CN111517356B - Cu2O nanotube and method for producing the same - Google Patents
Cu2O nanotube and method for producing the same Download PDFInfo
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- 239000002071 nanotube Substances 0.000 title claims abstract description 96
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 title abstract description 16
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 title abstract description 16
- 238000004519 manufacturing process Methods 0.000 title description 2
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims abstract description 92
- 239000010949 copper Substances 0.000 claims abstract description 91
- 239000002243 precursor Substances 0.000 claims abstract description 60
- 238000006243 chemical reaction Methods 0.000 claims abstract description 59
- 238000003756 stirring Methods 0.000 claims abstract description 56
- 239000008367 deionised water Substances 0.000 claims abstract description 51
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 51
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000001035 drying Methods 0.000 claims abstract description 34
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000002360 preparation method Methods 0.000 claims abstract description 23
- 238000000137 annealing Methods 0.000 claims abstract description 21
- 238000001816 cooling Methods 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 17
- 238000005406 washing Methods 0.000 claims abstract description 17
- 229910052786 argon Inorganic materials 0.000 claims abstract description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052802 copper Inorganic materials 0.000 claims abstract description 5
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 33
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 6
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 6
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 5
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 13
- 229940112669 cuprous oxide Drugs 0.000 abstract description 12
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- 238000007146 photocatalysis Methods 0.000 abstract description 2
- 238000011049 filling Methods 0.000 description 13
- -1 step six Substances 0.000 description 13
- 238000009826 distribution Methods 0.000 description 7
- 239000002086 nanomaterial Substances 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910001431 copper ion Inorganic materials 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 125000004430 oxygen atom Chemical group O* 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- LBJNMUFDOHXDFG-UHFFFAOYSA-N copper;hydrate Chemical group O.[Cu].[Cu] LBJNMUFDOHXDFG-UHFFFAOYSA-N 0.000 description 1
- 230000000875 corresponding effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/72—Copper
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention relates to a cuprous oxide nanotube and a preparation method thereof, wherein the preparation method comprises the following steps: step one, preparing a certain amount of copper source to be dissolved in a certain amount of deionized water, and stirring for a certain time to form a solution A; step two, preparing a certain amount of pyrrole to be dissolved in a certain amount of deionized water, and stirring for a certain time to form a solution B; dropwise adding the solution B into the solution A, and stirring for a certain time to form a solution C; step four, putting the solution C into a reaction kettle, putting the reaction kettle into a constant-temperature drying box, reacting for several hours at a certain temperature, step five, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing the solution C with ethanol and deionized water for multiple times respectively, and drying to obtain Cu2Placing precursor powder into a tube furnace, annealing for several hours in an argon environment at a certain temperature to obtain Cu2And (3) O nanotubes. The invention has the advantages of simple process, low cost, high controllable degree, uniform product and excellent visible light photocatalysis performance.
Description
Technical Field
The invention relates to a photocatalytic nano material and the field of preparation technology and application thereof, in particular to a preparation method of a cuprous oxide nanotube.
Background
Cuprous oxide is an important p-type metal oxide semiconductor, the band gap energy of the cuprous oxide is 1.9ev-2.2ev, the absorption coefficient in a visible light region is high, and the energy conversion rate can reach 12% theoretically. It has unique cuprite structure, i.e. oxygen atom is body-centered cubic pile, copper atom is face-centered cubic pile, and copper atom occupies the regular tetrahedron gap formed by oxygen atoms. In recent years, due to unique optical, electrical and magnetic properties, no toxicity, abundant reserves, low preparation cost and low price, the application of the nano-silver/nano-silver composite material has gradually been researched and developed by people in various fields, and has proved to have good applications, such as potential applications in solar energy conversion, electronics, magnetic storage devices, biosensing and catalysis.
