Sample positioning clamp, sample stage, sample detection device and X-ray electron spectrometer

By designing a sample positioning clamp and a temperature sensing platform, the problems of unstable sample fixation and abnormal temperature detection in X-ray electron spectrometers were solved, achieving stable sample fixation and accurate temperature detection, thus improving the overall efficiency and data reliability of the experiment.

CN114509461BActive Publication Date: 2025-10-28CHINA PETROLEUM & CHEMICAL CORP +1
View PDF 2 Cites 0 Cited by

Patent Information

Application Number
CN202011173635.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2020-10-28
Publication Date
2025-10-28
Estimated Expiration
2040-10-28

AI Technical Summary

Technical Problem

The existing in-situ heating and cooling sample stage of X-ray electron spectrometers presents challenges in sample fixation and temperature measurement, leading to unstable sample fixation and abnormal temperature detection, which affects the accuracy and stability of experimental results.

Method used

A sample positioning clamp was designed, comprising multiple mounting arms and a clamping structure. The sample positioning arms are clamped by pressing and holding the guide plate through the positioning gap to ensure stable fixation of the sample. The accuracy of temperature detection is improved by the elastic clamping plate structure and the temperature sensing platform.

Benefits of technology

This method achieves stable and reliable sample fixation, improves the stability and accuracy of temperature detection, avoids abnormal sample temperature detection, and enhances the overall efficiency and data reliability of the experiment.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN114509461B_ABST
    Figure CN114509461B_ABST
Patent Text Reader

Abstract

This invention relates to the field of sample detection and fixation technology, and discloses a sample positioning clamp, a sample stage, a sample detection device, and an X-ray electron spectrometer. The sample positioning clamp includes multiple mounting arms arranged at intervals and a sample positioning arm connected between adjacent mounting arms. Each of the mounting arms has a clamping structure at one end on the same side of the sample positioning arm. Each clamping structure includes a positioning slot for pressing and clamping a guide plate on a mounting base. The sample positioning arm and the clamping structures on both sides form a sample receiving space. In practical use, this sample positioning clamp can quickly and conveniently fix and position a sample placed on a mounting base, providing a good foundation for sample temperature detection, avoiding abnormal sample temperature detection, and improving the stability and accuracy of sample temperature detection.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] This invention relates to the field of sample detection and fixation technology, specifically to a sample positioning clamp, a sample stage, a sample detection device, and an X-ray electron spectrometer. Background Technology

[0002] X-ray photoelectron spectroscopy (XPS) is a complex, bulky, and expensive instrument specifically designed for testing the chemical information of material surfaces. It can analyze the composition and chemical valence state of sample surfaces and is widely used in metallurgy, corrosion science, adhesive science, ceramics, polymers, microelectronics, semiconductor materials, and various catalyst research. In practical applications, in-situ heating of XPS is often used, requiring an in-situ heated and cooled sample stage. However, the in-situ heated and cooled sample stage has some shortcomings in practical use. For example, in sample fixation, researchers need to use tweezers to hold stainless steel clips and screws to secure the sample, which greatly increases the difficulty and time required, slowing down the overall experimental process. Regarding temperature measurement, to meet the temperature measurement range requirement (-200℃~800℃), a K-type thermocouple is selected as the sensing element. However, the K-type thermocouple integrated into the in-situ heated and cooled sample stage has one of the larger measurement errors among various temperature sensors, and its sensing part is a circular contact, meaning the actual temperature measured is limited to the area contacted by the circular contact.

[0003] In addition, when the sample is in an irregular block shape, the existing stainless steel clips and screws cannot fix it well; when the sample is powder, and the powder sample needs to be pressed into a sample tablet, the stainless steel clips apply force to fix the sample tablet, but because the temperature-sensing circular contact is placed under the sample tablet, the sample tablet is often crushed, resulting in the inability to continue the heating process, and so on.

[0004] Furthermore, when samples are fixed on the in-situ heating / cooling stage for in-situ heating or cooling, problems arise due to improper sample fixation. These problems can cause the temperature-sensing circular contact to slip off the sample, fail to maintain proper contact, or even break under the pressure of the stainless steel clips and the temperature-sensing contact. Ultimately, poor contact between the sample and the thermocouple sensing point leads to abnormal temperature measurements during in-situ heating / cooling, resulting in unreadable temperature values, abrupt temperature increases, or even direct error reports. This makes it impossible for researchers to determine the sample's condition during in-situ processing, casting doubt on the obtained data, and may even interrupt the in-situ processing, causing the entire experiment to fail and requiring a restart, resulting in various forms of waste. Summary of the Invention

[0005] Firstly, the purpose of this invention is to provide a sample positioning clip that can quickly and conveniently fix and position a sample placed on an installation base in practical use, thereby providing a good fixed positioning basis for sample temperature detection, avoiding abnormal sample temperature detection, and improving the stability and accuracy of sample temperature detection.

[0006] To achieve the above objectives, the present invention provides a sample positioning clip, which includes a plurality of mounting arms arranged sequentially at intervals and a sample positioning arm connected between adjacent mounting arms. Each of the mounting arms has a clamping structure at one end on the same side of the sample positioning arm. Each clamping structure includes a positioning slot for pressing and clamping a guide plate positioned on a mounting base. The sample positioning arm and the clamping structures on both sides form a sample receiving space.

