Sample loading device for glow discharge spectrometer and sample analysis method

Abstract

The invention relates to the technical field of material component analysis, and provides a sample loading device for a glow discharge spectrometer and a sample analysis method. The sample loading device comprises a shell, a placement frame, an elastic piece and a first sealing piece, a containing cavity is formed in the shell, and a first opening communicated with the containing cavity is further formed in the top end of the shell; the placing frame is detachably arranged in the containing cavity, the top of the placing frame is suitable for penetrating through the first opening, a placing groove is further formed in the top end of the placing frame, and samples are suitable for being placed in the placing groove; the placing rack is elastically arranged in the accommodating cavity through the elastic piece; the first sealing piece is arranged at the top end of the shell. The placing frame is detachably arranged in the containing cavity of the shell, the placing frame with the matched placing groove can be selected according to the size specification of a sample, and the loading requirements of small-size samples of different specifications are met; when a sample is loaded, the elastic piece can be adaptively adjusted according to the thickness of the sample to ensure that the first sealing piece at the top of the shell can play a role, so that the vacuum state of the glow discharge cavity is ensured.

Description

Technical Field

[0001] The invention relates to the technical field of material component analysis, and further to a sample loading device for a glow discharge spectrometer and a sample analysis method. Background Art

[0002] The rapid development of advanced materials has promoted the progress of science and technology and society, and at the same time has put forward higher and higher requirements on the characterization technology and methods of materials. With the continuous emergence of new materials, not only the traditional characterization technology is required to be continuously improved in accuracy and resolution, but also new characterization methods and technologies need to be developed to cope with the complexity and diversity of new materials. For the composition of the material, the uniformity of its composition and the distribution of impurity elements will seriously affect the properties of the material. For example, the segregation, diffusion, enrichment and other behaviors of the elements in the material will significantly affect the optical, electrical, mechanical and other properties of the material. The development of efficient characterization devices and methods to achieve accurate characterization of the deep distribution of each element in the material is of vital importance for the control of the material preparation process, in-depth exploration of the growth mechanism and optimization and improvement of performance.

[0003] Glow discharge spectrometer is an important means to characterize the element composition and depth distribution in advanced materials. It can provide advanced materials with element depth distribution information from the surface to the inside, revealing the segregation, diffusion, enrichment and other behaviors of elements in materials, and has become an indispensable and important research method in the field of material research and production. Glow discharge spectrometer can quickly and sensitively directly analyze the element composition distribution in material surface coatings / platings, organic film coatings, lithium battery electrode multilayer structures, aviation protection multilayer films, and nano-scale functional multilayer films. It is widely used in steel, nonferrous metals, organic materials, battery electrodes, silicon materials, aerospace and semiconductors.

[0004] As a direct analysis method for solid materials, glow discharge spectroscopy has small matrix effect, and the type of matrix has almost no effect on the signal of the measured element; low power, the sputtered ion energy used for glow discharge spectroscopy depth spectrum measurement is low, and the depth resolution can reach sub-nanometer level; low-energy level excitation, the atoms of the sample being measured are mainly excited by electron collisions in the plasma, and the spectral lines generated are often simple linear spectral lines of atoms or ions, so the interference between spectral lines is small; all elements can be detected, and the sample atoms entering the plasma can be distinguished; small self-absorption effect, the confined light source makes the plasma thickness small when the sample is excited, and the generated self-absorption effect is small; fast analysis speed, it only takes a few minutes to analyze a sample, and the sputtering rate can reach several microns to tens of microns per minute.

[0005] When performing deep analysis with a glow discharge spectrometer, the sample needs to be smooth and flat on both sides and the outer periphery of the copper anode needs to be sealed with a device that covers the size of the sample to ensure that a closed environment is formed inside the glow source and glow discharge is generated. However, when the size of the sample to be analyzed is small (side length or diameter less than 14mm), and the size of the sample is smaller than the sealing device of the glow discharge spectrometer, the sealing device cannot properly seal the glow source, and the glow discharge spectrometer cannot generate glow discharge, which ultimately makes it impossible to conduct deep analysis.