In recent years, Cu with controllable shape and size is prepared by different methods2O nanocrystals have become a focus of attention for researchers in various countries. At present, there are many references to Cu2The research results of optimizing the corresponding properties of O nano-materials by controlling the shape and size of the O nano-materials in the preparation process are reported, for example, researchers have used magnetron sputtering method, low-temperature solid phase method, hydrothermal method, vapor deposition method, solvothermal method, electrochemical deposition method and other methods to prepare and synthesize Cu2The shapes of O nanospheres, nanowires, cubes, hollow spheres, films, octahedrons, dodecahedrons and the like. Although the methods are used for preparing cuprous oxide, the cuprous oxide with stable performance and uniform particle size can be rarely obtained, and many preparation methods are complicated, such as a magnetron sputtering method, which is not only complicated, but also has high requirements on equipment; cuprous oxide prepared by a solid phase method often has no uniform appearance. Therefore, the nano Cu with controllable appearance and high purity is prepared by a simple method and low cost2O has important significance.
Disclosure of Invention
The invention aims to solve the primary technical problem of providing the cuprous oxide nanotube with simple process, low cost, short reaction period and uniformity and the preparation method thereof.
Cu2The preparation method of the O nanotube comprises the following steps:
step one, preparing a certain amount of copper source to be dissolved in a certain amount of deionized water, and stirring for a certain time to form a solution A;
step two, preparing a certain amount of pyrrole to be dissolved in a certain amount of deionized water, and stirring for a certain time to form a solution B;
dropwise adding the solution B into the solution A, and stirring for a certain time to form a solution C;
step four, putting the solution C into a reaction kettle, putting the reaction kettle into a constant-temperature drying box, reacting for several hours at a certain temperature,
taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing the reaction kettle with ethanol and deionized water for multiple times respectively, and drying to obtain Cu2An O nanotube precursor;
step six, adding Cu2Placing the O nanotube precursor powder in a tube furnace, annealing for several hours in an inert gas environment at a certain temperature to obtain Cu2And (3) O nanotubes.
Further, the copper source is one or a mixture of more of copper acetate, copper sulfate, copper nitrate or copper chloride.
Further, the stirring time in the step one is 10-60 min; the concentration of the solution A is 2-8 mmol/L.
Further, the stirring time in the step two is 10-60 min; the concentration of the solution B is 0.05-0.2 mol/L.
Further, the stirring time of the third step is 10-60 minutes.
Further, the reaction temperature of the step four is 120-200 ℃; the reaction time is 8-20 hours.
Further, the annealing temperature of the sixth step is 200-400 ℃; the annealing time is 60-300 minutes; the inert gas is nitrogen or argon.
The invention also comprises a second technical scheme, namely Cu2O nanotubes prepared by the above-mentioned preparation method, Cu2The diameter of the O nano tube is 50nm-1 μm.
The invention has the beneficial effects that: the preparation method of the cuprous oxide nanotube does not need expensive instruments and equipment, and realizes the preparation of the cuprous oxide nanotube by reasonable process control. The invention has the advantages of cheap and easily obtained raw materials, simple synthesis process, low cost, short reaction period and no pollution to the environment.The prepared Cu2The O nano tube has uniform size, adjustable size, good dispersion and large specific surface area, and can be applied to the fields of photocatalysis, gas sensitivity, adsorption and the like.
Drawings
Fig. 1 is an X-ray diffraction pattern of cuprous oxide nanotube material prepared in example 1.
Fig. 2 is a Transmission Electron Microscope (TEM) photograph of the cuprous oxide nanotube material prepared in example 1.
Detailed Description
The following examples are presented to further illustrate the methods of the present invention and are not intended to limit the invention to these examples.
