Sample protection device

Abstract

The utility model provides a kind of sampling protection device, including bottle body, two sealing gaskets, catheter and adsorption filler.Bottle body includes two bottle mouths respectively located at its both ends, two sealing gaskets are covered in two bottle mouths one by one, catheter is installed in bottle body, catheter includes several adsorption holes on its peripheral wall, two ends of catheter are open, two ends of catheter are respectively one by one correspondingly towards two sealing gaskets, adsorption filler is filled in bottle body and located at the outside of catheter.The utility model is through the synergistic effect of bottle body, sealing gasket, catheter and adsorption filler, in the whole process of sample from reagent bottle extraction to transfer into analytical instrument sample inlet, continue to adsorb infiltrated or residual water vapor and oxygen, form local low water low oxygen environment around the needle head of sampling needle, effectively avoid that sample is contaminated, improve the accuracy of sample detection analysis result.

Description

Technical Field

[0001] This utility model belongs to the field of semiconductor material analysis technology, and specifically relates to a sampling protection device. Background Technology

[0002] In semiconductor manufacturing processes, high-purity precursors are key raw materials for core structures such as epitaxial layers, metal wiring, and dielectric layers. Their purity level directly determines the chip's performance, yield, and reliability. As integrated circuit manufacturing processes reach below 7nm, the impact of trace impurities in precursors (including metal ions, non-metallic impurities, and particulate matter) on device characteristics becomes increasingly prominent. Impurities can significantly interfere with carrier mobility, reduce breakdown voltage, and even directly lead to device failure.

[0003] Materials analysis is the core method for evaluating whether the purity of precursors meets the aforementioned stringent standards. However, high-purity precursors typically possess high chemical reactivity, making them highly susceptible to interference from water vapor and oxygen in the environment during analysis. The presence of water vapor and oxygen can not only trigger side reactions such as hydrolysis and oxidation of the precursors, generating new components and thus interfering with the accurate determination of the purity of the main component, but may even prevent the effective quantification of the target analyte. Furthermore, modern precision analytical instruments such as inductively coupled plasma mass spectrometry, atomic absorption spectrometry, gas chromatography-mass spectrometry, and X-ray photoelectron spectroscopy are extremely sensitive to water vapor and oxygen. Detecting water vapor and oxygen in the sample introduces background noise, spectral interference, and equipment wear, severely impacting the accuracy and reproducibility of the analytical results.

[0004] However, current methods for sampling precursors typically involve using a sampling needle to extract the precursor sample from a reagent bottle. During the sampling process, the sampling needle and the bottle opening are not protected with an inert atmosphere or dried. Moisture and oxygen remaining on the needle tip, the stopper puncture site, or in the outside air can directly mix into the sample, causing subsequent analytical data to deviate from the true values, resulting in inaccurate detection and analysis results. Utility Model Content

[0005] The purpose of this invention is to provide a sampling protection device to solve the problem that samples are easily contaminated when sampling with a sampling needle.

[0006] To achieve the above objectives, a specific embodiment of this utility model provides a sampling protection device, which includes a bottle body, two sealing gaskets, a conduit, and an adsorption filler. The bottle body includes two openings located at its two ends, and the two sealing gaskets cover the two openings respectively. The conduit is installed inside the bottle body and includes a plurality of adsorption holes on its peripheral wall. The two ends of the conduit are open and face the two sealing gaskets respectively. The adsorption filler fills the bottle body and is located outside the conduit.

[0007] In one or more embodiments of this utility model, the outer circumferential surface of the conduit is provided with a one-way water-permeable and air-permeable layer, and water vapor and gas inside the conduit can enter the adsorption packing through the adsorption pores.

[0008] In one or more embodiments of this utility model, the bottle body includes a bottle body portion and two bottle neck portions disposed at both ends of the bottle body portion, with the bottle mouth formed at the bottle neck portion; the sampling protection device also includes two bottle caps, which are installed at the two bottle neck portions, and each bottle cap includes a through hole that exposes a sealing gasket.

