An alkane gas adsorbent used in semiconductor processing and a method for preparing the same

Abstract

This invention relates to the field of gas adsorbents, specifically to an adsorbent for alkane gases used in semiconductor manufacturing processes and its preparation method. The adsorbent comprises the following raw materials: 50-65 parts activated manganese dioxide, 40-50 parts modified activated carbon, 27-32 parts activated copper oxide, 105-110 parts potassium permanganate aqueous solution, 0.2-0.6 parts lubricant, 0.01-0.03 parts manganese nitrate, and 1-4 parts silica. By controlling the amounts of modified activated carbon, activated manganese dioxide, activated copper oxide, and potassium permanganate, this invention enables the prepared adsorbent to exhibit high adsorption and decomposition capacity for silane, phosphine, and arsine waste gases, with a large adsorption capacity and excellent long-lasting effect.

Description

Technical Field

[0001] This invention relates to the field of gas adsorbents, and more specifically to an alkane gas adsorbent for use in semiconductor manufacturing processes and its preparation method. Background Technology

[0002] As a crucial branch of the electronics and information manufacturing industry, the semiconductor sector is experiencing rapid growth thanks to the successful implementation of new infrastructure initiatives such as 5G, artificial intelligence, the Internet of Things, cloud computing, and big data. The semiconductor industry chain, encompassing foundry, packaging and testing, design, equipment, and materials, will continue to thrive, with various semiconductor manufacturing companies emerging rapidly.

[0003] Semiconductors, as a high-tech industry, are often mistakenly considered a "clean" industry. However, in reality, the processes of semiconductor manufacturing, such as cleaning, etching, deposition, coating, photolithography, and development, require the use of various special gases, including alkanes such as silanes, phosphines, and arsines. These gases are basic chemical raw materials with high risks, being flammable, explosive, toxic, and corrosive. If the waste gases generated after use are not specially treated, they can cause incalculable adverse effects on the environment and human health.

[0004] Alkane gas adsorbents are adsorbents used to purify and treat alkane waste gases. They can effectively adsorb alkane gases from gases or liquids and react with them to generate harmless and stable compounds, reducing harm to human health and the environment. They are widely used in new energy, pharmaceutical and chemical industries, and semiconductor chip manufacturing. Currently, the adsorption capacity of alkane gas adsorbents produced by related technologies is relatively weak, requiring large dosages and long adsorption times to meet the emission standards for alkane gases.

[0005] Therefore, developing an alkane gas adsorbent plays a crucial role in the treatment of waste gases in semiconductor manufacturing processes. Summary of the Invention

[0006] To address the aforementioned technical problems, this invention provides an alkane gas adsorbent for use in semiconductor manufacturing processes and its preparation method. This gas adsorbent has good adsorption capacity for special gaseous waste gases generated in various processes of semiconductor manufacturing, and its effective action time is long-lasting, resulting in excellent purification effect.

[0007] To achieve the above objectives, the technical solution adopted by the present invention is as follows:

[0008] This invention provides an alkane gas adsorbent for use in semiconductor manufacturing processes. The adsorbent comprises the following raw materials by weight: 50-65 parts activated manganese dioxide, 40-50 parts modified activated carbon, 27-32 parts activated copper oxide, 105-110 parts potassium permanganate aqueous solution, 0.2-0.6 parts lubricant, 0.01-0.03 parts manganese nitrate, and 1-4 parts silica.

[0009] In some embodiments, the weight ratio between the active manganese dioxide and the active copper oxide is (1.9-2.3):1.

[0010] Preferably, the weight ratio between the active manganese dioxide and the active copper oxide is 2:1.

[0011] In some embodiments, the silica comprises precipitated silica and fumed silica in a weight ratio of 1:(2-5).

[0012] Preferably, the weight ratio between precipitated silica and fumed silica is 1:3.

[0013] In some embodiments, the precipitated silica has an average particle size of 10-15 μm and a BET specific surface area of ​​150-200 m². 2 / g.

[0014] Preferably, the precipitated silica has an average particle size of 13 μm and a BET specific surface area of ​​161-190 m². 2 / g.

