CN117339555B - Integral monolithic activated carbon adsorption material and application thereof - Google Patents
Integral monolithic activated carbon adsorption material and application thereofInfo
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Abstract
The invention relates to the technical field of semiconductor manufacturing, and discloses an integral monolithic active carbon adsorption material which is used for adsorbing and desorbing special gas in the process of preparing a semiconductor wafer, wherein the active carbon adsorption material contains 0.005-10% by mass of metal ions, and the metal ions are selected from one metal ion or a plurality of mixed ions in a first main group, a second main group, a third main group, an IB auxiliary group and an IIB auxiliary group. The activated carbon adsorption material is used for improving the adsorption capacity of the monolithic activated carbon adsorbent material to the special gas by introducing a certain content of metal hetero ions into the monolithic activated carbon adsorbent.
Description
Technical Field
The invention relates to the technical field of semiconductor manufacturing, in particular to an integral monolithic activated carbon adsorption material and application thereof, which are used for adsorbing and desorbing special gas in the preparation process of a semiconductor wafer.
Background
In the production and manufacturing process of ultra-large scale semiconductor integrated circuits, hazardous and toxic special gases are often used. The special gases refer to chemical gases, namely electron gases in gas categories, such as SiH4、PH3、AsH3、B2H6、N2O、NH3、SF6、NF3、CF4、BCl3、BF3、HCl、Cl2 with high purity and the like, used in the processes of extending, ion implantation, doping, washing and covering film formation in the semiconductor production links, and have important roles in the performance, the integration level and the yield of semiconductor integrated circuits.
In the process of manufacturing semiconductors, these specialty gases are usually transported by compression or liquefaction and stored in a specific container in a high density form, such as a high pressure gas cylinder. Once accidents occur in the transportation process, the special gases with hazard and toxicity can leak, such as the accidental release of high-pressure gases, the leakage of the gas cylinder and the like. Accidental leakage of these toxic gases can cause serious injury and even death to nearby personnel. There is a need for safer storage and transportation of specialty gases that are highly toxic or dangerous.
CN1132662 patent describes a negative pressure gas cylinder employing a packed molecular sieve adsorbent for safe and efficient use in high toxicity specialty gas related operations. The negative pressure gas steel cylinder utilizes the special regular nano-pore structure of the molecular sieve to provide the adsorption force to gas molecules so as to adsorb special gas with high toxicity, thereby reducing the pressure in the steel cylinder and reducing the chance of unexpected leakage of the gas. The release of the adsorbed specialty gas on the molecular sieve adsorbent may be accomplished by a pressure differential, by providing a pressure outside the vessel that is lower than the pressure inside the vessel. The release of the adsorbed specialty gas may also be accomplished by heating the physical adsorbent media to break the low association bonds between the adsorbed gas and the physical adsorbent media. In addition, the release of the adsorbed specialty gas can also be accomplished by a carrier gas flowing through the interior of the cylinder vessel, thereby effecting a concentration differential on the adsorbed gas to cause a substantial influx of the adsorbed gas into the carrier gas stream.
In order to increase the adsorption capacity of the negative pressure gas steel cylinder to the high-toxicity special gas, the activated carbon is used for filling the negative pressure gas steel cylinder due to the fact that the activated carbon has a higher surface area and a rich nano-sized pore structure than a molecular sieve, so that the adsorption of the high-toxicity special gas is improved. US5704965 describes a negative pressure gas cylinder employing filled activated carbon pellets as the adsorbent. In contrast to the use of molecular sieves as the adsorbent material in CN1132662, the negative pressure gas cylinders described in US5704965 patent utilize activated carbon adsorbents having a higher adsorption capacity for highly toxic specialty gases than molecular sieve adsorbents.