[0009] In one or more embodiments of this utility model, the through hole is coaxially arranged with the conduit, and the diameter of the through hole is less than or equal to the inner diameter of the conduit.

[0010] In one or more embodiments of this invention, a sealing gasket is clamped between the bottle neck and the bottle cap.

[0011] In one or more embodiments of this utility model, the bottle body includes a bottle body portion and two bottle neck portions disposed at both ends of the bottle body portion, and the two ends of the conduit extend into the interior of the two bottle neck portions respectively, with the outer diameter of the conduit equal to the inner diameter of the bottle neck portion.

[0012] In one or more embodiments of this utility model, the sealing gasket is adhered to the bottle mouth.

[0013] In one or more embodiments of this utility model, the two ends of the conduit are respectively abutted against two sealing gaskets.

[0014] In one or more embodiments of this utility model, the conduit includes a main body segment wrapped with adsorption filler, wherein the spacing between the adsorption holes in the middle region of the main body segment is smaller than the spacing between the adsorption holes in the end region of the main body segment, and the diameter of the adsorption holes in the middle region of the main body segment is larger than the diameter of the adsorption holes in the end region of the main body segment.

[0015] In one or more embodiments of this utility model, the sealing gasket is made of polypropylene, polytetrafluoroethylene, perfluoroalkoxy resin or silicone.

[0016] In one or more embodiments of this utility model, the adsorption filler includes silica gel, activated molecular sieve, montmorillonite, iron particle oxygen absorber, or particle desiccant.

[0017] In one or more embodiments of this invention, the conduit is made of glass, quartz, or stainless steel.

[0018] Compared with existing technologies, this invention utilizes the synergistic effect of the bottle, sealing gasket, conduit, and adsorption filler to continuously adsorb infiltrated or residual water vapor and oxygen throughout the entire process from sample extraction from the reagent bottle to transfer into the sample inlet of the analytical instrument. This creates a localized low-water, low-oxygen environment around the sampling needle tip, effectively preventing sample contamination and improving the accuracy of sample detection and analysis results. Attached Figure Description

[0019] To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0020] Figure 1 This is a schematic diagram of the sampling protection device in one embodiment of the present invention;

[0021] Figure 2 This is an exploded structural diagram of the sampling protection device in one embodiment of the present invention;

[0022] Figure 3 for Figure 2 A magnified view of part A in the middle;

[0023] Figure 4 This is a flowchart illustrating the operation of a sampling protection device in one embodiment of the present invention.

[0024] Explanation of main reference numerals: 1. Bottle body, 11. Bottle body, 12. Bottle neck, 121. Bottle mouth, 2. Sealing gasket, 3. Conduit, 31. Adsorption pore, 4. Adsorption packing material, 5. One-way water and air permeable layer, 6. Bottle cap, 61. Through hole, 7. Reagent bottle, 8. Sampling needle, 81. Syringe, 9. Analytical instrument. Detailed Implementation

[0025] To enable those skilled in the art to better understand the technical solutions in this disclosure, the technical solutions in the embodiments of this disclosure will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this disclosure, and not all embodiments. Based on the embodiments in this disclosure, all other embodiments obtained by those skilled in the art without creative effort should fall within the scope of protection of this disclosure.

[0026] In the description of this utility model, it should be understood that the terms "top", "bottom", "upper", "lower", "front", "rear", "left", "right", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this utility model.

[0027] Furthermore, the term "first" is used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Thus, features defined as "first" or "second" may explicitly or implicitly include one or more of the stated features. In the description of this utility model, "a plurality of" means two or more, unless otherwise explicitly specified.

