In-situ reaction sample holder for XPS test

Abstract

The utility model belongs to the technical field of X-ray photoelectron spectrometer analysis, and particularly relates to an in-situ reaction sample support for XPS (X-ray photoelectron spectroscopy) test, which comprises a base and an upper cover which are matched with each other, the base is detachably connected with the upper cover, the upper cover is provided with a plurality of sample holes, the sample holes comprise a sample upper hole b and a sample lower hole a, and the sample upper hole b and the sample lower hole a are communicated with each other. The lower sample hole a is used for placing a to-be-detected sample, the size of the lower sample hole a is matched with that of the to-be-detected sample, one side, provided with the lower sample hole, of the upper cover is in contact with the base, the upper sample hole b is communicated with at least one part of the corresponding lower sample hole a, and the area of the communicated part is smaller than the size of the to-be-detected sample. The sample support can effectively position and fix the sample to be tested under the condition of avoiding using an adhesive tape.

Description

Technical Field

[0001] The utility model belongs to the technical field of X-ray photoelectron spectrometer analysis, and in particular relates to an in-situ reaction sample holder for XPS testing. Background Art

[0002] X-ray photoelectron spectroscopy (XPS), an advanced surface analysis technology with minimal destructiveness to samples, can analyze all elements except H and He, providing information on elemental composition, relative content, chemical state, molecular structure, chemical bonds, etc. for material surface research. It is widely used in material surface research.

[0003] Before conventional XPS testing, the sample needs to be fixed to a sample strip using double-sided tape or conductive adhesive. During the transfer or sample preparation process, the sample will be exposed to the atmosphere. For environmentally sensitive materials, components such as O2 and H2O in the air will affect their surface electronic or chemical state, making it difficult for the XPS test results to reflect the true information of the material surface.

[0004] Currently, many laboratories achieve quasi-in-situ XPS characterization of materials by building in-situ reaction cells in combination with XPS. This technology allows the test samples to be directly vacuumed after pretreatment or reaction in the XPS in-situ reaction cell and then sent to the analysis room for testing. The entire process is isolated from air, so that the XPS test results can truly reflect the chemical state changes of species on the surface of the test samples.

[0005] However, the original quartz sample holder used in the existing X-ray photoelectron spectrometer for in-situ reaction characterization has certain defects: (1) The multiple grooves for storing samples on the sample holder are not marked. When testing samples of the same series, the samples cannot be distinguished from each other in terms of appearance. After the sample holder is transferred between the chambers of the XPS instrument, the sample serial number cannot be identified, resulting in the final test results being unusable; (2) When performing in-situ reactions, the sample usually needs to be heated. After the sample is fixed using the conventional tape fixing method, the tape will volatilize organic matter during the heating process, posing a risk of contaminating the sample. In addition, the grooves on the surface of the sample holder are shallow. When the atmosphere reaction is carried out in the reaction pool, the unfixed sample It is easy to fall or lose, thus affecting subsequent detection; (3) Although quartz material is resistant to high temperatures, it is easy to break. When transferring between the XPS sampling chamber, analysis chamber, and reaction pool, a slight difference in the angle and force of the transfer rod inserted into the quartz sample holder slot will cause the quartz sample holder to break, thus affecting subsequent experiments; (4) During the test of insulating samples, the quartz sample holder is not conductive and can easily lead to abnormal charge neutralization on the sample surface, which ultimately leads to abnormal XPS spectrum peak results. Therefore, it is not suitable for testing insulating samples; (5) Magnetic samples are magnetic. If they are not fixed during XPS testing, they may be adsorbed on the open magnetic lens, thereby affecting normal detection. Therefore, the existing sample holder is not suitable for testing magnetic materials. Utility Model Content

[0006] In order to improve the deficiencies of the prior art, the utility model provides an in-situ reaction sample holder for XPS testing, which can effectively position and fix the sample to be tested without using tape.

