Electronic gas absorption liquid continuous sample injection detection equipment

Abstract

The utility model relates to detection equipment for continuous sample introduction of electronic gas absorption liquid. The detection equipment comprises an ion chromatograph, a peristaltic pump and at least one group of sample introduction components, each group of sample introduction assembly comprises a plurality of gas absorption bottles, a cleaning bottle and a first switching valve, the first switching valve is provided with a plurality of first liquid inlets and a first liquid outlet, the gas absorption bottles and the cleaning bottle are respectively communicated with the corresponding first liquid inlets, the first liquid outlet is communicated with the ion chromatograph, and the first liquid inlet is communicated with the ion chromatograph; a peristaltic pump for providing power for liquid feeding of the ion chromatograph is arranged on an output pipeline of the ion chromatograph; the detection equipment disclosed by the utility model adopts a simple and low-cost structure to replace an existing automatic sampler, and a high-cost long-time nitrogen protection mode is not needed; under the condition of ensuring that the samples are not in contact with the external environment, automatic and continuous sample injection of a plurality of samples is realized, and the accuracy of ultra-trace detection of anions and cations in the electronic gas absorption liquid can be ensured in a specific detection scene aiming at the electronic gas absorption liquid.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of electronic gas detection, in particular to a continuous sampling detection equipment for electronic gas absorption liquid. BACKGROUND

[0002] Electronic gas is the second largest semiconductor manufacturing material next to substrate material, accounting for about 20% of the cost of chip manufacturing materials, including bulk electronic gas, ion implantation gas, thin film deposition gas (chemical vapor deposition, atomic layer deposition, precursor), etching / cleaning gas, etc. Electronic gas is a core material that affects chip manufacturing and device performance.

[0003] With the development of the integrated circuit industry, the use of electronic gas is increasing, and the detection requirements for trace anion and cation impurities in electronic gas are also increasing. For example, GB / T 43772-2024 "Electronic Gas Carbon Dioxide" implemented on October 1, 2024, requires the purity of carbon dioxide products to be 99.999% or higher. So far, related enterprises have required the purity of carbon dioxide products to be 9N, and the limit of anion and cation impurities to be ppb-ppt.

[0004] At present, the detection of trace anion and cation impurities in electronic gas is mainly carried out by enrichment through absorption method. After enrichment is completed, the sample absorption liquid (hereinafter referred to as sample liquid) is transferred to a sampling bottle in an automatic sampler, and then the sample liquid is sucked into an ion chromatograph by the automatic sampler for analysis.

[0005] For general substance detection, the "sampling needle" of the automatic sampler only needs to be inserted into the sample detection bottle, and a small amount of sample substance can be taken "at one time". The bottle opening can be sealed.

[0006] However, the detection of trace anion and cation impurities in electronic gas is relatively special.

[0007] On the one hand, electronic gas sample liquid needs to be transferred from a gas absorption bottle to a specific sampling bottle matched with an automatic sampler. The transfer process can easily contaminate the sample liquid and affect the accuracy of the detection results.

[0008] On the other hand, the content of anion and cation impurities in the sample liquid is very low, so a large amount (volume) of sample liquid is required for detection. For example, the volume of each sample liquid usually reaches several hundred milliliters, and the ion chromatography sampling + detection analysis time for a single sample can be up to about 1 hour. According to the existing "electronic gas trace anion and cation impurity" sampling and detection device, in order to facilitate sampling by the sampling needle, the sampling bottle is designed in an open manner, and the sample liquid is easily affected by the environment, especially when the limit of anion and cation impurities in the sample liquid reaches ppb-ppt, the influence of the environment cannot be ignored.

[0009] Furthermore, not only is the sampling time of each sample liquid long, if multiple sample liquids are sequentially sampled and detected (after the sampling of the sample liquid in a sample bottle is completed, the sampling needle is automatically moved to the next sample bottle to achieve automatic continuous detection), in such a long sampling scenario, it is easy to be contaminated; the nitrogen protection method of the prior art is high in cost and it is troublesome to replace the next batch of samples. Practical new type content

[0010] The present application aims to at least solve one of the technical problems existing in the prior art. To this end, the present application provides a detection equipment for continuous sampling of electronic gas absorption liquid, wherein the detection equipment comprises an ion chromatograph, a peristaltic pump and at least one set of sampling assembly, each set of the sampling assembly comprises a plurality of gas absorption bottles for containing sample liquid, at least one cleaning bottle for containing cleaning liquid and a first switching valve, the first switching valve is a multi-channel switching valve with multiple first liquid inlets and one first liquid outlet, the number of the first liquid inlets is not less than the total number of the gas absorption bottles and the cleaning bottles, a plurality of the gas absorption bottles and the cleaning bottles are respectively communicated with the corresponding first liquid inlets of the first switching valve, the first liquid outlet is communicated with the input pipeline of the ion chromatograph, and the peristaltic pump is arranged on the output pipeline of the ion chromatograph to provide power for the liquid inlet of the ion chromatograph.