[0028] In one embodiment, reference is made to Figures 1 to 3 As shown, this utility model provides a sampling protection device, which includes a bottle body 1, two sealing gaskets 2, a conduit 3, and an adsorption filler 4. The bottle body 1 includes two bottle openings 121 located at its two ends. The two sealing gaskets 2 can be attached to and fixed to the two bottle openings 121 one-to-one by means of adhesive, sealing the bottle openings 121 and enclosing the internal space of the bottle body 1. The conduit 3 is installed inside the bottle body 1, and several adsorption holes 31 are formed on its peripheral wall. Both ends of the conduit 3 are open, and each end faces one-to-one towards the two sealing gaskets 2. The adsorption filler 4 fills the interior of the bottle body 1 and is located outside the conduit 3. The adsorption filler 4 can adsorb impurities such as water vapor and oxygen inside the bottle body 1, and in particular, it can adsorb impurities such as water vapor and oxygen inside the conduit 3 through the adsorption holes 31.

[0029] Reference Figure 4 As shown, during the actual sampling process, the operator can tightly attach one end of the sampling protection device to the mouth 121 of the reagent bottle 7 (containing a high-purity precursor sample). The operator inserts the needle tube 81 of the sampling needle 8 into the bottle 1 from the top of the sampling protection device. The needle tube 81 passes through the sealing gasket 2 at the top, the inner cavity of the conduit 3, and the sealing gasket 2 at the bottom, finally entering the interior of the reagent bottle 7. The conduit 3 provides a penetration path for the needle tube 81, preventing the needle tube 81 from directly contacting the adsorption packing 4, and limiting the needle tube 81 from making large deviations. After the needle tube 81 enters the reagent bottle 7, the operator can pull the piston rod of the sampling needle 8 to extract the sample into the interior of the sampling needle 8.

[0030] After sampling, the syringe 81 is withdrawn from the reagent bottle 7, allowing the needle tip to retract into the interior of the delivery tube 3. At this point, the needle tip is positioned between the two sealing gaskets 2, without retracting from the top sealing gasket 2. Subsequently, the sampling protection device, along with the sampling needle 8, is transferred to the inlet of the analytical instrument 9. During the transfer process, the adsorption packing 4 continuously absorbs impurities such as water vapor and oxygen that have seeped into or remained in the delivery tube 3 through the adsorption pores 31 on the delivery tube 3, creating a localized low-water, low-oxygen environment inside the delivery tube 3 and outside the syringe 81, thus preventing contamination of the outer wall of the syringe 81 and the sample by impurities during the transfer process.

[0031] After reaching the inlet of the analyzer 9, the operator first places the bottom end of the sampling protection device against the inlet of the analyzer 9, then pushes the sampling needle 8 so that the needle tube 81 pierces the sealing gasket 2 at the bottom and enters the inlet of the analyzer 9. Then, the operator pushes the piston rod of the sampling needle 8 to accurately inject the sample into the inlet, thus completing the injection.

[0032] Throughout the sampling process, the two sealing gaskets 2 maintain a seal after puncture due to the elasticity of the material. Together with the physical isolation of the catheter 3 and the continuous purification of the adsorption packing 4, they achieve the adsorption of impurities throughout the entire process from sample extraction to injection, thereby ensuring the accuracy of high-purity precursor purity analysis.

[0033] In one embodiment, reference is made to Figure 3 As shown, the outer circumferential surface of the conduit 3 is provided with a one-way permeable and breathable layer 5. This layer 5 only allows water vapor and gas inside the conduit 3 to enter the adsorption packing 4 through the adsorption holes 31, but does not allow water vapor and gas outside the conduit 3 that has not been absorbed by the adsorption packing 4 in time to enter the conduit 3 in the reverse direction. Furthermore, the one-way permeable and breathable layer 5 also intercepts solid particles, preventing the adsorption packing 4 from entering the adsorption holes 31 and causing blockage, thus maintaining the long-term conductivity of the adsorption holes 31 and ensuring that impurities such as water and oxygen can be continuously and efficiently adsorbed. In addition, the one-way permeable and breathable layer 5 also prevents the adsorption packing 4 from falling into the conduit 3 through the adsorption holes 31, preventing the adsorption packing 4 from contacting the needle tube 81 inside the conduit 3, avoiding contamination of the needle tube 81 by the adsorption packing 4, and also preventing the adsorption packing 4 from entering the conduit 3 and obstructing the movement of the needle tube 81.

