A test paper for silane or phosphine detection and a method for preparing the same

Abstract

The application provides a preparation method of test paper for silane or phosphine detection, comprising the following steps: S1: preparing a reagent solution; the reagent solution contains a silane coupling agent, a dispersing agent, a hydrolysis solution, a cosolvent and an indicator; S2: spraying the reagent solution on filter paper at room temperature or soaking the filter paper in the reagent solution, and then performing drying treatment, and obtaining the test paper after cutting. The application also provides the test paper for silane or phosphine detection obtained by using the above preparation method. The test paper of the application has a white appearance, is portable and easy to store, has a sensitive detection, a short response time, and can quickly and accurately reflect the concentration of trace silane or phosphine in the environment.

Description

Technical Field

[0001] This invention belongs to the field of chemical detection and relates to a technology for detecting trace gases in the environment, and more particularly to a test strip for detecting silanes or phosphines and its preparation method. Background Technology

[0002] Alkane gases such as silanes and phosphines are widely used in the microelectronics and optoelectronics industries. Silicon thin films deposited on wafers using chemical vapor deposition are the basic materials for building core components such as transistors. However, silanes, phosphines, and other alkane gases are highly dangerous gases with a very wide spontaneous ignition range and extremely high combustion energy. They may spontaneously combust upon contact with air and can form explosive mixtures when mixed with air.

[0003] Alkane gas leaks can directly lead to production interruptions, wafer contamination, and even product scrapping, causing serious economic losses. Simultaneously, inhaling leaked alkane gases can irritate the respiratory tract and potentially cause poisoning, threatening personnel health and production safety. Silanes and phosphines are colorless, toxic gases with an irritating odor at room temperature. Current methods for detecting these gases include electrochemical and gas chromatography, but these equipment are expensive and inconvenient to carry. Colorimetric methods can provide a timely visual response to trace amounts of target gases in the environment. For example, JP 62021061 A reports a colored silica gel column loaded with copper salts of organic acids, which changes color from blue-green to black upon contact with hydride gases such as silanes. However, its detection limit for silanes and germanes is only 50 ppm, far exceeding industrial safety requirements. Furthermore, this method requires manual sampling and passing the gas through a detection tube, making continuous, real-time online monitoring impossible. Therefore, designing a silane and phosphine test strip that is colorimetrically sensitive, ready to use, stable, and durable, meeting the needs of rapid industrial detection, is of great significance. Summary of the Invention

[0004] In view of the above-mentioned technical problems in the prior art, the present invention provides a test strip for the detection of silanes or phosphines and a method for preparing the same. The test strip for the detection of silanes or phosphines and the method for preparing the same are intended to solve the technical problems of the complexity and low sensitivity of the existing methods for detecting silanes or phosphines.

[0005] This invention provides a method for preparing test strips for the detection of silanes or phosphines, comprising the following steps: S1: Prepare the reagent solution; The reagent solution contains a silane coupling agent, a dispersant, a hydrolysate, a co-solvent, and an indicator; The volume ratio of the silane coupling agent to the dispersant is (1~2):5; The hydrolysate is an aqueous solution of glacial acetic acid, and the volume percentage concentration of glacial acetic acid in the aqueous solution is 1-20%. The volume ratio of the silane coupling agent to the hydrolysate is (2:1) to (2:10). The volume ratio of the co-solvent to the silane coupling agent is (1~2):1; The indicator is a salt solution containing silver ions, the solvent in the indicator is acetone, and the concentration of the indicator is 1-5 g / L; The volume ratio of the silane coupling agent to the indicator is 2:3; S2: Spray the reagent solution onto the filter paper at room temperature or immerse the filter paper in the reagent solution, then dry it and cut it to obtain the test strip.

[0006] Furthermore, the silane coupling agent is tetraethyl orthosilicate, γ-aminopropyltriethoxysilane, or N-aminoethyl- γ Any one of -aminopropyltriethoxysilane.

[0007] Furthermore, the dispersant is acetone; the co-solvent is acetonitrile.

[0008] Furthermore, the indicator is a salt solution of silver nitrate or silver perchlorate.

[0009] The present invention also provides test strips for the detection of silanes or phosphines obtained by the above preparation method.

[0010] This invention also provides a rapid determination method for detecting silane or phosphine gases, comprising the following steps: Place the test strips in an environment that may contain silanes or phosphines. After the test strips change color, compare the color shown on the test strips with the standard color chart to obtain the concentration of silanes or phosphines.