[0015] This invention does not impose any special restrictions on the source of precipitated silica, which can be purchased commercially, including but not limited to the precipitated silica purchased from Guangzhou Housheng New Materials Co., Ltd.

[0016] In some embodiments, the fumed silica is a hydrophobic fumed silica with an average particle size of 10-20 nm and a specific surface area of ​​170-230 m². 2 / g.

[0017] Preferably, the hydrophobic fumed silica has an average particle size of 15 nm and a specific surface area of ​​175-225 m². 2 / g.

[0018] The present invention does not impose any special restrictions on the source of the fumed silica, which can be obtained through commercial purchases, including but not limited to the fumed silica purchased from Shanghai Yingcheng New Materials Co., Ltd., model YC-SI15.

[0019] This application, by adding specific precipitated silica and fumed silica, not only ensures that they are uniformly dispersed in the adsorbent, but also endows the adsorbent with many different adsorption sites through different particle sizes and specific surface areas, enabling the adsorption of different alkane waste gas molecules, which is beneficial to improving the adsorption capacity of the adsorbent.

[0020] In some embodiments, the average particle size of the active manganese dioxide is 40-60 nm, and the specific surface area is 1800-2200 m². 2 / g.

[0021] Preferably, the active manganese dioxide has an average particle size of 50 nm and a specific surface area of ​​2000 m². 2 / g.

[0022] The present invention does not impose any special restrictions on the source of the active manganese dioxide, which can be obtained through commercial purchases, including but not limited to the active manganese dioxide purchased from Yumu (Ningbo) New Materials Co., Ltd., model YM-MnO2-05.

[0023] In some embodiments, the preparation steps of the modified activated carbon include: wetting the dried activated carbon with deionized water, soaking it in deionized water, then adding copper chloride solution for impregnation treatment, condensing and refluxing after vacuum heating, then discarding the impregnation liquid, and washing, drying and calcining the solid to obtain the modified activated carbon.

[0024] Preferably, the preparation steps of the modified activated carbon include: wetting the dried activated carbon with an equal mass of deionized water, then adding twice the weight of deionized water to soak the activated carbon, then adding copper chloride solution for impregnation treatment, heating at 95°C for 10 hours under vacuum conditions, condensing and refluxing, then discarding the impregnation solution, washing the solid with deionized water, drying under vacuum at 110°C for 2 hours, and calcining to obtain the modified activated carbon.

[0025] In some embodiments, the activated carbon has a particle size of 200-400 mesh, preferably 325 mesh.

[0026] The present invention does not impose any special restrictions on the source of the activated carbon, which can be obtained through commercial purchases, including but not limited to the activated carbon purchased from Shanghai Xitan Environmental Protection Technology Co., Ltd.

[0027] In some embodiments, the conditions for the immersion treatment are: a copper chloride solution with a mass fraction of 15-20%, an immersion ratio of 1:(8-12), and an immersion time of 0.5-1h.

[0028] Preferably, the conditions for the immersion treatment are: a copper chloride solution with a mass fraction of 18%, an immersion ratio of 1:10, and an immersion time of 0.8 h.

[0029] In some embodiments, the calcination conditions are 280-310°C for 1.5-2.5 hours.

[0030] Preferably, the calcination conditions are 300°C and the time is 2 hours.

[0031] In some embodiments, the activated copper oxide has a particle size of 10-30 nm and a specific surface area of ​​40-80 m². 2 / g.

[0032] Preferably, the activated copper oxide has a particle size of 20 nm and a specific surface area of ​​50-60 m². 2 / g.

[0033] The present invention does not impose any special restrictions on the source of the active copper oxide, which can be obtained through commercial purchases, including but not limited to the active copper oxide purchased from Zhejiang Zhitai Nano Micro New Materials Co., Ltd.

[0034] In some embodiments, the lubricant is ethylene bis-stearamide. The addition of a certain amount of ethylene bis-stearamide in this application can promote the uniform dispersion of each component, prevent adsorbent agglomeration, improve the uniformity and molding performance of the adsorbent, and ensure its adsorption performance.