CN1723072 describes a method for increasing the adsorption of highly toxic specialty gases by filling monolithic carbon physical adsorbents in a negative pressure gas cylinder. CN1723072 patent describes the characteristics of monolithic carbon physical adsorbents, i.e., monolithic carbon physical adsorbents that form pores with crack shapes of less than 2 nanometers greater than 20% and 0.3 to 0.7 nanometers greater than 30% by pyrolysis and activation of some polymers. The monolithic carbon adsorbent material has an adsorption of higher than 50% of the specialty gas AsH3 calculated on a cylinder volume basis.
In these molecular sieve or activated carbon physical adsorbent based gas storage and distribution systems, the adsorption and desorption capacity of the adsorbent media for highly toxic specialty gases is a major limitation in practical applications. The formation of monolithic carbon sorbents by pyrolysis and activation of some polymers is not greatly enhanced by the choice of process parameters or different polymer precursors due to the limited amount of highly toxic specialty gases that can be adsorbed by the process conditions. The method is used for improving the adsorption capacity of the monolithic activated carbon adsorbent material to the special gas by introducing a certain content of metal hetero ions into the monolithic activated carbon adsorbent.
In these molecular sieve or activated carbon physical adsorbent based gas storage and distribution systems, the adsorption and desorption capacity of the adsorbent media for highly toxic specialty gases is a major limitation in practical applications. Therefore, the technical problem of how to further increase the adsorption and desorption capacity of the physical adsorbent is a direction of research by those skilled in the art.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide an integral monolithic activated carbon adsorption material, which improves the adsorption capacity of the monolithic activated carbon adsorbent material to special gas by introducing metal ions.
In order to achieve the aim, the technical scheme adopted by the invention is that the integral monolithic active carbon adsorption material is used for adsorbing and desorbing special gas in the preparation process of a semiconductor wafer, wherein the active carbon adsorption material contains 0.005-10% of metal ions by mass percent, and the metal ions are selected from one metal ion or a plurality of mixed ions in a first main group, a second main group, a third main group, an IB auxiliary group and an IIB auxiliary group.
As a specific embodiment, the activated carbon adsorption material is prepared from high molecular polymers, polysaccharide sugar compounds or cellulose through extrusion molding, pyrolysis and activation processes.
The high molecular polymer comprises a biological polymer, a copolymer, a conductive polymer, a natural high polymer or a synthetic polymer, and the polymer comprises at least one or a mixture of a plurality of polyethylene, polypropylene, polyvinyl chloride, polystyrene, polytetrafluoroethylene, polyethylene terephthalate, polystyrene, polycarbonate, polyvinylidene fluoride, polyvinylidene chloride, phenolic resin, polyvinyl chloride resin, polyester resin, polyamide resin, BS resin and epoxy resin.
The saccharide compound includes disaccharide and polysaccharide compounds. The saccharide compound comprises maltose, sucrose, lactose, cellobiose, melibiose, cellodextrin, fructo-oligosaccharide, galactooligosaccharide, isomaltooligosaccharide, maltodextrin, mannooligosaccharide, raffinose, agar, amylopectin, amylose, arabinoxylan, chitin sugar, chitosan, glucose, dextrin, levan, galactomannan, glucan, glycogen, guar gum, hemicellulose, lentinan, lichenin, mannans, natural gums, pectin, polysaccharide peptides, agarose, welan gum, xanthan gum, xylan and the like.
The cellulose includes wood pulp, sawdust, newsprint, coconut shell, olivine, peach blossom stone, apricot kernel, viscose rayon, cotton linter, melon nut shell, macadamia nut shell, cellulose acetate, bacterial cellulose, lignin, black thorn stone, walnut shell, jujube wood, rice hull, coffee parchment, coffee grounds, bagasse, sorghum millet, bamboo, mango kernel, almond shell, corncob, cherry stone and grape seed.
As a specific embodiment, the activated carbon adsorption material adopts one or more of polyvinylidene fluoride, polyvinylidene chloride and phenolic resin. The activated carbon adsorption material preferably adopts polyvinylidene fluoride and/or polyvinylidene chloride. More preferably, polyvinylidene chloride is used as the activated carbon adsorption material.
