CN113683115A - Preparation method of semiconductor material for 5G signal transmission - Google Patents
Preparation method of semiconductor material for 5G signal transmission Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 52
- 239000004065 semiconductor Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 230000008054 signal transmission Effects 0.000 title claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 65
- 238000000227 grinding Methods 0.000 claims abstract description 59
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229920002239 polyacrylonitrile Polymers 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 23
- 238000001914 filtration Methods 0.000 claims abstract description 22
- 239000011265 semifinished product Substances 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims description 91
- 239000000243 solution Substances 0.000 claims description 75
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 63
- 238000005406 washing Methods 0.000 claims description 46
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 42
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 42
- 239000002244 precipitate Substances 0.000 claims description 39
- 239000007787 solid Substances 0.000 claims description 38
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 37
- 239000008367 deionised water Substances 0.000 claims description 35
- 229910021641 deionized water Inorganic materials 0.000 claims description 35
- 238000004140 cleaning Methods 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 22
- 239000007810 chemical reaction solvent Substances 0.000 claims description 21
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 21
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 21
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 16
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 14
- 229910000366 copper(II) sulfate Inorganic materials 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- JJLJMEJHUUYSSY-UHFFFAOYSA-L Copper hydroxide Chemical compound [OH-].[OH-].[Cu+2] JJLJMEJHUUYSSY-UHFFFAOYSA-L 0.000 claims description 7
- 239000005750 Copper hydroxide Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 229910001956 copper hydroxide Inorganic materials 0.000 claims description 7
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 7
- 229960004887 ferric hydroxide Drugs 0.000 claims description 7
- 239000011790 ferrous sulphate Substances 0.000 claims description 7
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 7
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 claims description 7
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 claims description 7
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 abstract description 19
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 abstract description 19
- 229940112669 cuprous oxide Drugs 0.000 abstract description 19
- 239000013078 crystal Substances 0.000 abstract description 11
- 239000000126 substance Substances 0.000 abstract description 7
- 239000005416 organic matter Substances 0.000 abstract description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 abstract description 4
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- 238000005119 centrifugation Methods 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 239000005751 Copper oxide Substances 0.000 description 2
- 206010057040 Temperature intolerance Diseases 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 229910000431 copper oxide Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000008543 heat sensitivity Effects 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 238000010295 mobile communication Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000008542 thermal sensitivity Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Inorganic Chemistry (AREA)
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Abstract
The invention discloses a preparation method of a semiconductor material for 5G signal transmission, which particularly relates to the technical field of semiconductor preparation and specifically comprises the following steps: the method comprises the following steps: preparing raw materials, and step two: preparing a reaction device, and step three: preparing a solvent, and step four: preparing a semi-finished product, and step five: filtering, and a sixth step: grinding, step seven: and (5) purifying. According to the invention, the semiconductor organic matter is added in the existing cuprous oxide preparation process, on the basis of not changing the mechanical property of an inorganic semiconductor, the property of the organic matter is increased, and the added polyacrylonitrile and phthalocyanine enable the cuprous oxide surface to adsorb partial substances with benzene ring property and increase hydroxyl, so that the mixture crystal enhances the hydrophobicity on the mechanical property and the semiconductor property of the cuprous oxide, and the service life of a semiconductor material is prolonged.
Description
Technical Field
The invention relates to the technical field of semiconductor preparation, in particular to a preparation method of a semiconductor material for 5G signal transmission.
Background
The 5G network, i.e. the fifth generation mobile communication network (5th generation mobile networks or 5th generation wireless systems, abbreviated as 5G), is the latest generation cellular mobile communication technology. The performance goals are high data rates, reduced latency, energy savings, reduced cost, increased system capacity, and large-scale device connectivity. With the 5G technology, semiconductor materials are inevitably involved, cuprous oxide has equivalent semiconductor properties, is a monovalent copper oxide, is bright red powdery solid, is almost insoluble in water, is disproportionated into bivalent copper and a copper simple substance in an acid solution, and is gradually oxidized into black copper oxide in wet air.
When copper oxide is actually used as a semiconductor material, cuprous oxide has poor environmental adaptability, such as poor water resistance and poor hydrophobicity.