[0034] Furthermore, the one-way permeable and breathable layer 5 can be made of porous materials with microporous structures, such as polytetrafluoroethylene microporous membranes, polyethersulfone microporous membranes, cellulose acetate membranes, or nylon microporous filter membranes. These materials themselves have a large number of microporous structures, and the pore size of the micropores is usually controlled between 0.1 and 1.0 μm. This pore size range allows water molecules and gas molecules such as oxygen to pass through freely, while effectively intercepting larger adsorption filler particles 4.

[0035] In one embodiment, reference is made to Figure 2As shown, the bottle body 1 includes a bottle body portion 11 and two bottle neck portions 12. The two bottle neck portions 12 are respectively disposed at both ends of the bottle body portion 11, and the two bottle neck portions 12 are integrally formed with the bottle body portion 11. The outer diameter of the bottle neck portion 12 is usually smaller than the outer diameter of the bottle body portion 11. The bottle body portion 11 is used to accommodate the adsorbent filler 4, and the bottle mouth 121 is formed at the end of the bottle neck portion 12 away from the bottle body portion 11.

[0036] Furthermore, the sampling protection device also includes two bottle caps 6, which are respectively installed at the two bottle necks 12. The outer circumference of the bottle neck 12 is provided with external threads, and the inner circumference of the bottle cap 6 is provided with internal threads that mate with these external threads, allowing the bottle neck 12 and bottle cap 6 to be threadedly connected, achieving a tight fit. Alternatively, a snap-fit ​​structure can be used between the bottle neck 12 and bottle cap 6 for quick assembly and disassembly. Each bottle cap 6 has a through hole 61 along its axial direction, positioned directly opposite the sealing gasket 2 to expose the sealing gasket 2 covering the bottle opening 121. The bottle cap 6 protects the sealing gasket 2, preventing damage to its surface due to impact or scratches, thereby ensuring the sealing integrity of the sealing gasket 2.

[0037] Furthermore, the through hole 61 is coaxially arranged with the conduit 3. The cross-sectional shape of the through hole 61 and the conduit 3 is circular. The diameter of the through hole 61 is less than or equal to the inner diameter of the conduit 3. This ensures that after the sampling needle 8 is inserted through the through hole 61, the needle tube 81 can smoothly enter the inner cavity of the conduit 3, avoiding bending, jamming or scratching of the needle tube 81 due to eccentricity or sudden change in diameter, thereby improving the smoothness of the sampling operation and the positioning accuracy.

[0038] Furthermore, the sealing gasket 2 is clamped between the neck portion 12 and the cap 6, thereby better fixing the position of the sealing gasket 2 and preventing it from shifting or deflecting during sampling. In some cases, the position of the sealing gasket 2 can be fixed solely by the clamping force applied to it by the neck portion 12 and the cap 6, eliminating the need to use adhesive to attach the sealing gasket 2 to the bottle opening 121, thus avoiding potential contamination from adhesive residues.

[0039] Furthermore, the two ends of the conduit 3 extend into the interior of the two bottleneck sections 12 respectively. The outer diameter of the conduit 3 is equal to the inner diameter of the bottleneck section 12. The outer circumferential surface of the conduit 3 and the inner circumferential surface of the bottleneck section 12 can form a tight fit, realizing the axial and circumferential positioning of the conduit 3, preventing the conduit 3 from shaking or shifting within the bottle body 1, and ensuring that the conduit 3 and the through holes 61 at both ends remain coaxial. In addition, the gapless fit between the conduit 3 and the bottleneck section 12 can effectively prevent the adsorption packing 4 from migrating from the gap between the conduit 3 and the bottleneck section 12 to the bottle mouth 121 area, avoiding contamination of the bottle mouth 121 area by the packing particles, and preventing external gas from entering the interior of the conduit 3 along the gap between the conduit 3 and the bottleneck section 12, thereby enhancing the overall airtightness of the sampling protection device.