[0007] In this technical solution, each of the multiple mounting arms has a clamping structure on the same side of the sample positioning arm. Each clamping structure includes a positioning slot, which is used to press and clamp the sample onto the guide plate on the mounting base. The sample positioning arm and the clamping structures on both sides form a sample receiving space. In actual use, the experimenter can place the sample on the sample stage and clamp each positioning slot of the sample positioning clamp onto the guide plate on both sides of the sample on the sample stage. Then, the experimenter can press the sample positioning clamp downwards, so that the sample positioning arm presses down on the sample. In this way, through the pressing and clamping positioning of the positioning slots of each mounting arm, the experimenter can quickly and conveniently press and reliably fix the sample on the sample stage. This stable and reliable pressing and fixing positioning of the sample can make good contact between the sample and the temperature measuring element, so as to avoid abnormal sample temperature detection and improve the stability and accuracy of sample temperature detection.

[0008] Furthermore, the clamping structure includes clamping plate structures, each of which is arranged in parallel, and each of which includes a sheet-like positioning slot.

[0009] Furthermore, the clamping plate structure is elastic so that it can return to its original shape after the positioning slot is formed.

[0010] Furthermore, one end of the mounting arm is a mounting piece, and a portion of the mounting piece is formed into a suspension piece by a cut. The suspension piece can be flipped open to the side of the mounting piece so that the positioning slot is formed between the side pieces of the mounting piece and the side pieces on both sides of the suspension piece. The suspension piece and the side pieces on both sides form the clamping piece structure.

[0011] Furthermore, the cut is a U-shaped cut and is spaced from all edges of the mounting piece.

[0012] Furthermore, the clamping plate structure includes two clamping plates connected together, which form the positioning gap between them when not subjected to an expansion force, and which can expand the positioning gap when subjected to an expansion force.

[0013] In addition, the sample positioning arm is capable of elastic movement over the distance between the two ends of the mounting arm.

[0014] In addition, the sample positioning arm can be adjusted and positioned to a predetermined position within the distance between the two ends of the mounting arm.

[0015] Furthermore, the mounting arms at both ends of the sample positioning arm are each formed with a plurality of positioning holes spaced apart between the two ends of their respective mounting arms, and the two ends of the sample positioning arm can be selectively connected to the desired positioning holes.

[0016] In addition, the two ends of the sample positioning arm are respectively connected to the mounting arms on both sides via connecting arms. The two ends of the sample positioning arm maintain a distance from the mounting arms on their respective sides, and the sample positioning arm is located between the two ends of the mounting arms.

[0017] Furthermore, the connecting arm includes a horizontal straight arm and a vertical straight arm, wherein,

[0018] One end of the horizontal straight arm is connected to the mounting arm, the other end of the horizontal straight arm is connected to the upper end of the vertical straight arm, and both ends of the sample positioning arm are connected to the lower ends of the vertical straight arms on both sides.

[0019] Furthermore, the vertical straight arm includes multiple arm sections that are sequentially sleeved and can be extended and retracted to the required length, so that the sample positioning arm can be adjusted and positioned to a predetermined position over the distance between the two ends of the mounting arm.

[0020] In addition, the sample positioning clamp includes at least one of the following methods: Method 1: The sample positioning arm includes a sample contact plane for forming surface contact with the sample; Method 2: The sample positioning clamp is a sheet-like component; Method 3: The number of mounting arms is two.

[0021] Secondly, the present invention provides a sample stage, the sample stage including a table surface, wherein a plurality of parallel guide strips are provided on the table surface, and the table surface area between adjacent guide strips includes a sample placement and positioning area, wherein the plurality of guide strips are used to press and clamp the sample positioning arm of the sample positioning clamp at a plurality of spaced-apart mounting arms to maintain the sample placed on the sample placement and positioning area.

[0022] In this technical solution, the sample stage has multiple parallel guide bars arranged at intervals. The area between adjacent guide bars includes a sample placement and positioning area. These guide bars are used to press and clamp the sample positioning arms of the sample positioning clamp at intervals, ensuring that the sample positioning arms of the clamp maintain the sample placed in the sample placement and positioning area. In practical use, the experimenter can place the sample in the sample placement and positioning area, press and clamp each mounting arm of the sample positioning clamp onto its corresponding guide bar, and press the clamp downwards, causing the sample positioning arms to press down on the sample. Through the pressing and clamping positioning between the mounting arms and guide bars, the experimenter can quickly and easily and reliably press and fix the sample in the sample placement and positioning area. This stable and reliable pressing and fixing positioning ensures good contact between the sample and the temperature measuring element, preventing abnormal sample temperature detection and improving the stability and accuracy of sample temperature detection.

[0023] Furthermore, the guide bar is a guide groove that sinks down from the platform.

[0024] Furthermore, the guide strip is a guide piece that extends upward from the platform and is used to clamp and position the sample positioning clamp.

[0025] Furthermore, the outermost guide piece is the edging piece of the outer peripheral surface of the table edge.

[0026] Furthermore, the platform area is provided with a temperature-sensing platform for sensing the detection temperature of the sample, and the temperature-sensing platform includes the sample placement and positioning area.

[0027] Furthermore, the platform area is formed with a receiving groove, and a temperature sensing block is disposed in the receiving groove, with the upper surface of the temperature sensing block serving as the temperature sensing platform.

[0028] Furthermore, the temperature sensing block is disposed within the receiving groove by means of an elastic element; and / or, the temperature sensing block is the temperature sensing element of a platinum resistance thermometer.

[0029] Thirdly, the present invention provides a sample testing device, which includes a sample positioning clamp and a sample stage as described in any of the second aspects above, wherein the sample positioning clamp includes a plurality of spaced mounting arms and a sample positioning arm connected between adjacent mounting arms; the plurality of guide bars can be pressed and clamped with the plurality of mounting arms respectively, so that the sample positioning arm can maintain the position of the sample placed on the sample placement and positioning area.