As another specific embodiment, the activated carbon adsorption material is prepared by directly extruding and molding activated carbon particles or mixing the activated carbon particles with a binder and then extruding and molding, pyrolyzing and activating the activated carbon adsorption material, wherein the added mass of the binder in the activated carbon adsorption material is 0-99%, and the activated carbon particles are prepared from at least one of wood chip activated carbon, shell activated carbon, coconut shell activated carbon, biomass activated carbon and asphalt-based microsphere activated carbon. The activated carbon particles have a specific surface area of at least 100m 2/g, preferably greater than 500m 2/g, more preferably greater than 800m 2/g, more preferably greater than 1000m 2/g, more preferably greater than 1500m 2/g. The activated carbon particles have a pore volume of at least greater than 0.05cm 3/g, preferably greater than 0.1cm 3/g, more preferably greater than 0.3cm 3/g, more preferably greater than 0.5cm 3/g, more preferably greater than 0.8cm 3/g, more preferably greater than 1.0cm 3/g. The activated carbon particles have a pore diameter of less than 20 nanometers, preferably less than 15 nanometers, more preferably less than 10 nanometers, more preferably less than 8 nanometers, more preferably less than 5 nanometers, more preferably less than 3 nanometers.
The addition mass of the binder in the monolithic activated carbon material adsorbent is 0-99%. In some embodiments the binder is added at a mass of at least 1%, preferably at least 10%, preferably at least 30%, more preferably at least 60%. In some embodiments the binder is preferably added to the monolithic activated carbon material adsorbent in a mass of 0-99％,1-99％,10-99％,20-99％,30-99％,40-99％,50-99％,60-99％,70-99％,80-99％,0-90％,1-90％,10-90％,20-90％,30-90％,40-90％,50-90％,60-90％,70-90％,80-90％,0-80％,1-80％,10-80％,20-80％,30-80％,40-80％,50-80％,60-80％,70-80％,0-70％,1-70％,10-70％,20-70％,30-70％,40-70％,50-70％,60-70％. -99%,50-99%,70-99%,80-99%,5-90%,50-90%,50-90%,70-90%,80-90%.
In a specific embodiment, the binder is added in an amount of at least 1%, and the binder is a polymer, a polysaccharide compound or cellulose, preferably polyvinylidene fluoride and/or polyvinylidene chloride. The binder is preferably polyvinylidene fluoride and/or polyvinylidene chloride. More preferably, polyvinylidene chloride is used as the binder.
As another specific embodiment, the activated carbon adsorption material may further include a certain inorganic porous material including, but not limited to, various types of molecular sieves, porous silicon materials, metal organic framework compounds (MOFs), or a certain inorganic binder including, but not limited to, halloysite, attapulgite, alumina, pseudo-boehmite, silica, destoner, rectorite, sepiolite, and the like. In some embodiments the inorganic porous material or binder is added in an amount of at least 1%.
As another specific embodiment, the activated carbon adsorption material does not contain any inorganic porous material and inorganic binder.
The metal ions are selected from metal ions in the first main group, the second main group, the third main group, the IB subgroup and the IIB subgroup or mixed ions thereof. The metal ions in the first main group and the second main group are preferable, and lithium ion, sodium ion, potassium ion, rubidium ion, cesium ion, beryllium ion, magnesium ion, calcium ion, strontium ion, barium ion, aluminum ion, gallium ion are more preferable.
More preferred are magnesium ions, calcium ions, strontium ions and barium ions, in particular one of magnesium ions and calcium ions or a mixture thereof. More preferably calcium ions.
The metal ions described in some embodiments may not comprise or comprise a concentration of metal ions of the IB and IIB sub-groups or mixtures thereof of not more than 1000ppm, preferably not more than 500ppm or not more than 100ppm, in certain embodiments not more than 50ppm, in certain embodiments not more than 10ppm.
As a specific embodiment, the metal ion is selected from the first main group and/or the second main group.
As a specific embodiment, magnesium ion and/or calcium ion is used as the metal ion, and preferably, calcium ion is used as the metal ion.
