Sample injection and post-treatment device for industrial analysis of GeF4 isotope and implementation method thereof

Abstract

The invention belongs to the technical field of pretreatment and aftertreatment of industrial analysis of stable isotope gas products, and particularly relates to a sample introduction and aftertreatment device for industrial analysis of GeF4 isotope and an implementation method of the sample introduction and aftertreatment device. The device comprises an on-line and off-line sample introduction system, an industrial analysis system and a product recovery and tail gas collection system which are connected in sequence. The on-line and off-line sample introduction system comprises a sample introduction pipeline, and an on-line sample introduction system, an off-line sample introduction system, an evacuation system and a purging system which are respectively connected to the sample introduction pipeline, the on-line sample introduction system comprises a material supply sampling point, a concentrated material sampling point and a lean material sampling point, and at least one sampling point is selected for sample introduction when the on-line sample introduction system is used for sample introduction; the product recovery and tail gas collection system comprises two or more than two cold traps which are connected in parallel or in series. On-line and off-line sample introduction devices are designed, and a tail gas and product post-treatment device is designed, so that the requirements of GeF4 stable isotope industrial analysis sample introduction and post-treatment are met, and isotope gas detection and recovery are realized.

Description

Technical Field

[0001] The invention belongs to the technical field of pre-processing and post-processing of industrial analysis of stable isotope gas products, and in particular relates to a sampling and post-processing device for industrial analysis of GeF4 isotopes and an implementation method thereof. Background Art

[0002] All stable isotopes of germanium have application value or potential. 72Ge isotopes are mainly used in chip manufacturing in the semiconductor industry. High-purity 72GeF4 gas is used as a preformed implant before the dopant implantation process of silicon wafers to prevent the channeling effect of dopants implanted in silicon wafers. In addition, it can optimize the performance and speed of components and has a significant effect on improving chip performance. 76Ge isotopes have important applications in the field of detectors, especially in cutting-edge scientific fields such as the search for dark matter and the measurement of neutrino mass.

[0003] In recent years, my country has carried out relevant research using germanium, and there is also a certain demand for germanium isotopes. The domestic semiconductor industry has a demand for 100 kilograms of 72Ge isotopes (in the form of GeF4, abundance>50%). In recent years, with the development of science and technology, the application field of GeF4 stable isotopes has continued to expand. After the isotope product is produced, its abundance needs to be detected. In order to realize the online and offline abundance detection of GeF4 stable isotopes, it is necessary to design online and offline sampling and analysis pipelines for the samples to be tested to realize automatic sample injection. The post-processing system is designed to realize sample and exhaust gas post-processing. At present, there is no automatic sampling and sample recovery and exhaust gas collection and post-processing device for industrial analysis of GeF4 stable isotopes in China. Summary of the invention

[0004] In order to solve the problems existing in the above-mentioned prior art, the present invention provides a sampling and post-processing device for industrial analysis of GeF4 isotopes and an implementation method thereof, which can meet the sampling and post-processing requirements of GeF4 stable isotope industrial analysis and realize isotope gas detection and recovery.

[0005] The technical solution adopted by the present invention to solve this problem is: A sampling and post-processing device for industrial analysis of GeF4 isotopes, comprising an online and offline sampling system, an industrial analysis system, a product recovery and tail gas collection system connected in sequence, wherein: An online and offline sampling system, comprising a sampling pipeline and an online sampling system, an offline sampling system, an evacuation system and a purge system respectively connected to the sampling pipeline, wherein the online sampling system comprises a feed sampling point, a concentrate sampling point and a lean material sampling point, and at least one of the sampling points is selected for sampling when the online sampling system is used for sampling, and when the offline sampling system is used for sampling, an offline sampler is used to realize offline sampling; The product recovery and tail gas collection system comprises two or more cold traps which are interconnected in parallel or series and can be converted into each other in series or parallel.

[0006] In the above technical solution, the feed sampling point is connected to the sample injection line through a feed pipeline, and the feed pipeline is provided with a first DN3 valve and a first pneumatic solenoid valve.

[0007] In the above technical solution, the concentrate sampling point is connected to the sample feeding pipeline via a concentrate pipeline, and the concentrate pipeline is provided with a second DN3 valve and a second pneumatic solenoid valve.