Disclosure of Invention
In order to overcome the above defects in the prior art, embodiments of the present invention provide a method for preparing a semiconductor material for 5G signal transmission, in which a semiconductor organic substance is added in the existing preparation process of cuprous oxide, on the basis of not changing the mechanical properties of an inorganic semiconductor, the properties of the organic substance are increased, and polyacrylonitrile and phthalocyanine are added, so that a part of substances with benzene ring properties are adsorbed on the surface of cuprous oxide, and hydroxyl groups are added, so that the crystal of the mixture enhances the hydrophobicity and prolongs the service life of the semiconductor material on the mechanical properties and the semiconductor properties of cuprous oxide.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a semiconductor material for 5G signal transmission specifically comprises the following steps:
the method comprises the following steps: preparing raw materials, namely enough deionized water, toluene, N-dimethylformamide, sodium hydroxide solution, polyacrylonitrile, phthalocyanine, CuSO4 solution, FeSO4 solution, ethylene glycol and absolute ethyl alcohol;
step two: preparing a reaction device, selecting a proper agate grinding kettle, a proper reaction kettle, a proper drying box and a proper centrifugal machine according to the use specification, cleaning the required device and then drying for later use;
step three: preparing a solvent, namely mixing toluene and N-dimethylformamide according to a molar ratio of 1: 1, uniformly mixing and placing in a reaction kettle to be used as a reaction solvent in the subsequent steps;
step four: firstly, adding a sodium hydroxide solution into a solvent in a reaction kettle to make the reaction solvent alkaline, and then mixing polyacrylonitrile and phthalocyanine according to a ratio of 1: 1-1: 1.5, then injecting the mixed solution of CuSO4 and FeSO4 into a reaction solvent, sealing and reacting for 30-60 minutes, and simultaneously shaking a reaction kettle to uniformly disperse the separated precipitates in the reaction solution into the mixture;
step five: filtering, stripping the precipitate obtained by the reaction, washing with deionized water for multiple times, and filtering to obtain a mixture of copper hydroxide, ferrous hydroxide and ferric hydroxide;
step six: grinding, namely placing the mixture obtained in the fifth step into a grinding kettle for continuous grinding to enable the mixture to be more fully contacted, grinding for 60-120 minutes until the color of all the mixtures in the grinding kettle is completely changed into black to obtain a material A, washing the obtained material A with deionized water for multiple times, filtering, collecting water-insoluble solids, placing the solids into a drying box for drying, and then further finely grinding to obtain semi-finished product powder;
step seven: and purifying, dissolving the semi-finished product powder obtained in the sixth step in ethylene glycol, then placing the solution in a heating kettle, heating to 150-.
In a preferred embodiment, the molar ratio of the sodium hydroxide solution to the mixture of polyacrylonitrile and phthalocyanine in said step four is 20: 1-50: 1, wherein the molar ratio of the copper sulfate solution to the ferrous sulfate solution in the mixture is 1: 10.
in a preferred embodiment, the step four mixture first presents a white precipitate which after a period of time turns reddish brown and finally to a grayish green precipitate.
In a preferred embodiment, the temperature of the material a during drying in the sixth step is 60-100 ℃, and the drying temperature is kept for 1-5 hours, the fineness of the semi-finished powder obtained by fine grinding of the dried material a is 500-1000 meshes, and the fine grinding time is controlled to be 30-60 minutes.
In a preferred embodiment, the red solid cleaning mode in the step seven is as follows: firstly, washing with absolute ethyl alcohol, drying, washing with deionized water, drying again, then continuously washing with absolute ethyl alcohol, then drying again and washing with deionized water, drying, then washing with absolute ethyl alcohol, and finally washing with absolute ethyl alcohol.
In a preferred embodiment, the drying temperature of the drying oven used for drying the red solid washed by the absolute ethyl alcohol in the step seven is 80-90 ℃.