[0007] As mentioned above, the utility model provides an in-situ reaction sample holder for XPS testing, comprising a base and an upper cover that cooperate with each other, the base and the upper cover being detachably connected, a plurality of sample holes being opened on the upper cover, the sample holes comprising a sample upper hole b and a sample lower hole a, the sample lower hole a being used to place the sample to be tested, the size of the sample lower hole a being adapted to the sample to be tested, and one side of the upper cover where the sample lower hole is provided is in contact with the base, the sample upper hole b is at least partially connected to the corresponding sample lower hole a, and the area of ​​the connected portion is smaller than the size of the sample to be tested.

[0008] According to the embodiment of the present invention, the diameter of the lower sample hole a is larger than the diameter of the upper sample hole b.

[0009] According to an embodiment of the present invention, the upper sample hole b and the lower sample hole a are concentrically arranged.

[0010] According to the implementation scheme of the present utility model, the sum of the heights of the sample lower hole a and the sample upper hole b is the thickness of the upper cover, and the specific thicknesses of the sample lower hole a and the sample upper hole b are not limited.

[0011] According to the embodiment of the present invention, the diameter of the upper sample hole b is 3.50-3.70 mm, and the diameter of the lower sample hole a is 3.75-3.90 mm.

[0012] As an example, the diameter of the upper hole b of the sample is 3.65 mm; the diameter of the lower hole a of the sample is 3.85 mm.

[0013] According to an embodiment of the present invention, a mark is provided on the upper cover at a position corresponding to each sample well, and different sample wells have different marks.

[0014] According to the embodiment of the present invention, the number of the sample holes is set according to actual needs, and can be 1, 2, 4, 6 or more, and the sizes of different sample holes are the same or different.

[0015] As an example, the number of the sample holes is 4, and the 4 sample holes are symmetrically distributed, have the same size and shape, and are marked as 1, 2, 3, and 4 respectively.

[0016] According to the implementation scheme of the present utility model, the base and the upper cover are connected by screws, and screw holes are provided in the base and the upper cover at positions corresponding to the screws.

[0017] According to the implementation scheme of the present invention, the material of the screw is selected according to actual needs, and a suitable material can be selected according to parameters such as the vacuum degree of the detection environment, for example, SS316 stainless steel can be used.

[0018] According to the implementation scheme of the present invention, two positioning slots are provided on the side of the base: a first positioning slot and a second positioning slot. The position and shape of the first positioning slot are adapted to the fork at one end of the XPS test sample strip, and the position and shape of the second positioning slot match the transfer fork in the in-situ reaction chamber (in fact, the sizes of these forks and slots are adapted).

[0019] According to an embodiment of the present invention, the first positioning slot and the second positioning slot are both in the shape of a circular ring.

[0020] According to an embodiment of the present invention, the first positioning slot is located above the second positioning slot.

[0021] According to the implementation scheme of the present utility model, the height of the first positioning slot and the second positioning slot is 2.00 mm, the slot depth is 2.06 mm, the distance between the top of the first positioning slot and the upper surface of the base is 1.08 mm, and the distance between the bottom of the second positioning slot and the lower surface of the base is 1.89 mm.

[0022] According to the embodiment of the present utility model, a connection hole is opened at the lower part of the base, and the connection hole is used to connect and fix with the XPS reaction cell base.

[0023] According to an embodiment of the present invention, the outer diameter of the base is 14.50 mm, and the height of the base is 9.05 mm.

[0024] According to an embodiment of the present invention, the outer diameter of the upper cover is 14.50 mm, and the thickness of the upper cover is 2.00 mm.

[0025] According to the implementation scheme of the present utility model, the diameter of the lower connecting hole of the base is 3.88 mm and the depth is 7.30 mm.

[0026] According to an embodiment of the present invention, the material of the sample holder is selected from any one of quartz, tantalum, molybdenum, tungsten, copper or stainless steel.