[0006] Therefore, it is necessary to design a small-size sample depth analysis loading device for glow discharge spectrometer to solve the above problems. Summary of the invention

[0007] In view of the above technical problems, the purpose of the present invention is to provide a sample loading device and a sample analysis method for a glow discharge spectrometer. The placement rack can be detachably arranged in the accommodating cavity of the shell, and the placement rack with an adaptive placement slot can be selected according to the size specifications of the sample to meet the loading requirements of small-sized samples of different specifications; the bottom of the placement rack and the bottom of the accommodating cavity are connected by an elastic member. When the sample is loaded, the elastic member can be adaptively adjusted according to the thickness of the sample to ensure that the first sealing member on the top of the shell can play a role, thereby ensuring the vacuum state of the glow discharge cavity, and finally realizing the in-depth analysis of small-sized samples of the glow discharge spectrometer.

[0008] In order to achieve the above object, the present invention provides a sample loading device for a glow discharge spectrometer, the sample loading device comprising a housing, a placement frame, an elastic member and a first sealing member, a housing cavity is provided inside the housing, and a first opening communicating with the housing cavity is also provided at the top of the housing;

[0009] The placement rack is detachably arranged in the accommodating cavity, the top of the placement rack is suitable for passing through the first opening and abutting against the glow discharge spectrometer, and the top of the placement rack is also provided with a placement groove, and the placement groove is suitable for placing the sample;

[0010] The elastic member is elastically arranged between the bottom of the placement rack and the bottom of the accommodating chamber, so that the placement rack is elastically arranged in the accommodating chamber;

[0011] The first sealing member is disposed at the top of the housing and is relatively located outside the first opening.

[0012] In some embodiments, the housing includes a detachably connected top shell and a base, the first opening and the second opening are respectively provided at two ends of the accommodating cavity, and the base is adapted to be detachably mounted at the second opening and abut against the elastic member;

[0013] A sealing groove is provided on the top of the top shell, and the first sealing member is arranged in the sealing groove.

[0014] In some embodiments, the accommodating cavity includes a first cavity and a second cavity, the first cavity is connected to the first opening, the second cavity is connected to the second opening, the diameter of the second opening is larger than the diameter of the first opening, and the placement rack is suitable for passing through the second opening and being arranged in the accommodating cavity;

[0015] The placement rack is in the shape of a boss and matches the accommodating cavity. The placement rack includes a first frame body matching the first cavity and a second frame body matching the second cavity.

[0016] In some embodiments, the shell is cylindrical; the shell, the placement frame and the elastic member are all made of conductive materials.

[0017] In some embodiments, a first groove is further provided at the bottom of the placement rack, and one end of the elastic member is disposed in the first groove;

[0018] The top of the base is also provided with a second groove, and the other end of the elastic member is arranged in the second groove.

[0019] In some embodiments, the placement groove is relatively located in the center of the top of the placement rack, and the placement rack, the shell and the placement groove are relatively coaxially arranged, so that the sample is suitable for matching with the discharge chamber of the glow discharge spectrometer.

[0020] In some embodiments, a rib is further provided at the outer edge of the top of the shell, and the rib is suitable for abutting against the outer side wall of the glow discharge spectrometer, so that the sample in the placement groove matches the discharge cavity of the glow discharge spectrometer.

[0021] In some embodiments, a plurality of limiting posts are further disposed on the top of the shell. The limiting posts are spaced around the outer edge of the top of the shell and are suitable for abutting against the outer side wall of the glow discharge spectrometer.

[0022] In some embodiments, a second sealing member is disposed outside the discharge chamber of the glow discharge spectrometer, and the first sealing member is relatively located outside the second sealing member;

[0023] The placement groove has a diameter of 3.0-8.0 mm and a depth of 2.0-6.0 mm.

[0024] According to another aspect of the present application, there is further provided a sample analysis method, which is applied to any one of the sample loading devices in the above preferred embodiments, comprising drying the sample;

[0025] According to the sample size, select a placement rack with a suitable placement slot;

[0026] Assembling the placement rack into the shell and arranging an elastic member between the placement rack and the shell;

[0027] Disposing a first sealing member at the top end of the housing;

[0028] Install the sample loading device at the test port of the glow discharge spectrometer.

[0029] Compared with the prior art, the sample loading device and sample analysis method for a glow discharge spectrometer provided by the present invention have at least one of the following beneficial effects:

[0030] 1. The placement rack can be detachably arranged in the accommodating cavity of the shell. A placement rack with an adaptable placement slot can be selected according to the size specifications of the sample to meet the loading requirements of small-sized samples of different specifications; the bottom of the placement rack and the bottom of the accommodating cavity are connected by an elastic member. When the sample is loaded, the elastic member can be adaptively adjusted according to the thickness of the sample to ensure that the first sealing member on the top of the shell can play a role, thereby ensuring the vacuum state of the glow discharge cavity, and finally realizing the in-depth analysis of small-sized samples of the glow discharge spectrometer.

