Scanning electron microscope sample stage for deep-sea complex environment corrosion sample and operation method

Abstract

Provided are a scanning electron microscope sample stage for deep-sea complex environment corrosion samples and an operating method. The sample stage comprises a carrier frame and N clamping blocks, with a cuboid containing space comprising sequentially connected first, second, third and fourth side walls; the first and third side walls each have a long strip-shaped guide groove. Each clamping block can be placed in the containing space, and the first and second ends thereof can be respectively slid and fixed in the long strip-shaped guide grooves of the first and third side walls. The N clamping blocks can divide the containing space into N+1 independent sample clamping spaces, and each clamping block can have two clamping surfaces of different shapes, suitable for clamping different samples.

Description

Technical Field

[0001] This application relates to the field of electron microscopy, specifically to a scanning electron microscope sample stage and operating method for corroded samples in complex deep-sea environments. Background Technology

[0002] Deep-sea equipment and engineering structures are subjected to the combined effects of complex environmental factors during service. Localized corrosion damage to their metal components (such as crevice corrosion) often leads to major accidents and huge economic losses. Researching and solving the problem of material corrosion failure in the complex environment of the deep sea is of great significance for ensuring the safe service of deep-sea equipment and engineering structures.

[0003] Scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) are key techniques for obtaining surface morphology and compositional information of samples in corrosion failure studies in complex deep-sea environments. To obtain reliable SEM and EDS results, the following basic conditions must be met: a good and stable electrical connection between the sample and the SEM to avoid image distortion caused by charging effects; stable sample fixation to ensure its position remains unchanged during observation to avoid image drift; and during EDS analysis, the observation surfaces of multiple samples should be at similar heights to ensure that each sample is located near the focal plane with optimal signal intensity (usually within a few millimeters of the microscope pole piece). Excessive height differences between samples can cause some samples to deviate from the optimal detection area, resulting in signal weakening or undetectable signals.

[0004] Conventional scanning electron microscope (SEM) stages have a circular, flat surface, allowing samples to be placed directly or fixed to the stage using conductive adhesive. This is suitable for standardized, regularly shaped samples. However, a significant portion of the samples involved in corrosion failure studies in complex deep-sea environments are electrochemical samples with insulating coatings and external guide wires. These samples also include non-standard slit configurations, U-shaped bends, etc., exhibiting significant differences in size and shape. Conventional detection methods present several problems: For conductive samples with insulating coatings, conventional surface conductive treatments such as carbon deposition or gold sputtering introduce foreign elements that interfere with component analysis and alter the original surface state, affecting subsequent analysis and detection. Furthermore, they result in blurred image details during high-magnification SEM observations. Removing the coating may damage the sample and is a cumbersome process. Using conductive tape to fix samples is prone to drift due to its elasticity; for irregularly shaped samples or those with external guide wires, this method is ineffective, often requiring the external guide wires to be cut, compromising sample integrity and failing to meet the sample reuse requirements of corrosion failure studies in complex deep-sea environments. Conventional operations also cannot ensure that multiple sample surfaces are at similar heights. In addition, existing clamping devices are mostly designed for specific sample types, making it difficult to stably adapt to and simultaneously detect samples of various shapes and sizes on the same platform, resulting in low detection efficiency. Summary of the Invention

[0005] To address the aforementioned problems, this application provides a scanning electron microscope sample stage for corrosion samples from complex deep-sea environments, comprising:

[0006] A platform frame includes sequentially connected first, second, third, and fourth side walls, as well as a bottom and a top surface. The side walls, bottom, and top surfaces form a cuboid-shaped accommodating space. The top surface is open. The first and third side walls are opposite each other, and the second and fourth side walls are opposite each other. Specifically: a long, narrow guide groove is formed on the first side wall, penetrating the side wall in a direction perpendicular to it, and its length direction is parallel to the top surface of the platform frame; a long, narrow guide groove is formed on the third side wall, penetrating the side wall in a direction perpendicular to it, and its length direction is parallel to the top surface of the platform frame, and is parallel to the long, narrow guide groove on the first side wall; and:

[0007] There are N clamping blocks, where N is an integer greater than or equal to 1. Each clamping block is rectangular and has a first end and a second end opposite to each other along its length. It is placed in the receiving space and spans between the first sidewall and the third sidewall. One of its first end and the second end can be slidably engaged with the elongated guide groove of the first sidewall, and the other of its first end and the second end can be slidably engaged with the elongated guide groove of the third sidewall. Each clamping block has a first fastener detachably provided at its first end and the second end. The first fastener is a screw fastener. Each clamping block has a screw hole at its first end and the second end. After the clamping block slides to a predetermined position, the first fastener can pass vertically through the first sidewall guide groove and the third sidewall guide groove from the outside of the first sidewall or the third sidewall and be screwed into the screw hole at the first end and the second end. The clamping block is fixed by the first fastener abutting against the sidewall where the first sidewall guide groove and the third sidewall guide groove are located.