[0011] Preferably, the detection equipment comprises a plurality of sets of the sampling assembly.

[0012] The detection equipment further comprises a second switching valve, the second switching valve is a multi-channel switching valve with multiple second liquid inlets and at least one second liquid outlet; the first liquid outlet of each set of the sampling assembly is respectively communicated with the corresponding second liquid inlet; and the second liquid outlet is communicated with the input pipeline of the ion chromatograph.

[0013] Preferably, the detection equipment comprises two sets of the sampling assembly, and the second switching valve is a two-position three-way reversing valve; or the detection equipment comprises more than three sets of the sampling assembly, and the second switching valve is a multi-channel switching valve with multiple second liquid inlets.

[0014] Preferably, the first switching valve and the second switching valve are low-pressure valves.

[0015] Preferably, the first switching valve and the second switching valve are low-pressure valves suitable for 2.5mm-4.5mm pipeline diameter.

[0016] Preferably, the first switching valve and the second switching valve are made of PEEK.

[0017] Preferably, the first switching valve is a multi-channel switching valve with four, six, eight or ten channels; preferably, the first switching valve is a multi-channel switching valve with six channels; preferably, the first switching valve is an SV-07 multi-channel switching valve.

[0018] Preferably, the detection device further comprises a waste liquid container for collecting liquid flowing out of the output pipe of the ion chromatograph; the peristaltic pump is arranged between the ion chromatograph and the waste liquid container.

[0019] Preferably, the peristaltic pump has a pump pipe for communicating the ion chromatograph and the waste liquid container, and the pump pipe is a BPT rubber hose.

[0020] Preferably, the liquid outlet pipe of the gas absorption bottle or the washing bottle is communicated with the corresponding first liquid inlet pipe through a two-way joint.

[0021] The electronic gas absorption liquid continuous sampling detection device of the present application has the following advantages: on the one hand, by arranging a liquid outlet pipe on each gas absorption bottle, the sample liquid in the gas absorption bottle can be output through the liquid outlet pipe, so as to realize the closure of the "sampling bottle mouth" and avoid the pollution of the open gas absorption bottle; on the other hand, a plurality of gas absorption bottles and washing bottles can be communicated with the ion chromatograph in turn through the first switching valve and the related pipes, and further, a plurality of sampling assemblies can be communicated with the ion chromatograph in turn through the second switching valve, so as to ensure that a plurality of sample liquids are continuously input into the ion chromatograph by the power provided by the peristaltic pump without contacting the external environment, thereby realizing automatic and continuous sampling; the electronic gas absorption liquid continuous sampling detection device of the present application uses a simple and low-cost structure to replace the existing automatic sampler (which uses an automatic sampling needle for continuous sampling), and does not need to use a high-cost long-time nitrogen protection mode; in the case of ensuring that the sample does not contact the external environment, the automatic and continuous sampling of a plurality of samples is realized, and in the specific detection scene of the electronic gas absorption liquid, the accuracy of the ultra-trace detection of anions and cations in the electronic gas absorption liquid can be ensured. BRIEF DESCRIPTION OF DRAWINGS

[0022] The present application will be further described below with reference to the accompanying drawings.

[0023] Figure 1 Fig. 1 is a structural schematic diagram of an electronic gas absorption liquid continuous sampling detection device according to an embodiment of the present application.

[0024] BRIEF DESCRIPTION OF DRAWINGS

[0025] 1, ion chromatograph; 2, peristaltic pump; 21, output pipeline; 3, sample injection assembly; 31, gas absorption bottle; 32, cleaning bottle; 33, first switching valve; 334, first liquid inlet; 332, first liquid outlet; 34, liquid outlet pipe; 35, first liquid inlet pipe; 36, two-way joint; 4, second switching valve; 41, second liquid inlet; 52, second liquid outlet; 5, connecting pipeline; 6, three-way joint; 7, waste liquid container; 8, connecting pipeline. DETAILED DESCRIPTION

[0026] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative work fall within the scope of protection of the present application.