[0031] 2. The placement rack and the accommodating cavity are both in the shape of bosses, and the second frame body is suitable for abutting the end of the second cavity, which can effectively prevent the placement rack from separating from the shell and ensure the stability of the sample loading device; the elastic member is abutted and installed in the first groove at the bottom of the placement rack and the second groove at the top of the base, so that both ends of the elastic member are fixedly connected to the placement rack and the base, avoiding misalignment or malposition of the elastic member and maintaining the stability of the placement rack's movement.

[0032] 3. The rib is suitable for contacting with the outer wall of the glow discharge spectrometer, which can effectively ensure that the small-sized sample fixed by the sample loading device is always in the plasma excitation center, ensuring that the sample will not be displaced and stably excited during the loading, injection and analysis process, avoiding plasma leakage caused by displacement during sample loading.

[0033] 4. The limiting column is also used to limit the glow discharge spectrometer and the sample loading device to ensure the assembly stability of the glow discharge spectrometer and the sample loading device, and to maintain the relative position of the sample and the plasma emission port when the sample is loaded.

[0034] 5. Glow discharge spectrometer can directly perform in-depth analysis on small-sized samples. Its structure is simple and reasonable, and it is suitable for glow discharge spectrometer or similar devices. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] The preferred implementation modes will be described below in a clear and understandable manner with reference to the accompanying drawings to further illustrate the above-mentioned characteristics, technical features, advantages and implementation methods of the present invention.

[0036] Figure 1 It is a position diagram of a sample loading device for a glow discharge spectrometer;

[0037] Figure 2is a cross-sectional view of a sample loading device for a glow discharge spectrometer;

[0038] Figure 3 It is an installation diagram of a sample loading device for a glow discharge spectrometer;

[0039] Figure 4 is a sputtering crater morphology image obtained when a small-size sample is deeply analyzed using a sample loading device in this embodiment;

[0040] Figure 5 This is the element distribution diagram obtained when a small-size sample is deeply analyzed using a sample loading device in this embodiment.

[0041] Description of Figure Numbers:

[0042] Shell 1, accommodating cavity 10, first opening 101, second opening 102, top shell 11, first cavity 111, second cavity 112, base 12, second groove 121, retaining edge 13, placement frame 2, first frame 21, placement groove 211, second frame 22, first groove 221, elastic member 3, first sealing member 4, glow discharge spectrometer 5, second sealing member 51, discharge cavity 52. DETAILED DESCRIPTION

[0043] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the specific implementation methods of the present invention will be described below with reference to the accompanying drawings. Obviously, the accompanying drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings and other implementation methods can be obtained based on these drawings without creative work.

[0044] In order to simplify the drawings, only the parts related to the invention are schematically shown in each figure, and they do not represent the actual structure of the product. In addition, in order to simplify the drawings and facilitate understanding, in some figures, only one of the parts with the same structure or function is schematically drawn or marked. In this article, "one" not only means "only one", but also means "more than one".

[0045] It should be further understood that the term “and / or” used in the specification and appended claims refers to any combination and all possible combinations of one or more of the associated listed items, and includes these combinations.

[0046] In this document, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0047] In addition, in the description of the present application, the terms "first", "second", etc. are only used to distinguish the description and cannot be understood as indicating or implying relative importance. It should be noted that the above embodiments can be freely combined as needed. The above are only preferred implementations of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention, and these improvements and modifications should also be regarded as the scope of protection of the present invention.

[0048] refer to Figures 1 to 3 The present invention provides a sample loading device for a glow discharge spectrometer, the sample loading device is used for sample depth analysis of the glow discharge spectrometer 5, the sample loading device comprises a shell 1, a placement rack 2, an elastic member 3 and a first sealing member 4, a housing 1 is provided with a housing chamber 10 inside the shell 1, and a first opening 101 communicating with the housing chamber 10 is also provided at the top of the shell 1; the placement rack 2 is detachably arranged in the housing chamber 10, the top of the placement rack 2 is suitable for passing through the first opening 101 and abutting against the glow discharge spectrometer 5, and a placement groove 211 is also provided at the top of the placement rack 2, and the placement groove 211 is suitable for placing the sample; the elastic member 3 is elastically arranged between the bottom of the placement rack 2 and the bottom of the housing chamber 10, so that the placement rack 2 is elastically arranged in the housing chamber 10; the first sealing member 4 is arranged at the top of the shell 1 and is relatively located outside the first opening 101.