[0008] In the above technical solution, the lean material sampling point is connected to the sample feeding line through a lean material pipeline, and the lean material pipeline is provided with a third DN3 valve and a third pneumatic solenoid valve.

[0009] In the above technical solution, the evacuation system includes an evacuation pipeline, and a fourth pneumatic solenoid valve is arranged on the evacuation pipeline.

[0010] In the above technical solution, the purge system includes a purge pipeline, and a fifth pneumatic solenoid valve is arranged on the purge pipeline.

[0011] In the above technical solution, the offline sampling system is connected to the sampling pipeline through an offline pipeline, and the offline pipeline is provided with a fourth DN3 valve and a seventh pneumatic solenoid valve. When using the offline sampling system for sampling, an offline sampler is selected to be connected to the rear end of the fourth DN3 valve.

[0012] In the above technical solution, the sample inlet line is connected to the industrial analysis system through a connecting line, and the connecting line is provided with a sixth pneumatic solenoid valve, a particle filter, and a flow controller.

[0013] In the above technical solution, the industrial analysis system is connected to the product recovery and exhaust gas collection system through a recovery pipeline. One end of the recovery pipeline is branched into at least two recovery input pipelines connected to the industrial analysis system, and the other end is branched into several recovery output pipelines corresponding to each level of cold trap.

[0014] In the above technical solution, each of the cold traps has a cold trap input pipeline and a cold trap output pipeline, the cold trap input pipeline is connected to the recovery output pipeline one by one, the cold trap output pipeline is connected to the discharge pipeline, and a conversion pipeline is also connected between two adjacent cold traps, and the conversion pipeline is connected between the cold trap output pipeline of the upper-level cold trap and the cold trap input pipeline of the next-level cold trap.

[0015] In the above technical solution, the recovery input pipeline, recovery output pipeline, cold trap input pipeline, cold trap output pipeline, discharge pipeline and conversion pipeline are respectively provided with valves for controlling the opening or closing thereof.

[0016] The second invention object of the present invention is to provide an implementation method of a sampling and post-processing device for industrial analysis of GeF4 isotopes, comprising the following steps: S1. Choose to use an online sampling system or an offline sampling system for sampling. If the online sampling system is used for sampling, select one of the feed sampling point, the concentrate sampling point and the lean material sampling point for sampling; S2. If an offline sampling system is used for sampling, an offline sampler is connected to the rear end of the fourth DN3 valve, and offline sampling is realized through the valve of the offline sampler itself and the switch of the fourth DN3 valve; S3, evacuate the industrial analysis system through the evacuation system, replace and purge the vacuum system through the purge system, and the sample enters the online and offline sampling system, and then passes through the particle filter and flow controller to enter the industrial analysis system; S4. Two or more cold traps in the product recovery system can be connected in series or in parallel. Taking a two-stage cold trap as an example, it is divided into a primary cold trap and a secondary cold trap. When conventional tail gas is recovered, the sample enters the secondary cold trap; when product gas is recovered, the sample enters the primary cold trap. When the test sample flow rate is large, the two-stage cold trap is connected in series, and the sample first enters the primary cold trap as a product recovery, and then enters the secondary cold trap, so as to enhance the GeF4 stable isotope gas capture capacity.

[0017] The advantages and positive effects of the present invention are: 1. The present invention designs online and offline sampling devices, designs tail gas and product post-processing devices, realizes the sampling and post-processing requirements of GeF4 stable isotope industrial analysis, and realizes isotope gas detection and recovery.

[0018] 2. The present invention can realize automatic online and offline sampling during industrial analysis of GeF4 stable isotope gas, and realize the collection of GeF4 stable isotope gas tail gas and product gas recovery. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] The technical solution of the present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments, but it should be understood that these drawings are designed only for explanation purposes and are not intended to limit the scope of the present invention. In addition, unless otherwise specified, these drawings are intended only to conceptually illustrate the structural configurations described herein and are not necessarily drawn to scale.

[0020] Figure 1 It is a schematic diagram of the connection between the online and offline injection systems and the industrial analysis system; Figure 2 It is a schematic diagram of the connection of the sampling and post-processing device for industrial analysis of GeF4 isotopes.

