Preparation device of ultrathin sheet sample for glow discharge mass spectrometer

By using a preparation device to press ultrathin sheet samples together with high-purity indium sheets, the problems of sample breakdown and contamination in glow discharge mass spectrometry testing are solved. This achieves accurate positioning and tight compaction of ultrathin sheet samples, ensuring the accuracy and stability of the test.

CN224163438UActive Publication Date: 2026-04-24INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
Filing Date
2025-05-15
Publication Date
2026-04-24

AI Technical Summary

Technical Problem

When testing ultrathin sheet samples, existing glow discharge mass spectrometers are prone to sample breakdown and unstable discharge. Furthermore, inadequate compaction can lead to contamination, affecting the accuracy of the test results.

Method used

A preparation apparatus is used, which consists of a dustproof box and an internal sample preparation system. 6N high-purity indium sheet is used as a substrate. The sample preparation system combines and presses the ultrathin sample with the high-purity indium sheet to prevent contamination and ensure stable discharge.

Benefits of technology

It achieves accurate positioning and tight compaction of ultrathin sheet samples, reduces the risk of contamination, ensures the accuracy and stability of testing, and is simple and convenient to operate.

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Abstract

The utility model provides a preparation device of an ultrathin sheet sample for a glow discharge mass spectrometer. The preparation device comprises an external dustproof box and an internal sample preparation system, the dustproof box comprises an air port, an air outlet with a silencer, a dustproof box side door, a side door lock catch, an internal sample preparation system and a tool table; in the internal sample preparation system, fixed seats and a lower fixed mold are respectively arranged on two sides and the center of a bottom plate, and the upper ends of the fixed seats on two sides are connected with a guide rail; the two sliding plates drive the upper die to move downwards, so that the sample and the indium sheet are compressed; the center of the lower end of the upper die moving sliding plate is sequentially connected with an upper die pressing spring, an upper die and a pressing head. Tension springs, pressing claws and pressing wheels are sequentially arranged on the two sides of the center of the lower end of the upper die moving sliding plate. The lower ends of the air inlet pipes are connected with a manual control valve to drive the two sliding plates to move. The device has the advantages that the ultrathin sheet sample for the glow discharge mass spectrometer can be prepared, and the device is simple to operate and not easy to pollute. The sample center can be accurately positioned, and subsequent accurate testing is facilitated.
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Description

Technical Field

[0001] This utility model relates to the field of glow discharge mass spectrometry analysis in chemical composition analysis, specifically to a device for preparing ultrathin sample for glow discharge mass spectrometry. Background Technology

[0002] Material chemical composition analysis is an important part of physicochemical testing. Glow discharge mass spectrometry, as the most effective method for trace element detection, has advantages such as direct solid sample introduction, full element analysis, fast detection speed, wide range, weak matrix effect, stable ion source, and excellent gas element analysis capability. It is widely used in various industries such as pure metals, alloys, ceramics and coatings, and has an irreplaceable position, especially in the fields of high-purity metals and semiconductors. It also provides an important basis for the selection of raw materials for products in various fields.

[0003] In practical applications, glow discharge mass spectrometers are equipped with standard sample clamps, including pin-shaped and flat-shaped clamps. For testing non-standard samples, sample preparation and analysis are necessary, especially for ultrathin sheet samples. Direct testing can result in samples that are too thin and quickly penetrate the clamps, leading to inaccurate results. Thin samples also pose a risk of insufficient compaction, causing discharge gas leakage and unstable discharge. Manually pressing with PTFE rods can result in insufficient pressure, causing samples to detach during testing and more easily contaminating the sample surface. Utility Model Content

[0004] To address the aforementioned issues, this invention provides a device for preparing ultrathin sheet samples for glow discharge mass spectrometry. This device uses 6N high-purity indium sheets as substrates and directly combines and presses the ultrathin sheet samples with the high-purity indium sheets in a dustproof box, ensuring safety, preventing contamination, and achieving high efficiency.