[0030] As described above, in practical use, the experimenter can place the sample in the sample placement positioning area. Simultaneously, the experimenter can press and hold each mounting arm of the sample positioning clamp onto its corresponding guide strip, and then press the sample positioning clamp downwards, causing the sample positioning arms to press down on the sample. In this way, through the pressing and clamping positioning between the mounting arms and the guide strips, the experimenter can quickly and conveniently and reliably press and fix the sample in the sample placement positioning area. This stable and reliable pressing and fixing positioning of the sample ensures good contact between the sample and the temperature measuring element, avoiding abnormal sample temperature detection and improving the stability and accuracy of sample temperature detection.

[0031] Furthermore, when the sample positioning clamp is held and positioned on the guide strip, it can also move along the extension direction of the guide strip to adjust to the desired position.

[0032] Furthermore, the sample positioning clamp includes a first sample positioning clamp and a second sample positioning clamp, wherein the plurality of mounting arms of the first sample positioning clamp are pressed and clamped in the vertical direction with their respective corresponding guide strips, and the second sample positioning clamp is arranged horizontally, wherein the plurality of mounting arms of the second sample positioning clamp are pressed and clamped in the horizontal direction with their respective corresponding mounting arms of the first sample positioning clamp, so that the first sample positioning clamp is used for vertical positioning of the sample, and the second sample positioning clamp is used for horizontal positioning of the sample.

[0033] Alternatively, the sample positioning clip may be any of the sample positioning clips described in the first aspect above.

[0034] Fourthly, the present invention provides an X-ray electron spectrometer, which includes any of the sample detection devices described in the third aspect above. Thus, through the sample detection device, the overall quality of the X-ray electron spectrometer is effectively improved. Attached Figure Description

[0035] Figure 1 This is a schematic diagram of the structure of a sample positioning clip provided in a specific embodiment of the present invention;

[0036] Figure 2 yes Figure 1A side view of the sample positioning clip;

[0037] Figure 3 yes Figure 1 Another side view of the sample positioning clamp structure;

[0038] Figure 4 This is a schematic diagram of a positioning slot of a sample positioning clamp provided in a specific embodiment of the present invention;

[0039] Figure 5 This is a schematic diagram of another structure of the positioning slot of a sample positioning clamp provided in a specific embodiment of the present invention;

[0040] Figure 6 This is a schematic diagram of the mounting arm of a sample positioning clamp provided in a specific embodiment of the present invention;

[0041] Figure 7 This is a top view of a sample stage according to a specific embodiment of the present invention;

[0042] Figure 8 This is a schematic diagram of the viewing structure of a sample stage provided in a specific embodiment of the present invention;

[0043] Figure 9 This is a schematic diagram of another sample stage viewing structure provided in a specific embodiment of the present invention;

[0044] Figure 10 This is a schematic diagram of the structure in which two sample positioning clamps are perpendicularly clamped to each other, according to a specific embodiment of the present invention;

[0045] Figure 11 This is a schematic diagram of a sample positioning clamp pressing and fixing a sample on a sample stage, provided by a specific embodiment of the present invention;

[0046] Figure 12 This is a test spectrum of a carbon-based supported catalyst sample from the prior art, after being fixed on an in-situ heated sample stage.

[0047] Figure 13 This is a test spectrum of the carbon-based supported catalyst sample of the present invention after it was fixed on an in-situ heated sample stage.

[0048] Explanation of reference numerals in the attached figures

[0049] 1- Mounting arm, 2- Sample positioning arm, 3- Positioning slot, 4- Sample receiving space, 5- Clamping plate structure, 6- Mounting plate, 7- Cut slit, 8- Suspension plate, 9- Side plate, 10- Clamping plate, 11- Positioning hole, 12- Connecting arm, 13- Horizontal straight arm, 14- Vertical straight arm, 15- Sample contact plane, 16- Platform, 17- Guide strip, 18- Platform area, 19- Sample placement and positioning area, 20- Guide plate, 21- Edge banding plate, 22- Receiving groove, 23- Temperature sensing block, 24- Elastic element, 25- Temperature sensing platform, 26- First sample positioning component, 27- Second sample positioning clamp, 28- Guide groove, 29- Sample. Detailed Implementation

[0050] The specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings. It should be understood that the specific embodiments described herein are for illustration and explanation only and are not intended to limit the present invention.

[0051] In a first aspect, the present invention provides a sample positioning clip, with reference to Figures 1-5 The four embodiments of the sample positioning clamp include a plurality of mounting arms 1 arranged sequentially at intervals and a sample positioning arm 2 connected between adjacent mounting arms 1. Each of the mounting arms 1 has a clamping structure at one end on the same side of the sample positioning arm 2. Each clamping structure includes a positioning slot 3, which is used to press and clamp the guide plate positioned on the mounting base. The sample positioning arm 2 and the clamping structures on both sides form a sample receiving space 4.

[0052] In this technical solution, multiple mounting arms have clamping structures at one end on the same side of the sample positioning arm. Each clamping structure includes a positioning slot, which is used to press and clamp the sample onto the guide plate on the mounting base. The sample positioning arm and the clamping structures on both sides form a sample receiving space. In actual use, the experimenter can place the sample on the sample stage surface and clamp each positioning slot of the sample positioning clamp onto the guide plates on both sides of the sample on the sample stage surface. The experimenter then presses down on the sample positioning clamp, causing the sample positioning arm to press down on the sample. Through the pressing and clamping positioning of the positioning slots of each mounting arm, the experimenter can quickly and conveniently and reliably press and fix the sample onto the sample stage surface. This stable and reliable pressing and fixing positioning of the sample ensures good contact between the sample and the temperature measuring element, avoiding abnormal sample temperature detection and improving the stability and accuracy of sample temperature detection. Figure 12 and Figure 13 .