[0008] Specifically, between the inner surfaces of the second and fourth sidewalls, the N clamping blocks can divide the accommodating space into N+1 sample clamping spaces of adjustable size.

[0009] The second sidewall inner surface has a predetermined shape; the fourth sidewall inner surface has a predetermined shape; each clamping block has a first clamping surface and a second clamping surface, the first clamping surface having a predetermined shape and the second clamping surface having a predetermined shape. Through the combination of the second sidewall inner surface and the fourth sidewall inner surface, as well as the first clamping surface and the second clamping surface of each clamping block, it is possible to fasten samples of different shapes.

[0010] In addition, the predetermined shape of the inner surface of the second sidewall includes one of a concave cylindrical surface extending along its height direction, a concave cylindrical surface extending along its lateral direction, a spherical surface, and a plane;

[0011] The predetermined shape of the inner surface of the fourth sidewall includes one of the following: a concave cylindrical surface extending along its height direction, a concave cylindrical surface extending along its lateral direction, a sphere, and a plane.

[0012] In addition, the predetermined shape of the first clamping surface of each clamping block includes one of a concave cylindrical surface extending along its height direction, a concave cylindrical surface extending along its lateral direction, a spherical surface, and a plane;

[0013] The predetermined shape of the second clamping surface of each clamping block includes one of a concave cylindrical surface extending along its height direction, a concave cylindrical surface extending along its lateral direction, a spherical surface, and a plane.

[0014] In addition, the fourth sidewall has one or more through holes perpendicular to the fourth sidewall along the bottom edge direction near the bottom edge, for electrically connecting the outer guide wire of the sample under test, wherein the conductive part of the outer guide wire can make electrical contact with the inner wall of the one or more through holes.

[0015] A predetermined gap is left between the lower edge of each clamping block and the bottom surface of the platform so that the outer guide wire of the sample under test can be led out through the gap via the one or more through holes.

[0016] Additionally, in the fourth sidewall, a vertical screw through-hole is correspondingly provided directly below each of the one or more through holes. One end of the screw through-hole communicates with the corresponding through hole, and the other end extends vertically downward to the bottom surface of the stage. Each screw through-hole is detachably provided with a second fastener. The second fastener can pass through the screw through-hole from bottom to top and abut against the conductive part of the outer guide wire of the sample to ensure its electrical contact with the inner wall of the one or more through holes, so that the sample and the stage can form a stable electrical connection. The second fastener is a screw fastener.

[0017] In addition, the lower surface of the base of the stage is provided with a connecting structure for adapting to the sample holders of different scanning electron microscopes. The connecting structure is at least one of a flat surface, a dovetail groove, or a positioning pin hole.

[0018] In addition, each clamping block is detachably provided with one or more third fasteners, which are screw fasteners. The third fasteners can act on the clamped sample through one or more corresponding screw through holes perpendicular to the clamping surface on the clamping block for further fixing the sample.

[0019] In addition, the platform frame, the clamping block, and each fastener are all made of non-magnetic metal materials.

[0020] According to another aspect of the present invention, a method for operating the above-described scanning electron microscope sample stage for corroded samples in complex deep-sea environments is also provided, characterized by comprising the following steps:

[0021] S1. Depending on the quantity, shape, and size of the sample, select to use a single clamping block to cooperate with the second sidewall or the fourth sidewall to form a clamping space, or use two or more clamping blocks to cooperate relative to each other to form a clamping space;

[0022] S2. Place the sample in the selected clamping space. When there are two or more samples, adjust the height of the sample detection surface to make them basically the same, and slide the clamping block to initially clamp the sample.

[0023] S3. Secure the position of the clamping block using the first fastener;

[0024] S4. For samples that require electrical connection or reinforced fixation, the second fastener or the third fastener may be used selectively for electrical connection and auxiliary fixation.

[0025] S5. The sample stage with the sample installed is then installed into the sample chamber of the scanning electron microscope for testing.