The invention has the technical effects and advantages that:
1. according to the invention, the semiconductor organic matter is added in the existing cuprous oxide preparation process, on the basis of not changing the mechanical property of an inorganic semiconductor, the property of the organic matter is increased, and the added polyacrylonitrile and phthalocyanine enable the cuprous oxide surface to adsorb partial substances with benzene ring property and increase hydroxyl, so that the mixture crystal has enhanced hydrophobicity on the mechanical property and the semiconductor property of the cuprous oxide, and the service life of a semiconductor material is prolonged;
2. the semiconductor material prepared by the process has high heat sensitivity, the conductivity is enhanced with the continuous rise of temperature, the process is simple, the equipment requirement is low, the operability is strong, and the method has good social popularization and application.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the invention provides a preparation method of a semiconductor material for 5G signal transmission, which specifically comprises the following steps:
the method comprises the following steps: preparing raw materials, namely enough deionized water, toluene, N-dimethylformamide, sodium hydroxide solution, polyacrylonitrile, phthalocyanine, CuSO4 solution, FeSO4 solution, ethylene glycol and absolute ethyl alcohol;
step two: preparing a reaction device, selecting a proper agate grinding kettle, a proper reaction kettle, a proper drying box and a proper centrifugal machine according to the use specification, cleaning the required device and then drying for later use;
step three: preparing a solvent, namely mixing toluene and N-dimethylformamide according to a molar ratio of 1: 1, uniformly mixing and placing in a reaction kettle to be used as a reaction solvent in the subsequent steps;
step four: firstly, adding a sodium hydroxide solution into a solvent in a reaction kettle to make the reaction solvent alkaline, and then mixing polyacrylonitrile and phthalocyanine according to a ratio of 1: 1, then injecting a mixture solution of CuSO4 and FeSO4 which is mixed according to a certain proportion into a reaction solvent, carrying out a sealing reaction for 30 minutes, firstly generating a white precipitate, converting the white precipitate into reddish brown after a period of time, and finally converting the reddish green precipitate, and simultaneously oscillating a reaction kettle to uniformly disperse the precipitate which is separated from the reaction solution into the mixture, wherein the molar ratio of a sodium hydroxide solution to the mixture of polyacrylonitrile and phthalocyanine is 20: 1, wherein the molar ratio of the copper sulfate solution to the ferrous sulfate solution in the mixture is 1: 10;
step five: filtering, stripping the precipitate obtained by the reaction, washing with deionized water for multiple times, and filtering to obtain a mixture of copper hydroxide, ferrous hydroxide and ferric hydroxide;
step six: grinding, namely putting the mixture obtained in the fifth step into a grinding kettle for continuous grinding to enable the mixture to be more fully contacted, grinding for 60 minutes until the color of the whole mixture in the grinding kettle is completely changed into black to obtain a material A, washing the obtained material A with deionized water for multiple times, filtering, collecting water-insoluble solids, and putting the solids into a drying box for drying at the temperature of 60 ℃ for 1 hour, finely grinding the dried material A to enable the fineness to be 500 meshes, and controlling the fine grinding time to be 30 minutes to obtain semi-finished product powder;
step seven: purifying, dissolving the semi-finished product powder obtained in the sixth step in ethylene glycol, then placing the solution in a heating kettle, heating to 150 ℃, keeping the temperature for 30 minutes, naturally cooling the mixed solution to room temperature, then, placing the heated and cooled mixture solution in a centrifuge, controlling the speed of the centrifuge to 10000rpm, keeping the centrifugal speed for sufficient centrifugation for 5min, separating red solid, cleaning the separated red solid with absolute ethyl alcohol once, drying, cleaning with deionized water once, and then drying, then continuously washing with absolute ethyl alcohol, drying and washing with deionized water, drying, washing with absolute ethyl alcohol for the last time, drying in a drying oven after washing, and the drying temperature of a drying box for drying the red solid cleaned by the absolute ethyl alcohol is 80 ℃, and finally the purified cuprous oxide crystal is obtained.