As a specific embodiment, the metal ions are added to the activated carbon adsorbent material in the form of metal ion salts, oxides, hydroxides, or mixtures of metal ions.
Preferably, the metal ions are added to the activated carbon adsorption material in the form of an aqueous solution using a metal ion salt.
The metal ions can be added before the activated carbon is molded, or can be added after the activated carbon is molded. Or the active carbon prepared by adopting a specific material with the metal ion content can contain the metal ion concentration.
The metal ions are added in a mode of 1) directly mixing the metal ions with active carbon or active carbon preparation raw materials in the form of ionic metal salts, 2) carrying out ion exchange on the metal ions and the active carbon preparation raw materials, and 3) directly immersing the active carbon preparation raw materials in a metal ion salt solution. Preferably, the activated carbon is used to prepare the raw material which is directly immersed in the metal ion salt solution.
The introduced metal ions described in one particular embodiment are used without direct activation. In a specific embodiment, the activation of the metal ions is performed by heating at a certain temperature and under a certain atmosphere. The heating temperature includes 50 to 500 ℃, preferably 50 to 400 ℃,50 to 300 ℃,50 to 200 ℃,50 to 150 ℃,50 to 100 ℃,100 to 500 ℃,100 to 400 ℃,100 to 300 ℃,100 to 200 ℃, more preferably 100 to 200 ℃, and the atmosphere includes inert gases such as nitrogen, argon, helium and reactive gases such as air, oxygen, hydrogen, carbon dioxide, carbon monoxide, or a mixture of two or more of the foregoing gases. Nitrogen is preferably used.
As a specific embodiment, the content of metal ions in the activated carbon adsorption material is 0.001% -10%, 0.01% -10%, 0.05% -10%, preferably 0.01% -5%, 0.01% -2%, 0.01% -1%, more preferably 0.05% -2%.
The activated carbon activation method includes a chemical activation method and a gas activation method or a combination of both.
The chemical activation method comprises the steps of uniformly mixing various carbon-containing raw materials with chemical activation reagents, and then carbonizing, activating, recovering chemicals, rinsing, drying and the like at a certain temperature to prepare the activated carbon. Among them, phosphoric acid, zinc chloride, potassium hydroxide, sodium hydroxide, sulfuric acid, potassium carbonate, polyphosphoric acid, phosphoric acid esters, and the like can be used as the activating agent. The gas activation method comprises the step of contacting carbonized raw materials with activating gases such as water vapor, CO 2、N2, CO or air at a high temperature of 800-1000 ℃ so as to perform an activation reaction.
The heating temperature herein includes 150 to 1500 ℃, preferably 200 to 1000 ℃,200 to 800 ℃,200 to 600 ℃,300 to 1000 ℃,300 to 800 ℃,300 to 600 ℃,400 to 1000 ℃,400 to 800 ℃,400 to 600 ℃, more preferably 400 to 800 ℃. The atmosphere includes inert gases such as nitrogen, argon, helium and reactive gases such as air, oxygen, hydrogen, carbon dioxide, carbon monoxide or a mixture of two or more thereof. Nitrogen is preferred.
The final molding of the activated carbon extrusion molding process can be integrated monolithic molecular sieve materials such as cylinder type, square column type, polygonal column type, large sphere type, large polygonal type and the like. The cylindrical and square column types are preferable, and the cylindrical type is more preferable.
It is a further object of the present invention to provide for the use of the monolithic activated carbon adsorbent material described above in specialty gas storage and dispensing systems in negative pressure gas cylinders. Such gases that are adsorbed include, but are not limited to, silane, diborane, arsine, phosphane, chlorine, boron trichloride, boron trifluoride, trimethylantimony, tungsten hexafluoride, hydrogen fluoride, hydrogen chloride, hydrogen bromide, hydrogen iodide, germane, ammonia, stibine, hydrogen sulfide, nitrogen trifluoride.