[0011] Specifically, when the test strip is placed in a trace amount of silane environment, a clear color spot appears on the test strip within 1 minute, enabling the detection of silane gas with a concentration of ≤10 ppm in the environment.

[0012] Specifically, when the test strip is placed in a trace amount of phosphine environment, a clear color spot appears on the test strip within 1 minute, enabling the detection of silane gas with a concentration of ≤500 ppb in the environment.

[0013] Furthermore, the method for preparing the standard colorimetric card is as follows: (1) Place the test strip of the present invention in a silane environment of different concentrations, and record the color of the test strip and the values ​​of L, a, and b after the color of the test strip changes.

[0014] (2) Prepare a standard color card and a Lab value variation table based on the known concentrations of silane and phosphine.

[0015] The working principle of this invention is as follows: the silane coupling agent undergoes hydrolysis and condensation to form a silica matrix with a three-dimensional network structure. The spontaneously generated siloxane oligomers in this process effectively adsorb free silver ions in the solution and enrich them on the surface of each silica particle. This structure inhibits excessive aggregation of silver ions, maintaining their high dispersion and long-term stability within the system. When the test paper comes into contact with reducing alkane gases such as silanes and phosphines, the enriched silver ions are reduced in situ to silver nanoparticles (silver colloids). This reduction reaction triggers a significant change in the plasmon resonance optical properties of the material surface, macroscopically manifested as a sharp color change of the test paper from white to yellow. Based on this colorimetric phenomenon, real-time visual monitoring of leaks of target alkane gases can be achieved.

[0016]

[0017] This invention aims to provide a timely and efficient detection method for trace amounts of toxic alkane gases such as silanes and phosphines present during the manufacturing process of electronic devices in the semiconductor industry, ensuring the safety of industrial production. The trace silane and phosphine test strip prepared using the method of this invention is white in appearance, portable and easy to store, has high detection sensitivity and a short response time, and can quickly and accurately reflect the concentration of trace silanes and phosphines in the environment.

[0018] Compared with existing technologies, the technical effects of this invention are positive and obvious: (1) The prepared test paper reacts with silane with extreme sensitivity and has a low detection limit. It can detect silane with a concentration of 0-10 ppm and phosphine with a concentration of 0-500 ppb, and generates two different colored spots.

[0019] (2) The prepared test strip has obvious color development effect and can remain stable under indoor light irradiation. It can be used in conjunction with paper tape gas detection equipment.

[0020] (3) This test paper is prepared by spraying or soaking. It is operated at room temperature in the dark, without the need for complex temperature control equipment. The process is simple and stable, and can be adapted to rapid and stable industrial production.

[0021] (4) Experimental verification shows that under sealed and light-proof storage conditions (25℃, 40% humidity), the shelf life of this test strip is ≥3 months. During the storage period, the detection sensitivity (ΔE value ±5%), color contrast and response time remain stable. The detection is sensitive and the response time is short, which can quickly and accurately reflect the concentration of trace silane in the environment, and meet the needs of long-term stocking and immediate use in industrial scenarios.

[0022] (5) Experimental verification showed that the test paper did not undergo any visible color change when in contact with other reducing gases commonly found in integrated circuit manufacturing environments (such as ammonia and hydrogen chloride), indicating that it has good anti-interference ability. This characteristic enables the present invention to specifically identify and respond to silane and phosphine gases, thereby achieving highly selective visual monitoring of target leaked gases. Attached Figure Description

[0023] Figure 1 To illustrate the color change of the test paper of the present invention when placed in a silane or phosphine gas atmosphere, (a) the original test paper; (b) after reaction with silane; and (c) after reaction with phosphine.

[0024] Figure 2 The color change of the test paper after reacting with 1-10 ppm of silane gas for 1 min is shown (ambient temperature 25 ℃, humidity 40%).

[0025] Figure 3 The test paper of this invention reacts with silane gas for 1 minute. Δb The relationship between the value and concentration.

[0026] Figure 4 The color change of the test paper after reacting with 100-500 ppb of phosphine gas for 1 min (ambient temperature 25 ℃, humidity 40%) is shown.

[0027] Figure 5 The relationship between the Δb value and the concentration after the test paper of the present invention reacts with phosphine gas for 1 min is shown.