[0053] Additionally, the guide plate on the mounting base can be a guide plate on the sample stage surface, and / or, the guide plate on the mounting base can be a mounting arm of another sample clamp. For example, the sample positioning clamp can be set on a guide plate on the mounting base, such as the sample stage surface. Furthermore, if needed, multiple sample positioning clamps can be used in combination. For example, multiple mounting arms of the first sample positioning clamp 26 can be vertically pressed and clamped with their respective corresponding guide bars 17, while the second sample positioning clamp 27 is horizontally arranged, with multiple mounting arms of the second sample positioning clamp 27 horizontally pressed and clamped with their respective corresponding mounting arms of the first sample positioning clamp 26. This allows the first sample positioning clamp 26 to be used for vertical sample positioning, and the second sample positioning clamp 27 to be used for horizontal sample positioning. This combination of sample positioning clamps can effectively fix and position irregularly shaped samples.

[0054] Furthermore, the clamping structure in this sample positioning clamp can have various structural forms. For example, in one form of the clamping structure, the positioning arm 2 can be a cylinder or a rod, with an axial slit formed on the front end face of the cylinder or rod, which can serve as a positioning slot 3. Alternatively, in another form of the clamping structure, one end of the positioning arm 2 includes two clamping rods rotatably connected together to form a clamping structure. A torsion spring is provided between the two clamping rods. Squeezing the two clamping rods will cause them to open to form the positioning slot 3, and releasing them will cause them to return to their original position under the action of the torsion spring. Or, in yet another form of the clamping structure, refer to... Figure 1-5 The clamping structure includes clamping plate structures 5, which are arranged in parallel. Each clamping plate structure 5 includes a sheet-like positioning slot 3. For example, the clamping structure is formed as a sheet-like structure, so that the positioning slot 3 is formed as a sheet-like slot. In this way, the sheet-like positioning slot 3 can increase the contact area with the guide plate of the mounting base, so that a clamping mating surface is formed between the positioning slot 3 and the guide plate, thereby making the pressing clamping and positioning of the sample positioning clamp and the guide plate more stable and reliable.

[0055] In addition, to improve the clamping and positioning stability of the sample positioning clamp and the guide plate of the mounting base, the clamping plate structure 5 is further made elastic so that it can return to its original shape after the positioning gap 3 is formed. In this way, after the positioning gap 3 and the guide plate are clamped, the clamping plate structure can clamp the guide plate more tightly under the action of elastic force, which can further improve the clamping and positioning stability between the clamping plate structure 3 and the guide plate.

[0056] Of course, the positioning gap 3 can be formed in various structural forms. For example, in one structural form of forming the positioning gap 3, refer to... Figure 1 and Figure 2One end of the mounting arm 1 is a mounting piece 6, that is, one end of the mounting arm 1 is a plate-shaped end. A portion of the mounting piece 6 is formed into a suspension piece 8 through a slit 7. The suspension piece 8 can be flipped open to the side of the mounting piece 6, for example, flipped open to the outside. Figure 1 The position indicated by the dotted line is such that a positioning slot 3 is formed between the side pieces 9 on both sides of the suspension piece 8 and the mounting piece 6, forming a clamping structure 5. In use, the suspension piece 8 is flipped to the side to form the positioning slot 3, and then the positioning slot 3 is pressed onto the guide piece. The pressing depth between the positioning slot 3 and the guide piece can be controlled as needed until the sample positioning arm 2 of the sample positioning clamp presses against the sample to fix the sample from top to bottom. When the sample positioning clamp is pulled out, causing the positioning slot 3 to separate from the guide piece, the suspension piece 8 may not return to its original position, or it may elastically return to its initial position, for example, returning to the initial position where the surface of the suspension piece 8 and the surface of the side pieces 9 are flush, for future use. Alternatively, after a portion of the mounting piece 6 is formed into a suspension piece 8 through the slit 7, the suspension piece 8 can be flipped open to a certain angle to the side of the mounting piece 6 to be in the initial position of forming a pre-slit, so that the pre-slit can be directly pressed onto the guide piece during use.

[0057] Alternatively, the cut 7 can begin from the front end face of the mounting piece 6, or the cut 7 can be spaced apart from the edges of the mounting piece 6, for example, refer to Figure 3 The cut 7 is a U-shaped cut and maintains a distance from all edges of the mounting piece 6. This allows the side pieces 9 on both sides of the suspension piece 8 to be connected together via the front ends of the mounting piece 6, thereby improving the stability of the side pieces 9 on both sides of the suspension piece 8 and making the positioning gap 3 formed by the suspension piece 8 and the side pieces 9 on both sides more stable and reliable. It should be noted that the two opposing vertical edges of the U-shaped cut can be parallel to each other or inclined to each other, for example, in... Figure 3 In the graphical interface, the upper gap between the two opposite vertical seam edges of the U-shaped cut is greater than the lower gap, or the upper gap is less than the lower gap.

[0058] For example, in another structural form that forms the positioning slot 3, refer to Figure 3 and Figure 4 The two structures shown include a clamping plate structure 5 comprising two clamping plates 10 connected together. When not subjected to an expansion force, the initial position of the two clamping plates 10 forms a positioning gap 3 between them. When subjected to an expansion force, the positioning gap 3 expands. Alternatively, the two clamping plates 10 may not return to their original position, or they may elastically return to their initial position for future use.