[0026] In addition, for conductive samples with insulating coating and external guide wires, in step S4, the conductive part of the external guide wire is inserted into the through hole of the fourth side wall and fixed by pressing with the second fastener so that the sample is electrically connected to the stage; and before detection, conductive adhesive is used to cover the exposed insulating coating of the sample to protect the scanning electron microscope.

[0027] The above solution solves the problems in existing technologies, such as the inability to perform non-destructive testing on samples with external guide wires and insulating coatings, sample drift, difficulty in fixing the position of irregularly shaped samples, inconsistent sample surface height, and the inability to simultaneously test multiple types of samples, which makes it difficult to perform scanning electron microscopy and energy dispersive spectroscopy quickly and effectively.

[0028] Beneficial effects:

[0029] This invention provides a scanning electron microscope (SEM) sample stage and its operating method for corroded samples in complex deep-sea environments. By fixing the conductive portion of the sample's external guide wire to the stage frame, a good electrical connection is formed between the sample and the SEM via the stage frame, meeting the conductivity requirements of SEM detection, effectively avoiding the charging effect, and supporting the sample to retain its original surface, external guide wire, and insulating coating, achieving non-destructive testing of the sample and meeting the sample reuse requirements for corrosion failure research in complex deep-sea environments. It effectively solves the image drift problem caused by unstable sample fixation during SEM detection. The operating method can stably clamp irregularly shaped samples, ensuring their fixed position. The operating method can easily adjust the positions of multiple samples, ensuring that their detection surface heights are basically consistent, guaranteeing optimal working conditions for energy dispersive spectroscopy (EDS). The operating method can simultaneously and stably install and fix multiple samples of different sizes, shapes, and types on the sample stage, significantly improving detection efficiency and reliability. Attached Figure Description

[0030] To more clearly illustrate the technical solutions in the embodiments of this application or the background art, the accompanying drawings used in the embodiments of this application or the background art will be described below.

[0031] Figure 1 An exploded view of the sample stage of the present invention is shown;

[0032] Figure 2 yes Figure 1 View from direction A;

[0033] Figure 3 The structure of the sample stage of the present invention is shown, wherein a sample with insulating coating and external guide wires is loaded;

[0034] Figure 4 yes Figure 3 View from direction B;

[0035] Figure 5 The structure of the sample stage of the present invention is shown, wherein a sheet-like sample is loaded;

[0036] Figure 6 The structure of the sample stage of the present invention is shown, wherein samples with insulating coating and external guide wires, sheet samples, block samples and filament samples are simultaneously loaded;

[0037] Figure 7 yes Figure 6 The C-direction view;

[0038] Figure 8 The structure of the sample stage of the present invention is shown, wherein the first clamping surface of the clamping block has a predetermined circular groove (concave spherical surface) to accommodate the loaded spherical sample;

[0039] Figure 9 The actual effect of embodiment 3 of the sample stage of the present invention is shown, wherein conductive samples with insulating coating and external guide wires, sheet samples, block samples and irregularly shaped failed samples are loaded simultaneously.

[0040] Figure 10 The following diagram illustrates a comparison between conventional and present invention methods for scanning electron microscopy (SEM) observation of conductive samples with insulating coatings and external leads: (a) is an SEM image of the sample after sputtering gold plating using a conventional sample stage; (b) is... Figure 9 Scanning electron microscope images of the original surface of the corresponding similar samples.

[0041] Wherein: 1-Platform; 1a-Accommodation space; 11-First sidewall; 111-First sidewall guide groove; 12-Second sidewall; 13-Third sidewall; 131-Third sidewall guide groove; 14-Fourth sidewall; 141-Through hole; 142-Screw through hole; 1421-Second fastening screw; 15-Bottom surface; 16-Top surface; 2-Clamping block; 21-First end and second end; 211-Screw hole; 2111-First fastening screw; 22-First clamping surface; 221-Screw through hole; 2211-Third fastening screw; 222-Circular groove (concave spherical surface); 23-Second clamping surface; 3-Conductive sample with insulating coating and external guide wire; 31-External guide wire; 32-Sample detection surface; 4-Thin sheet sample; 5-Block sample; 6-Filament sample; 7-Spherical sample;

[0042] In the attached diagram, the labels consist of multiple digits, read from left to right. The first digit identifies the primary component; subsequent adjacent digits represent the lower-level features of that component; the feature represented by the digit to the right is structurally or logically subordinate to the feature represented by its immediately adjacent digit to the left. Figure 1 For example, label 111 represents the guide groove 111 of the first side wall 11 of the platform 1. Detailed Implementation

[0043] In the following description, exemplary embodiments will be described in more detail with reference to the accompanying drawings, in which the same reference numerals refer to the same elements throughout the drawings. This application may be embodied in a variety of different forms and should not be considered as limited to the embodiments shown herein. Rather, these embodiments are provided as examples so that this application will be sufficient and complete, and will fully convey aspects and features of the invention to those skilled in the art. Unless otherwise stated, the same reference numerals denote the same elements throughout the drawings and written description, and in the drawings, the relative dimensions of elements, layers, and regions may be exaggerated for clarity.