[0035] In some embodiments, the mass concentration of the potassium permanganate aqueous solution is 5-7%, preferably 6%.

[0036] During the research process, the applicant discovered that by controlling the dosage of specific modified activated carbon, activated manganese dioxide, activated copper oxide, and potassium permanganate, this application can achieve a high adsorption and decomposition capacity for silane, phosphine, and arsine waste gases, with a large adsorption capacity and excellent long-lasting effect. The applicant believes that this may be due to two factors: firstly, the high functional group density, large contact area, and high dispersibility of the active metal oxides in this system give them strong oxidizing properties, allowing them to fully react with silane, phosphine, and arsine gases to generate stable, non-toxic, or low-toxic inorganic salts, ensuring the safety of the reaction and making it unaffected by temperature and humidity; secondly, the addition of specially modified activated carbon allows copper salts to be loaded onto the porous carrier surface, and the calcination process generates copper oxide, which promotes the reaction with silane, phosphine, and arsine waste gases. Simultaneously, the high adsorption capacity of the porous structure endows the adsorbent with a long-lasting purification effect. In addition, the applicant unexpectedly discovered that adding precipitated silica and fumed silica of different particle sizes not only fixes various alkane gases, but also adjusts the density of activated copper oxide and activated manganese dioxide, which is more conducive to the full reaction with silane, phosphine and arsine waste gases and improves reaction efficiency.

[0037] Another aspect of the present invention provides a method for preparing an alkane gas adsorbent for use in semiconductor manufacturing processes, comprising the following steps:

[0038] (1) Weigh out each raw material according to the proportion;

[0039] (2) Add activated manganese dioxide, modified activated carbon, activated copper oxide, silica and lubricant to a kneader, mix and stir for 30-60 minutes, add potassium permanganate aqueous solution, and continue to stir and mix for 10-30 minutes to obtain a mixture;

[0040] (3) Add the mixture obtained in step (2) to a molding machine for pelletizing;

[0041] (4) The shaped particles are dried to obtain the alkane gas adsorbent.

[0042] In some embodiments, the drying process in step (4) includes two stages: the temperature of the first stage is 100-200℃ and the holding time is 40-70 min; the temperature of the second stage is 400-500℃ and the holding time is 120-180 min.

[0043] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0044] (1) By adjusting the dosage of modified activated carbon, activated manganese dioxide, activated copper oxide and potassium permanganate, this invention can achieve high adsorption and decomposition capacity for silane, phosphine and arsine waste gas, and has a large adsorption capacity and excellent long-lasting effect.

[0045] (2) By adding specific precipitated silica and fumed silica, this invention can not only make them uniformly dispersed in the adsorbent, but also endow the adsorbent with many different adsorption sites through different particle sizes and specific surface areas, which can adsorb different alkane waste gas molecules, thus improving the adsorption capacity of the adsorbent; and can adjust the density of active copper oxide and active manganese dioxide, which is more conducive to the full reaction with silane, phosphine and arsine waste gases, thus improving the reaction efficiency.

[0046] (3) The ethylene bis-stearamide added in this invention can promote the uniform dispersion of each component, prevent adsorbent from clumping, improve the uniformity and molding performance of the adsorbent, and ensure its adsorption performance. Detailed Implementation

[0047] The technical solution of the present invention will be clearly and completely described below with reference to the embodiments. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0048] Example 1

[0049] An alkane gas adsorbent for use in semiconductor manufacturing processes, comprising, by weight, the following raw materials: 60 parts activated manganese dioxide, 45 parts modified activated carbon, 30 parts activated copper oxide, 108 parts potassium permanganate aqueous solution, 0.4 parts lubricant, 0.02 parts manganese nitrate, and 2.5 parts silica.

[0050] Silica includes precipitated silica and fumed silica, with a weight ratio of 1:3.