Compared with the prior art, the monolithic activated carbon adsorption material has the advantages that the monolithic activated carbon adsorption material is used for improving the adsorption capacity of the monolithic activated carbon adsorption material to special gases by introducing a certain content of metal hetero ions into the monolithic activated carbon adsorption material.
Detailed Description
The technical scheme of the invention is further described below in conjunction with specific embodiments.
In some embodiments, the monolithic activated carbon adsorbent is prepared by extrusion, pyrolysis, and activation of a high molecular polymer, a polysaccharide carbohydrate, or cellulose.
In other embodiments, the monolithic activated carbon adsorbent is prepared by uniformly mixing a high molecular polymer, a polysaccharide saccharide compound or cellulose as a binder with activated carbon particles in a certain proportion, and then pressing under a certain pressure, such as 8 MPa. The formed monolithic adsorbent precursor is pyrolyzed and activated to form the monolithic activated carbon adsorbent. The binder is selected from high molecular polymer, saccharide compound of polysaccharide or organic polymer of cellulose. The binder adopts polyvinylidene fluoride and/or polyvinylidene chloride. The binder is preferably polyvinylidene fluoride and/or polyvinylidene chloride. More preferably, polyvinylidene chloride is used as the binder.
The testing method comprises the following steps:
1) The specific surface area of the monolithic activated carbon adsorbent is measured by a Jin Aipu V-Sorb 2800 specific surface area and a pore diameter tester according to weight;
2) Density measurements are determined by measuring size and mass;
3) The determination of the adsorption of ammonia, phosphane and phosphorus trifluoride was carried out in a self-made adsorption device:
a certain amount of monolithic activated carbon is placed in an adsorption vessel, vacuumized for at least 6 hours under 0.1Mpa, and then the corresponding adsorption gas is added until the adsorption is balanced. The amount of gas adsorbed was estimated from the increased weight change of the monolithic activated carbon. Then vacuum is applied for at least 6 hours at 0.1Mpa, and the desorption amount of the gas is estimated from the reduced weight change of the monolithic activated carbon.
1. Influence of preparation conditions on the performance of monolithic activated carbon adsorbents
The effect of the preparation conditions on the performance of monolithic activated carbon adsorbents is studied in table 1. Specific surface area of activated carbon, and other characteristics.
In some of the following examples, phenolic resin, polyvinylidene chloride and polyvinylidene fluoride were each prepared by extrusion, pyrolysis and activation processes to give monolithic activated carbon adsorbents. In other embodiments, polyvinylidene chloride and polyvinylidene fluoride are used as binders, respectively, and are mixed with a coconut activated carbon particle according to a certain proportion, and then the mixture is subjected to extrusion molding, pyrolysis and activation processes to prepare the monolithic activated carbon adsorbent. The coconut shell activated carbon particles have specific surface areas of more than 1000m 2/g, pore volumes of more than 0.30cm 2/g and pore diameters of more than 4 nanometers.
The monolithic porous inorganic material adsorbent is mixed together according to the proportion of each component, and is molded under certain extrusion and activation conditions. The monolithic porous inorganic material adsorbent in the examples is cylindrical, and monolithic cylindrical adsorbents with different volumes, which can be 10 mm to 100 mm in diameter and 5mm to 200 mm in height, are prepared according to different experimental conditions.
TABLE 1 preparation of monolithic activated carbon adsorbents
In table 1, samples 1, 2 and 5 were directly extruded using phenolic resin, polyvinylidene fluoride or polyvinylidene fluoride as raw materials to form monolithic activated carbon adsorbent materials. In addition, the results of samples 3, 4, 6, 7 and 8 show that the polyvinylidene fluoride or the polyvinylidene fluoride and the activated carbon particles are matched to show good bonding effect and influence the sintering density and the specific surface area.
2. Effect of calcium ion loading on monolithic activated carbon adsorbent Performance
The effect of calcium ion loading on the performance of monolithic activated carbon adsorbents was studied in this example and is specifically shown in table 2.