[0027] Beneficial effects

[0028] 1) The sample holder of the present invention includes an upper cover, which is provided with a plurality of sample holes, including a sample upper hole b and a sample lower hole a. The sample lower hole a is used to place the sample to be tested. The size of the sample lower hole a is adapted to the sample to be tested, and the side of the upper cover where the sample lower hole is provided is in contact with the base. The sample upper hole b is at least partially connected to the corresponding sample lower hole a, and the area of ​​the connected portion is smaller than the size of the sample to be tested. During use, the sample to be tested is pressed into a sheet with a diameter equal to or slightly smaller than the sample lower hole a and larger than the sample upper hole b. The sample to be tested is first placed in the sample lower hole a, and the upper cover and the base are fixed and then turned over. Since the diameter of the sheet is larger than the area of ​​the communication between the sample upper hole b and the sample lower hole a, the sheet is confined in the sample lower hole a and will not fall from the sample upper hole b, thereby achieving sample fixation and positioning. This not only avoids the contamination problem caused by tape fixation, but also avoids the wear and breakage of the quartz sample holder caused by the sample holder being transferred between XPS chambers, and the charge neutralization anomaly that is prone to occur when testing insulating samples. In addition, magnetic samples can be fixed and tested, effectively improving the test accuracy and expanding the test range of the test samples.

[0029] 2) The sample holder of the present invention has a mark on the upper cover corresponding to each sample hole. After adding the sample, the sample can be distinguished according to the mark, which facilitates the one-to-one correspondence between the sample and the corresponding test result. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 It is a structural schematic diagram of the in-situ reaction sample holder used for XPS testing in the present invention.

[0031] Among them, 1-base, 2-upper cover, 3-first positioning slot, 4-second positioning slot, 5-connecting hole, 6-sample hole, 7-screw. DETAILED DESCRIPTION

[0032] The following will further explain the structure of the present invention in detail with reference to specific embodiments. It should be understood that the following embodiments are merely exemplary illustrations and explanations of the present invention and should not be construed as limiting the scope of protection of the present invention. All technologies implemented based on the above-mentioned content of the present invention are included within the scope of protection intended by the present invention.

[0033] It should be noted that the terms used herein are only for describing specific embodiments and are not intended to limit the exemplary embodiments according to the present invention. As used herein, unless the context clearly indicates otherwise, the singular form is also intended to include the plural form. In addition, it should be understood that when the terms "comprise" and / or "include" are used in this specification, they indicate the presence of features, steps, operations, devices, components and / or combinations thereof.

[0034] Unless otherwise specified, the relative arrangement of the parts and steps, numerical expressions and numerical values ​​set forth in these embodiments do not limit the scope of the present invention. At the same time, it should be clear that, for ease of description, the sizes of the various parts shown in the accompanying drawings are not drawn according to actual proportional relationships. The technology, methods and equipment known to those of ordinary skill in the relevant art may not be discussed in detail, but in appropriate cases, the technology, methods and equipment should be considered as part of the specification. In all examples shown and discussed here, any specific value should be interpreted as being merely exemplary, rather than as a limitation. Therefore, other examples of the exemplary embodiments may have different values. It should be noted that similar numbers and letters represent similar items in the following figures, and therefore, once an item is defined in one figure, it does not need to be further discussed in subsequent figures.

[0035] In the description of the present invention, it should be noted that the terms "center", "up", "down", "left", "right", "vertical", "horizontal", "inside", "outside", etc., indicating directions or positional relationships, are based on the directions or positional relationships shown in the accompanying drawings. They are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific direction, be constructed and operated in a specific direction. Therefore, they cannot be understood as limitations on the present invention.

[0036] In the description of this utility model, it should be noted that, unless otherwise expressly specified or limited, the terms "mounted," "connected," and "connected" should be understood in a broad sense. For example, they can refer to fixed connections, detachable connections, or integral connections; mechanical connections, electrical connections; direct connections, indirect connections through an intermediate medium, and internal communication between two components. Those skilled in the art will understand the specific meanings of the above terms in this utility model based on the specific circumstances.

[0037] Example 1

[0038] In a specific embodiment of the present invention, Figure 1 As shown, an in-situ reaction sample holder for XPS testing includes a base 1 and an upper cover 2 that cooperate with each other. The base 1 and the upper cover 2 are detachably connected. The cross-sectional shapes of the base 1 and the upper cover 2 can be set according to actual needs, such as circular, rectangular or other polygonal shapes.