[0049] In this embodiment, the placement rack 2 is detachably arranged in the accommodating cavity 10 of the shell 1. The placement rack 2 with an adaptable placement groove 211 can be selected according to the size specifications of the sample to meet the loading requirements of small-sized samples of different specifications; the bottom of the placement rack 2 and the bottom of the accommodating cavity 10 are connected by an elastic member 3. When the sample is loaded, the elastic member 3 can be adaptively adjusted according to the thickness of the sample to ensure that the first sealing member 4 on the top of the shell 1 can play a role, thereby ensuring the vacuum state of the glow discharge cavity 52, and finally realizing the in-depth analysis of small-sized samples of the glow discharge spectrometer 5.

[0050] Specifically, the glow discharge spectrometer 5 is a prior art in the art. The glow discharge spectrometer 5 has a discharge chamber 52. A second seal 51 is also provided outside the discharge chamber 52. The second seal 51 is used to seal the discharge chamber 52. The diameter of the second seal 51 is generally 15 mm. The existing glow discharge spectrometer 5 cannot test small-sized samples because the size of the sample to be tested is small. Before the test starts, the vacuum degree of the discharge chamber 52 cannot meet the requirements, and glow discharge cannot be generated. The small-sized sample cannot be deeply analyzed. The small-sized sample can only be enlarged to meet the sealing requirements of the second seal 51 of the glow discharge spectrometer 5. The cost is very high if the diameter of the second seal 51 on the glow discharge spectrometer 5 is designed according to the size of the sample to be tested. Moreover, because the discharge chamber 52 of the glow discharge spectrometer 5 requires a certain wall thickness, the second seal 51 needs to maintain a certain distance from the discharge chamber 52, which makes the second seal 51 unable to meet the requirements of smaller-sized samples.

[0051] Therefore, when the sample loading device loaded with the sample is loaded into the glow discharge spectrometer 5 for glow discharge spectrum depth analysis, the present application provides a first seal 4 at the top of the shell 1 of the sample loading device, and the first seal 4 abuts against the top of the shell 1 and the end of the glow discharge spectrometer 5, and seals the discharge chamber 52 to meet the vacuum requirement. The first seal 4 is installed through the sealing groove at the top of the top shell 11, and the first seal 4 is arranged in the sealing groove. At the same time, the diameter of the first seal 4 at the periphery of the first opening 101 at the center of the shell 1 is preferably 26.0 mm. Preferably, a second seal 51 is provided on the outside of the discharge chamber 52 of the glow discharge spectrometer 5, and the first seal 4 is relatively located on the outside of the second seal 51. In a modified embodiment, the first seal 4 can also be located on the inside of the second seal 51 and relatively located on the outside of the first opening 101.

[0052] The top of the placement rack 2 is provided with a placement groove 211 suitable for placing the sample, and the placement groove 211 is adapted to the discharge chamber 52. The shape of the placement groove 211 is not further limited in this application, and it can be circular, square, rectangular, etc. In this application, the diameter of the placement groove 211 is 3.0-8.0 mm and the depth is 2.0-6.0 mm. The height of the placement rack 2 is 8.0-15.0 mm, the diameter is 3.0-8.0 mm, and it can also be other reasonable sizes.

[0053] At the same time, in order to achieve effective abutment between the first seal 4 and the end of the glow discharge spectrometer 5, the present application sets the placement rack 2 as an elastically displaceable structure, that is, the placement rack 2 and the shell 1 are connected by an elastic member 3. When the sample is loaded, the elastic member 3 will be adaptively adjusted according to the thickness of the sample to ensure that the first seal 4 on the top of the sample loading device plays a role, thereby ensuring the vacuum state of the glow discharge chamber 52, and finally realizing the in-depth analysis of small-size samples of the glow discharge spectrometer 5. Specifically, a accommodating cavity 10 is provided inside the shell 1, and a first opening 101 is provided at the top of the accommodating cavity 10, and the first opening 101 is adapted to the end of the placing rack 2, and the top of the placing rack 2 is suitable for passing through the first opening 101 and abutting against the end of the glow discharge spectrometer 5, and elastic members 3 are provided at the bottom of the placing rack 2 and the bottom of the accommodating cavity 10. When the sample loading device and the glow discharge spectrometer 5 are assembled, the end of the glow discharge spectrometer 5 pushes the placing rack 2 to extrude the elastic member 3, so that the placing rack 2 moves into the accommodating cavity 10, and when the top of the placing rack 2 is flush with the top of the shell 1, the sample loading device and the glow discharge spectrometer 5 are assembled, and the first sealing member 4 is abutted between the sample loading device and the glow discharge spectrometer 5 and seals the discharge cavity 52.