[0059] Alternatively, the sample positioning arm 2 may be non-elastic. Or, alternatively, the sample positioning arm 2 may be elastically movable within the distance between the two ends of the mounting arm 1. This allows the sample positioning clamp to press and hold the sample onto the guide plate, and then further press, causing the sample positioning arm 2 to undergo a certain degree of elastic deformation. This elastic deformation increases the pressing and fixing force of the sample positioning arm 2 on the sample without crushing or cracking it. In one embodiment, the sample positioning arm 2 itself may be an elastic arm, for example, a rubber sheet arm with a certain degree of hardness. Of course, other methods can be used to enable the sample positioning arm 2 to elastically move within the distance between the two ends of the mounting arm 1; these other methods will be described below.

[0060] In addition, to enable the sample positioning clamp to be used for fixing and positioning samples of different sizes, in one embodiment, the sample positioning arm 2 can be adjusted and positioned to a predetermined position based on the distance between the two ends of the mounting arm 1. Thus, before fixing and positioning the sample, the sample positioning arm 2 can be adjusted to the required predetermined position according to the size of the sample to meet the pressing and fixing positioning requirements of samples of different sizes.

[0061] Of course, the ability of "sample positioning arm 2 to be positioned at a predetermined location within the distance between the two ends of mounting arm 1" can be achieved through various adjustment methods. For example, in one adjustment method, referencing... Figure 6 The sample positioning arm 2 has multiple positioning holes 11 spaced apart at both ends of its mounting arms 1. Each end of the sample positioning arm 2 can be selectively connected to a desired positioning hole 11. Thus, by mounting the sample positioning arm 2 from one positioning hole to another, it can be adjusted to a predetermined position. Alternatively, the sample positioning arm 2 can also be elastically moved within the distance between the two ends of the mounting arms 1 at each predetermined position. Other adjustment methods will be described below.

[0062] Additionally, in this sample positioning clamp, both ends of the sample positioning arm 2 can be directly connected to the mounting arms 1 on both sides. Alternatively, refer to... Figure 1 The two ends of the sample positioning arm 2 are connected to the mounting arms 1 on both sides via connecting arms 12. The two ends of the sample positioning arm 2 maintain a distance from their respective mounting arms 1, and the sample positioning arm 2 is positioned between the two ends of the mounting arms 1. This allows the sample positioning arm 2 to more easily abut against the sample via the connecting arms 12.

[0063] Alternatively, the connecting arm 12 may be elastic. Alternatively, the connecting arms 12 at both ends may be selectively connected to the desired positioning holes 11 of their respective mounting arms 1, so that the sample positioning arm 2 can be adjusted and positioned to a predetermined position over the distance between the two ends of the mounting arm 1.

[0064] Of course, the connecting arm 12 can be of various types. For example, the connecting arm 12 can be an inclined arm that extends downward at an angle toward the middle of the gap between the two mounting arms 1. Or, as... Figure 1 As shown, the connecting arm 12 includes a horizontal straight arm 13 and a vertical straight arm 14. One end of the horizontal straight arm 13 is connected to the mounting arm 1, and the other end of the horizontal straight arm 13 is connected to the upper end of the vertical straight arm 14. Both ends of the sample positioning arm 2 are connected to the lower ends of the two vertical straight arms 14 respectively. In this way, the two horizontal straight arms 13 allow the sample positioning arm 2 to be located in the middle of the interval between the two mounting arms 1, while the two vertical straight arms 14 allow the sample positioning arm 2 to be located in the middle of the mounting arm 1 or close to the clamping structure of the mounting arm 1.

[0065] Additionally, the horizontal straight arms 13 at both ends can be elastic, allowing the sample positioning arm 2 to move elastically within the distance between the two ends of the mounting arm 1. Furthermore, the horizontal straight arms 13 at both ends can be mounted from a positioning hole at one position to a positioning hole at another position, allowing the sample positioning arm 2 to be adjusted to a predetermined position.

[0066] Alternatively, the vertical straight arm 14 may include a plurality of arm segments that are sequentially fitted and extendable to a desired length, so that the sample positioning arm 2 can be adjusted and positioned at a predetermined position within the distance between the two ends of the mounting arm 1. In this way, by extending and retracting the arm segments and holding them at the desired length, the sample positioning arm 2 can be adjusted and positioned at a predetermined position within the distance between the two ends of the mounting arm 1.

[0067] In addition, the sample positioning clamp includes at least one of the following methods: Method 1: The sample positioning arm 2 includes a sample contact plane 15 for forming surface contact with the sample. This increases the contact area between the sample positioning arm 2 and the sample through the sample contact plane 15, making the sample easier to fix and position, and preventing it from being crushed or cracked; Method 2: (Refer to...) Figure 1 and Figure 2 The sample positioning clamp is a sheet-like component, for example, it can be formed by bending a stainless steel strip. Figure 1 and Figure 2 The structure shown can be formed by cutting slits to create the suspension piece 8; alternatively, it can also be formed by injection molding of plastic material. Figure 1 and Figure 2The sheet-shaped sample positioning clip shown; Method 3: The number of mounting arms 1 is two, or the number of mounting arms 1 can be three or four, and adjacent mounting arms 1 are connected by sample positioning arms 2.

[0068] Secondly, the present invention provides a sample stage, with reference to Figure 7 The sample stage includes a tabletop 16, on which multiple parallel guide bars 17 are arranged at intervals. The tabletop area 18 between adjacent guide bars 17 includes a sample placement and positioning area 19. The multiple guide bars 17 are used to press and clamp the sample positioning arm of the sample positioning clamp at intervals so that the sample positioning arm of the sample positioning clamp maintains the position of the sample placed on the sample placement and positioning area 19.