[0039] In this embodiment, the base 1 and the upper cover 2 are cylindrical, and the base 1 and the upper cover 2 are detachably connected by existing methods. For example, a lower screw hole is provided on the base 1, and an upper screw hole is provided on the upper cover 2 at a position corresponding to the lower screw hole of the base 1. A screw 7 is provided in the upper screw hole. The screw 7 passes through the upper screw hole and is inserted into the lower screw hole to fix the upper cover 2 to the upper surface of the base 1. The material of the screw 7 is selected according to actual needs. The appropriate material can be selected according to parameters such as the vacuum degree of the detection environment, for example, SS316 stainless steel can be used.

[0040] In this specific embodiment, the size of the sample holder is compatible with the XPS test sample strip, the spatial structure of the XPS injection chamber, and the spatial structure of the XPS in-situ reaction cell.

[0041] Two positioning slots are set on the side of the base 1: a first positioning slot 3 and a second positioning slot 4. The position and shape of the first positioning slot 3 are adapted to the fork at one end of the XPS test sample strip, and the position and shape of the second positioning slot 4 are adapted to the position, height and shape of the transfer fork in the in-situ reaction chamber; the relative positions of the first positioning slot 3 and the second positioning slot 4 are not particularly limited. In this embodiment, the first positioning slot 3 and the second positioning slot 4 are both circular, and the first positioning slot 3 is located above the second positioning slot 4; the height of the first positioning slot 3 and the second positioning slot 4 is 2.00 mm, the groove depth is 2.06 mm, the distance between the top of the first positioning slot 3 and the upper surface of the base 1 is 1.08 mm, and the distance between the bottom of the second positioning slot 4 and the lower surface of the base 1 is 1.89 mm.

[0042] A connecting hole 5 is provided at the lower part of the base 1, which is used to connect and fix to the base of the XPS reaction cell; a plurality of sample holes 6 are provided on the upper cover 2, and the sample holes 6 pass through the upper cover 2. A mark is provided on the upper cover 2 corresponding to each sample hole 6. Different sample holes 6 have different marks. The number of sample holes 6 is set according to actual needs, and can be 1, 2, 4, 6 or more. The sizes of different sample holes 6 are the same or different. In this embodiment, the number of sample holes 6 is 4, and the 4 sample holes 6 are symmetrically distributed, the same size and shape, and are marked as 1, 2, 3, and 4 respectively.

[0043] The sample hole 6 includes a sample lower hole a and a sample upper hole b. The sample upper hole b and the sample lower hole a are concentrically arranged. The diameter of the sample lower hole a is larger than the diameter of the sample upper hole b. The specific diameters and heights of the sample upper hole b and the sample lower hole a are set according to actual needs. The total height of the sample upper hole b and the sample lower hole a is the thickness of the upper cover 2. The diameter of the sample upper hole b is 3.50~3.70mm, and the diameter of the sample lower hole a is 3.75~3.90mm. For example, the diameter of the sample upper hole b is 3.65mm; the diameter of the sample lower hole a is 3.85mm.

[0044] The sample hole 6 is the sample placement area. The sample to be tested is pressed into a shape that matches the sample hole 6 by a customized tablet pressing mold and then placed in the sample hole 6; the center of the upper surface of the base 1 is aligned with the center of the lower surface of the upper cover. After the whole is flipped over, the bottom of the base 1 faces downward, and the upper surface of the upper cover 2 faces upward and stands on a plane. The upper cover 2 is fixed to the base 1 by screws, and the sample to be tested is installed on the XPS sample strip along with the sample holder to realize the transfer between the in-situ reaction system and the XPS detection system.

[0045] In a preferred embodiment, the outer diameter of the base 1 is 14.50 mm and the height is 9.05 mm; the outer diameter of the upper cover 2 is 14.50 mm and the thickness of the upper cover 2 is 2.00 mm; the diameter of the lower connecting hole 5 of the base 1 is 3.88 mm and the height is 7.30 mm, and the connecting hole 5 can be connected to the lower screw hole.