TABLE 2
In Table 2, sample 9 was a monolithic activated carbon adsorbent prepared from polyvinylidene chloride as a binder and activated carbon particles by a process of co-extrusion, pyrolysis, and activation. Wherein sample 10 was prepared by immersing sample 9 in 0.5M aqueous calcium nitrate solution, at room temperature for at least 10 minutes, then blowing off the excess solution with nitrogen, and firing at 120℃for 3 hours. The net weight of the introduced calcium ions in the monolithic activated carbon adsorbent was 0.48%. The specific surface area of the monolithic molecular sieve is obviously reduced by 21% due to the loading of the calcium ions.
3. Adsorption influence of monolithic activated carbon adsorbent carried by calcium ions on ethanol and water
The effect of a calcium ion-loaded monolithic activated carbon adsorbent on ethanol and water adsorption was studied mainly in this example, see table 3.
TABLE 3 Table 3
In Table 3, the weight measurement was performed after immersing samples 9 and 10 in pure water and pure ethanol liquid, respectively, and then purging off the excess liquid with nitrogen gas. The resulting adsorption amounts of ethanol and water were converted into calculated adsorption amounts of 100 g or 1 liter of sample 9 and sample 10. Obviously, the adsorption amount of the monolithic activated carbon adsorbent to water and ethanol is not obviously changed after the calcium ions are carried.
4. Adsorption of pH 3 by calcium ion-loaded monolithic activated carbon adsorbent
The adsorption effect of a calcium ion-loaded monolithic activated carbon adsorbent on pH 3 was studied in this example, and the specific results are shown in Table 4.
TABLE 4 Table 4
In Table 4, a certain amount of sample 9 and sample 10 were taken and placed in a gas cylinder and evacuated, respectively. The phosphane gas is gradually introduced into the steel cylinder under vacuum at room temperature until the balance state. The adsorbed weight gain of the phosphine for the monolithic activated carbon adsorbent was then determined. The resulting adsorption amount of phosphane was converted into the adsorption amount calculated as 100 g or 1 liter of sample 9 and sample 10. It can be seen from Table 4 that both sample 9 and sample 10 produced significant adsorption of phosphane. Although it is clear from Table 2 that the specific surface area of sample 10 is lower than that of sample 9, it is clear from Table 4 that the amount of the adsorbed phosphane by sample 10 is significantly increased, the amount of the adsorbed phosphane by sample 10 is increased by 20.9% calculated as 100 g of activated carbon adsorbent, and the amount of the adsorbed phosphane by sample 10 is increased by about 24.8% calculated as 1 liter of activated carbon adsorbent, for example, the amount of the adsorbed phosphane by sample 10 is significantly increased by 56% in consideration of the amount of the adsorbed phosphane by unit specific surface area, compared with sample 9.
5. Influence of the activation conditions of the monolithic activated carbon adsorbent on the adsorption amount of ammonia molecules
The adsorption performance of the monolithic activated carbon adsorbent on ammonia gas is mainly studied in this example. Sample 11 was prepared by mixing, extrusion molding, pyrolysis and activation of polyvinylidene chloride as a binder and activated carbon particles to obtain a monolithic activated carbon adsorbent, wherein the content of calcium ions was 0.1%, and placing the monolithic activated carbon adsorbent in a self-made gas adsorption and desorption device for vacuum pumping. Ammonia gas was gradually introduced into sample 11 under vacuum at room temperature until equilibrium. The adsorption weight gain of the monolithic activated carbon adsorbent for ammonia was then determined. The adsorption results are shown in Table 5.
TABLE 5
| Sample of | Concentration of calcium ion | Density/(g/ml) | Specific area/(m 2/g) | Adsorption rate g/100g | Adsorption rate g/L |
| 11 | 0.1% | 1.18 | 670 | 9.83 | 116.3 |
As can be seen from Table 5, the adsorption amount of sample 11 to ammonia molecules was 9.83g calculated as 100 g of activated carbon adsorbent and 116.3g calculated as 1L of activated carbon adsorbent for the monolithic activated carbon adsorbent prepared from polyvinylidene chloride having a calcium ion concentration of 0.1%.