[0069] In this technical solution, the sample stage has multiple parallel guide bars arranged at intervals. The area between adjacent guide bars includes a sample placement and positioning area. These guide bars are used to press and clamp the sample positioning arms of the sample positioning clamp at intervals, ensuring that the sample positioning arms of the clamp maintain the sample positioned in the sample placement and positioning area. In practical use, the experimenter can place the sample in the sample placement and positioning area, press and clamp each mounting arm of the sample positioning clamp onto its corresponding guide bar, and press down on the clamp, causing the positioning arms to press down on the sample. Through the pressing and clamping positioning between the mounting arms and guide bars, the experimenter can quickly and easily and reliably press and fix the sample in the sample placement and positioning area. This stable and reliable pressing and fixing positioning ensures good contact between the sample and the temperature measuring element, preventing abnormal sample temperature detection and improving the stability and accuracy of sample temperature detection. Figure 12 and Figure 13 .

[0070] In this sample stage, the guide bar 17 can have various structural types. For example, in one structural type, the guide bar 17 is a guide groove 28 that sinks down from the stage surface. (Refer to...) Figure 8 The dotted lines in the diagram represent the guide grooves. Each side may have one guide groove 28 or multiple guide grooves spaced apart. In this way, the mounting arm of the sample positioning clamp can be pressed and inserted into the guide groove 28, and the guide groove 28 clamps and positions the mounting arm to press and hold the sample positioning clamp in the guide groove 28.

[0071] Alternatively, in another structural type of guide strip 17, guide strip 17 is a guide piece 20 extending upward from the table surface for clamping and positioning with the positioning slot of the sample positioning clamp. Each side may have one guide piece 20 or multiple guide pieces arranged at intervals. In this way, the positioning slot of the mounting arm of the sample positioning clamp can be pressed and inserted into the guide piece 20, forming a clamping and positioning mechanism to press and hold the sample positioning clamp onto the guide piece 20.

[0072] Of course, guide grooves 28 and guide plates 20 can be formed on the sample stage to facilitate the pressing, clamping and positioning of sample positioning clips with different structures.

[0073] In addition, the outermost guide piece is the edge banding piece 21 on the outer periphery of the edge of the platform 16. In this way, the edge banding piece 21 not only protects the edge of the sample stage, but also presses and clamps it with the positioning slot for positioning.

[0074] Furthermore, to improve the accuracy and comprehensiveness of sample temperature detection, in one embodiment, a reference is used. Figure 7 , Figure 8 and Figure 9 The platform area 18 is provided with a temperature-sensing platform 25 for sensing the detection temperature of the sample. The temperature-sensing platform 25 includes a sample placement and positioning area 19. In this way, samples, such as sheet-like samples or irregularly shaped samples, can be placed on the temperature-sensing platform 25, so that a temperature-sensing surface contact is formed between the sample and the temperature-sensing platform 25. For example, sheet-like samples form a temperature-sensing surface contact with the temperature-sensing platform 25, and irregularly shaped samples will form a temperature-measuring contact with the temperature-sensing platform 25 regardless of their placement. Therefore, the accuracy and comprehensiveness of sample temperature detection can be improved more effectively.

[0075] Of course, the temperature sensor can be fixedly mounted on the surface of the tabletop area 18. Or, refer to... Figure 8 and Figure 9 The platform area 18 has a receiving groove 22, and a temperature sensing block 23 is disposed in the receiving groove 22. The upper surface of the temperature sensing block 23 serves as the temperature sensing platform 25. In this way, by limiting the temperature sensing block 23 through the receiving groove 22, it can be ensured that the sample can be stably and reliably fixed and positioned on the upper surface of the temperature sensing block 23 by the sample positioning clamp.

[0076] Or, refer to Figure 8The temperature-sensing block 23 is positioned within the receiving groove 22 via an elastic element 24, such as a spring or elastic pad. After the sample positioning clamp presses and positions itself on the guide plate to contact the sample, it can be further pressed, causing the elastic element 24 to undergo a certain elastic deformation. This elastic deformation increases the pressing and fixing force of the sample positioning arm 2 on the sample without crushing or cracking it. Alternatively, the temperature-sensing block 23 can be the temperature-sensing block of any type of temperature measuring device. For example, the temperature-sensing block 23 can be the temperature-sensing element of a platinum resistance thermometer. In this way, by using a platinum resistance thermometer, while increasing the temperature-sensing contact area and reducing temperature measurement error, the platinum resistance thermometer can overcome the shortcomings of existing K-type thermocouples with large temperature measurement errors and S-type thermocouples with small temperature measurement errors only above 300℃ and inability to measure low temperatures. It retains the integrated characteristics of temperature measurement and control. Therefore, the platinum resistance thermometer can be used to meet the temperature measurement needs of samples below 300℃.

[0077] Thirdly, the present invention provides a sample detection device, which includes a sample positioning clamp and a sample stage as described in any of the second aspects above. The sample positioning clamp includes a plurality of spaced-apart mounting arms and a sample positioning arm connected between adjacent mounting arms. Multiple guide bars 17 can be pressed and clamped to the plurality of mounting arms for positioning, so that the sample positioning arm can maintain the position of the sample 29 placed on the sample placement and positioning area 19. (Refer to...) Figure 11 One embodiment is shown.

[0078] As described above, in practical use, the experimenter can place the sample in the sample placement area. Simultaneously, the experimenter can press and hold each mounting arm of the sample positioning clamp onto its corresponding guide strip, and then press the sample positioning clamp downwards, causing the sample positioning arms to press down on the sample. In this way, through the pressing and clamping positioning between the mounting arms and the guide strips, the experimenter can quickly and conveniently and reliably press and fix the sample in the sample placement area. This stable and reliable pressing and fixing positioning of the sample ensures good contact between the sample and the temperature measuring element, avoiding abnormal sample temperature detection and improving the stability and accuracy of sample temperature detection. (Reference) Figure 12 and Figure 13 .