[0028] Figure 6 (a) The test strip of the present invention one month before production; (b) The color change of the test strip one month after production.

[0029] Figure 7 The color change of the test paper of the present invention is shown in (a) after the test paper is fully contacted with a 50 ppm ammonia atmosphere for 5 min; and (b) after the test paper is fully contacted with a 10 ppm hydrogen chloride atmosphere for 5 min.

[0030] Figure 8 This is a simplified diagram illustrating the working principle of the test strip of the present invention. Detailed Implementation

[0031] To enable those skilled in the art to better understand the technical solutions of the present invention, the present invention will be further described in detail below with reference to specific embodiments and accompanying drawings. It should be understood that the preferred embodiments described herein are only for explaining the present invention and are not intended to limit the scope of protection of the present invention. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without inventive effort are within the scope of protection of the present invention. Example 1

[0032] At room temperature, 2 ml of tetraethyl orthosilicate was dissolved in 5 ml of acetone to obtain a 40 vol% tetraethyl orthosilicate-acetone solution. 2 ml of acetonitrile was then slowly added to the solution to obtain a mixed solution. 0.1 ml of glacial acetic acid was dissolved in 10 ml of water to obtain a 1 vol% acetic acid aqueous solution. After complete dissolution, the acetic acid aqueous solution was slowly added dropwise to the mixed solution at a rate of 1 drop / s, maintaining a rotation speed of 100 rpm during the addition. After all the solution was added, the mixture was allowed to react for 30 min to obtain a clear pre-hydrolyzed solution.

[0033] 0.1 g of silver perchlorate was dissolved in 100 ml of acetone at room temperature to obtain a 1 g / L silver perchlorate acetone solution. 3 ml of the silver perchlorate acetone solution was slowly added dropwise to the pre-hydrolyzed solution at a constant speed of 100 rpm. After all the solution was added, the reaction was allowed to proceed for 10 min to obtain the detection reagent solution. All procedures were performed in the dark.

[0034] Immerse 90 mm diameter qualitative filter paper in the above-mentioned test reagent solution for 10 minutes. After thorough saturation, place the paper in a fume hood to dry in the dark for 2 hours. Once completely dry, cut the paper into 1 cm pieces. 2 Square pieces of paper were used to obtain white silane and phosphine test strips. The indicator was 1 g / L silver perchlorate, which reacted directly with silanes and phosphines in the environment to form yellow silver nanoparticles. Example 2

[0035] At room temperature, 1 ml of tetraethyl orthosilicate was dissolved in 5 ml of acetone to obtain a 20 vol% tetraethyl orthosilicate-acetone solution. 1 ml of acetonitrile was then slowly added to the solution to obtain a mixed solution. 0.1 ml of glacial acetic acid was dissolved in 10 ml of water to obtain a 1 vol% acetic acid aqueous solution. After complete dissolution, the acetic acid aqueous solution was slowly added dropwise to the mixed solution at a rate of 1 drop / s, maintaining a rotation speed of 100 rpm during the addition. After all the solution was added, the mixture was allowed to react for 30 min to obtain a clear pre-hydrolyzed solution.

[0036] 0.1 g of silver perchlorate was dissolved in 100 ml of acetone at room temperature to obtain a 1 g / L silver perchlorate acetone solution. 3 ml of the silver perchlorate acetone solution was slowly added dropwise to the pre-hydrolyzed solution at a constant speed of 100 rpm. After all the solution was added, the reaction was allowed to proceed for 10 min to prepare the silane detection reagent solution. All operations were performed in the dark.

[0037] Immerse 90 mm diameter qualitative filter paper in the above-mentioned test reagent solution for 10 minutes. After thorough saturation, place the paper in a fume hood to dry in the dark for 2 hours. Once completely dry, cut the paper into 1 cm pieces. 2 Square pieces of paper were used to obtain white silane and phosphine test strips. The indicator was 1 g / L silver perchlorate, which reacted directly with silanes and phosphines in the environment to form yellow silver nanoparticles. Example 3

[0038] At room temperature, 2 ml of tetraethyl orthosilicate was dissolved in 5 ml of acetone to obtain a 40 vol% tetraethyl orthosilicate-acetone solution. 2 ml of acetonitrile was then slowly added to the solution to obtain a mixed solution. 0.2 ml of glacial acetic acid was dissolved in 10 ml of water to obtain a 2 vol% acetic acid aqueous solution. After complete dissolution, the acetic acid aqueous solution was slowly added dropwise to the mixed solution at a rate of 1 drop / s, maintaining a rotation speed of 100 rpm during the addition. After all the solution was added, the mixture was allowed to react for 30 min to obtain a clear pre-hydrolyzed solution.