[0005] To solve the above problems, the technical solution adopted by this utility model is as follows:

[0006] An apparatus for preparing ultrathin sample slides for glow discharge mass spectrometry, characterized in that: the apparatus consists of a dustproof box and an internal sample preparation system, wherein:

[0007] The dustproof box includes a dustproof box shell, a dustproof box back door, an air inlet, an air outlet with a silencer, a dustproof box side door, a side door latch, an internal sample preparation system, and a tool table; the sample preparation system consists of a base plate, a fixed seat, a lower fixed mold, a manual control valve, an air inlet pipe one, an air inlet pipe two, a cylinder, an upper fixed plate, a guide rail, an upper mold fixing slide plate, an upper mold moving slide plate, an upper mold clamping spring, an upper mold, a pressure head, a tension spring, pressure claws, and pressure rollers.

[0008] In the sample preparation system, fixed seats and lower fixed molds are respectively located on both sides and the center of the base plate. The upper ends of the fixed seats on both sides are connected to guide rails. The guide rails are respectively equipped with upper mold fixed slide plates and upper mold moving slide plates. The two slide plates drive the upper mold to move downward. When the upper mold fixed slide plate moves to a specific position, it stops moving, while the upper mold moving slide plate continues to move, thus completing the pressing of the sample with the indium sheet. The lower center of the upper mold moving slide plate is connected in sequence with an upper mold clamping spring, the upper mold, and a pressure head. On both sides of its lower center are arranged tension springs, pressure claws, and pressure rollers. The top of the guide rail is equipped with an upper fixed plate. The lower end of the upper fixed plate is connected to a cylinder. The left side of the cylinder is connected to two air inlet pipes, one above the other. The lower end of the air inlet pipes is connected to a manual control valve. Three parallel pipelines at the rear end of the valve are connected to the air inlet and exhaust port of the dustproof box, respectively. Opening the valve will activate the cylinder, thereby driving the movement of the two slide plates.

[0009] As a preferred technical solution:

[0010] The dustproof box has a back door, an air inlet, and an exhaust outlet on the back of the outer shell; a side door and a side door latch on the side; and a sample preparation system and a tool table inside.

[0011] The dustproof box serves to prevent dust contamination of the sample during the sample preparation process by airborne impurities.

[0012] The dustproof box has an exhaust port on the back to allow gas to escape outside the dustproof box, reducing the contamination of the sample by compressed gas; the exhaust port is equipped with a silencer to reduce noise pollution.

[0013] In the sample preparation system, the manual control valve can control the pressure of the pressure head on the sample according to the gas flow rate.

[0014] In the sample preparation system, a circular protrusion is provided at the center of the pressure head, which can mark the center of the sample during the pressing process to avoid improper sample positioning and unstable discharge signal during subsequent clamping.

[0015] In the sample preparation system, the sample can be pressed onto an indium sheet, with the edge of the indium sheet wrapped around the lower fixing mold. After the sample preparation is completed, the lower fixing mold can be directly removed and placed into the sheet-like fixture of the glow discharge mass spectrometer. The operation is simple and not prone to contamination.

[0016] The beneficial effects of this utility model are as follows:

[0017] This instrument enables the preparation of ultrathin sample sheets for glow discharge mass spectrometry (GFMS), offering simple operation and minimizing contamination. It features a dustproof enclosure and exhaust vents to reduce air and gas contamination of the sample surface. The manual control valve allows for adjustment of the gas flow rate based on sample characteristics, enabling the preparation of ultrathin sample sheets at different pressures. A circular protrusion at the center of the pressure head ensures accurate sample centering, facilitating subsequent accurate testing. The instrument tightly presses the ultrathin sheet onto an indium sheet, then firmly presses the edges of the indium sheet into the lower fixing mold. After sample preparation, the lower fixing mold can be directly removed and placed into the sheet-like fixture of the GFMS, making operation convenient. Attached Figure Description

[0018] Figure 1 A three-dimensional view of the dustproof box in the apparatus for preparing ultrathin slide samples for glow discharge mass spectrometry;

[0019] Figure 2 A front view of the dustproof box in the apparatus for preparing ultrathin samples for glow discharge mass spectrometry;

[0020] Figure 3 Rear view of the dustproof box in the apparatus for preparing ultrathin samples for glow discharge mass spectrometry;

[0021] Figure 4 Side view of the dustproof box in the apparatus for preparing ultrathin samples for glow discharge mass spectrometry;

[0022] Figure 5 The sample preparation system inside the dustproof box of the apparatus for preparing ultrathin slide samples for glow discharge mass spectrometry;