Example 1:
cu2The preparation method of the O nanotube comprises the following steps: step one, dissolving 0.08g of copper acetate in 80ml of deionized water, and stirring for 30min to form a copper acetate solution; dissolving 0.14ml of pyrrole in 20ml of deionized water, and stirring for 30min to form a dilute pyrrole solution; dropwise adding the prepared dilute pyrrole solution into the copper acetate solution, and stirring for 30min to obtain a precursor solution; step four, filling the precursor solution into a reaction kettle, putting the reaction kettle into a constant-temperature drying box, reacting for 16 hours at 160 ℃, step five, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Cu2The precursor of the O nano tube, step six, Cu2Placing the O nanotube precursor powder in a tube furnace, and annealing at 300 ℃ for 180min under an argon environment to obtain Cu2And (3) O nanotubes.
FIGS. 1 and 2 are Cu, respectively, produced in this example2XRD and TEM images of O nanotubes, from which the Cu produced can be seen2Better dispersity of O nanotube and Cu2The distribution of O nano-tubes is relatively uniform, Cu2The diameter of the O nanotubes was 1 μm. From the XRD pattern, the prepared Cu can be seen2The O nanotube has good crystallinity, is Cu2And (4) O crystals.
Example 2:
this example differs from example 1 in that the amount of copper acetate in step 1 was changed to 0.12g,the rest is the same as example 1, specifically as follows: step one, 012g of copper acetate is dissolved in 80ml of deionized water and stirred for 30min to form a copper acetate solution; dissolving 0.14ml of pyrrole in 20ml of deionized water, and stirring for 30min to form a dilute pyrrole solution; dropwise adding the prepared dilute pyrrole solution into the copper acetate solution, and stirring for 30min to obtain a precursor solution; step four, filling the precursor solution into a reaction kettle, putting the reaction kettle into a constant-temperature drying box, reacting for 16 hours at 160 ℃, step five, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Cu2The precursor of the O nano tube, step six, Cu2Placing the O nanotube precursor powder in a tube furnace, and annealing at 300 ℃ for 180min under an argon environment to obtain Cu2And (3) O nanotubes. Obtained Cu2Better dispersity of O nanotube and Cu2The distribution of O nano-tubes is relatively uniform, Cu2The diameter of the O nanotubes was 0.8. mu.m.
Example 3:
this example differs from example 1 in that the amount of pyrrole in step two was changed to 0.21ml, and the other steps are the same as in example 1, specifically as follows: step one, dissolving 0.08g of copper acetate in 80ml of deionized water, and stirring for 30min to form a copper acetate solution; dissolving 0.21ml of pyrrole in 20ml of deionized water, and stirring for 30min to form a dilute pyrrole solution; dropwise adding the prepared dilute pyrrole solution into the copper acetate solution, and stirring for 30min to obtain a precursor solution; step four, filling the precursor solution into a reaction kettle, putting the reaction kettle into a constant-temperature drying box, reacting for 16 hours at 160 ℃, step five, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Cu2The precursor of the O nano tube, step six, Cu2Placing the O nanotube precursor powder in a tube furnace, and annealing at 300 ℃ for 180min under an argon environment to obtain Cu2And (3) O nanotubes. Cu2Better dispersity of O nanotube and Cu2The distribution of O nano-tubes is relatively uniform, Cu2The diameter of the O nanotubes was 0.9. mu.m.
Example 4:
this embodiment and examples1, except that the reaction temperature was changed to 140 ℃ in the fourth step, the same as in example 1 was repeated, specifically as follows: step one, dissolving 0.08g of copper acetate in 80ml of deionized water, and stirring for 30min to form a copper acetate solution; dissolving 0.14ml of pyrrole in 20ml of deionized water, and stirring for 30min to form a dilute pyrrole solution; dropwise adding the prepared dilute pyrrole solution into the copper acetate solution, and stirring for 30min to obtain a precursor solution; step four, filling the precursor solution into a reaction kettle, putting the reaction kettle into a constant-temperature drying box, reacting for 16 hours at the temperature of 140 ℃, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Cu2The precursor of the O nano tube, step six, Cu2Placing the O nanotube precursor powder in a tube furnace, and annealing at 300 ℃ for 180min under an argon environment to obtain Cu2And (3) O nanotubes. Cu2Better dispersity of O nanotube and Cu2The distribution of O nano-tubes is relatively uniform, Cu2The diameter of the O nanotubes was 0.5. mu.m.