[0039] 0.1 g of silver perchlorate was dissolved in 100 ml of acetone at room temperature to obtain a 1 g / L silver perchlorate acetone solution. 3 ml of the silver perchlorate acetone solution was slowly added dropwise to the pre-hydrolyzed solution at a constant speed of 100 rpm. After all the solution was added, the reaction was allowed to proceed for 10 min to prepare the silane detection reagent solution. All operations were performed in the dark.

[0040] Immerse 90 mm diameter qualitative filter paper in the above-mentioned test reagent solution for 10 minutes. After thorough saturation, place the paper in a fume hood to dry in the dark for 2 hours. Once completely dry, cut the paper into 1 cm pieces. 2 Square pieces of paper were used to obtain white silane and phosphine test strips. The indicator was 1 g / L silver perchlorate, which reacted directly with silanes and phosphines in the environment to form yellow silver nanoparticles. Example 4

[0041] At room temperature, 2 ml of tetraethyl orthosilicate was dissolved in 5 ml of acetone to obtain a 40 vol% tetraethyl orthosilicate-acetone solution. 2 ml of acetonitrile was then slowly added to the solution to obtain a mixed solution. 0.1 ml of glacial acetic acid was dissolved in 10 ml of water to obtain a 1 vol% acetic acid aqueous solution. After complete dissolution, the acetic acid aqueous solution was slowly added dropwise to the mixed solution at a rate of 1 drop / s, maintaining a rotation speed of 100 rpm during the addition. After all the solution was added, the mixture was allowed to react for 30 min to obtain a clear pre-hydrolyzed solution.

[0042] 0.5 g of silver perchlorate was dissolved in 100 ml of acetone at room temperature to obtain a 5 g / L silver perchlorate acetone solution. 3 ml of the silver perchlorate acetone solution was slowly added dropwise to the pre-hydrolyzed solution at a constant speed of 100 rpm. After all the solution was added, the reaction was allowed to proceed for 10 min to obtain the silane detection reagent solution. All operations were performed in the dark.

[0043] Immerse 90 mm diameter qualitative filter paper in the above-mentioned test reagent solution for 10 minutes. After thorough saturation, place the paper in a fume hood to dry in the dark for 2 hours. Once completely dry, cut the paper into 1 cm pieces. 2 Square pieces of paper were used to obtain white silane and phosphine test strips. The indicator was 5 g / L silver perchlorate, which reacted directly with silanes and phosphines in the environment to form yellow silver nanoparticles. Example 5

[0044] At room temperature, 2 ml of γ-aminopropyltriethoxysilane was dissolved in 5 ml of acetone to obtain a 40 vol% γ-aminopropyltriethoxysilane acetone solution. 2 ml of acetonitrile was slowly added to the solution to obtain a mixed solution. 0.1 ml of glacial acetic acid was dissolved in 10 ml of water to obtain a 1 vol% acetic acid aqueous solution. After complete dissolution, the acetic acid aqueous solution was slowly added dropwise to the mixed solution at a rate of 1 drop / s, maintaining a rotation speed of 100 rpm during the addition. After all the solution was added, the reaction was allowed to proceed for 30 min to obtain a clear pre-hydrolyzed solution.

[0045] 0.1 g of silver perchlorate was dissolved in 100 ml of acetone at room temperature to obtain a 1 g / L silver perchlorate acetone solution. 3 ml of the silver perchlorate acetone solution was slowly added dropwise to the pre-hydrolyzed solution at a constant speed of 100 rpm. After all the solution was added, the reaction was allowed to proceed for 10 min to prepare the silane detection reagent solution. All operations were performed in the dark.