[0054] The placement rack 2 is detachably mounted on the accommodating chamber 10. The sample loading device can select a placement rack 2 with an adaptable placement groove 211 according to the size specifications of the sample to meet the loading requirements of small-sized samples of different specifications, so as to improve the loading convenience of small-sized samples of different specifications. In one embodiment, the housing 1 includes a detachably connected top shell 11 and a base 12, and the two ends of the accommodating chamber 10 are respectively provided with a first opening 101 and a second opening 102, and the base 12 is suitable for being detachably mounted at the second opening 102 and abutting against the elastic member 3; a sealing groove is provided at the top of the top shell 11, and the first sealing member 4 is arranged in the sealing groove. In this embodiment, the accommodating chamber 10 is located inside the top shell 11, and the base 12 is detachably mounted on the top shell 11 and abuts against the bottom of the placement rack 2. A second opening 102 is provided at the bottom of the accommodating chamber 10, and the base 12 is detachably mounted at the bottom of the top shell 11 and seals the accommodating chamber 10, and the elastic member 3 abuts between the bottom of the placement rack 2 and the top of the base 12. The base 12 and the top shell 11 are fixedly connected by fasteners such as screws, and the assembly and disassembly are simple. When installing the placement rack 2, it is only necessary to remove the base 12, then place the top of the placement rack 2 and the elastic member 3 in the accommodating cavity 10 and make the top of the placement rack 2 pass through the first opening 101, and then install the base 12 on the bottom of the top shell 11 to complete the assembly of the placement rack 2. The sample loading device of the present invention reduces the requirements of the glow discharge spectrometer 5 on the size of the sample to be tested. The structure of the present invention is simple and reasonable, and can effectively solve the problem that the glow discharge spectrometer 5 cannot directly analyze the depth analysis requirements of small-sized samples, and is suitable for glow discharge mass spectrometers or similar devices.

[0055] In a modified embodiment, the housing 1 includes a detachably connected top shell 11 and a base 12, a second opening 102 is provided at the top of the base 12, and the top shell 11 is detachably mounted at the second opening 102 of the base 12. This embodiment is different from the above embodiment in that, in this embodiment, a receiving chamber 10 is provided on the base 12, the top shell 11 is detachable from the base 12, and the top shell 11 is suitable for abutting against the top of the placement rack 2. When installing the placement rack 2, the top shell 11 needs to be disassembled, and then the bottom of the placement rack 2 and the elastic member 3 are placed in the receiving chamber 10, and then the top shell 11 is installed on the top of the base 12 and the first opening 101 of the top shell 11 is aligned with the top of the placement rack 2, so that the top of the placement rack 2 passes through the first opening 101. It is worth noting that the detachable structure of the placement rack 2 is diverse, and this application does not make further restrictions. In another modified embodiment, the housing 1 can also be detachably connected to the left and right, and this application does not make further redundant descriptions here.

[0056] Further, refer to Figure 2 The accommodating cavity 10 includes a first cavity 111 and a second cavity 112. The first cavity 111 is connected to the first opening 101, and the second cavity 112 is connected to the second opening 102. The diameter of the second opening 102 is larger than the diameter of the first opening 101. The placement rack 2 is suitable for passing through the second opening 102 and being arranged in the accommodating cavity 10; the placement rack 2 is boss-shaped and matches the accommodating cavity 10. The placement rack 2 includes a first frame body 21 matching the first cavity 111 and a second frame body 22 matching the second cavity 112.

[0057] In this embodiment, the placement rack 2 and the accommodating cavity 10 are both boss-shaped, and the second frame 22 is suitable for abutting against the end of the second cavity 112, which can effectively prevent the placement rack 2 from separating from the shell 1 and ensure the stability of the sample loading device.