[0046] In a preferred embodiment, the sample holder is made of at least one of the following: quartz, tantalum, molybdenum, tungsten, copper, or stainless steel. During the in-situ reaction, the sample is subjected to high-temperature and high-pressure heating, exposing the sample holder to high-temperature and high-pressure environments. Therefore, the material of the sample holder must possess excellent high-temperature and high-pressure resistance. Quartz, tantalum, molybdenum, tungsten, copper, or stainless steel, as materials with excellent high-temperature and high-pressure resistance, can ensure normal use during the in-situ reaction. The specific material used can be selected based on the actual sample conditions.

[0047] Although the embodiments of the present invention have been shown and described above, it can be understood that the above embodiments are illustrative and cannot be understood as limitations on the present invention. Ordinary technicians in this field can change, modify, replace and modify the above embodiments within the scope of the present invention without departing from the principles and purpose of the present invention.

[0048] The above examples illustrate the specific implementation methods of the present invention. However, the scope of protection of the present invention is not limited to the above-mentioned exemplary implementation methods. Any modifications, equivalent substitutions, improvements, etc. made by those skilled in the art within the spirit and principles of the present invention shall be included in the scope of protection of the claims of the present invention.

Claims

1. An in-situ reaction sample holder for XPS testing, comprising a base and an upper cover that cooperate with each other, characterized in that: The base and the upper cover are detachably connected, and a plurality of sample holes are provided on the upper cover, wherein the sample holes include an upper sample hole b and a lower sample hole a. The lower sample hole a is used to place the sample to be tested, and the size of the lower sample hole a is adapted to the sample to be tested, and the side of the upper cover where the lower sample hole is provided is in contact with the base, and the upper sample hole b is at least partially connected to the corresponding lower sample hole a, and the area of ​​the connected portion is smaller than the size of the sample to be tested.

2. The in-situ reaction sample holder for XPS testing according to claim 1, characterized in that: The diameter of the sample lower hole a is larger than the diameter of the sample upper hole b.

3. The in-situ reaction sample holder for XPS testing according to claim 1, characterized in that: The diameter of the sample upper hole b is 3.50-3.70 mm, and the diameter of the sample lower hole a is 3.75-3.90 mm.

4. The in-situ reaction sample holder for XPS testing according to claim 1, characterized in that: A mark is provided on the upper cover at a position corresponding to each sample hole, and different sample holes have different marks.

5. The in-situ reaction sample holder for XPS testing according to claim 1, characterized in that: The base and the upper cover are connected by screws, and screw holes are provided at positions of the base and the upper cover corresponding to the screws.

6. The in-situ reaction sample holder for XPS testing according to any one of claims 1 to 5, characterized in that: Two positioning slots are set on the side of the base: a first positioning slot and a second positioning slot. The position and shape of the first positioning slot are adapted to the fork at one end of the XPS test sample strip, and the position and shape of the second positioning slot match the transfer fork in the in-situ reaction chamber.

7. The in-situ reaction sample holder for XPS testing according to claim 6, characterized in that: The first positioning slot and the second positioning slot are both in the shape of a circular ring.

8. The in-situ reaction sample holder for XPS testing according to any one of claims 1 to 4, characterized in that: A connection hole is provided at the lower portion of the base, and the connection hole is used for connecting and fixing with the XPS reaction cell base.

9. The in-situ reaction sample holder for XPS testing according to any one of claims 1 to 4, characterized in that: The outer diameter of the base is 14.50 mm, and the height of the base is 9.05 mm; the outer diameter of the upper cover is 14.50 mm, and the thickness of the upper cover is 2.00 mm.

10. The in-situ reaction sample holder for XPS testing according to any one of claims 1 to 4, characterized in that: The material of the sample holder is selected from any one of quartz, tantalum, molybdenum, tungsten, copper or stainless steel.

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