[0051] Precipitated silica was purchased from Guangzhou Housheng New Materials Co., Ltd., with an average particle size of 13 μm and a BET specific surface area of ​​161-190 m². 2 / g; Hydrophobic fumed silica was purchased from Shanghai Yingcheng New Materials Co., Ltd., model YC-SI15, with an average particle size of 15nm and a specific surface area of ​​175-225m². 2 / g; Active manganese dioxide was purchased from Yumu (Ningbo) New Materials Co., Ltd., model YM-MnO2-05, with an average particle size of 50nm and a specific surface area of ​​2000m². 2 / g; Activated copper oxide was purchased from Zhejiang Zhitai Nano-Micro New Materials Co., Ltd., with a particle size of 20nm and a specific surface area of ​​50-60m². 2 / g; the lubricant is ethylene bis-stearamide; the mass concentration of potassium permanganate aqueous solution is 6%.

[0052] The preparation steps of the modified activated carbon include: wetting the dried activated carbon with an equal mass of deionized water, then adding twice the weight of deionized water to soak the activated carbon, then adding copper chloride solution for impregnation treatment, heating at 95°C for 10 hours under vacuum conditions, condensing and refluxing, then discarding the impregnation solution, washing the solid with deionized water, drying under vacuum at 110°C for 2 hours, and calcining at 300°C for 2 hours to obtain the modified activated carbon.

[0053] The activated carbon was purchased from Shanghai Xitan Environmental Protection Technology Co., Ltd., with a particle size of 325 mesh.

[0054] The conditions for the immersion treatment were: a copper chloride solution with a mass fraction of 18%, an immersion ratio of 1:10, and an immersion time of 0.8 h.

[0055] The preparation method of the alkane gas adsorbent in this embodiment includes the following steps:

[0056] (1) Weigh out each raw material according to the proportion;

[0057] (2) Add activated manganese dioxide, modified activated carbon, activated copper oxide, white carbon black and lubricant to a kneader, mix and stir for 45 min, add potassium permanganate aqueous solution, and continue to stir and mix for 20 min to obtain a mixture;

[0058] (3) Add the mixture obtained in step (2) to a molding machine for pelletizing;

[0059] (4) The shaped particles are dried to obtain the alkane gas adsorbent.

[0060] The drying process in step (4) consists of two stages: the temperature of the first stage is 160℃ and the holding time is 50min; the temperature of the second stage is 450℃ and the holding time is 150min.

[0061] Example 2

[0062] An alkane gas adsorbent for use in semiconductor manufacturing processes, comprising, by weight, the following raw materials: 52 parts activated manganese dioxide, 40 parts modified activated carbon, 27 parts activated copper oxide, 105 parts potassium permanganate aqueous solution, 0.2 parts lubricant, 0.01 parts manganese nitrate, and 1 part silica.

[0063] Silica includes precipitated silica and fumed silica, with a weight ratio of 1:3.

[0064] Precipitated silica was purchased from Guangzhou Housheng New Materials Co., Ltd., with an average particle size of 13 μm and a BET specific surface area of ​​161-190 m². 2 / g; Hydrophobic fumed silica was purchased from Shanghai Yingcheng New Materials Co., Ltd., model YC-SI15, with an average particle size of 15nm and a specific surface area of ​​175-225m². 2 / g; Active manganese dioxide was purchased from Yumu (Ningbo) New Materials Co., Ltd., model YM-MnO2-05, with an average particle size of 50nm and a specific surface area of ​​2000m². 2 / g; Activated copper oxide was purchased from Zhejiang Zhitai Nano-Micro New Materials Co., Ltd., with a particle size of 20nm and a specific surface area of ​​50-60m². 2 / g; the lubricant is ethylene bis-stearamide; the mass concentration of potassium permanganate aqueous solution is 6%.

[0065] The preparation steps of the modified activated carbon include: wetting the dried activated carbon with an equal mass of deionized water, then adding twice the weight of deionized water to soak the activated carbon, then adding copper chloride solution for impregnation treatment, heating at 95°C for 10 hours under vacuum conditions, condensing and refluxing, then discarding the impregnation solution, washing the solid with deionized water, drying under vacuum at 110°C for 2 hours, and calcining at 300°C for 2 hours to obtain the modified activated carbon.