[0058] Specifically, the placement rack 2 is convex, including a first frame 21 and a second frame 22, the first frame 21 is located on the top of the second frame 22, the diameter of the first frame 21 is smaller than the diameter of the second frame 22, the accommodating cavity 10 is also convex, including a first cavity 111 and a second cavity 112, the inner wall of the first cavity 111 matches the outer wall of the first frame 21, and the inner wall of the second cavity 112 matches the outer wall of the second frame 22, that is, the first frame 21 is suitable for being placed in the first cavity 111, and the second frame 22 is suitable for being placed in the second cavity 112. Suitable for placement in the second cavity 112, the length of the first frame 21 is longer than the length of the first cavity 111, under normal conditions, the elastic member 3 drives the first frame 21 of the placement rack 2 to pass through the first cavity 111 and the top of the first frame 21 is relatively located outside the accommodating cavity 10, and the second frame 22 abuts against the top of the second cavity 112; when the glow discharge spectrometer 5 and the sample loading device are assembled, the glow discharge spectrometer 5 drives the first frame 21 to enter the second cavity 112 until the top of the first frame 21 is flush with the top of the shell 1. The shell 1 includes but is not limited to a cylindrical type, and the shell 1 can also be understood as a torus, with a diameter of 34.0 mm and a height of 30.0 mm. Of course, it can also be other reasonable sizes, and this application does not make further restrictions.

[0059] Preferably, the housing 1, the rack 2 and the elastic member 3 are all made of conductive materials. The rack 2 is made of high-purity conductive metal tantalum, copper or stainless steel; the housing 1 is made of conductive stainless steel or copper; and the elastic member 3 is made of conductive stainless steel or copper alloy.

[0060] Further, refer to Figure 3 A first groove 221 is further provided at the bottom of the placement rack 2, and one end of the elastic member 3 is arranged in the first groove 221; a second groove 121 is further provided at the top of the base 12, and the other end of the elastic member 3 is arranged in the second groove 121.

[0061] In this embodiment, the elastic member 3 is installed in abutment with the first groove 221 at the bottom of the placement rack 2 and the second groove 121 at the top of the base 12, so that both ends of the elastic member 3 are fixedly connected to the placement rack 2 and the base 12, avoiding misalignment or dislocation of the elastic member 3 and maintaining the stability of the movement of the placement rack 2.

[0062] Furthermore, the placement groove 211 is relatively located in the center of the top of the placement rack 2 , and the placement rack 2 , the housing 1 and the placement groove 211 are relatively coaxially arranged, so that the sample is suitable for matching with the discharge chamber 52 of the glow discharge spectrometer 5 .

[0063] In this embodiment, the placement rack 2, the shell 1 and the placement slot 211 are relatively coaxially arranged, so that the sample is suitable for matching with the discharge chamber 52 of the glow discharge spectrometer 5. The small-sized sample fixed by the sample loading device is at the plasma excitation center, and the detection is more accurate.

[0064] Specifically, the placement rack 2 on which the sample is fixed is connected to the shell 1 through an elastic member 3, and the center of the size of the top of the placement rack 2 is adapted to be arranged at the center position of the first opening 101 of the shell 1, that is, the axes of the placement rack 2 and the shell 1 coincide; the placement groove 211 is located at the center of the top of the placement rack 2, so that the axes of the placement rack 2 and the placement groove 211 coincide, thereby ensuring that the placement rack 2, the shell 1 and the placement groove 211 are relatively coaxially arranged.

[0065] Further, refer to Figure 2 and Figure 3 A rib 13 is also provided at the outer edge of the top of the shell 1 , and the rib 13 is suitable for abutting against the outer side wall of the glow discharge spectrometer 5 , so that the sample in the placement groove 211 matches the discharge chamber 52 of the glow discharge spectrometer 5 .

[0066] In this embodiment, the retaining edge 13 is suitable for abutting against the outer wall of the glow discharge spectrometer 5, which can effectively ensure that the small-sized sample fixed by the sample loading device is always in the plasma excitation center, ensuring that the sample will not be displaced and stably excited during the loading, injection and analysis processes, thereby avoiding plasma leakage caused by displacement during sample loading.

[0067] Specifically, the rib 13 is relatively located at the top of the shell 1, and the rib 13 extends axially along the shell 1 to a side away from the shell 1. When assembled, the rib 13 is suitable for abutting against the outer side wall of the glow discharge spectrometer 5, so that the axis of the shell 1 and the end of the discharge chamber 52 of the glow discharge spectrometer 5 are coaxially arranged, so that the small-sized sample fixed by the sample loading device is always in the plasma excitation center; at the same time, the rib 13 can also ensure the stability of the assembly of the sample loading device and the glow discharge spectrometer 5, ensuring that the sample will not be displaced and stably excited during the loading, injection and analysis processes, avoiding the plasma leakage caused by displacement and dislocation during sample loading, and improving the safety performance of the sample loading device.