[0046] Immerse 90 mm diameter qualitative filter paper in the above-mentioned test reagent solution for 10 minutes. After thorough saturation, place the paper in a fume hood to dry in the dark for 2 hours. Once completely dry, cut the paper into 1 cm pieces. 2 Square pieces of paper were used to obtain white silane and phosphine test strips. The indicator was 1 g / L silver perchlorate, which reacted directly with silanes and phosphines in the environment to form yellow silver nanoparticles. Example 6

[0047] At room temperature, 2 ml of tetraethyl orthosilicate was dissolved in 5 ml of acetone to obtain a 40 vol% tetraethyl orthosilicate-acetone solution. 2 ml of acetonitrile was then slowly added to the solution to obtain a mixed solution. 0.1 ml of glacial acetic acid was dissolved in 10 ml of water to obtain a 1 vol% acetic acid aqueous solution. After complete dissolution, the acetic acid aqueous solution was slowly added dropwise to the mixed solution at a rate of 1 drop / s, maintaining a rotation speed of 100 rpm during the addition. After all the solution was added, the mixture was allowed to react for 30 min to obtain a clear pre-hydrolyzed solution.

[0048] 0.1 g of silver nitrate was dissolved in 100 ml of acetone at room temperature to obtain a 1 g / L silver nitrate acetone solution. 3 ml of the silver nitrate acetone solution was slowly added dropwise to the pre-hydrolyzed solution at a rotation speed of 100 rpm. After all the solution was added, the reaction was allowed to proceed for 10 min to obtain the silane detection reagent solution. All operations were performed in the dark.

[0049] Immerse 90 mm diameter qualitative filter paper in the above-mentioned test reagent solution for 10 minutes. After thorough saturation, place the paper in a fume hood to dry in the dark for 2 hours. Once completely dry, cut the paper into 1 cm pieces. 2 Square pieces of paper were used to obtain white silane and phosphine test strips. The indicator was 1 g / L silver perchlorate, which reacted directly with silanes and phosphines in the environment to form yellow silver nanoparticles. Example 7

[0050] At room temperature, 2 ml of tetraethyl orthosilicate was dissolved in 5 ml of acetone to obtain a 40 vol% tetraethyl orthosilicate-acetone solution. 2 ml of acetonitrile was then slowly added to the solution to obtain a mixed solution. 0.1 ml of glacial acetic acid was dissolved in 10 ml of water to obtain a 1 vol% acetic acid aqueous solution. After complete dissolution, the acetic acid aqueous solution was slowly added dropwise to the mixed solution at a rate of 1 drop / s, maintaining a rotation speed of 100 rpm during the addition. After all the solution was added, the mixture was allowed to react for 30 min to obtain a clear pre-hydrolyzed solution.

[0051] 0.1 g of silver perchlorate was dissolved in 100 ml of acetone at room temperature to obtain a 1 g / L silver perchlorate acetone solution. 3 ml of the silver perchlorate acetone solution was slowly added dropwise to the pre-hydrolyzed solution at a constant speed of 100 rpm. After all the solution was added, the reaction was allowed to proceed for 10 min to obtain the detection reagent solution. All procedures were performed in the dark.

[0052] Lay a 90 mm diameter qualitative filter paper flat on a clean glass plate. Using a handheld sprayer (nozzle orifice diameter 0.3–0.5 mm), evenly spray the reagent solution onto the filter paper surface. Maintain a spraying distance of 20–30 cm, and spray at a rate that is sufficient to moisten the filter paper surface without dripping (approximately 0.1–0.15 mL / cm²). Place the sprayed filter paper in a fume hood to dry in the dark for 2 hours. After complete drying, cut the paper into 1 cm pieces. 2 Square pieces of paper were used to obtain white silane and phosphine test strips. The indicator was 1 g / L silver perchlorate, which reacted directly with silanes and phosphines in the environment to form yellow silver nanoparticles. Example 8

[0053] The test strips prepared in Example 1 were placed in silane gas atmospheres of different concentrations, and the test strips were measured after five minutes. L, a, b Values ​​(in the CIE Lab color space): : Indicates brightness (lightness), ranging from 0 (black) to 100 (white).

[0054] : Represents the red-green axis, with positive values ​​for red and negative values ​​for green.

[0055] : Indicates the yellow-blue axis, with positive values ​​for yellow and negative values ​​for blue.

[0056] Color difference (ΔE) represents the overall difference between two colors, and is calculated using the following formula:

[0057] in, 、 、 Two colors are respectively in 、 、 The difference on the axis. The results are shown in Table 1, where... ΔE A color change of >5 is perceptible to the naked eye. When the silane concentration is ≤10 ppm, the color change of the test paper is measured by a colorimeter (in this experiment, a 3nh SC-10 high-precision colorimeter was used to analyze the color parameters of the test paper). Δb The value has a good linear relationship with the silane concentration, and a colorimeter was established. Δb A standard curve of the value versus silane concentration is attached. Figure 3 .