6. Results of adsorption and desorption of ammonia molecules by monolithic activated carbon adsorbent
The present example is a main study of adsorption and desorption of ammonia molecules by monolithic activated carbon adsorbent sample 11. Placing the sample in a self-made gas adsorption and desorption device, vacuumizing, and gradually inputting ammonia gas into the sample at room temperature under the vacuum condition until the sample is in an equilibrium state. The adsorption amount was measured by measuring the adsorption weight gain of the monolithic activated carbon adsorbent for ammonia gas. And then carrying out vacuumizing treatment on the sample, and measuring the unreleased amount, namely the residual amount, of the ammonia gas in the sample after balancing. The results are shown in Table 6.
TABLE 6
From the results in table 6, it can be seen that ammonia adsorption is greater than 85% reversible in adsorption and desorption cycle tests of ammonia molecules in monolithic activated carbon.
7. Results of adsorption of boron trifluoride by monolithic activated carbon adsorbent
The adsorption result test of boron trifluoride on the monolithic activated carbon adsorbent sample 11 showed that the adsorption of boron trifluoride by sample 11 was remarkable, and 30 g of boron trifluoride per 100 g of the sample was adsorbed, which corresponds to 355 g of boron trifluoride in 1 liter of sample 11.
The above embodiments are provided to illustrate the technical concept and features of the present invention and are intended to enable those skilled in the art to understand the content of the present invention and implement the same, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention.
Claims (7)
1. The application of the integral monolithic activated carbon adsorption material in adsorbing and desorbing special gas in the preparation process of a semiconductor wafer is characterized in that the integral monolithic activated carbon adsorption material contains 0.005-10% of metal ions by mass, wherein the metal ions are calcium ions, metal ion salts are adopted for the metal ions, the metal ions are added into the activated carbon adsorption material in a water solution mode, and the special gas is PH 3 or BF 3.
2. The use of an integrated monolithic activated carbon adsorption material for adsorbing and desorbing a specialty gas in a semiconductor wafer manufacturing process of claim 1, wherein said integrated monolithic activated carbon adsorption material is prepared from a carbohydrate of a high molecular polymer or polysaccharide by extrusion, pyrolysis and activation processes.
3. The use of an integral monolithic activated carbon adsorption material for adsorbing and desorbing a specialty gas in a semiconductor wafer manufacturing process of claim 2, wherein said integral monolithic activated carbon adsorption material is a blend of one or more of polyvinylidene fluoride, polyvinylidene chloride, phenolic resin.
4. The use of an integrated monolithic activated carbon adsorption material for adsorbing and desorbing a specialty gas in a semiconductor wafer manufacturing process according to claim 1, wherein the integrated monolithic activated carbon adsorption material is prepared by directly extrusion molding activated carbon particles or by mixing activated carbon particles with a binder and then performing extrusion molding, pyrolysis and activation, wherein the added mass of the binder in the integrated monolithic activated carbon adsorption material is 0-99%, and the activated carbon particles are prepared from at least one of wood chip activated carbon, shell activated carbon, coconut shell activated carbon, biomass activated carbon and asphalt-based microsphere activated carbon.
5. The use of an integrated monolithic activated carbon adsorption material for adsorbing and desorbing a specialty gas in a semiconductor wafer process of claim 4 wherein said binder is added in an amount of at least 1% by weight, said binder being a carbohydrate of a high molecular polymer or polysaccharide.
6. The use of an integral monolithic activated carbon adsorption material for adsorbing and desorbing a specialty gas in a semiconductor wafer manufacturing process of claim 1, wherein the content of metal ions in said integral monolithic activated carbon adsorption material is between 0.05% and 2%.
7. The use of an integral monolithic activated carbon adsorbent material for adsorbing and desorbing specialty gases in semiconductor wafer fabrication as set forth in claim 1 wherein said integral monolithic activated carbon adsorbent material is used in specialty gas storage and dispensing systems in negative pressure gas cylinders.
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