[0068] Preferably, a plurality of limiting columns are further provided on the top of the housing 1 , and the limiting columns are arranged at intervals around the outer edge of the top of the housing 1 and are suitable for abutting against the outer side wall of the glow discharge spectrometer 5 .

[0069] In this embodiment, the limiting column is also used to limit the glow discharge spectrometer 5 and the sample loading device, to ensure the assembly stability of the glow discharge spectrometer 5 and the sample loading device, and to maintain the relative position of the sample and the plasma emission port when the sample is loaded. Specifically, four limiting columns distributed in a central symmetrical manner are provided on the periphery of the shell 1, that is, distributed in two mutually perpendicular diameter directions on the upper surface of the shell 1, and the center of the limiting column is 16.0 mm away from the center of the circle of the shell 1. The bottom surface of the limiting column is circular, with a diameter of 1.00 mm and a height of 0.50 mm. It is worth noting that the retaining edge 13 and the limiting column can exist at the same time or one of them can exist selectively, and this application does not make further restrictions.

[0070] Furthermore, the present application provides a sample analysis method, which is applied to the sample loading device in any of the above embodiments, including drying the sample; selecting a placement rack 2 with a suitable placement slot 211 according to the sample size specifications; assembling the placement rack 2 into the interior of the shell 1 and arranging an elastic member 3 between the placement rack 2 and the shell 1; arranging a first sealing member 4 at the top of the shell 1; and installing the sample loading device at the test port of the glow discharge spectrometer 5.

[0071] In this embodiment, the glow discharge spectrometer 5 can directly perform depth analysis on small-sized samples, and its structure is simple and reasonable, and is suitable for the glow discharge spectrometer 5 or similar devices.

[0072] Specifically, first, the small-sized sample to be tested is cleaned and dried with ultrapure water and anhydrous ethanol in sequence. Subsequently, according to the size specifications of the sample to be tested, a placement rack 2 of suitable size is selected and loaded into the housing 1, and the housing 1 and the placement rack 2 are connected and fixed by the elastic member 3. After fixing, the base 12 is installed so that the elastic member 3 is stably arranged between the housing 1 and the placement rack 2. Then the first sealing member 4 is loaded into the top of the housing 1 fixed with the placement rack 2 to play a vacuum sealing role, and then the sample is placed in the placement groove 211 at the top of the placement rack 2 so that the sample is arranged in the central area of ​​the placement rack 2. Then the above-mentioned assembled sample loading device fixed with small-sized samples is loaded on the test port of the glow discharge spectrometer 5, and the retaining edge 13 and the limiting column at the top of the housing 1 of the sample loading device ensure that the sample will not be displaced and stably excited during loading, injection and analysis. Finally, the sample is tested, the signal intensity of the element to be measured is recorded, and the sputtering pit of the depth analysis is detected. The sample analysis method in this embodiment is simple in sample pre-treatment, and does not require special preparation of large-size samples. Small-size samples can be directly sampled, and only a placement rack 2 with a placement slot 211 suitable for small-size samples needs to be found. Moreover, the small-size sample loading device can meet the vacuum degree of the glow discharge chamber 52 during the loading process of the small-size samples, and can prevent the samples from falling off, and always ensure that the small-size samples are at the excitation center of the glow light source; it has strong universality and a wide range of applications.

[0073] Furthermore, a Horiba GD Profile 2 type glow discharge spectrometer 5 was selected to perform a depth analysis on a galvanized steel sheet with a size of 4.0 mm × 4.0 mm × 1.0 mm. A placement rack 2 with a pit diameter of 4.0 mm and a depth of 1.0 mm was used to form a small-size sample loading device with an elastic member 3, a shell 1, etc. according to the above description. The test conditions were an argon pressure of 700 Pa, a power of 30 W, a copper anode diameter of 2.0 mm, that is, a sputtering aperture of 2.0 mm, and a glow discharge spectrum depth analysis time of 3.0 min.