[0066] The activated carbon was purchased from Shanghai Xitan Environmental Protection Technology Co., Ltd., with a particle size of 325 mesh.

[0067] The conditions for the immersion treatment were: a copper chloride solution with a mass fraction of 18%, an immersion ratio of 1:10, and an immersion time of 0.8 h.

[0068] The preparation method of the alkane gas adsorbent in this embodiment includes the following steps:

[0069] (1) Weigh out each raw material according to the proportion;

[0070] (2) Add activated manganese dioxide, modified activated carbon, activated copper oxide, white carbon black and lubricant to a kneader, mix and stir for 45 min, add potassium permanganate aqueous solution, and continue to stir and mix for 20 min to obtain a mixture;

[0071] (3) Add the mixture obtained in step (2) to a molding machine for pelletizing;

[0072] (4) The shaped particles are dried to obtain the alkane gas adsorbent.

[0073] The drying process in step (4) consists of two stages: the temperature of the first stage is 160℃ and the holding time is 50min; the temperature of the second stage is 450℃ and the holding time is 150min.

[0074] Example 3

[0075] An alkane gas adsorbent for use in semiconductor manufacturing processes, comprising, by weight, the following raw materials: 65 parts activated manganese dioxide, 50 parts modified activated carbon, 32 parts activated copper oxide, 110 parts potassium permanganate aqueous solution, 0.6 parts lubricant, 0.03 parts manganese nitrate, and 4 parts silica.

[0076] Silica includes precipitated silica and fumed silica, with a weight ratio of 1:3.

[0077] Precipitated silica was purchased from Guangzhou Housheng New Materials Co., Ltd., with an average particle size of 13 μm and a BET specific surface area of ​​161-190 m². 2 / g; Hydrophobic fumed silica was purchased from Shanghai Yingcheng New Materials Co., Ltd., model YC-SI15, with an average particle size of 15nm and a specific surface area of ​​175-225m². 2 / g; Active manganese dioxide was purchased from Yumu (Ningbo) New Materials Co., Ltd., model YM-MnO2-05, with an average particle size of 50nm and a specific surface area of ​​2000m². 2 / g; Activated copper oxide was purchased from Zhejiang Zhitai Nano-Micro New Materials Co., Ltd., with a particle size of 20nm and a specific surface area of ​​50-60m². 2 / g; the lubricant is ethylene bis-stearamide; the mass concentration of potassium permanganate aqueous solution is 6%.

[0078] The preparation steps of the modified activated carbon include: wetting the dried activated carbon with an equal mass of deionized water, then adding twice the weight of deionized water to soak the activated carbon, then adding copper chloride solution for impregnation treatment, heating at 95°C for 10 hours under vacuum conditions, condensing and refluxing, then discarding the impregnation solution, washing the solid with deionized water, drying under vacuum at 110°C for 2 hours, and calcining at 300°C for 2 hours to obtain the modified activated carbon.

[0079] The activated carbon was purchased from Shanghai Xitan Environmental Protection Technology Co., Ltd., with a particle size of 325 mesh.

[0080] The conditions for the immersion treatment were: a copper chloride solution with a mass fraction of 18%, an immersion ratio of 1:10, and an immersion time of 0.8 h.

[0081] The preparation method of the alkane gas adsorbent in this embodiment includes the following steps:

[0082] (1) Weigh out each raw material according to the proportion;

[0083] (2) Add activated manganese dioxide, modified activated carbon, activated copper oxide, white carbon black and lubricant to a kneader, mix and stir for 45 min, add potassium permanganate aqueous solution, and continue to stir and mix for 20 min to obtain a mixture;

[0084] (3) Add the mixture obtained in step (2) to a molding machine for pelletizing;

[0085] (4) The shaped particles are dried to obtain the alkane gas adsorbent.

[0086] The drying process in step (4) consists of two stages: the temperature of the first stage is 160℃ and the holding time is 50min; the temperature of the second stage is 450℃ and the holding time is 150min.