[0021] In the figure: 1-feed sampling point, 2-fine material sampling point, 3-lean material sampling point, 4-evacuation pipeline, 5-purge pipeline, 6-injection pipeline, 7-cold trap, 8-connection pipeline, 9-recovery pipeline, 10-discharge pipeline, 11-conversion pipeline, 101-first DN3 valve, 102-second DN3 valve, 103-third DN3 valve, 104-fourth DN3 valve, 105-fifth DN3 valve, 106-sixth DN3 valve, 201 -first DN25 valve, 202-second DN25 valve, 203-third DN25 valve, 204-fourth DN25 valve, 205-fifth DN25 valve, 206-sixth DN25 valve, 301-first pneumatic solenoid valve, 302-second pneumatic solenoid valve, 303-third pneumatic solenoid valve, 304-fourth pneumatic solenoid valve, 305-fifth pneumatic solenoid valve, 306-sixth pneumatic solenoid valve, 307-seventh pneumatic solenoid valve. DETAILED DESCRIPTION

[0022] First of all, it should be noted that the specific structure, features and advantages of the present invention will be specifically described below by way of example, but all descriptions are only for illustration and should not be understood as limiting the present invention. In addition, any single technical feature described or implied in the embodiments mentioned herein, or any single technical feature displayed or implied in the drawings, can still be combined or deleted between these technical features (or their equivalents) to obtain more other embodiments of the present invention that may not be directly mentioned in this document. In addition, in order to simplify the drawings, the same or similar technical features may be marked only in one place in the same drawing.

[0023] In the present invention, unless otherwise clearly specified and limited, the terms "installation", "setting", "connection", "fixation", "screwing" and the like should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral one; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements, unless otherwise clearly defined, for ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to the specific circumstances. The present invention is described in detail below with reference to the accompanying drawings. Example

[0024] A sampling and post-processing device for industrial analysis of GeF4 isotopes, comprising an online and offline sampling system, an industrial analysis system, a product recovery and tail gas collection system connected in sequence, wherein: An online and offline sampling system, comprising a sampling line 6 and an online sampling system, an offline sampling system, an evacuation system and a purge system respectively connected to the sampling line 6, wherein the online sampling system comprises a feed sampling point 1, a concentrate sampling point 2 and a lean material sampling point 3, and at least one of the sampling points is selected for sampling when the online sampling system is used for sampling; when the offline sampling system is used for sampling, an offline sampler is used to realize offline sampling; The product recovery and tail gas collection system comprises two or more cold traps 7 which are interconnected in parallel or in series and can be converted into each other in series or in parallel.

[0025] Furthermore, in this embodiment, it can also be considered that the feed sampling point 1 is connected to the sample injection line 6 through a feed pipeline, and the feed pipeline is provided with a first DN3 valve 101 and a first pneumatic solenoid valve 301.

[0026] Furthermore, in this embodiment, it can also be considered that the concentrate sampling point 2 is connected to the sampling pipeline 6 through a concentrate pipeline, and the concentrate pipeline is provided with a second DN3 valve 102 and a second pneumatic solenoid valve 302 .

[0027] Furthermore, in this embodiment, it can also be considered that the lean material sampling point 3 is connected to the sampling pipeline 6 through a lean material pipeline, and the lean material pipeline is provided with a third DN3 valve 103 and a third pneumatic solenoid valve 303.

[0028] Furthermore, in this embodiment, it can also be considered that the evacuation system includes an evacuation pipeline 4 , and a fourth pneumatic solenoid valve 304 is provided on the evacuation pipeline 4 .

[0029] Furthermore, in this embodiment, it can also be considered that the purge system includes a purge pipeline 5 , and a fifth pneumatic solenoid valve 305 is provided on the purge pipeline 5 .

[0030] Furthermore, in this embodiment, it can also be considered that the offline sampling system is connected to the sampling pipeline 6 through an offline pipeline, and the offline pipeline is provided with a fourth DN3 valve 104 and a seventh pneumatic solenoid valve 307. When using the offline sampling system for sampling, an offline sampler is selected to be connected to the rear end of the fourth DN3 valve 104.