[0074] Without the small-size sample loading device of the present application, due to the small size of the galvanized sheet to be tested, the vacuum degree of the discharge chamber cannot meet the requirements before the test begins, and glow discharge cannot be generated, so the small-size sample cannot be deeply analyzed. However, the sputtering pits left on the sample surface are detected by using a profilometer. The small-size sample loading device of the present application can smoothly perform a deep analysis of the galvanized steel. The sputtering pits left on the sample surface are detected by using a profilometer. The detection results are as follows: Figure 4 shown. Figure 4 The sputtering pit morphology obtained after the depth analysis of the embodiment shows that the use of the small-size sample loading device designed by the present invention can ensure that the depth analysis of small-size samples can be carried out smoothly. Figure 5 As shown, by comparing the signal intensity of each element obtained in the embodiment with the change of depth, it can be found that the signal intensity of each element is stable, indicating that the small-size sample loading device designed by the present invention has high stability and good accuracy during the depth test.

[0075] It should be noted that the above embodiments can be freely combined as needed. The above are only preferred embodiments of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be regarded as the protection scope of the present invention.

Claims

1. A sample loading device for a glow discharge spectrometer, characterized in that: include: A housing, wherein a receiving cavity is provided inside the housing, and a first opening communicating with the receiving cavity is also provided at the top of the housing; A placement rack, the placement rack is detachably arranged in the accommodating cavity, the top of the placement rack is suitable for passing through the first opening and abutting against the glow discharge spectrometer, and the top of the placement rack is also provided with a placement groove, and the placement groove is suitable for placing a sample; An elastic member, wherein the elastic member is elastically arranged between the bottom of the placement rack and the bottom of the accommodating chamber, so that the placement rack is elastically arranged in the accommodating chamber; A first sealing member is disposed at the top of the housing and relatively located outside the first opening.

2. A sample loading device for a glow discharge spectrometer according to claim 1, characterized in that: The housing comprises a detachably connected top shell and a base, the first opening and the second opening are respectively provided at two ends of the accommodating cavity, and the base is adapted to be detachably mounted at the second opening and abut against the elastic member; A sealing groove is provided on the top of the top shell, and the first sealing member is arranged in the sealing groove.

3. A sample loading device for a glow discharge spectrometer according to claim 2, characterized in that: The accommodating cavity includes a first cavity and a second cavity, the first cavity is connected to the first opening, the second cavity is connected to the second opening, the diameter of the second opening is larger than the diameter of the first opening, and the placement rack is suitable for passing through the second opening and being arranged in the accommodating cavity; The placement rack is in the shape of a boss and matches the accommodating cavity. The placement rack includes a first frame body matching the first cavity and a second frame body matching the second cavity.

4. A sample loading device for glow discharge spectrometer according to claim 3, characterized in that: The shell is cylindrical; the shell, the placement frame and the elastic member are all made of conductive materials.

5. The sample loading device for glow discharge spectrometer according to claim 2, characterized in that: The bottom of the placement rack is also provided with a first groove, and one end of the elastic member is arranged in the first groove; The top of the base is also provided with a second groove, and the other end of the elastic member is arranged in the second groove.

6. A sample loading device for a glow discharge spectrometer according to any one of claims 1 to 5, characterized in that: The placement groove is relatively located in the center of the top of the placement rack, and the placement rack, the shell and the placement groove are relatively coaxially arranged, so that the sample is suitable for matching with the discharge chamber of the glow discharge spectrometer.

7. A sample loading device for glow discharge spectrometer according to claim 6, characterized in that: A rib is also provided at the outer edge of the top of the shell, and the rib is suitable for abutting against the outer side wall of the glow discharge spectrometer, so that the sample in the placement groove matches the discharge cavity of the glow discharge spectrometer.

8. The sample loading device for glow discharge spectrometer according to claim 7, characterized in that: The top of the shell is also provided with a plurality of limiting columns, which are arranged at intervals around the outer edge of the top of the shell and are suitable for abutting against the outer side wall of the glow discharge spectrometer.

9. The sample loading device for glow discharge spectrometer according to claim 6, characterized in that: A second sealing member is provided outside the discharge chamber of the glow discharge spectrometer, and the first sealing member is relatively located outside the second sealing member; The placement groove has a diameter of 3.0-8.0 mm and a depth of 2.0-6.0 mm.

10. A sample analysis method, applied to the sample loading device according to any one of claims 1 to 9, characterized in that: include: Dry the sample; According to the sample size, select a placement rack with appropriate placement slots; Assembling the placement rack into the shell and arranging an elastic member between the placement rack and the shell; Disposing a first sealing member at the top end of the housing; Install the sample loading device at the test port of the glow discharge spectrometer.

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