[0087] Example 4

[0088] An alkane gas adsorbent for use in semiconductor manufacturing processes, comprising, by weight, the following raw materials: 55 parts activated manganese dioxide, 42 parts modified activated carbon, 28 parts activated copper oxide, 107 parts potassium permanganate aqueous solution, 0.3 parts lubricant, 0.02 parts manganese nitrate, and 2 parts silica.

[0089] Silica includes precipitated silica and fumed silica, with a weight ratio of 1:2.

[0090] Precipitated silica was purchased from Guangzhou Housheng New Materials Co., Ltd., with an average particle size of 13 μm and a BET specific surface area of ​​161-190 m². 2 / g; Hydrophobic fumed silica was purchased from Shanghai Yingcheng New Materials Co., Ltd., model YC-SI15, with an average particle size of 15nm and a specific surface area of ​​175-225m². 2 / g; Active manganese dioxide was purchased from Yumu (Ningbo) New Materials Co., Ltd., model YM-MnO2-05, with an average particle size of 50nm and a specific surface area of ​​2000m². 2 / g; Activated copper oxide was purchased from Zhejiang Zhitai Nano-Micro New Materials Co., Ltd., with a particle size of 20nm and a specific surface area of ​​50-60m². 2 / g; the lubricant is ethylene bis-stearamide; the mass concentration of potassium permanganate aqueous solution is 6%.

[0091] The preparation steps of the modified activated carbon include: wetting the dried activated carbon with an equal mass of deionized water, then adding twice the weight of deionized water to soak the activated carbon, then adding copper chloride solution for impregnation treatment, heating at 95°C for 10 hours under vacuum conditions, condensing and refluxing, then discarding the impregnation solution, washing the solid with deionized water, drying under vacuum at 110°C for 2 hours, and calcining at 280°C for 2.5 hours to obtain the modified activated carbon.

[0092] The activated carbon was purchased from Shanghai Xitan Environmental Protection Technology Co., Ltd., with a particle size of 325 mesh.

[0093] The conditions for the immersion treatment were: a copper chloride solution with a mass fraction of 20%, an immersion ratio of 1:8, and an immersion time of 0.5 h.

[0094] The preparation method of the alkane gas adsorbent in this embodiment includes the following steps:

[0095] (1) Weigh out each raw material according to the proportion;

[0096] (2) Add activated manganese dioxide, modified activated carbon, activated copper oxide, white carbon black and lubricant to a kneader, mix and stir for 30 min, add potassium permanganate aqueous solution, and continue to stir and mix for 30 min to obtain a mixture;

[0097] (3) Add the mixture obtained in step (2) to a molding machine for pelletizing;

[0098] (4) The shaped particles are dried to obtain the alkane gas adsorbent.

[0099] The drying process in step (4) consists of two stages: the temperature of the first stage is 100℃ and the holding time is 70 min; the temperature of the second stage is 400℃ and the holding time is 180 min.

[0100] Example 5

[0101] An alkane gas adsorbent for use in semiconductor manufacturing processes, comprising, by weight, the following raw materials: 65 parts activated manganese dioxide, 48 parts modified activated carbon, 28 parts activated copper oxide, 106 parts potassium permanganate aqueous solution, 0.5 parts lubricant, 0.02 parts manganese nitrate, and 3 parts silica.

[0102] Silica includes precipitated silica and fumed silica, with a weight ratio of 1:5.

[0103] Precipitated silica was purchased from Guangzhou Housheng New Materials Co., Ltd., with an average particle size of 13 μm and a BET specific surface area of ​​161-190 m². 2 / g; Hydrophobic fumed silica was purchased from Shanghai Yingcheng New Materials Co., Ltd., model YC-SI15, with an average particle size of 15nm and a specific surface area of ​​175-225m². 2 / g; Active manganese dioxide was purchased from Yumu (Ningbo) New Materials Co., Ltd., model YM-MnO2-05, with an average particle size of 50nm and a specific surface area of ​​2000m². 2 / g; Activated copper oxide was purchased from Zhejiang Zhitai Nano-Micro New Materials Co., Ltd., with a particle size of 20nm and a specific surface area of ​​50-60m². 2 / g; the lubricant is ethylene bis-stearamide; the mass concentration of potassium permanganate aqueous solution is 6%.