[0079] Additionally, the guide bar 17 can have any desired extension length, so that when the sample positioning clip is clamped and positioned on the guide bar 17, it can also be moved and adjusted to the desired position along the extension direction of the guide bar 17. This allows the sample positioning clip to be moved along the guide bar to the desired position for pressing and clamping the sample at different locations.

[0080] Furthermore, in this sample detection device, multiple sample positioning clamps can be used in combination, for example, reference Figure 10 The sample positioning clamps include a first sample positioning clamp 26 and a second sample positioning clamp 27. The multiple mounting arms of the first sample positioning clamp 26 are vertically pressed and clamped to their respective corresponding guide strips 17 for positioning. The second sample positioning clamp 27 is horizontally arranged, and its multiple mounting arms are horizontally pressed and clamped to their respective corresponding mounting arms of the first sample positioning clamp 26 for positioning. This allows the first sample positioning clamp 26 to be used for vertical positioning of the sample, and the second sample positioning clamp 27 to be used for horizontal positioning of the sample. This combination of sample positioning clamps can effectively fix and position irregularly shaped samples. For example, using two sample positioning clamps arranged at 90° intervals can define the range of irregularly shaped samples from the side. Furthermore, because the temperature-sensing contact surface of the irregularly shaped platinum resistance thermometer is large, fixing the sample within the range of the temperature-sensing surface can improve the testing effect of carbon-based supported catalyst samples during in-situ heating and cooling on a sample stage. This can be compared with reference... Figure 12 and Figure 13 .

[0081] Furthermore, the sample positioning clamp in this sample testing device can be of various types, which can be selected according to the guide strip 17 on the sample stage. For example, the guide strip 17 is a guide groove 28, and one end of the mounting arm of the sample positioning clamp can be an insert without a positioning slot 3. Alternatively, the sample positioning clamp can be any of the sample positioning clamps described in the first aspect above.

[0082] In another embodiment, a trimetallic TiZrV oxide sample used in the aerospace field is typically a sheet-like metal sample. When fixed on an in-situ heating and cooling sample stage using existing clamps, the thermocouple contacts are small and slippery for the sheet-like sample. During heating, the sample often experiences poor contact, resulting in unreadable temperature values ​​or abrupt temperature increases, due to accidental slippage of the thermocouple contacts. This affects the overall multi-stage in-situ heating process. Using the sample detection device of this application, the sheet-like sample is positioned using a sample positioning clamp and guide strip 17, and then directly pressed onto the sensing surface 25, such as the sensing element of a shaped platinum resistance thermometer. This reduces the occurrence of poor contact leading to unreadable temperature values ​​or abrupt temperature increases, optimizing the temperature difference during vacuum heating from ±10℃ to ±3℃, and the temperature error during constant temperature from ±5℃ to ±1℃.

[0083] In another embodiment, ordinary powdered samples need to be pressed into sheets to be fixed on the in-situ heating and cooling stage. Using existing clamps to hold the sample sheet and thermocouple contacts can sometimes cause the sample to break during or after in-situ processing due to excessive fixing force or uneven sample stress, making further XPS testing impossible. With the sample testing device of this application, after positioning by the sample positioning clamp and guide strip 17, the metal sheet sample is directly pressed onto the temperature sensing surface 25, such as the sensing element of a shaped platinum resistance thermometer. This ensures that the sample sheet is no longer subjected to force at a single point, but rather to a small area with uniform force. The large area of ​​the shaped platinum resistance thermometer's sensing element provides a large contact area with the pressed powder sheet sample, resulting in uniform force distribution. This reduces the probability of sample breakage during in-situ processing and also allows for more uniform heating or cooling, leading to better results.

[0084] Fourthly, the present invention provides an X-ray electron spectrometer, which includes any of the sample detection devices described in the third aspect above. Thus, through the sample detection device, the overall quality of the X-ray electron spectrometer is effectively improved.

[0085] The preferred embodiments of the present invention have been described in detail above; however, the present invention is not limited thereto. Within the scope of the inventive concept, various simple modifications can be made to the technical solutions of the present invention, including combinations of various technical features in any other suitable manner. These simple modifications and combinations should also be considered as the content disclosed in the present invention and are all within the protection scope of the present invention.

Claims

1. A sample positioning clamp, characterized in that, The sample positioning clamp is used for X-ray electron spectroscopy testing. The sample positioning clamp includes a plurality of mounting arms (1) arranged sequentially at intervals and sample positioning arms (2) connected between adjacent mounting arms (1). Each of the multiple mounting arms (1) has a clamping structure at one end located on the same side of the sample positioning arm (2), and each clamping structure includes a positioning slot (3), which is used to press and clamp the guide piece positioned on the mounting base; The sample positioning arm (2) and the clamping structures on both sides form a sample receiving space (4). The clamping structure includes clamping plate structures (5), each of the clamping plate structures (5) is arranged in parallel, and each of the clamping plate structures (5) includes a sheet-like positioning slot (3). One end of the mounting arm (1) is a mounting piece (6), and a portion of the mounting piece (6) is formed into a suspension piece (8) through a slit (7). The suspension piece (8) can be flipped open to the side of the mounting piece (6) so that the positioning slot (3) is formed between the suspension piece (8) and the side pieces (9) of the mounting piece (6) located on both sides of the suspension piece (8). The suspension piece (8) and the side pieces (9) on both sides form the clamping piece structure (5). The mounting arms (1) at both ends of the sample positioning arm (2) are respectively formed with a plurality of positioning holes (11) arranged at intervals between the two ends of the respective mounting arms. The two ends of the sample positioning arm (2) can be selectively connected to the desired positioning holes (11). The two ends of the sample positioning arm (2) are respectively connected to the mounting arms (1) on both sides via connecting arms (12), wherein the two ends of the sample positioning arm (2) maintain a distance from the mounting arms (1) on their respective sides, and the sample positioning arm (2) is located between the two ends of the mounting arms (1). The connecting arm (12) includes a horizontal straight arm (13) and a vertical straight arm (14), wherein one end of the horizontal straight arm (13) is connected to the mounting arm (1), the other end of the horizontal straight arm (13) is connected to the upper end of the vertical straight arm (14), and both ends of the sample positioning arm (2) are connected to the lower ends of the vertical straight arms (14) on both sides respectively.