[0058] The regression linear equation is y= 3.44 x + 0.29 (0 <x ≤ 3.44), y = 0.28 x + 8.32 (3.44 <x ≤ 7), y = 1.29 x + 1.25 (x > 7); linear correlation coefficient R 2 = 0.99 ( x This refers to the concentration of silane (unit: ppm). y (Refers to the Δb value of the colorimeter).

[0059] The concentration of silane in the environment can be calculated using a formula based on the color change of the test strip.

[0060] Table 1. Results of the reaction between the test strip and different concentrations of silane after 1 min. L, a, b Values ​​(Temperature: 25℃; Humidity: 40%) 5.30 6.01 6.52 7.77 8.16 8.49 4.05 -3.27 -6.57 -1.34 -0.25 0.25 1.29 1.77 1.92 1.66 2.08 2.88 3.13 3.17 4.31 6.86 9.26 9.09 9.97 10.01 9.77 11.84 13.30 13.76 6.83 9.12 11.40 12.09 13.03 13.23 10.78 12.62 15.16 14.19 Example 9

[0061] This invention also proposes an application of a trace silane detection test strip in an integrated circuit manufacturing environment, which is used for the detection of trace silanes in the environment. The test strip is placed in a silane gas atmosphere of less than 10 ppm, as shown in the attached... Figure 1 As shown, a distinct yellow spot appears on the test strip surface within 1 minute. The presence of silane in the environment can be observed with the naked eye. Figure 2 Color development at concentrations of 0-10 ppm.

[0062] If precise data is required, use a colorimeter to read the values ​​of the color-changing portion of the test strip. y , put the value y Substitute into the formula y = 3.44 x + 0.29 (0< x ≤ 3.44), y = 0.28 x + 8.32 (3.44< x ≤ 7), y = 1.29 x +1.25 ( x >7), then the equation can be used to calculate x (Silane concentration (unit: ppm)). Example 10

[0063] The test strips prepared in Example 1 were placed in phosphine gas atmospheres of different concentrations, and the test strips were measured after five minutes. L, a, b Values ​​(in the CIE Lab color space): : Indicates brightness (lightness), ranging from 0 (black) to 100 (white).

[0064] : Represents the red-green axis, with positive values ​​for red and negative values ​​for green.

[0065] : Indicates the yellow-blue axis, with positive values ​​for yellow and negative values ​​for blue.

[0066] Color difference (ΔE) represents the overall difference between two colors, and is calculated using the following formula:

[0067] in, 、 、 Two colors are respectively in 、 、 The difference on the axis. The results are shown in Table 2, where... ΔE A color change of >5 is visible to the naked eye. When the phosphine concentration is ≤ 500 ppb, the color change of the test paper is measured by a colorimeter (in this experiment, a 3nh SC-10 high-precision colorimeter was used to analyze the color parameters of the test paper). Δb The value has a good linear relationship with the silane concentration, and a colorimeter was established. Δb A standard curve of the value versus silane concentration is attached. Figure 5 .

[0068] The regression linear equation is y = -0.02 x +2.77, linear correlation coefficient R 2 = 0.99 ( x Phosphine concentration (unit: ppb), Y refers to the colorimeter. Δb (Value). The concentration of phosphine in the environment can be calculated using a formula based on the color change of the test strip.

[0069] Table 2. Results of the reaction between the test strip and different concentrations of phosphine after 1 min L, a, b Values ​​(Temperature: 25℃; Humidity: 40%) 4.13 2.90 1,98 0.21 -2.54 -4.13 -0.31 -0.06 -0.07 0.86 1.42 2.21 3.70 4.57 6.26 8.35 9.93 10.58 5.55 5.41 6.56 8.40 10.34 11.57 Example 11

[0070] This invention also proposes an application of a trace phosphine test strip in an integrated circuit manufacturing environment, which is used for the detection of trace phosphine in the environment. The test strip is placed in a phosphine gas atmosphere of less than 500 ppb, as shown in the attached... Figure 1 As shown, a distinct brown spot appears on the test strip surface within 1 minute. The presence of phosphine in the environment can be observed with the naked eye. Figure 4 The color development range is 0-500 ppb.