[0044] It will be understood that although the terms "first," "second," etc., may be used herein to describe parts, these parts should not be limited by these terms. Unless otherwise defined, the technical terms used in this application should have the ordinary meaning understood by one of ordinary skill in the art to which this application pertains, and should not be construed as limiting the application.

[0045] The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of this application. As used herein, the singular forms “a,” “an,” and “the” are intended to include the plural forms as well, unless otherwise expressly stated. It will be further understood that, when used herein, the terms “comprising” and “including” describe the presence of stated features, integers, steps, operations, elements, components, and / or combinations thereof, but do not exclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and / or combinations thereof. As used herein, the term “and / or” includes any and all combinations of one or more of the associated listed items. When placed before a list of elements, expressions such as “at least one” modify the entire list of elements, rather than individual elements within that list.

[0046] To make the technical problems solved by this application, the technical solutions adopted, and the technical effects achieved clearer, the technical solutions of the embodiments of this application will be further described in detail below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, and not all embodiments.

[0047] The scanning electron microscope sample stage for corrosion samples in complex deep-sea environments provided by this invention has the following structure for each component: Figures 1 to 2 As shown, it includes a platform frame 1, a clamping block 2, and various fasteners.

[0048] In a specific embodiment of the present invention, the platform 1 is 56mm long, 52mm wide, and 16mm high, and has a accommodating space 1a for placing samples. The accommodating space 1a is 49mm long, 46mm wide, and 15mm deep, and includes a first sidewall 11, a second sidewall 12, a third sidewall 13, a fourth sidewall 14, a bottom surface 15, and a top surface 16 connected in sequence. The first sidewall 11 and the third sidewall 13 are arranged opposite each other, and the second sidewall 12 and the fourth sidewall 14 are arranged opposite each other. Among them, a guide groove 111 with a length of 39mm and a height of 4.2mm is opened on the first sidewall. The guide groove 111 penetrates the sidewall in a direction perpendicular to the first sidewall 11, and its length direction is parallel to the top surface 16. A guide groove 131 with a length perpendicular to the third sidewall 13 is opened on the third sidewall 13. The guide groove 131 penetrates the sidewall in a direction perpendicular to the third sidewall 13, and its length direction is parallel to the top surface 16. It is parallel to the guide groove 111 of the first sidewall and has the same size.

[0049] The clamping block 2 is 45mm long, 10mm high, 3mm thick in the middle, and 6mm thick at both ends. It has a first end and a second end 21 that are opposite each other and the same size along its length. The first end and the second end 21 are 2mm long, 4mm high, and 6mm thick. The clamping block 2 is placed in the receiving space 1a. One of its first end and the second end 21 can be slidably engaged with the first sidewall guide groove 111, and the other of its first end and the second end 21 can be slidably engaged with the third sidewall guide groove 131, so that the clamping block 2 can move along the first sidewall guide groove 111 and the third sidewall guide groove 131. Sliding along the length direction; the first end and the second end 21 of the clamping block 2 are respectively provided with an M3 screw hole 211, and a first fastening screw 2111 is detachably provided in the screw hole 211. After the clamping block 2 slides to the predetermined position, the first fastening screw 2111 can pass vertically through the first side wall guide groove 111 and the third side wall guide groove 131 from the outside of the first side wall 11 and the third side wall 13, and be screwed into the two screw holes 211. The clamping block 2 is fixed by abutting the first fastening screw 2111 against the side wall where the first side wall guide groove 111 and the third side wall guide groove 131 are located.

[0050] In addition, when fixed, the clamping block 2 can also be configured to leave a 5mm gap between its lower edge and the upper surface of the bottom surface 15 of the platform, so that the outer guide wire of the sample can pass through the gap to reach one of the through holes 141 to complete the electrical connection.

[0051] In addition, one or more through holes 141 perpendicular to the fourth sidewall 14 can be provided on the fourth sidewall 14. In this embodiment, there are four through holes 141 with a diameter of 4 mm, a hole center spacing of 11 mm, and a hole center spacing of 4 mm from the lower surface of the bottom surface 15, which are used to electrically connect the outer guide wire of the sample. The conductive part of the outer guide wire 31 can make electrical contact with the inner wall of the multiple through holes 141.