2. The sample positioning clamp according to claim 1, characterized in that, The clamping plate structure (5) is elastic so that it can return to its original shape after the positioning gap (3) is formed.

3. The sample positioning clamp according to claim 1, characterized in that, The cut (7) is a U-shaped cut and is spaced from all edges of the mounting piece (6).

4. The sample positioning clamp according to claim 1, characterized in that, The clamping plate structure (5) includes two clamping plates (10) connected together, which form the positioning gap (3) between the two clamping plates (10) when not subjected to an expansion force, and which can expand the positioning gap (3) when subjected to an expansion force.

5. The sample positioning clamp according to any one of claims 1-4, characterized in that, The sample positioning arm (2) is capable of elastic movement over the distance between the two ends of the mounting arm (1).

6. The sample positioning clamp according to any one of claims 1-4, characterized in that, The sample positioning arm (2) can be adjusted to a predetermined position over the distance between the two ends of the mounting arm (1).

7. The sample positioning clamp according to claim 1, characterized in that, The vertical straight arm (14) includes multiple arm sections that are sequentially fitted and can be extended and retracted to the required length, so that the sample positioning arm (2) can be adjusted and positioned at a predetermined position at the distance between the two ends of the mounting arm (1).

8. The sample positioning clamp according to claim 1, characterized in that, The sample positioning clip includes at least one of the following methods: Method 1: The sample positioning arm (2) includes a sample contact plane (15) for contacting the sample forming surface; Method 2: The sample positioning clamp is a sheet-like component; Method 3: The number of mounting arms (1) is two.

9. A sample stage, characterized in that, The device includes a tabletop (16) with multiple parallel guide strips (17) spaced apart. The tabletop area (18) between adjacent guide strips (17) includes a sample placement positioning area (19). The multiple guide strips (17) are used to press and clamp the sample positioning clamp with the mounting arm (1) of the sample positioning clamp according to any one of claims 1-8 so that the sample positioning arm (2) maintains the position of the sample placed on the sample placement positioning area (19).

10. The sample stage according to claim 9, characterized in that, The guide strip (17) is a guide groove (28) that sinks down from the platform.

11. The sample stage according to claim 9, characterized in that, The guide strip (17) is a guide piece (20) that extends upward from the table surface and is used to clamp and position the sample positioning clamp.

12. The sample stage according to claim 11, characterized in that, The outermost guide piece is the edging piece (21) of the outer periphery of the edge of the table (16).

13. The sample stage according to any one of claims 9-12, characterized in that, The platform area (18) is provided with a temperature-sensing platform (25) for sensing the detection temperature of the sample, and the temperature-sensing platform (25) includes the sample placement and positioning area (19).

14. The sample stage according to claim 13, characterized in that, The platform area (18) has a receiving groove (22), and a temperature sensing block (23) is provided in the receiving groove (22). The upper surface of the temperature sensing block (23) serves as the temperature sensing platform (25).

15. The sample stage according to claim 14, characterized in that, The temperature sensing block (23) is disposed in the receiving groove (22) by means of an elastic element (24); and / or, the temperature sensing block (23) is the temperature sensing element of a platinum resistance thermometer.

16. A sample testing device, characterized in that, Includes the sample positioning clamp according to any one of claims 1-8 and the sample stage according to any one of claims 9-15, wherein, The multiple guide bars (17) can be pressed and clamped to position the multiple mounting arms (1) respectively, so that the sample positioning arm (2) can maintain the position of the sample (29) placed on the sample placement positioning area (19).

17. The sample detection device according to claim 16, characterized in that, When the sample positioning clip is clamped and positioned on the guide strip (17), it can also move along the extension direction of the guide strip (17) to adjust to the desired position.

18. The sample detection device according to claim 16, characterized in that, The sample positioning clamp includes a first sample positioning clamp (26) and a second sample positioning clamp (27). The multiple mounting arms of the first sample positioning clamp (26) are pressed and clamped in the vertical direction with their respective corresponding guide strips (17). The second sample positioning clamp (27) is arranged horizontally. The multiple mounting arms of the second sample positioning clamp (27) are pressed and clamped in the horizontal direction with their respective corresponding mounting arms of the first sample positioning clamp (26), so that the first sample positioning clamp (26) is used for vertical positioning of the sample and the second sample positioning clamp (27) is used for horizontal positioning of the sample.

19. An X-ray photoelectron spectrometer, characterized in that, Includes the sample detection device according to any one of claims 16-18.

Citation Information

Patent Citations

  • Sample platform

    CN105628723A

  • Scanning electron microscope sample stage fixing device for nano-indentation experiment

    CN110609049A