[0023] Figure 6 A three-dimensional view of the sample preparation system in the apparatus for preparing ultrathin slide samples for glow discharge mass spectrometry;

[0024] Figure 7 A front view of the sample preparation system in the apparatus for preparing ultrathin samples for glow discharge mass spectrometry;

[0025] Figure 8 Rear view of the sample preparation system in the apparatus for preparing ultrathin samples for glow discharge mass spectrometry;

[0026] Figure 9 A top view of the sample preparation system in the apparatus for preparing ultrathin samples for glow discharge mass spectrometry;

[0027] Figure 10 A bottom view of the sample preparation system in the apparatus for preparing ultrathin samples for glow discharge mass spectrometry;

[0028] Figure 11 A detailed view of the upper mold indenter of the sample preparation system in the apparatus for preparing ultrathin slide samples for glow discharge mass spectrometry.

[0029] Figure 12Detailed image of the sample after pressing using the ultrathin sample preparation device of glow discharge mass spectrometry;

[0030] In the diagram: 1. Dustproof box outer shell, 2. Dustproof box back door, 3. Air inlet, 4. Exhaust port with silencer, 5. Side door latch, 6. Dustproof box side door, 7. Sample preparation system, 8. Tool table, 9. Manual control valve, 10. Pressure head, 11. Upper mold, 12. Upper mold clamping spring, 13. Upper mold fixing slide plate, 14. Second air inlet pipe, 15. First air inlet pipe, 16. Cylinder, 17. Upper fixing plate, 18. Guide rail, 19. Upper mold moving slide plate, 20. Tension spring, 21. Pressure claw, 22. Pressure roller, 23. Lower fixing mold, 24. Fixing base, 25. Base plate. Detailed Implementation

[0031] The present invention will be further described below with reference to the embodiments and the accompanying drawings, but is not limited thereto.

[0032] like Figures 1-4 As shown in the figure, the dustproof box is an external dustproof box for a device used to prepare ultrathin sheet samples for glow discharge mass spectrometry. The dustproof box consists of a dustproof box shell 1, a dustproof box back door 2, an air inlet 3, an air outlet with a silencer 4, a side door latch 5, a dustproof box side door 6, a sample preparation system 7, and a tool table 8. The process involves opening the side door latch 5, cleaning the ultrathin sheet sample and indium sheet from the dustproof box side door 6 and placing them on the tool table 8, closing the dustproof box side door 6, and locking the side door latch 5.

[0033] like Figures 5-10 As shown in the figure, the internal sample preparation system of an ultrathin sample preparation device for glow discharge mass spectrometer is a sample preparation device. The sample preparation system consists of a base plate 25, a fixed seat 24, a lower fixed mold 23, a guide rail 18, an upper mold moving slide plate 19, an upper mold fixing slide plate 13, an upper mold clamping spring 12, an upper mold 11, a pressure head 10, a tension spring 20, a pressure claw 21, a pressure wheel 22, an upper fixed plate 17, a cylinder 16, an air inlet pipe 15, an air inlet pipe 2 14, and a manual control valve 9.

[0034] In the sample preparation system, a fixed seat 24 and a lower fixed mold 23 are respectively provided on both sides and the center of the base plate 25. The upper ends of the fixed seats 24 are connected to guide rails 18. The guide rails 18 are respectively provided with an upper mold fixing slide plate 13 and an upper mold moving slide plate 19. The two slide plates drive the upper mold to move downward. When the pressure head contacts the sample to be tested, the upper mold fixing slide plate 13 stops moving, and the upper mold moving slide plate 19 continues to move downward, completing the pressing of the sample with the indium sheet and the combination of the indium sheet with the lower fixed mold. The lower center of the upper mold moving slide plate 19 is connected in sequence with an upper mold pressing spring. 12. The upper mold 11 and the pressure head 10 are respectively equipped with tension springs 20, pressure claws 21 and pressure rollers 22 on both sides of their lower center; the top of the guide rail 18 is equipped with an upper fixing plate 17, the lower end of which is connected to a cylinder 16. The left side of the cylinder 16 is connected to an air inlet pipe 2 14 and an air inlet pipe 15, respectively. The lower end of the air inlet pipe is connected to a manual control valve 9. The three parallel pipelines at the rear end of the valve are respectively connected to the air inlet 3 and the exhaust port 2 of the dustproof box; opening the manual control valve 9 can realize the operation of the cylinder, and the pressure can be controlled by the air flow.