[0052] Directly below the four through holes 141 on the fourth side wall, four M3 screw through holes 142 are provided, perpendicular to and communicating with the through holes 141. The screw through holes 142 are located in the fourth side wall, with the other end extending vertically downward to the lower surface of the stage frame bottom 15. A second fastening screw 1421 is provided in each screw through hole 142, which is screwed upward into the screw through hole 142 to press and fix the sample guide wire inside the through hole 141, ensuring that its conductive part is in electrical contact with the inner wall of the plurality of through holes, so that the sample and the stage frame 1 form a stable electrical connection. The lower surface of the stage frame bottom 15 can be a flat surface structure.

[0053] The inner surface of the second side wall 12 of the stage can be constructed as a concave cylindrical surface extending along its height direction, with a radius of 11 mm. The inner surface of the fourth side wall 14 of the stage is constructed as a plane to more firmly fix the sample to be tested.

[0054] In another embodiment, the inner surfaces of the second sidewall 12 and the fourth sidewall 14 of the platform can be configured into other predetermined shapes. For example, the inner surface of the second sidewall 12 can be a plane, a concave cylindrical surface extending laterally therein, or a spherical surface (including concave spherical surfaces and / or convex spherical surfaces). The inner surface of the fourth sidewall 14 can be a concave cylindrical surface extending along its height direction, a concave cylindrical surface extending laterally therein, or a spherical surface (including concave spherical surfaces and / or convex spherical surfaces). Alternatively, the inner surfaces of both the second sidewall 12 and the fourth sidewall 14 can be planes, or both can be concave cylindrical surfaces, or both can be spherical surfaces (including concave spherical surfaces and / or convex spherical surfaces).

[0055] The clamping block 2 includes a first clamping surface 22 and a second clamping surface 23, wherein the first clamping surface 22 is a plane and the second clamping surface 23 is a concave cylindrical surface extending along its height direction, and the radius of the concave cylindrical surface is 11mm.

[0056] It is easy to understand that, in order to achieve a more secure clamping of the sample, the shapes of the first clamping surface 22 and the second clamping surface 23 included in the clamping block 2 are not limited to planar or concave cylindrical surfaces; other shapes are also possible. For example, for samples with special shapes, one or more clamping blocks can be customized or pre-ordered so that the shape of their clamping surfaces matches the sample to achieve more reliable fixation. For example, the first clamping surface 22 or the second clamping surface 23 may be a concave cylindrical surface, a spherical surface (including concave spherical surfaces and / or convex spherical surfaces), etc., extending laterally.

[0057] One or more screw through holes 221 may be provided on the first clamping surface 22. In this embodiment, four M3 screw through holes 221 with a center-to-center spacing of 8 mm are provided. The four screw through holes 221 may all be located on the same side of the center line in the length direction of the first clamping surface 22, and the distance from the center of each screw through hole 221 to the center line is 2.5 mm. A third fastening screw 2211 can be detachably provided in each screw through hole 221. The third fastening screw 2211 can press the clamped sample through the screw through hole 221 for further fixing of the sample.

[0058] The platform frame 1 and the clamping block 2 can be made of aluminum, and the first fastening screw 2111, the second fastening screw 1421 and the third fastening screw 2211 can all be made of brass.

[0059] The dimensions of the scanning electron microscope (SEM) stage for corroded samples in the above embodiments can be adapted, for example, to the Nak Microbeam FE-1050 SEM. It should be understood that the specific dimensions of the stage can be adjusted accordingly to suit other different SEM models without departing from the design principles of this invention. The scope of protection of this invention is not limited to the specific structures and embodiments listed in the specification.

[0060] Example 1: Fixation of a conductive sample with insulating coating and external conductor

[0061] The scanning electron microscope sample stage of this invention, used for corroded samples in complex deep-sea environments, is used to mount conductive samples with insulating coatings and external leads, such as... Figures 3 to 4 As shown, it includes a platform 1, a clamping block 2, and two conductive samples 3 with insulating coating and external guide wires.

[0062] A clamping block 2 is placed into the receiving space 1a, with its first end and second end 21 inserted into the first side wall guide groove 111 and the third side wall guide groove 131, respectively. The clamping block 2 can slide along the length direction of the guide groove 111 and the guide groove 131. At this time, the second clamping surface 23 of the clamping block 2 is opposite to the second side wall 12 of the platform 1, forming an elongated cylindrical clamping space.