Example 5:
this example differs from example 1 in that the reaction time was changed to 12 hours in step four, and otherwise is the same as example 1, specifically as follows: step one, dissolving 0.08g of copper acetate in 80ml of deionized water, and stirring for 30min to form a copper acetate solution; dissolving 0.14ml of pyrrole in 20ml of deionized water, and stirring for 30min to form a dilute pyrrole solution; dropwise adding the prepared dilute pyrrole solution into the copper acetate solution, and stirring for 30min to obtain a precursor solution; step four, filling the precursor solution into a reaction kettle, putting the reaction kettle into a constant-temperature drying box, reacting for 12 hours at 160 ℃, step five, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Cu2The precursor of the O nano tube, step six, Cu2Placing the O nanotube precursor powder in a tube furnace, and annealing at 300 ℃ for 180min under an argon environment to obtain Cu2And (3) O nanotubes. Cu2Better dispersity of O nanotube and Cu2The distribution of O nano-tubes is relatively uniform, Cu2The diameter of the O nanotubes was 0.9. mu.m.
Example 6:
the difference between this example and example 1 is that the annealing temperature is changed to 350 ℃ in step six, and the other steps are the same as those of example 1, specifically as follows: step one, dissolving 0.08g of copper acetate in 80ml of deionized water, and stirring for 30min to form a copper acetate solution; dissolving 0.14ml of pyrrole in 20ml of deionized water, and stirring for 30min to form a dilute pyrrole solution; dropwise adding the prepared dilute pyrrole solution into the copper acetate solution, and stirring for 30min to obtain a precursor solution; step four, filling the precursor solution into a reaction kettle, putting the reaction kettle into a constant-temperature drying box, reacting for 16 hours at 160 ℃, step five, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Cu2The precursor of the O nano tube, step six, Cu2Placing the O nanotube precursor powder in a tube furnace, and annealing at 350 ℃ for 180min under an argon environment to obtain Cu2And (3) O nanotubes. Cu2Better dispersity of O nanotube and Cu2The distribution of O nano-tubes is relatively uniform, Cu2The diameter of the O nanotubes was 50 nm.
Example 7:
the difference between this example and example 1 is that the annealing time is changed to 120min in step six, and the rest is the same as example 1, specifically as follows: step one, dissolving 0.08g of copper acetate in 80ml of deionized water, and stirring for 30min to form a copper acetate solution; dissolving 0.14ml of pyrrole in 20ml of deionized water, and stirring for 30min to form a dilute pyrrole solution; dropwise adding the prepared dilute pyrrole solution into the copper acetate solution, and stirring for 30min to obtain a precursor solution; step four, filling the precursor solution into a reaction kettle, putting the reaction kettle into a constant-temperature drying box, reacting for 16 hours at 160 ℃, step five, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Cu2The precursor of the O nano tube, step six, Cu2Placing the O nanotube precursor powder in a tube furnace, and annealing at 300 ℃ for 120min in an argon environment to obtain Cu2And (3) O nanotubes. Cu2Better dispersity of O nanotube and Cu2The distribution of O nano-tubes is relatively uniform, Cu2The diameter of the O nanotube is 100 nm.
Example 8:
this example is different from example 1 in that the stirring time is changed to 60min in the first to third steps, and the other steps are the same as example 1, specifically as follows: step one, dissolving 0.08g of copper acetate in 80ml of deionized water, and stirring for 60min to form a copper acetate solution; dissolving 0.14ml of pyrrole in 20ml of deionized water, and stirring for 60min to form a dilute pyrrole solution; dropwise adding the prepared dilute pyrrole solution into the copper acetate solution, and stirring for 60min to obtain a precursor solution; step four, filling the precursor solution into a reaction kettle, putting the reaction kettle into a constant-temperature drying box, reacting for 16 hours at 160 ℃, step five, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Cu2The precursor of the O nano tube, step six, Cu2Placing the O nanotube precursor powder in a tube furnace, and annealing at 300 ℃ for 180min under an argon environment to obtain Cu2And (3) O nanotubes.