[0035] Details of the upper mold pressing head in the sample preparation system of the ultrathin sample preparation apparatus for glow discharge mass spectrometry, and details of the sample after pressing using the apparatus. Figure 11 and Figure 12 As shown.

[0036] The sample preparation system can select the pressure according to the characteristics of the sample and the preparation requirements, and can also locate and mark the center of the sample.

[0037] The device is used to polish rod-shaped samples for glow discharge mass spectrometry. The specific steps are as follows: the cleaned and dried indium sheet is placed on the lower fixed mold 23 through the dustproof glove area. The power and compressor are turned on, the manual control valve 9 is opened, and after selecting a suitable gas flow rate, the gas enters the first gas inlet pipe 15 and the second gas inlet pipe 14 through the gas inlet 2. The cylinder 16 starts to move, which in turn drives the upper mold fixed slide plate 13 and the upper mold moving slide plate 19 to move downward together. When the pressure head 10 contacts the sample and begins to apply pressure, the upper mold fixed slide plate 13 stops moving, and the upper mold moving slide plate 19 continues to move downward. The upper mold compression spring 12 begins to contract and receive force. At the same time, the tension springs 20, pressure claws 21, and pressure rollers on both sides continue to move downward close to the lower fixed mold 23, so that the ultrathin sheet sample is pressed firmly onto the indium sheet. The excess part of the indium sheet is pressed firmly onto both sides of the lower fixed mold 23. After the pressing is completed, the lower fixed mold 23 is removed and placed in the sheet sample holder of the glow discharge mass spectrometer, and the experiment can begin. When the manual control valve 9 is closed, excess gas is discharged from the exhaust port 4 with a silencer to the outside of the dustproof box.

[0038] Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the present invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. An apparatus for preparing ultrathin sample for glow discharge mass spectrometry, characterized in that: The apparatus for preparing ultrathin sample for glow discharge mass spectrometry includes an external dustproof box and an internal sample preparation system. The external dust box includes a dust box shell (1), a dust box back door (2), an air inlet (3), an air outlet with a silencer (4), a side door latch (5), a dust box side door (6), a sample preparation system (7), and a tool table (8); Among them: open the side door latch (5), clean the ultra-thin sheet sample and indium sheet to be tested from the side door (6) of the dust box and place them on the tool table (8), close the side door (6) of the dust box and lock the side door latch (5); The internal sample preparation system includes a base plate (25), a fixed seat (24), a lower fixed mold (23), a guide rail (18), an upper mold moving slide plate (19), an upper mold fixing slide plate (13), an upper mold clamping spring (12), an upper mold (11), a pressure head (10), a tension spring (20), a pressure claw (21), a pressure roller (22), an upper fixed plate (17), a cylinder (16), an air inlet pipe one (15), an air inlet pipe two (14), and a manual control valve (9); In the sample preparation system, a fixed seat (24) and a lower fixed mold (23) are respectively provided on both sides and the center of the base plate (25). The upper ends of the fixed seats (24) on both sides are connected to guide rails (18). The guide rails (18) are respectively provided with an upper mold fixed slide plate (13) and an upper mold moving slide plate (19). The two slide plates drive the upper mold to move downward. When the pressure head contacts the sample to be tested, the upper mold fixed slide plate (13) stops moving, and the upper mold moving slide plate (19) continues to move downward, completing the pressing of the sample with the indium sheet and the combination of the indium sheet with the lower fixed mold. The lower center of the upper mold moving slide plate (19) is connected to an upper mold pressing spring (12). The upper mold (11) and the pressure head (10) are provided with tension springs (20), pressure claws (21) and pressure rollers (22) on both sides of the lower center of the mold (11). The top of the guide rail (18) is provided with an upper fixing plate (17). The lower end of the upper fixing plate is connected to the cylinder (16). The upper and lower sides of the left side of the cylinder (16) are connected to the second air inlet pipe (14) and the first air inlet pipe (15). The lower end of the air inlet pipe is connected to the manual control valve (9). The three parallel pipelines at the rear end of the valve are connected to the air inlet (3) and the exhaust port (2) of the dustproof box. The cylinder can be operated by opening the manual control valve (9), and the pressure can be controlled by the air flow.