[0027] Please refer to Figure 1 As shown in the drawings, the present application provides a detection device for continuous sample injection of electronic gas absorption liquid, which comprises an ion chromatograph 1, a peristaltic pump 2 and at least one set of sample injection assembly 3. Each sample injection assembly 3 comprises a plurality of gas absorption bottles 31 for containing sample liquid, a cleaning bottle 32 for containing cleaning liquid and a first switching valve 33. The first switching valve 33 is a multi-channel switching valve with a plurality of first liquid inlets 334 and a first liquid outlet 332. The number of first liquid inlets 334 is not less than the total number of gas absorption bottles 31 and cleaning bottles 32. The plurality of gas absorption bottles 31 and cleaning bottles 32 are respectively communicated with the corresponding first liquid inlets 334 of the first switching valve 33, and the first liquid outlet 332 is communicated with the input pipeline (not labeled in the figure) of the ion chromatograph 1. The peristaltic pump 2 is arranged on the output pipeline 21 of the ion chromatograph 1, and provides power for the liquid inlet of the ion chromatograph 1.

[0028] The detection device of the embodiment is powered by the peristaltic pump 2, so that the sample liquid in each gas absorption bottle 31 and the cleaning liquid in the cleaning bottle 32 can be transported into the ion chromatograph 1 through the input pipeline. By setting the first switching valve 33, the communication state of each gas absorption bottle 31 and the cleaning bottle 32 with the ion chromatograph 1 can be switched. For example, first, the cleaning bottle 32 is communicated through the first switching valve 33, the peristaltic pump 2 is started, so that the cleaning liquid enters the ion chromatograph 1 through the first liquid outlet 332 and the input pipeline of the ion chromatograph 1 to perform pipeline cleaning work (to prevent the ion chromatograph 1 and the pipeline along the way from being contaminated by the residual sample liquid and causing pollution to the subsequent detection); then the peristaltic pump 2 is closed; the first switching valve 33 is switched to communicate the first gas absorption bottle 31, and the peristaltic pump 2 is started to make the sample liquid in the first gas absorption bottle 31 continuously enter the ion chromatograph 1 through the first liquid outlet 332 and the input pipeline of the ion chromatograph 1 to perform detection, and after the detection of the first sample liquid is completed, the peristaltic pump 2 is closed; the first switching valve 33 is switched again to communicate the cleaning bottle 32 to perform pipeline cleaning work; then the detection of the second sample liquid is performed. That is, after the detection of the sample liquid in one gas absorption bottle 31 is completed, the cleaning bottle is communicated through the switching of the first switching valve 33 to perform pipeline cleaning work, and the next gas absorption bottle 31 is communicated through the switching of the first switching valve 33 to complete the detection of the next sample liquid, and the process is repeated until the detection of the sample liquid in all the gas absorption bottles 31 of the first sample injection assembly 3 is completed.

[0029] In the embodiment, the number of gas absorption bottles 31 included in each sample injection assembly 3 can be set according to the required amount of sample liquid.

[0030] In a preferred embodiment of the present application, the first switching valve 33 can be a multi-channel switching valve with four, six, eight or ten channels.

[0031] In particular, in the embodiment, the first switching valve 33 is a multi-channel switching valve with six channels.

[0032] In a preferred embodiment of the present application, the first switching valve 33 is a low-pressure valve. In particular, in the embodiment, the first switching valve 33 is a low-pressure multi-channel switching valve, specifically an SV-07 multi-channel switching valve with six channels.

[0033] In a preferred embodiment of the present application, the detection device includes multiple sample injection assemblies 3; the detection device further includes a second switching valve 4, which is a multi-channel switching valve with multiple channels or a multi-way reversing valve; the second switching valve 4 has multiple second liquid inlets 41 and at least one second liquid outlet 42; the first liquid outlet 332 of each sample injection assembly 3 is communicated with a corresponding second liquid inlet 41; and the second liquid outlet 42 is communicated with the input pipeline of the ion chromatograph 1.