[0040] Furthermore, each end of the catheter 3 abuts against one of the two sealing gaskets 2. This abutting structure axially limits the catheter 3 within the bottle body 1, preventing displacement during use or transportation. Simultaneously, the ends of the catheter 3 support the sealing gaskets 2. When the sampling needle 8 pierces the gasket, the gasket is held in place by the catheter 3 and does not excessively indent into the bottle body 1, thus maintaining the stability of the puncture point and the rebound sealing effect, preventing seal failure or puncture path deviation due to gasket deformation.

[0041] In one embodiment, the conduit 3 includes a main body segment wrapped with adsorbent packing 4. Generally, adsorption holes 31 can be formed only on the main body segment of the conduit 3, while other areas of the conduit 3 (e.g., the area within the bottleneck 12) may not have adsorption holes 31. The spacing between the adsorption holes 31 in the middle region of the main body segment is smaller than that in the end region of the conduit 3. During sampling, when the needle is withdrawn from the reagent bottle 7 and retracted into the conduit 3, the needle mostly remains in the middle region of the main body segment. Therefore, the adsorption demand for water and oxygen is higher in the middle region. By reducing the spacing between the holes in the middle region (i.e., increasing the pore density per unit length), the efficiency of water and oxygen diffusion from the inner cavity of the conduit 3 to the external adsorbent packing 4 can be significantly improved, thereby removing residual water vapor and oxygen around the needle more quickly and thoroughly. Correspondingly, the end region of the main body segment is closer to the sealing gasket 2. Using a larger pore spacing can reduce the local exposure of the adsorbent packing 4, reduce the risk of packing loosening or falling off due to puncture, and avoid excessive opening that weakens the structural strength of the conduit 3.

[0042] Furthermore, the pore diameter of the adsorption pores 31 in the middle region of the main body section is larger than that in the end region of the main body section. Increasing the pore diameter in the middle region can increase the flux of water vapor and oxygen diffused from the inner cavity of the conduit 3 to the outside per unit time, thereby enhancing the adsorption efficiency of the adsorption packing 4 for water and oxygen.

[0043] As a non-limiting reference example, the total length of the conduit 3 can be set to 50 mm to 140 mm, the length of the main body segment can be set to 30 mm to 100 mm, the area at each end of the conduit 3, which accounts for one-quarter of the length of the conduit 3, is the end region, and the remaining part in the middle of the conduit 3 (i.e., the area whose length accounts for half of the total length) is the middle region. The diameter of the adsorption holes 31 in the middle region can be set to 0.3 mm to 0.8 mm, and the hole spacing can be set to 1 mm to 3 mm. The diameter of the adsorption holes 31 in the end region can be set to 0.1 mm to 0.3 mm, and the hole spacing can be set to 4 mm to 8 mm.

[0044] In one embodiment, the sealing gasket 2 may be made of common flexible sealing materials such as polypropylene, polytetrafluoroethylene, perfluoroalkoxy resin or silicone.

[0045] In one embodiment, the adsorption filler 4 includes, but is not limited to, silica gel, activated molecular sieve, montmorillonite, iron particle oxygen absorber, and particle desiccant.

[0046] Furthermore, the adsorbent filler 4 can be wrapped in a breathable packaging bag, such as a bag made of non-woven fabric, filter paper or microporous breathable membrane, which allows water vapor and oxygen to pass freely while confining the filler particles inside the bag, making it easy to assemble and replace.

[0047] In one embodiment, the conduit 3 may be made of common hard materials such as glass, quartz, or stainless steel.