[0031] Furthermore, it can also be considered in this embodiment that the sampling line is connected to the industrial analysis system through a connecting line, and the connecting line is provided with a sixth pneumatic solenoid valve 306, a particle filter, and a flow controller. By designing the online and offline sampling systems of the industrial analysis system, during the operation of the dedicated process system, the working pressures of the three materials of the feed system, the refined material, the lean material, and the feed material are all less than 20 Torr. The online sampling design has 3 low-pressure inlets connected to the feed system. When the sample is injected, the stop valve is opened, and the sample enters the sampling system, and then the low-pressure sample passes through the particle filter and the flow controller and enters the industrial analysis system. When the sample is tested offline, the sample is taken from the purification pouring system to the sampler, and its sample pressure is about 0.1MPa. The sampler is connected to the offline sampling port to realize offline sampling, and then the sample enters the industrial analysis system through the MFC to control the injection pressure.

[0032] Furthermore, it can also be considered in this embodiment that the industrial analysis system is connected to the product recovery and tail gas collection system through a recovery pipeline, one end of the recovery pipeline is branched into at least two recovery input pipelines connected to the industrial analysis system, and the other end is branched into a plurality of recovery output pipelines correspondingly connected to each stage of cold trap 7. Taking this embodiment as an example, one end of the recovery pipeline is branched into two routes, on which the fifth DN3 valve 105 and the sixth DN3 valve 106 are respectively provided.

[0033] Furthermore, in this embodiment, it can also be considered that each of the cold traps 7 has a cold trap input pipeline and a cold trap output pipeline, the cold trap input pipeline is connected to the recovery output pipeline one by one, the cold trap output pipeline is connected to the discharge pipeline, and a conversion pipeline is also connected between two adjacent cold traps 7, and the conversion pipeline is connected between the cold trap output pipeline of the upper-level cold trap and the cold trap input pipeline of the next-level cold trap.

[0034] Furthermore, in this embodiment, it can also be considered that the recovery input pipeline, the recovery output pipeline, the cold trap input pipeline, the cold trap output pipeline, the discharge pipeline, and the conversion pipeline are respectively provided with valves for controlling the opening or closing thereof.

[0035] Taking this embodiment as an example, two-stage cold traps are provided, namely cold trap 1 and cold trap 2, corresponding to two recovery output pipelines, a first DN25 valve 201 is provided on the recovery output pipeline corresponding to cold trap 1, a second DN25 valve 202 and a third DN25 valve 203 are provided on the recovery output pipeline corresponding to cold trap 2, a fifth DN25 valve 205 and a sixth DN25 valve 206 are provided on the discharge pipeline, and a fourth DN25 valve 204 is provided on the conversion pipeline. By designing two-stage cold traps, they can be connected in series or in parallel. When conventional tail gas is recovered, the sample enters cold trap 1, and when product gas is recovered, the sample enters cold trap 2. When the flow rate of the test sample is large, the two-stage cold traps can be connected in series, the sample first enters cold trap 2 as a product recovery, and cold trap 1 is used as a secondary cold trap to enhance the gas capture capacity of GeF4 stable isotopes.

[0036] In this embodiment, as shown in the attached Figure 1-2 As shown, a sampling and post-processing device for industrial analysis of GeF4 isotopes includes online and offline automatic sampling devices, an evacuation system, a purge system, a sampling system, a product recovery and tail gas collection system.

[0037] A dedicated design is adopted to configure an online and offline sampling system for the GeF4 industrial analysis system. Since the working environment of the dedicated separation system is a negative pressure condition close to vacuum, the output samples to be tested are distributed in 1~3Torr. Using fine material (P), feed material (F), and lean material (W), feed material sampling point 1, fine material sampling point 2, and lean material sampling point 3 are set, and the three sampling points are respectively online sampled to achieve different analysis requirements of samples to be tested. When sampling, open one of the first DN3 valve 101, the second DN3 valve 102, and the third DN3 valve 103 for sampling; control one of the first pneumatic solenoid valve 301, the second pneumatic solenoid valve 302, and the third pneumatic solenoid valve 303, and cooperate to open the sixth pneumatic solenoid valve 306 to realize online automatic sampling of the sample to be tested. When sampling offline, open the fourth DN3 valve 104 and control the seventh pneumatic solenoid valve 307 to realize automatic sampling of offline samples. Open the fifth DN3 valve 105 and the sixth DN3 valve 106, control the fourth pneumatic solenoid valve 304 to evacuate the industrial analysis system, and control the fifth pneumatic solenoid valve 305 to achieve vacuum system replacement and purge. The sample enters the online and offline sampling system, and then passes through the particle filter and flow controller to enter the industrial analysis system.