Example 2:
the invention provides a preparation method of a semiconductor material for 5G signal transmission, which specifically comprises the following steps:
the method comprises the following steps: preparing raw materials, namely enough deionized water, toluene, N-dimethylformamide, sodium hydroxide solution, polyacrylonitrile, phthalocyanine, CuSO4 solution, FeSO4 solution, ethylene glycol and absolute ethyl alcohol;
step two: preparing a reaction device, selecting a proper agate grinding kettle, a proper reaction kettle, a proper drying box and a proper centrifugal machine according to the use specification, cleaning the required device and then drying for later use;
step three: preparing a solvent, namely mixing toluene and N-dimethylformamide according to a molar ratio of 1: 1, uniformly mixing and placing in a reaction kettle to be used as a reaction solvent in the subsequent steps;
step four: firstly, adding a sodium hydroxide solution into a solvent in a reaction kettle to make the reaction solvent alkaline, and then mixing polyacrylonitrile and phthalocyanine according to a ratio of 1: 1.2, then injecting a mixture solution of CuSO4 and FeSO4 mixed in proportion into a reaction solvent, sealing and reacting for 40 minutes, firstly generating a white precipitate, converting the white precipitate into reddish brown after a period of time, and finally converting the reddish green precipitate into a grayish green precipitate, and simultaneously oscillating a reaction kettle to uniformly disperse the precipitate separated from the reaction solution into the mixture, wherein the molar ratio of a sodium hydroxide solution to the mixture of polyacrylonitrile and phthalocyanine is 30: 1, wherein the molar ratio of the copper sulfate solution to the ferrous sulfate solution in the mixture is 1: 10;
step five: filtering, stripping the precipitate obtained by the reaction, washing with deionized water for multiple times, and filtering to obtain a mixture of copper hydroxide, ferrous hydroxide and ferric hydroxide;
step six: grinding, namely putting the mixture obtained in the fifth step into a grinding kettle for continuous grinding to enable the mixture to be more fully contacted, grinding for 70 minutes until the color of the whole mixture in the grinding kettle is completely changed into black to obtain a material A, washing the obtained material A with deionized water for multiple times, filtering, collecting water-insoluble solids, and putting the solids into a drying box for drying at the temperature of 70 ℃ for 2 hours, finely grinding the dried material A to enable the fineness to be 600 meshes, and controlling the fine grinding time to be 40 minutes to obtain semi-finished product powder;
step seven: purifying, dissolving the semi-finished product powder obtained in the sixth step in ethylene glycol, then placing the solution in a heating kettle, heating to 155 ℃, preserving the temperature for 32 minutes, naturally cooling the mixed solution to room temperature, then, placing the heated and cooled mixture solution in a centrifuge, controlling the speed of the centrifuge to be 11000rpm, keeping the centrifugal rotation speed for sufficient centrifugation for 6min, separating out red solid, cleaning the separated red solid, firstly cleaning the red solid with absolute ethyl alcohol once, drying the red solid, cleaning the red solid with deionized water once, and then drying the red solid again, then continuously washing with absolute ethyl alcohol, drying and washing with deionized water, drying, washing with absolute ethyl alcohol for the last time, drying in a drying oven after washing, and the drying temperature of a drying box for drying the red solid cleaned by the absolute ethyl alcohol is 82 ℃, and finally the purified cuprous oxide crystal is obtained.
Example 3:
the invention provides a preparation method of a semiconductor material for 5G signal transmission, which specifically comprises the following steps:
the method comprises the following steps: preparing raw materials, namely enough deionized water, toluene, N-dimethylformamide, sodium hydroxide solution, polyacrylonitrile, phthalocyanine, CuSO4 solution, FeSO4 solution, ethylene glycol and absolute ethyl alcohol;
step two: preparing a reaction device, selecting a proper agate grinding kettle, a proper reaction kettle, a proper drying box and a proper centrifugal machine according to the use specification, cleaning the required device and then drying for later use;
step three: preparing a solvent, namely mixing toluene and N-dimethylformamide according to a molar ratio of 1: 1, uniformly mixing and placing in a reaction kettle to be used as a reaction solvent in the subsequent steps;
step four: firstly, adding a sodium hydroxide solution into a solvent in a reaction kettle to make the reaction solvent alkaline, and then mixing polyacrylonitrile and phthalocyanine according to a ratio of 1: 1.2, then injecting a mixture solution of CuSO4 and FeSO4 which is mixed according to a certain proportion into a reaction solvent, sealing and reacting for 50 minutes, firstly generating a white precipitate, converting the white precipitate into reddish brown after a period of time, and finally converting the reddish green precipitate into a lime green precipitate, and simultaneously oscillating a reaction kettle to uniformly disperse the precipitate which is separated from the reaction solution into the mixture, wherein the molar ratio of a sodium hydroxide solution to the mixture of polyacrylonitrile and phthalocyanine is 40: 1, wherein the molar ratio of the copper sulfate solution to the ferrous sulfate solution in the mixture is 1: 10;
step five: filtering, stripping the precipitate obtained by the reaction, washing with deionized water for multiple times, and filtering to obtain a mixture of copper hydroxide, ferrous hydroxide and ferric hydroxide;
step six: grinding, namely putting the mixture obtained in the fifth step into a grinding kettle for continuous grinding to enable the mixture to be more fully contacted, grinding for 90 minutes until the color of the whole mixture in the grinding kettle is completely changed into black to obtain a material A, washing the obtained material A with deionized water for multiple times, filtering, collecting water-insoluble solids, and putting the solids into a drying box for drying at the temperature of 80 ℃ for 3 hours, finely grinding the dried material A to enable the fineness to be 700 meshes, and controlling the fine grinding time to be 50 minutes to obtain semi-finished product powder;
step seven: purifying, dissolving the semi-finished product powder obtained in the sixth step in ethylene glycol, then placing the solution in a heating kettle, heating to 160 ℃, keeping the temperature for 35 minutes, naturally cooling the mixed solution to room temperature, then, placing the heated and cooled mixture solution in a centrifuge, controlling the speed of the centrifuge to 12000rpm, keeping the centrifugal speed for sufficient centrifugation for 8min, separating out red solid, cleaning the separated red solid with absolute ethyl alcohol, drying, cleaning with deionized water, drying again, then continuously washing with absolute ethyl alcohol, drying and washing with deionized water, drying, washing with absolute ethyl alcohol for the last time, drying in a drying oven after washing, and the drying temperature of a drying box for drying the red solid cleaned by the absolute ethyl alcohol is 85 ℃, and finally the purified cuprous oxide crystal is obtained.