[0063] Place two samples 3 into the clamping space with the detection surface 32 of the sample 3 facing upward and parallel to the top surface 16 of the platform. Insert the conductive part of the outer guide wire 31 of the sample 3 into the through hole 141 of the fourth side wall, and screw the second fastening screw 1421 into the screw through hole 142 to press the outer guide wire 31 and fix it to ensure that the sample 3 and the platform 1 form a stable electrical connection.

[0064] Copper conductive adhesive was used to cover the exposed insulating part on the upper surface of sample 3 to protect the scanning electron microscope; the positions of the two samples 3 were adjusted so that the height difference between the two detection surfaces 32 was less than 1 mm, ensuring that the two detection surfaces 32 were simultaneously within the optimal detection range of the energy spectrum during energy spectroscopy.

[0065] Slide the clamping block 2 along the first sidewall guide groove 111 and the third sidewall guide groove 131, and clamp the two samples 3 with the second clamping surface 23 and the inner sidewall of the second sidewall 12. As before, use two first fastening screws 2111 to fix the clamping block 2 to the platform frame 1. Screw the third fastening screw 2211 into the screw through hole 221 to press the sample 3, thus completing the installation of the sample 3.

[0066] The entire SEM sample stage for the corrosion sample of the complex deep-sea environment, which has been installed with sample 3, is placed into the sample chamber of the SEM for testing.

[0067] Example 2: Fixation of thin-section samples

[0068] The conductive thin-film sample is mounted on the scanning electron microscope sample stage of the present invention for corrosion samples in complex deep-sea environments, such as... Figure 5 As shown, it includes a platform 1, two clamping blocks 2, and a sheet sample 4.

[0069] Two clamping blocks 2 are placed into the receiving space 1a in the same way as in Example 1. At this time, the first clamping surfaces 22 of the two clamping blocks are opposite to each other, forming a cuboid clamping space. The sample 4 is placed into the cuboid clamping space with the test surface of the sample 4 facing upward and parallel to the top surface 16 of the platform.

[0070] The two clamping blocks 2 slide relative to each other along the first side wall guide groove 111 and the third side wall guide groove 131, and clamp the sample 4 with the two first clamping surfaces 22 of the two clamping blocks. The two clamping blocks 2 are fixed to the platform frame 1 in the same way as in Embodiment 1. The third fastening screw 2211 is screwed into the screw through hole 221 to press the sample 4, thus completing the installation of the sample 4.

[0071] The entire SEM sample stage for the corrosion sample in the complex deep-sea environment, with sample 4 already installed, was placed into the sample chamber of the SEM for testing.

[0072] Example 3: Simultaneously fixing samples of different types and sizes

[0073] The scanning electron microscope sample stage of this invention, used for corroded samples in complex deep-sea environments, is used to load conductive samples, sheet samples, block samples, and filamentous samples with insulating coatings and external guide wires, such as... Figures 6 to 7 As shown, it includes a platform 1, two clamping blocks 2, and two conductive samples 3 with insulating coating and external guide wires, a sheet sample 4, a block sample 5, and a filament sample.

[0074] Two clamping blocks 2 are placed into the receiving space 1a in the same way as in embodiment 1; at this time, the clamping block 2 near the second side wall 12 has its second clamping surface 23 facing the second side wall 12 of the platform, forming an elongated cylindrical clamping space; the first clamping surfaces 22 of the two clamping blocks face each other, forming a cuboid clamping space.

[0075] The installation positions and methods of the two samples 3 are the same as those in Example 1.

[0076] The installation positions and methods of samples 4, 5 and 6 are the same as those in Example 2.

[0077] Copper conductive adhesive was used to cover the exposed insulating part on the upper surface of sample 3 to protect the scanning electron microscope; the positions of all samples were adjusted so that the height difference between the detection surfaces of the five samples was less than 1 mm, ensuring that the detection surfaces of the five samples were simultaneously within the optimal detection range of the energy spectrum during energy dispersive spectroscopy; thus, the positioning and installation of multiple samples of different types and sizes on the same sample stage were completed.

[0078] The entire SEM sample stage, containing five samples for corrosion testing in complex deep-sea environments, was placed into the SEM sample chamber for analysis.

[0079] Figure 9 The practical effect of the scanning electron microscope sample stage of the present invention for corrosion samples in complex deep-sea environments is shown in Embodiment 3, wherein samples with insulating coating and external guide wires, sheet samples, block samples and irregularly shaped failed samples are loaded simultaneously.