[0104] The preparation steps of the modified activated carbon include: wetting the dried activated carbon with an equal mass of deionized water, then adding twice the weight of deionized water to soak the activated carbon, then adding copper chloride solution for impregnation treatment, heating at 95°C for 10 hours under vacuum conditions, condensing and refluxing, then discarding the impregnation solution, washing the solid with deionized water, drying under vacuum at 110°C for 2 hours, and calcining at 310°C for 1.5 hours to obtain the modified activated carbon.

[0105] The activated carbon was purchased from Shanghai Xitan Environmental Protection Technology Co., Ltd., with a particle size of 325 mesh.

[0106] The conditions for the immersion treatment were: a copper chloride solution with a mass fraction of 15%, an immersion ratio of 1:12, and an immersion time of 1 hour.

[0107] The preparation method of the alkane gas adsorbent in this embodiment includes the following steps:

[0108] (1) Weigh out each raw material according to the proportion;

[0109] (2) Add activated manganese dioxide, modified activated carbon, activated copper oxide, silica and lubricant to a kneader, mix and stir for 60 min, add potassium permanganate aqueous solution, and continue stirring and mixing for 10 min to obtain a mixture;

[0110] (3) Add the mixture obtained in step (2) to a molding machine for pelletizing;

[0111] (4) The shaped particles are dried to obtain the alkane gas adsorbent.

[0112] The drying process in step (4) consists of two stages: the temperature of the first stage is 200℃ and the holding time is 40 min; the temperature of the second stage is 500℃ and the holding time is 120 min.

[0113] Example 6

[0114] This embodiment provides an alkane gas adsorbent and its preparation method. The specific implementation method is the same as that in Embodiment 1, except that the mass ratio between active manganese dioxide and active copper oxide is 1.5:1.

[0115] Example 7

[0116] This embodiment provides an alkane gas adsorbent and its preparation method. The specific implementation method is the same as that in Embodiment 1, except that the mass ratio between active manganese dioxide and active copper oxide is 1:1.

[0117] Example 8

[0118] This embodiment provides an alkane gas adsorbent and its preparation method. The specific implementation method is the same as that in Embodiment 1, except that the silica is fumed silica.

[0119] Example 9

[0120] This embodiment provides an alkane gas adsorbent and its preparation method. The specific implementation method is the same as that in Embodiment 1, except that the silica is precipitated silica.

[0121] Comparative Example 1

[0122] This comparative example provides an alkane gas adsorbent and its preparation method. The specific implementation method is the same as that in Example 1, except that the active manganese dioxide in the raw materials is replaced by an equal amount of active copper oxide.

[0123] Comparative Example 2

[0124] This comparative example provides an alkane gas adsorbent and its preparation method. The specific implementation method is the same as in Example 1, except that the modified activated carbon in the raw materials is replaced by unmodified activated carbon.

[0125] Comparative Example 3

[0126] This comparative example provides an alkane gas adsorbent and its preparation method. The specific implementation method is the same as that in Example 1, except that active copper oxide is not added to the raw materials.

[0127] Comparative Example 4

[0128] This comparative example provides an alkane gas adsorbent and its preparation method. The specific implementation method is the same as that in Example 1, except that silica is not added to the raw materials.

[0129] Performance testing

[0130] 1. Adsorption capacity

[0131] The adsorbents prepared in Examples 1-9 and Comparative Examples 1-4 were characterized by adsorption capacity method. The specific steps are as follows: 15g of adsorbent was weighed. The gas composition at the inlet of the adsorber was 1000ppm silane, 1000ppm phosphine, and 1000ppm arsine, respectively. Nitrogen was used as the carrier. Adsorption isotherm data were obtained by volumetric method. The adsorption capacity of silane, phosphine, and arsine was calculated respectively. The results are shown in Table 1.