Example 4:
the invention provides a preparation method of a semiconductor material for 5G signal transmission, which specifically comprises the following steps:
the method comprises the following steps: preparing raw materials, namely enough deionized water, toluene, N-dimethylformamide, sodium hydroxide solution, polyacrylonitrile, phthalocyanine, CuSO4 solution, FeSO4 solution, ethylene glycol and absolute ethyl alcohol;
step two: preparing a reaction device, selecting a proper agate grinding kettle, a proper reaction kettle, a proper drying box and a proper centrifugal machine according to the use specification, cleaning the required device and then drying for later use;
step three: preparing a solvent, namely mixing toluene and N-dimethylformamide according to a molar ratio of 1: 1, uniformly mixing and placing in a reaction kettle to be used as a reaction solvent in the subsequent steps;
step four: firstly, adding a sodium hydroxide solution into a solvent in a reaction kettle to make the reaction solvent alkaline, and then mixing polyacrylonitrile and phthalocyanine according to a ratio of 1: 1.4, then injecting a mixture solution of CuSO4 and FeSO4 mixed according to a certain proportion into a reaction solvent, sealing and reacting for 55 minutes, firstly generating a white precipitate, converting the white precipitate into reddish brown after a period of time, and finally converting the reddish green precipitate into a lime green precipitate, and simultaneously oscillating a reaction kettle to uniformly disperse the precipitate separated from the reaction solution into the mixture, wherein the molar ratio of a sodium hydroxide solution to the mixture of polyacrylonitrile and phthalocyanine is 45: 1, wherein the molar ratio of the copper sulfate solution to the ferrous sulfate solution in the mixture is 1: 10;
step five: filtering, stripping the precipitate obtained by the reaction, washing with deionized water for multiple times, and filtering to obtain a mixture of copper hydroxide, ferrous hydroxide and ferric hydroxide;
step six: grinding, namely putting the mixture obtained in the fifth step into a grinding kettle for continuous grinding to enable the mixture to be more fully contacted, grinding for 110 minutes until the color of the whole mixture in the grinding kettle is completely changed into black to obtain a material A, washing the obtained material A with deionized water for multiple times, filtering, collecting water-insoluble solids, and putting the solids into a drying box for drying at the temperature of 90 ℃ for 4 hours, finely grinding the dried material A to enable the fineness to be 900 meshes, and controlling the fine grinding time to be 55 minutes to obtain semi-finished product powder;
step seven: purifying, dissolving the semi-finished product powder obtained in the sixth step in ethylene glycol, then placing the solution in a heating kettle, heating to 165 ℃, keeping the temperature for 38 minutes, naturally cooling the mixed solution to room temperature, then, placing the heated and cooled mixture solution in a centrifuge, controlling the speed of the centrifuge to 14000rpm, keeping the centrifuge rotating speed for sufficient centrifugation for 9min, separating red solid, cleaning the separated red solid, firstly cleaning with absolute ethyl alcohol once, drying, then cleaning with deionized water once, then drying again, then continuously washing with absolute ethyl alcohol, drying and washing with deionized water, drying, washing with absolute ethyl alcohol for the last time, drying in a drying oven after washing, and the drying temperature of a drying box for drying the red solid cleaned by the absolute ethyl alcohol is 88 ℃, and finally the purified cuprous oxide crystal is obtained.