[0038] A two-stage cold trap is designed, which can be connected in series or in parallel. When conventional tail gas is recovered, the sample enters cold trap 1 (open the first DN25 valve 201 and the sixth DN25 valve 206, and close the second DN25 valve 202, the third DN25 valve 203, the fourth DN25 valve 204 and the fifth DN25 valve 205). When product gas is recovered, the sample enters cold trap 2 (close the first DN25 valve 201 and the fourth DN25 valve 204, and open the second DN25 valve 202, the third DN25 valve 203, the fifth DN25 valve 205 and the sixth DN25 valve 206). When the test sample flow is large, the two-stage cold trap can be connected in series (close the first DN25 valve 201 and the fifth DN25 valve 205, open the second DN25 valve 202, the third DN25 valve 203, the fourth DN25 valve 204 and the sixth DN25 valve 206), the sample first enters the cold trap 2 as product recovery, and the cold trap 1 is used as a secondary cold trap to enhance the GeF4 stable isotope gas capture capacity. Example

[0039] An implementation method of a sampling and post-processing device for industrial analysis of GeF4 isotopes, comprising the following steps: S1. Select to use an online sampling system or an offline sampling system for sampling. If the online sampling system is used for sampling, select one of the feed sampling point 1, the concentrate sampling point 2 and the lean material sampling point 3 for sampling; S2, if an offline sampling system is used for sampling, an offline sampler is connected to the rear end of the fourth DN3 valve 104, and offline sampling is realized through the valve of the offline sampler itself and the switch of the fourth DN3 valve 104; S3, evacuate the industrial analysis system through the evacuation system, replace and purge the vacuum system through the purge system, and the sample enters the online and offline sampling system, and then passes through the particle filter and flow controller to enter the industrial analysis system; S4. Two or more cold traps 7 in the product recovery system can be connected in series or in parallel. Taking a two-stage cold trap as an example, it is divided into a primary cold trap and a secondary cold trap. When conventional tail gas is recovered, the sample enters the secondary cold trap; when product gas is recovered, the sample enters the primary cold trap; when the test sample flow rate is large, the two-stage cold trap is connected in series, and the sample first enters the primary cold trap as a product recovery, and then enters the secondary cold trap, so as to enhance the GeF4 stable isotope gas capture capacity.

[0040] The above embodiments describe the present invention in detail, but the contents are only preferred embodiments of the present invention and cannot be considered to limit the scope of the present invention. All equivalent changes and improvements made within the scope of the present invention should still fall within the scope of the present invention.

Claims

1. A sampling and post-processing device for industrial analysis of GeF4 isotopes, characterized in that: It includes online and offline sampling systems, industrial analysis systems, product recovery and tail gas collection systems connected in sequence, including: An online and offline sampling system, comprising a sampling line (6) and an online sampling system, an offline sampling system, an evacuation system and a purge system respectively connected to the sampling line (6), wherein the online sampling system comprises a feed sampling point (1), a concentrate sampling point (2) and a lean material sampling point (3), and when the online sampling system is used for sampling, at least one of the sampling points is selected for sampling, and when the offline sampling system is used for sampling, an offline sampler is used to realize offline sampling; The product recovery and tail gas collection system comprises two or more cold traps (7) which are interconnected in parallel or series and can be converted into each other in series or parallel.