[0071] If precise data is needed, use a colorimeter to read the value y of the color-changing portion of the test paper, and substitute the value y into the formula. y = 0.02 x With +2.77, we can calculate the result using the equation. x (Phosphine concentration (unit: ppb)). Example 12

[0072] This invention also proposes a method for verifying the stability of silane and phosphine test strips, specifically including the following steps: The silane and phosphine test strips are stored in a light-proof, sealed environment at an ambient temperature of 25°C and a relative humidity of 45%, sealed in a black polyethylene self-sealing bag. After a one-month storage period, no significant color change was observed on the surface of the test strips, and their chromatic characteristics were consistent with those of freshly prepared test strips. To verify the functional activity of the test strips after storage, the aged test strips were placed in a silane detection environment of a set concentration. The test strips still exhibited the characteristic color change from white to yellow, proving that the test strips of this invention maintain stable gas-sensitive response characteristics (e.g., ...) even after long-term storage. Figure 6 (As shown). Example 13

[0073] This invention also proposes a specificity verification method for silane and phosphine test strips, specifically including the following steps: under ambient temperature of 25 ℃ and relative humidity of 45%, the silane test strip is placed in an atmosphere of 50 ppm ammonia and 10 ppm hydrogen chloride, respectively, and after full contact for 5 min, the color of the test strip surface is observed to show no obvious color change. Figure 7 This result indicates that the test strip of the present invention has no cross-response to other reducing gases commonly found in integrated circuit manufacturing environments.

[0074] In summary, the present invention provides a method for preparing and applying a test strip for detecting trace amounts of silane and phosphine in an integrated circuit manufacturing environment. Trace amounts of silane and phosphine in the environment can be detected by the test strip within 30 seconds to 1 minute, exhibiting a short response time and rapidly reflecting the gas conditions in the environment. Compared with traditional solution colorimetric methods, the test strip is more stable and exhibits clear color development, allowing for rapid visual observation while eliminating cumbersome experimental steps and offering strong scalability. Using silver ions as an indicator, a white-looking test strip is prepared, achieving a clear color change before and after the reaction.

Claims

1. A method for preparing a test strip for detecting silanes or phosphines, characterized in that, Includes the following steps: S1: Prepare the reagent solution; The reagent solution contains a silane coupling agent, a dispersant, a hydrolysate, a co-solvent, and an indicator; The volume ratio of the silane coupling agent to the dispersant is (1~2):5; The hydrolysate is an aqueous solution of glacial acetic acid, and the volume percentage concentration of glacial acetic acid in the aqueous solution is 1-20%. The volume ratio of the silane coupling agent to the hydrolysate is (2:1) to (2:10). The volume ratio of the co-solvent to the silane coupling agent is (1~2):1; The indicator is a salt solution containing silver ions, the solvent in the indicator is acetone, and the concentration of the indicator is 1-5 g / L; The volume ratio of the silane coupling agent to the indicator is 2:3; S2: Spray the reagent solution onto the filter paper at room temperature or immerse the filter paper in the reagent solution, then dry it and cut it to obtain the test strip.

2. The method for preparing a test strip for detecting silanes or phosphines as described in claim 1, characterized in that, The silane coupling agent is any one of tetraethyl orthosilicate, γ-aminopropyltriethoxysilane, and N-aminoethyl-γ-aminopropyltriethoxysilane.

3. The method for preparing a test strip for detecting silanes or phosphines as described in claim 1, characterized in that, The dispersant is acetone; the co-solvent is acetonitrile.

4. The method for preparing a test strip for detecting silanes or phosphines as described in claim 1, characterized in that, The indicator is a salt solution of silver nitrate or silver perchlorate.

5. A test strip for the detection of silanes or phosphines obtained by the preparation method according to claim 1.

6. A rapid method for determining silane or phosphine gas, characterized in that: The test strip described in claim 5 is placed in an environment that may contain silane or phosphine. After the color of the test strip changes, the color shown by the test strip is compared with the standard colorimetric card to obtain the concentration of silane or phosphine.

7. The rapid determination method for silane or phosphine gas according to claim 6, characterized in that: The method for preparing the standard colorimetric card is as follows: (1) Place the test paper according to claim 5 in a silane environment of different concentrations, and record the color of the test paper and the values ​​of L, a, and b after the color of the test paper changes. (2) Prepare a standard color card and a Lab value variation table based on the known concentrations of silane and phosphine.

Images