Example 5:
the invention provides a preparation method of a semiconductor material for 5G signal transmission, which specifically comprises the following steps:
the method comprises the following steps: preparing raw materials, namely enough deionized water, toluene, N-dimethylformamide, sodium hydroxide solution, polyacrylonitrile, phthalocyanine, CuSO4 solution, FeSO4 solution, ethylene glycol and absolute ethyl alcohol;
step two: preparing a reaction device, selecting a proper agate grinding kettle, a proper reaction kettle, a proper drying box and a proper centrifugal machine according to the use specification, cleaning the required device and then drying for later use;
step three: preparing a solvent, namely mixing toluene and N-dimethylformamide according to a molar ratio of 1: 1, uniformly mixing and placing in a reaction kettle to be used as a reaction solvent in the subsequent steps;
step four: firstly, adding a sodium hydroxide solution into a solvent in a reaction kettle to make the reaction solvent alkaline, and then mixing polyacrylonitrile and phthalocyanine according to a ratio of 1: 1.5, then injecting a mixture solution of CuSO4 and FeSO4 mixed in proportion into a reaction solvent, sealing and reacting for 60 minutes, firstly generating a white precipitate, converting the white precipitate into reddish brown after a period of time, and finally converting the reddish green precipitate into a grayish green precipitate, and simultaneously oscillating a reaction kettle to uniformly disperse the precipitate separated from the reaction solution into the mixture, wherein the molar ratio of a sodium hydroxide solution to the mixture of polyacrylonitrile and phthalocyanine is 50: 1, wherein the molar ratio of the copper sulfate solution to the ferrous sulfate solution in the mixture is 1: 10;
step five: filtering, stripping the precipitate obtained by the reaction, washing with deionized water for multiple times, and filtering to obtain a mixture of copper hydroxide, ferrous hydroxide and ferric hydroxide;
step six: grinding, namely putting the mixture obtained in the fifth step into a grinding kettle for continuous grinding to enable the mixture to be more fully contacted, grinding for 120 minutes until the color of the whole mixture in the grinding kettle is completely changed into black to obtain a material A, washing the obtained material A with deionized water for multiple times, filtering, collecting water-insoluble solids, and putting the solids into a drying box for drying at the temperature of 100 ℃ for 5 hours, finely grinding the dried material A to enable the fineness to be 1000 meshes, and controlling the fine grinding time to be 60 minutes to obtain semi-finished product powder;
step seven: purifying, dissolving the semi-finished product powder obtained in the sixth step in ethylene glycol, then placing the solution in a heating kettle, heating to 170 ℃, keeping the temperature for 40 minutes, naturally cooling the mixed solution to room temperature, then, placing the heated and cooled mixture solution in a centrifuge, controlling the speed of the centrifuge to 15000rpm, keeping the centrifugal speed for sufficient centrifugation for 10min, separating out red solid, cleaning the separated red solid, firstly cleaning with absolute ethyl alcohol once, drying, then cleaning with deionized water once, then drying again, then continuously washing with absolute ethyl alcohol, drying and washing with deionized water, drying, washing with absolute ethyl alcohol for the last time, drying in a drying oven after washing, and the drying temperature of a drying box for drying the red solid cleaned by the absolute ethyl alcohol is 90 ℃, and finally the purified cuprous oxide crystal is obtained.
Five semiconductor materials can be obtained through the five groups of embodiments, and the five semiconductor materials are respectively subjected to performance tests, wherein the semiconductor material in embodiment 3 has the best performance and the highest value, and in the test process, the obtained parameters are as follows:
heat sensitivity | Crystal particle (mesh) | Material yield | |
Example 1 | High strength | 500 | 97.6% |
Example 2 | High strength | 600 | 97.8% |
Example 3 | High strength | 700 | 97.9% |
Example 4 | High strength | 900 | 98.1% |
Example 5 | High strength | 1000 | 97.8% |
From the above table, it can be seen that the raw material mixing ratio in example 4 is moderate, the invention adds the semiconductor organic matter in the existing preparation process of cuprous oxide, on the basis of not changing the mechanical property of the inorganic semiconductor, the property of the organic matter is increased, the added polyacrylonitrile and phthalocyanine make the cuprous oxide surface adsorb part of the substances with benzene ring property, and the hydroxyl group is added, so that the crystal of the mixture enhances the hydrophobicity on the mechanical property and the semiconductor property of the cuprous oxide, prolongs the service life of the semiconductor material, and the prepared semiconductor material has higher yield and smaller particle fineness of the semiconductor crystal in the using process, thereby being convenient for manufacturing elements with various specifications, the semiconductor prepared by the process has higher thermal sensitivity, the conductivity is increasingly enhanced along with the continuous rise of temperature, the process is simple, and the equipment requirement is low, the operability is strong, and the method has good social popularization and application.