[0132] Table 1

[0133]

[0134] As shown in Table 1, the adsorbents prepared in Examples 1-5 have excellent adsorption effects on silanes, phosphines, and arsines, and have large adsorption capacities. In Examples 6 and 7, the ratio of activated manganese dioxide to activated copper oxide was changed, resulting in varying degrees of reduction in the adsorption effect of the adsorbents on silanes, phosphines, and arsines. In Examples 8 and 9, the type of silica was changed, resulting in varying degrees of reduction in the adsorption effect of the adsorbents on silanes, phosphines, and arsines.

[0135] In Comparative Example 1, replacing activated manganese dioxide with an equal amount of activated copper oxide significantly reduced the adsorption efficiency of the adsorbent for silanes, phosphines, and arsines, with the most significant reduction in silane adsorption efficiency. In Comparative Example 2, the addition of unmodified activated carbon significantly reduced the adsorption efficiency of the adsorbent for all three alkane gases. In Comparative Example 3, the absence of activated copper oxide in the raw material resulted in varying degrees of reduction in the adsorption efficiency of the adsorbent for the three alkane gases, with the most significant reduction for phosphine. The absence of silica in the raw material of Comparative Example 3 also resulted in varying degrees of reduction in the adsorption efficiency of the adsorbent for the three alkane gases.

[0136] Finally, it should be noted that the above specific embodiments are only used to illustrate the technical solutions of the present invention and not to limit it. Although the present invention has been described in detail with reference to examples, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all such modifications or substitutions should be covered within the scope of the claims of the present invention.

Claims

1. An alkyl gas adsorbent for use in a semiconductor process, characterized by, The adsorbent comprises, by weight, the following raw materials: 50-65 parts activated manganese dioxide, 40-50 parts modified activated carbon, 27-32 parts activated copper oxide, 105-110 parts potassium permanganate aqueous solution with a mass concentration of 5-7%, 0.2-0.6 parts lubricant, 0.01-0.03 parts manganese nitrate, and 1-4 parts silica. The silica includes precipitated silica and fumed silica in a weight ratio of 1:(2-5). The average particle size of the precipitated white carbon black is 10-15 μm, the BET specific surface area is 150-200 m 2 / g; The fumed white carbon black is a hydrophobic fumed white carbon black, with an average particle size of 10-20 nm, a specific surface area of 170-230 m 2 / g; The preparation steps of the modified activated carbon include: wetting the dried activated carbon with deionized water, soaking it in deionized water, then adding copper chloride solution for impregnation treatment, condensing and refluxing after vacuum heating, then discarding the impregnation liquid, washing, drying and calcining the solid to obtain the modified activated carbon. The conditions for the immersion treatment are as follows: the mass fraction of the copper chloride solution is 15-20%, the immersion ratio is 1:(8-12), and the immersion time is 0.5-1h.

2. The alkane gas adsorbent for semiconductor manufacturing processes according to claim 1, characterized in that, The weight ratio between the active manganese dioxide and the active copper oxide is (1.9-2.3):

1.

3. The alkane gas adsorbent for semiconductor manufacturing processes according to claim 1, characterized in that, The lubricant is ethylene bis-stearamide.

4. A method for preparing an alkane gas adsorbent for semiconductor manufacturing processes according to any one of claims 1-3, characterized in that, Includes the following steps: (1) Weigh each raw material according to the proportion; (2) Add activated manganese dioxide, modified activated carbon, activated copper oxide, silica and lubricant to a kneader and mix for 30-60 minutes. Add potassium permanganate aqueous solution and continue mixing for 10-30 minutes to obtain a mixture. (3) Add the mixture obtained in step (2) to the molding machine for pelletizing; (4) The formed particles are dried sequentially to obtain the alkane gas adsorbent.

5. The method for preparing an alkane gas adsorbent for semiconductor manufacturing according to claim 4, characterized in that, The drying process in step (4) includes two stages: the temperature of the first stage is 100-200℃ and the holding time is 40-70 min; the temperature of the second stage is 400-500℃ and the holding time is 120-180 min.

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