[0034] With such a structure, continuous detection of sample liquid of multiple sets of gas absorption bottles 31 can be achieved. Specifically, after the detection of sample liquid of all gas absorption bottles 31 of the first set of sampling assembly 3 is completed, the second switching valve 4 is switched to connect the second set of sampling assembly 3, and then the detection of sample liquid of all gas absorption bottles 31 of the second set of sampling assembly is sequentially completed through switching of the first switching valve 33 in the second set of sampling assembly 3. This is repeated. In specific detection practice, through setting of a control program, the automatic and continuous detection of multiple sample liquids per set and multiple sample liquids can be achieved.

[0035] The number of sampling assemblies 3 can be adjusted according to the number of sample liquids to be detected, and is not specifically limited herein.

[0036] Specifically in this embodiment, the detection device includes two sets of sampling assemblies 3, and the second switching valve 4 is a two-position three-way reversing valve. In alternative embodiments of the present application, the detection device includes more sampling assemblies 3, such as three or more sets of sampling assemblies 3, and the second switching valve 4 is a multi-channel switching valve with one inlet and multiple outlets.

[0037] In this embodiment, there are two sets of sampling assemblies 3, and the second switching valve 4 is a two-position three-way reversing valve, having two second liquid inlets 41 and one second liquid outlet 42. The first liquid outlets 332 of the two sets of sampling assemblies 3 are respectively communicated with the two second liquid inlets 41 of the second switching valve 4 through the connecting pipelines 5. The second liquid outlet 42 of the second switching valve 4 is communicated with the connecting pipeline 8.

[0038] Specifically in this embodiment, the connecting pipeline 8 is respectively communicated with the cation detection port and the anion detection port of the ion chromatograph 1 through the three-way joint 6, so that the sample liquid is divided through the three-way joint 6 and flows into the ion chromatograph 1 from the cation detection port and the anion detection port respectively to perform detection of anion content and detection of cation content respectively.

[0039] In the detection device of this embodiment, there are two sets of sampling assemblies 3, and the first switching valve 33 in each set of sampling assembly 3 is a multi-channel switching valve with one inlet and six outlets, which can be connected to and process at most 5 gas absorption bottles 31 (at least one cleaning bottle 32); in this way, sample liquid of 10 gas absorption bottles 31 can be processed continuously at one time.

[0040] In a preferred embodiment of the present application, the first switching valve 33 and the second switching valve 4 are low-pressure valves. In a more preferred embodiment of the present application, the first switching valve 33 and the second switching valve 4 are low-pressure valves suitable for a 2.5mm-4.5mm pipeline diameter. More preferably, in this embodiment, the first switching valve 33 and the second switching valve 4 are low-pressure valves suitable for an eighth of an inch (0.3175mm) pipeline diameter.

[0041] In this embodiment, the first switching valve 33 and the second switching valve 4 are made of PEEK, so as to avoid corrosion of the first switching valve 33 and the second switching valve 4 and improve the durability of the first switching valve 33 and the second switching valve 4.

[0042] In this technical field, the place for preparing the sample liquid is usually different from the place for detecting the sample liquid. After the sample liquid is prepared, the gas absorption bottle 31 containing the sample liquid needs to be transported to the place for detecting the sample liquid and connected with the first switching valve 33.

[0043] In order to avoid the sample liquid from being contaminated in the transportation process and in the detection process, in a preferred embodiment of the present application, the liquid outlet pipe 34 is arranged on each of the gas absorption bottle 31 and the cleaning bottle 32 in each of the sample inlet assemblies 3, the first liquid inlet pipe 35 is arranged on the first liquid inlet port 334 of the first switching valve 33, and the first liquid outlet pipe 34 and the first liquid inlet pipe 35 are connected through the two-way joint 36.

[0044] In this embodiment, the two-way joint 36 is connected with the upstream and downstream pipes through the inverted taper joint to realize the sealed connection. In this embodiment, the connection between all the valves and the pipes is also realized through the inverted taper joint to realize the sealed connection. The inverted taper joint can be made of PEEK.

[0045] With such a structure, the liquid outlet pipe 34 is arranged on each of the gas absorption bottles 31, so that the sample liquid in the gas absorption bottle 31 can be output through the liquid outlet pipe 34, thereby realizing the closed “sample bottle mouth” and avoiding the sample liquid from being contaminated in the transportation process and especially in the detection process due to the open placement of the gas absorption bottle 34.

[0046] In a preferred embodiment of the present application, the detection device further comprises a waste liquid container 7 for collecting the liquid (sample liquid and cleaning liquid) flowing out of the output pipe 21 of the ion chromatograph 1, and the peristaltic pump 2 is arranged on the output pipe 21 between the ion chromatograph 1 and the waste liquid container 7.