2. The sampling and post-processing device for industrial analysis of GeF4 isotopes according to claim 1, characterized in that: The feed sampling point (1) is connected to the sample injection line (6) via a feed pipeline, and the feed pipeline is provided with a first DN3 valve (101) and a first pneumatic solenoid valve (301); The concentrate sampling point (2) is connected to the sample feeding pipeline (6) via a concentrate pipeline, and a second DN3 valve (102) and a second pneumatic solenoid valve (302) are provided on the concentrate pipeline; The lean material sampling point (3) is connected to the sampling pipeline (6) via a lean material pipeline, and the lean material pipeline is provided with a third DN3 valve (103) and a third pneumatic solenoid valve (303).

3. The sampling and post-processing device for industrial analysis of GeF4 isotopes according to claim 1, characterized in that: The evacuation system comprises an evacuation pipeline (4), and a fourth pneumatic solenoid valve (304) is arranged on the evacuation pipeline (4).

4. The sampling and post-processing device for industrial analysis of GeF4 isotopes according to claim 1, characterized in that: The purge system comprises a purge pipeline (5), and a fifth pneumatic solenoid valve (305) is arranged on the purge pipeline (5).

5. The sampling and post-processing device for industrial analysis of GeF4 isotopes according to claim 1, characterized in that: The offline sampling system is connected to the sampling pipeline (6) via an offline pipeline. The offline pipeline is provided with a fourth DN3 valve (104) and a seventh pneumatic solenoid valve (307). When the offline sampling system is used for sampling, an offline sampler is connected to the rear end of the fourth DN3 valve (104).

6. The sampling and post-processing device for industrial analysis of GeF4 isotopes according to claim 1, characterized in that: The sample inlet pipeline (6) is connected to the industrial analysis system via a connecting pipeline (8), and a sixth pneumatic solenoid valve (306), a particle filter, and a flow controller are provided on the connecting pipeline (8).

7. The sampling and post-processing device for industrial analysis of GeF4 isotopes according to claim 1, characterized in that: The industrial analysis system is connected to the product recovery and tail gas collection system via a recovery pipeline (9); one end of the recovery pipeline (9) is branched into at least two recovery input pipelines connected to the industrial analysis system, and the other end is branched into a plurality of recovery output pipelines correspondingly connected to each stage of the cold trap (7).

8. The sampling and post-processing device for industrial analysis of GeF4 isotopes according to claim 7, characterized in that: Each of the cold traps (7) has a cold trap input pipeline and a cold trap output pipeline, the cold trap input pipeline is connected to the recovery output pipeline in a one-to-one correspondence, the cold trap output pipeline is connected to the discharge pipeline (10), and a conversion pipeline (11) is also connected between two adjacent cold traps (7), and the conversion pipeline (11) is connected between the cold trap output pipeline of the upper-stage cold trap (7) and the cold trap input pipeline of the lower-stage cold trap (7).

9. The sampling and post-processing device for industrial analysis of GeF4 isotopes according to claim 8, characterized in that: The recovery input pipeline, the recovery output pipeline, the cold trap input pipeline, the cold trap output pipeline, the discharge pipeline (10), and the conversion pipeline (11) are respectively provided with valves for controlling the opening or closing thereof.

10. An implementation method of the sampling and post-processing device for industrial analysis of GeF4 isotopes according to any one of claims 1 to 9, characterized in that: The following steps are involved: S1. Select to use an online sampling system or an offline sampling system for sampling. If the online sampling system is used for sampling, select one of the feed sampling point (1), the concentrate sampling point (2) and the lean material sampling point (3) for sampling; S2, if an offline sampling system is used for sampling, an offline sampler is connected to the rear end of the fourth DN3 valve (104), and offline sampling is achieved through the valve of the offline sampler itself and the switch of the fourth DN3 valve (104); S3, evacuate the industrial analysis system through the evacuation system, replace and purge the vacuum system through the purge system, and the sample enters the online and offline sampling system, and then passes through the particle filter and flow controller to enter the industrial analysis system; S4. Two or more cold traps (7) in the product recovery system can be connected in series or in parallel. For example, a two-stage cold trap is divided into a primary cold trap and a secondary cold trap. When conventional tail gas is recovered, the sample enters the secondary cold trap. When product gas is recovered, the sample enters the primary cold trap. When the test sample flow rate is large, the two-stage cold trap is connected in series, and the sample first enters the primary cold trap for product recovery and then enters the secondary cold trap, thereby enhancing the GeF4 stable isotope gas capture capacity.

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