[0080] Figure 10 The results of scanning electron microscopy (SEM) observations of conductive samples with insulating coatings and external leads, using conventional methods and the method of this invention, are shown. (a) is an SEM image of the sample after sputtering gold plating and placing it on a conventional sample stage; (b) is... Figure 9 Scanning electron microscope (SEM) images of corresponding samples in their original surface condition, obtained using the sample stage of this invention, are shown in the comparison. It is evident that the resolution of the images obtained using the method of this invention is significantly superior to the imaging effect achieved using a conventional sample stage after sputtering gold plating.

[0081] Example 4: Fixing a spherical sample

[0082] Using the scanning electron microscope sample stage of the present invention for corroded samples in complex deep-sea environments, in the case of spherical samples, a circular groove is formed on the first clamping surface of the clamping block to accommodate the loaded spherical sample, such as... Figure 8 As shown, it includes a platform 1, two clamping blocks 2, and two spherical samples 7.

[0083] Here, for clamping spherical samples, the circular groove on the clamping surface plays the same role as the concave spherical surface.

[0084] Four circular grooves 222 with a radius of 2.25 mm and a depth of 1.5 mm are pre-defined on the first clamping surface 22 of the two clamping blocks 2, the center of which coincides with the center of the screw through hole 221.

[0085] Two clamping blocks 2 are placed into the receiving space 1a in the same way as in Example 1. At this time, the first clamping surfaces 22 of the two clamping blocks 2 are opposite each other, and the circular grooves 222 of the two clamping blocks 2 are opposite each other, thus constructing a predetermined clamping space that is suitable for the spherical sample 7.

[0086] Two spherical samples 7 are placed in the predetermined clamping space with their detection surfaces facing upwards; the two clamping blocks 2 slide towards each other along the first side wall guide groove 111 and the third side wall guide groove 131, and clamp the samples 7 with the two circular grooves 222 of the two clamping blocks 2. The two clamping blocks 2 are fixed on the platform frame 1 in the same way as in Example 1; the third fastening screw 2211 is screwed into the screw through hole 221 to press the samples 7, thus completing the installation of the samples 7.

[0087] The entire SEM sample stage for the corrosion sample of the complex deep-sea environment, with sample 7 already installed, was placed into the sample chamber of the SEM for testing.

[0088] In the above examples, the samples are spherical, and the clamping blocks employ a circular groove or a concave spherical surface structure. It can be understood that using the sample stage of this invention, even for samples with special shapes, the purpose of adapting to various sample shapes can be achieved through a simple operation of only customizing the clamping blocks. For example, for some samples, a convex spherical clamping surface can also be used.

[0089] The specific embodiments of the present invention have been described in detail above. However, the present invention is not limited to the above embodiments. Within the scope of knowledge possessed by those skilled in the art, various changes can be made without departing from the spirit of the present invention. Furthermore, the present application has been described illustratively with reference to the accompanying drawings, but is not limited thereto. The drawings show only one embodiment of the present invention. If researchers in the art propose a structural form similar to this technical solution without departing from the spirit of the present invention, it should fall within the protection scope of the present invention.