[0047] The peristaltic pump 2 has a pump pipe (arranged on the output pipe 21) for connecting the ion chromatograph 2 and the waste liquid container 7. In this embodiment, the pump pipe is made of BPT rubber hose, which has a long service life, reduces the frequency of replacing the pump pipe, and reduces the maintenance cost.

[0048] The above describes one embodiment of the present application in detail, but the above description is only a preferred embodiment of the present application and cannot be considered as limiting the scope of the present application. Any equivalent changes and improvements made within the scope of the present application should still belong to the scope of the patent coverage of the present application.

[0049] It should be noted that the terms "first", "second", and similar terms used in the present application do not denote any order, quantity, or importance, but are only used to distinguish different components. The description of the present application with respect to "left", "right", "left side", "right side", "upper", "lower", "top", "bottom", and the like are defined based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the structure must be constructed and operated in a particular orientation, therefore, it cannot be understood as a limitation on the present application. In the description of the present application, the meaning of "a plurality of" is two or more, unless otherwise explicitly specified and limited.

[0050] In the description of the present application, unless otherwise explicitly specified and limited, the terms "connected", "connected", "connected" should be understood broadly, for example, it can be fixedly connected, or it can be detachably connected, or integrally connected; it can be directly connected, or indirectly connected through an intermediate medium, it can be the communication inside two elements. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

Claims

1. An apparatus for detecting a continuous sample of an electronic gas absorption solution, characterized by, The detection device comprises an ion chromatograph, a peristaltic pump, and at least one set of sample injection assembly, each set of sample injection assembly comprising a plurality of gas absorption bottles for containing sample liquid, at least one cleaning bottle for containing cleaning liquid, and a first switching valve, the first switching valve being a multi-port multi-channel switching valve having a plurality of first liquid inlets and a first liquid outlet, the number of first liquid inlets being not less than the total number of gas absorption bottles and cleaning bottles, the plurality of gas absorption bottles and cleaning bottles being respectively communicated with the corresponding first liquid inlets of the first switching valve, the first liquid outlet being communicated with the input pipeline of the ion chromatograph, and the peristaltic pump being arranged on the output pipeline of the ion chromatograph to provide power for the liquid inlet of the ion chromatograph.

2. The detection apparatus of claim 1, wherein The detection device comprises a plurality of sets of sample injection assembly. The detection device further comprises a second switching valve, the second switching valve being a multi-port multi-channel switching valve or a multi-way reversing valve, the second switching valve having a plurality of second liquid inlets and at least one second liquid outlet, the first liquid outlet of each set of sample injection assembly being respectively communicated with the corresponding second liquid inlets, and the second liquid outlet being communicated with the input pipeline of the ion chromatograph.

3. The apparatus according to claim 2, wherein The detection device comprises two sets of sample injection assembly, and the second switching valve is a two-position three-way reversing valve; or the detection device comprises more than three sets of sample injection assembly, and the second switching valve is a multi-port multi-channel switching valve.

4. The apparatus according to claim 3, wherein The first switching valve and the second switching valve are low-pressure valves.

5. The apparatus according to claim 4, wherein The first switching valve and the second switching valve are low-pressure valves suitable for 2.5mm-4.5mm pipeline diameter.

6. The apparatus according to claim 4, wherein The first switching valve and the second switching valve are made of PEEK.

7. The apparatus according to claim 1, wherein The first switching valve is a one-port-four, one-port-six, one-port-eight, or one-port-ten multi-channel switching valve.

8. The apparatus according to claim 7, wherein The first switching valve is a one-port-six multi-channel switching valve.

9. The detection apparatus of claim 8, wherein, The first switching valve is an SV-07 multi-channel switching valve.

10. The apparatus according to any one of claims 1 to 9, wherein The detection device further comprises a waste liquid container for collecting liquid flowing out of the output pipeline of the ion chromatograph, and the peristaltic pump is arranged between the ion chromatograph and the waste liquid container.

11. The detection apparatus of claim 10, wherein, The peristaltic pump has a pump tube for communicating the ion chromatograph and the waste liquid container, and the pump tube is a BPT rubber hose.

12. The apparatus according to any one of claims 1 to 9, wherein The liquid outlet of the gas absorption bottle or the cleaning bottle is communicated with the corresponding first liquid inlet through a two-way joint.

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