[0048] The above describes the general structure of the sampling protection device provided by this utility model. As can be seen from the above, this utility model has the following beneficial effects:

[0049] First, through the synergistic effect of the bottle body 1, sealing gasket 2, conduit 3 and adsorption filler 4, water vapor and oxygen that have seeped in or remain are continuously adsorbed throughout the entire process from the extraction of the sample from the reagent bottle 7 to the transfer into the inlet of the analyzer 9, forming a local low-water and low-oxygen environment around the needle tip of the sampling needle 8, effectively avoiding sample contamination and improving the accuracy of sample detection and analysis results.

[0050] Second, the structure of the catheter 3 provides a clear penetration path for the needle tube 81 of the sampling needle 8, preventing the needle tip from directly contacting the adsorbent filler 4. At the same time, the two ends of the catheter 3 abut against the sealing gasket 2, forming support for the sealing gasket 2, ensuring the sealing reliability and repeatability of the puncture.

[0051] Third, the one-way permeable and breathable layer 5 set on the outer periphery of the conduit 3 allows water vapor to permeate outward to the adsorption filler 4 and prevents the filler particles from entering the inner cavity of the conduit 3 in the reverse direction, thus avoiding blockage of the adsorption pores 31 and preventing contamination of the inner cavity of the conduit 3.

[0052] It will be apparent to those skilled in the art that this disclosure is not limited to the details of the exemplary embodiments described above, and that this disclosure can be implemented in other specific forms without departing from its spirit or essential characteristics. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of this disclosure is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within this disclosure. No reference numerals in the claims should be construed as limiting the scope of the claims.

[0053] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A sampling protection device, characterized in that, The sampling protection device includes: The bottle body includes two bottle openings located at its two ends; Two sealing gaskets are placed one-to-one over the two bottle openings; A conduit is installed inside the bottle. The conduit includes several adsorption holes on its peripheral wall. Both ends of the conduit are open and face each of the two sealing gaskets. Adsorption filler is used to fill the bottle body and is located outside the conduit.

2. The sampling protection device according to claim 1, characterized in that, The outer circumferential surface of the conduit is provided with a one-way water-permeable and air-permeable layer, and water vapor and gas inside the conduit can enter the adsorption packing through the adsorption pores.

3. The sampling protection device according to claim 1, characterized in that, The bottle body includes a bottle body and two bottle necks that are correspondingly located at both ends of the bottle body, and the bottle mouth is formed in the bottle neck. The sampling protection device also includes two bottle caps, which are installed one-to-one at the two bottle necks, and each bottle cap includes a through hole that exposes the sealing gasket.

4. The sampling protection device according to claim 3, characterized in that, The through hole is coaxially arranged with the conduit, and the diameter of the through hole is less than or equal to the inner diameter of the conduit.

5. The sampling protection device according to claim 3, characterized in that, The sealing gasket is held between the bottle neck and the bottle cap.

6. The sampling protection device according to claim 1, characterized in that, The bottle body includes a bottle body and two bottle necks located at both ends of the bottle body. The two ends of the conduit extend into the interior of the two bottle necks respectively, and the outer diameter of the conduit is equal to the inner diameter of the bottle neck.

7. The sampling protection device according to claim 1, characterized in that, The sealing gasket is affixed to the bottle opening.

8. The sampling protection device according to claim 1, characterized in that, The two ends of the catheter are respectively abutted against two sealing gaskets.

9. The sampling protection device according to claim 1, characterized in that, The conduit includes a main body segment wrapped with adsorbent packing material. The spacing between the adsorbent pores in the middle region of the main body segment is smaller than the spacing between the adsorbent pores in the end region of the main body segment, and the pore diameter of the adsorbent pores in the middle region of the main body segment is larger than the pore diameter of the adsorbent pores in the end region of the main body segment.

10. The sampling protection device according to claim 1, characterized in that, The sealing gasket is made of polypropylene, polytetrafluoroethylene, perfluoroalkoxy resin, or silicone; and / or, The adsorption packing material includes silica gel, activated molecular sieves, montmorillonite, iron granules as oxygen absorbers or granular desiccants; and / or, The conduit is made of glass, quartz, or stainless steel.

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