Claims

1. A scanning electron microscope sample stage for corroded samples in complex deep-sea environments, characterized in that, include: A platform frame includes sequentially connected first, second, third, and fourth side walls, a bottom surface, and a top surface. These side walls, bottom surface, and top surface form a cuboid-shaped accommodating space. The top surface is open. The first and third side walls are positioned opposite each other, as are the second and fourth side walls. Specifically, the first side wall has an elongated guide groove that penetrates the side wall perpendicularly to it, with its length parallel to the top surface of the platform frame. The third side wall also has an elongated guide groove that penetrates the side wall perpendicularly to it, with its length parallel to the top surface of the platform frame and parallel to the elongated guide groove on the first side wall. There are N clamping blocks, where N is an integer greater than or equal to 1. Each clamping block is rectangular and has a first end and a second end opposite to each other along its length. It is placed in the receiving space and spans between the first sidewall and the third sidewall. One of its first end and the second end can be slidably engaged with the elongated guide groove of the first sidewall, and the other of its first end and the second end can be slidably engaged with the elongated guide groove of the third sidewall. Each clamping block has a first fastener detachably provided at its first end and the second end. The first fastener is a screw fastener. Each clamping block has a screw hole at its first end and the second end. After the clamping block slides to a predetermined position, the first fastener can pass vertically through the first sidewall guide groove and the third sidewall guide groove from the outside of the first sidewall or the third sidewall and be screwed into the screw hole at the first end and the second end. The clamping block is fixed by the first fastener abutting against the sidewall where the first sidewall guide groove and the third sidewall guide groove are located. Specifically, between the inner surfaces of the second and fourth sidewalls, the N clamping blocks can divide the accommodating space into N+1 sample clamping spaces of adjustable size. The second sidewall inner surface has a predetermined shape; the fourth sidewall inner surface has a predetermined shape; each clamping block has a first clamping surface and a second clamping surface, the first clamping surface having a predetermined shape and the second clamping surface having a predetermined shape. Through the combination of the second sidewall inner surface and the fourth sidewall inner surface, as well as the first clamping surface and the second clamping surface of each clamping block, it is possible to fasten samples of different shapes. The fourth sidewall has one or more through holes perpendicular to the fourth sidewall along the bottom edge direction near the bottom edge, for electrically connecting the outer guide wire of the sample under test, wherein the conductive part of the outer guide wire can make electrical contact with the inner wall of the one or more through holes; A predetermined gap is left between the lower edge of each clamping block and the bottom surface of the platform so that the outer guide wire of the sample under test can be led out through the gap via the one or more through holes; In the fourth sidewall, a corresponding vertical screw through hole is provided directly below each of the one or more through holes. One end of the screw through hole communicates with the corresponding through hole, and the other end extends vertically downward to the bottom surface of the stage frame. Each screw through hole is detachably provided with a second fastener. The second fastener can pass through the screw through hole from bottom to top and abut against the conductive part of the sample outer guide wire to ensure electrical contact with the inner wall of the one or more through holes, so that the sample and the stage frame form a stable electrical connection. The second fastener is a screw fastener.

2. The scanning electron microscope sample stage according to claim 1, characterized in that: The predetermined shape of the inner surface of the second sidewall includes one of a concave cylindrical surface extending along its height direction, a concave cylindrical surface extending along its lateral direction, a spherical surface, and a plane. The predetermined shape of the inner surface of the fourth sidewall includes one of the following: a concave cylindrical surface extending along its height direction, a concave cylindrical surface extending along its lateral direction, a sphere, and a plane.

3. The scanning electron microscope sample stage according to claim 1, characterized in that: The predetermined shape of the first clamping surface of each clamping block includes one of a concave cylindrical surface extending along its height direction, a concave cylindrical surface extending along its lateral direction, a spherical surface, and a plane. The predetermined shape of the second clamping surface of each clamping block includes one of a concave cylindrical surface extending along its height direction, a concave cylindrical surface extending along its lateral direction, a spherical surface, and a plane.

4. The scanning electron microscope sample stage according to claim 1, characterized in that, The lower surface of the stage frame is provided with a connecting structure for adapting to the sample holders of different scanning electron microscopes. The connecting structure is at least one of a flat surface, a dovetail groove, or a positioning pin hole.

5. The scanning electron microscope sample stage according to claim 1, characterized in that, Each clamping block can be detachably provided with one or more third fasteners, which are screw fasteners. The third fasteners can act on the clamped sample through one or more corresponding screw through holes perpendicular to the clamping surface on the clamping block for further fixing the sample.

6. The scanning electron microscope sample stage according to any one of claims 1-5, characterized in that, The platform, the clamping block, and all the fasteners are made of non-magnetic metal materials.

7. A method for operating a scanning electron microscope sample stage as described in claim 5, characterized in that, Including the following steps: S1. Depending on the quantity, shape, and size of the sample, select to use a single clamping block to cooperate with the second sidewall or the fourth sidewall to form a clamping space, or use two or more clamping blocks to cooperate relative to each other to form a clamping space; S2. Place the sample in the selected clamping space. When there are two or more samples, adjust the height of the sample detection surface to make them basically the same, and slide the clamping block to initially clamp the sample. S3. Secure the position of the clamping block using the first fastener; S4. For samples that require electrical connection or reinforced fixation, the second fastener or the third fastener may be used selectively for electrical connection and auxiliary fixation. S5. The sample stage with the sample installed is then installed into the sample chamber of the scanning electron microscope for testing.

8. The method according to claim 7, characterized in that, For conductive samples with an insulating coating and an external guide wire, in step S4, the conductive portion of the external guide wire is inserted into one or more through holes in the fourth sidewall and secured with the second fastener to form a stable electrical connection between the sample and the stage; and before detection, conductive adhesive is used to cover the exposed insulating coating of the sample to protect the scanning electron microscope.

Images