And finally: the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that are within the spirit and principle of the present invention are intended to be included in the scope of the present invention.
Claims (6)
1. A preparation method of a semiconductor material for 5G signal transmission is characterized by comprising the following steps: the method specifically comprises the following steps:
the method comprises the following steps: preparing raw materials, namely enough deionized water, toluene, N-dimethylformamide, sodium hydroxide solution, polyacrylonitrile, phthalocyanine, CuSO4 solution, FeSO4 solution, ethylene glycol and absolute ethyl alcohol;
step two: preparing a reaction device, selecting a proper agate grinding kettle, a proper reaction kettle, a proper drying box and a proper centrifugal machine according to the use specification, cleaning the required device and then drying for later use;
step three: preparing a solvent, namely mixing toluene and N-dimethylformamide according to a molar ratio of 1: 1, uniformly mixing and placing in a reaction kettle to be used as a reaction solvent in the subsequent steps;
step four: firstly, adding a sodium hydroxide solution into a solvent in a reaction kettle to make the reaction solvent alkaline, and then mixing polyacrylonitrile and phthalocyanine according to a ratio of 1: 1-1: 1.5, then injecting the mixed solution of CuSO4 and FeSO4 into a reaction solvent, sealing and reacting for 30-60 minutes, and simultaneously shaking a reaction kettle to uniformly disperse the separated precipitates in the reaction solution into the mixture;
step five: filtering, stripping the precipitate obtained by the reaction, washing with deionized water for multiple times, and filtering to obtain a mixture of copper hydroxide, ferrous hydroxide and ferric hydroxide;
step six: grinding, namely placing the mixture obtained in the fifth step into a grinding kettle for continuous grinding to enable the mixture to be more fully contacted, grinding for 60-120 minutes until the color of all the mixtures in the grinding kettle is completely changed into black to obtain a material A, washing the obtained material A with deionized water for multiple times, filtering, collecting water-insoluble solids, placing the solids into a drying box for drying, and then further finely grinding to obtain semi-finished product powder;
step seven: and purifying, dissolving the semi-finished product powder obtained in the sixth step in ethylene glycol, then placing the solution in a heating kettle, heating to 150-.
2. The method for preparing a semiconductor material for 5G signal transmission according to claim 1, wherein: in the fourth step, the molar ratio of the sodium hydroxide solution to the mixture of polyacrylonitrile and phthalocyanine is 20: 1-50: 1, wherein the molar ratio of the copper sulfate solution to the ferrous sulfate solution in the mixture is 1: 10.
3. the method for preparing a semiconductor material for 5G signal transmission according to claim 1, wherein: the mixture in the fourth step firstly generates white precipitate, the white precipitate is converted into reddish brown after a period of time, and finally the white precipitate is converted into grey green precipitate.
4. The method for preparing a semiconductor material for 5G signal transmission according to claim 1, wherein: and in the sixth step, the temperature of the material A during drying is 60-100 ℃, the drying temperature is kept for 1-5 hours, the fineness of the semi-finished powder obtained by finely grinding the dried material A is 500-1000 meshes, and the fine grinding time is controlled to be 30-60 minutes.
5. The method for preparing a semiconductor material for 5G signal transmission according to claim 1, wherein: the cleaning mode of the red solid in the seventh step is as follows: firstly, washing with absolute ethyl alcohol, drying, washing with deionized water, drying again, then continuously washing with absolute ethyl alcohol, then drying again and washing with deionized water, drying, then washing with absolute ethyl alcohol, and finally washing with absolute ethyl alcohol.
6. The method for preparing a semiconductor material for 5G signal transmission according to claim 5, wherein: and the drying temperature of the drying box used for drying the red solid cleaned by the absolute ethyl alcohol in the seventh step is 80-90 ℃.
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