204 are connected between the inner ring 203 and the outer ring 202. The four dividing bars 204 are located on two straight lines passing through the center of the inner ring 203 in a cross shape, dividing the grid area 201 between the inner ring 203 and the outer ring 202 into four sample preparation areas of equal area.

[0040] Similar, such as Fig. 9 As shown in B, three dividing bars 204 are connected between the inner ring 203 and the outer ring 202. The three dividing bars 204 are located on different straight lines passing through the center of the inner ring 203, and the angle between adjacent dividing bars 204 is 120°, dividing the grid area 201 between the inner ring 203 and the outer ring 202 into three sample preparation areas of equal area.

[0041] Similar, such as Fig. 9 As shown in A, two dividing strips 204 are connected between the inner ring 203 and the outer ring 202. The two dividing strips 204 are in a straight line passing through the center of the inner ring 203, and separate the mesh area 201 between the inner ring 203 and the outer ring 202 into two sample preparation areas of equal area.

[0042] Combination Fig.10 As shown, specifically, the dividing strip 204 is composed of two parallel connecting lines, and the area between the two connecting lines is a dividing strip, which is used to separate the mesh area 201 between the outer ring 202 and the inner ring 203 into different sample preparation areas, so that mutual contamination will not occur when comparative tests are performed on multiple groups of samples at the same time.

[0043] In the specific implementation process of the utility model, the TEM grid capable of multi-region sample preparation can be made of metal materials such as copper mesh, nickel mesh, molybdenum mesh, gold mesh, aluminum mesh, platinum mesh, titanium mesh, palladium mesh, beryllium copper mesh, gold-plated copper mesh, gold-plated nickel mesh, stainless steel mesh, etc., and can also be made of non-metallic materials such as graphite carbon mesh, nylon, nitrile rubber, polyamide-polyethylene oxide block compound, etc.; the diameter of the TEM grid is 3mm, and the thickness ranges from 20 to 100μm; the mesh size of the TEM grid is between 50 and 400 meshes, and the shapes of the mesh include but are not limited to round holes, square holes, diamond holes, single hole rings, etc.

[0044] Specifically, Fig.10 Taking the TEM grid that can prepare samples in four areas as an example, the width of the outer ring 202 is in the range of 0.2-0.5 mm, the diameter of the inner ring 203 is 0.2 mm, and the width of the inner ring 203 is in the range of 0.15-0.25 mm; the width of the dividing zone (i.e., the dividing area) between the two parallel connecting lines constituting the dividing strip 204 is in the range of 0.1-0.2 mm.

[0045] In order to better identify samples in multiple areas, it is better to set holes of different shapes and / or numbers on the inner ring 203 corresponding to different sample preparation areas, such as one or two round holes, triangular holes or square holes, or to set hollow Roman numeral patterns on the inner ring corresponding to different sample preparation areas; thereby, the samples can be quickly identified in the electron microscope observation window, avoiding confusion when comparative testing of multiple groups of samples is performed at the same time, and the testing work can be performed accurately and quickly.

[0046] If metal materials are used to make TEM grids, template etching method can be used; if non-metal materials are used to make TEM grids, 3D printers can be used for printing. For example, the pre-built model can be imported into the slicing software BMF 3Dslicer for slicing, and then the sliced ​​images can be imported into the 3D Printing System in sequence; then polyacrylic acid is loaded into the liquid tank, and the platform is debugged (including level, height and focus); finally, the printing mode is selected, and the parameters and imported slice image files can be started for printing.

[0047] In addition, combined Fig.11 As shown, some TEM grids also need to be coated with polyvinyl alcohol formal with a thickness of about 10 nm on their surface to form a polyvinyl alcohol formal film (commonly known as Fanghua film 205). It should be noted that the mesh size of the TEM grid coated with Fanghua film 205 is preferably 200 meshes; combined with Fig.12 As shown, in order to improve the conductivity of the Fanghua film 205, a carbon support film 206, a micro-grid carbon support film or an ultra-thin carbon support film with a thickness ranging from 10 to 20 nm may be sprayed on the surface of the Fanghua film 205.

[0048] It should be noted that the TEM grid of the utility model can be used for multi-region sample preparation, has a good user experience, does not use a complex structure to achieve a simple function, and does not use conventional or simple features for combination or stacking. Therefore, it conforms to the common sense of technological improvement and has certain practicality.

[0049] The contents not described in detail in this specification belong to the prior art known to ordinary technicians in this field, for example, template etching method.

[0050] It should be understood that the above description is only a preferred embodiment of the present invention and is not sufficient to limit the technical solution of the present invention. For ordinary technicians in this field, within the spirit and principles of the present invention, additions, substitutions, changes or improvements can be made according to the above description, and all these additions, substitutions, changes or improved technical solutions should fall within the scope of protection of the claims attached to the present invention.

Claims

1. A TEM grid capable of preparing samples in multiple regions, characterized in that: It consists of an inner ring, an outer ring and a grid area. The grid area is connected between the inner ring and the outer ring. At least two dividing strips are connected between the inner ring and the outer ring to separate the grid area between the inner ring and the outer ring into more than two sample preparation areas.

2. The TEM grid capable of preparing samples in multiple regions according to claim 1, characterized in that: Two dividing strips are connected between the inner ring and the outer ring. The two dividing strips are in a straight line passing through the center of the inner ring, and separate the mesh area between the inner ring and the outer ring into two sample preparation areas of equal area.

3. The TEM grid capable of preparing samples in multiple regions according to claim 1, characterized in that: Three dividing strips are connected between the inner ring and the outer ring. The three dividing strips are located on different straight lines passing through the center of the inner ring, and the angle between adjacent dividing strips is 120°, dividing the grid area between the inner ring and the outer ring into three sample preparation areas of equal area.

4. The TEM grid capable of preparing samples in multiple regions according to claim 1, characterized in that: Four dividing strips are connected between the inner ring and the outer ring. The four dividing strips are located on two straight lines passing through the center of the inner ring in a cross shape, and divide the grid area between the inner ring and the outer ring into four sample preparation areas of equal area.

5. The TEM grid capable of preparing samples in multiple regions according to claim 1, characterized in that: Five dividing strips are connected between the inner ring and the outer ring. The five dividing strips are evenly distributed on different straight lines passing through the center of the inner ring, and the angle between adjacent dividing strips is 72°, dividing the grid area between the inner ring and the outer ring into five sample preparation areas of equal area.

6. The TEM grid capable of preparing samples in multiple regions according to claim 1, characterized in that: Six dividing strips are connected between the inner ring and the outer ring. The six dividing strips are evenly distributed on three straight lines passing through the center of the inner ring, and the angle between adjacent dividing strips is 60°, dividing the grid area between the inner ring and the outer ring into six sample preparation areas of equal area.

7. The TEM grid capable of preparing samples in multiple regions according to claim 1, characterized in that: The separation strip is composed of two parallel connecting lines, and the area between the two connecting lines is a separation zone, which is used to separate different sample preparation areas.

8. The TEM grid capable of preparing samples in multiple regions according to claim 1, characterized in that: The surface of the sample preparation area is coated with a polyvinyl formal film, and the surface of the polyvinyl formal film is sprayed with a carbon support film.

9. The TEM grid capable of preparing samples in multiple regions according to claim 1, characterized in that: The TEM grid is a metal grid and is manufactured by a template etching method.

10. The TEM grid capable of preparing samples in multiple regions according to claim 1, characterized in that: The TEM grid is made of non-metallic material and is produced using a 3D printer.

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