Example 9:
this example differs from example 1 in that the reaction time was changed to 8 hours in step four, and otherwise is the same as example 1, specifically as follows: step one, dissolving 0.08g of copper acetate in 80ml of deionized water, and stirring for 30min to form a copper acetate solution; dissolving 0.14ml of pyrrole in 20ml of deionized water, and stirring for 30min to form a dilute pyrrole solution; dropwise adding the prepared dilute pyrrole solution into the copper acetate solution, and stirring for 30min to obtain a precursor solution; step four, filling the precursor solution into a reaction kettle, putting the reaction kettle into a constant-temperature drying box, reacting for 8 hours at 160 ℃, step five, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Cu2The precursor of the O nano tube, step six, Cu2Placing the O nanotube precursor powder in a tube furnace, and annealing at 300 ℃ for 180min under an argon environment to obtain Cu2And (3) O nanotubes.
Example 10:
this example differs from example 1 in that argon gas is changed to nitrogen gas in step six, and the other steps are the same as in example 1, specifically as follows: in the first step of the method,dissolving 0.08g of copper acetate in 80ml of deionized water, and stirring for 30min to form a copper acetate solution; dissolving 0.14ml of pyrrole in 20ml of deionized water, and stirring for 30min to form a dilute pyrrole solution; dropwise adding the prepared dilute pyrrole solution into the copper acetate solution, and stirring for 30min to obtain a precursor solution; step four, filling the precursor solution into a reaction kettle, putting the reaction kettle into a constant-temperature drying box, reacting for 16 hours at 160 ℃, step five, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Cu2The precursor of the O nano tube, step six, Cu2Placing the O nanotube precursor powder in a tube furnace, and annealing at 300 ℃ for 180min in a nitrogen environment to obtain Cu2And (3) O nanotubes.
Example 11:
cu2The preparation method of the O nanotube comprises the following steps: step one, dissolving 0.1024g of copper sulfate in 80ml of deionized water, and stirring for 30min to form a copper sulfate solution; dissolving 0.14ml of pyrrole in 20ml of deionized water, and stirring for 30min to form a dilute pyrrole solution; dropwise adding the prepared dilute pyrrole solution into the copper sulfate solution, and stirring for 30min to obtain a precursor solution; step four, filling the precursor solution into a reaction kettle, putting the reaction kettle into a constant-temperature drying box, reacting for 16 hours at 160 ℃, step five, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Cu2The precursor of the O nano tube, step six, Cu2Placing the O nanotube precursor powder in a tube furnace, and annealing at 300 ℃ for 180min in a nitrogen environment to obtain Cu2And (3) O nanotubes.
Example 12:
cu2The preparation method of the O nanotube comprises the following steps: step one, 0.0602g of copper nitrate is dissolved in 80ml of deionized water and stirred for 30min to form 4mmol/L of copper nitrate solution; dissolving 0.14ml of pyrrole in 20ml of deionized water, and stirring for 30min to form a dilute pyrrole solution; dropwise adding the prepared dilute pyrrole solution into the copper nitrate solution, and stirring for 30min to obtain a precursor solution; step four, the precursor is processedPutting the solution into a reaction kettle, putting the reaction kettle into a constant-temperature drying box, reacting for 16 hours at 160 ℃, taking the reaction kettle out, naturally cooling to room temperature, centrifuging, washing the solution with ethanol and deionized water for multiple times respectively, and drying to obtain Cu2The precursor of the O nano tube, step six, Cu2Placing the O nanotube precursor powder in a tube furnace, and annealing at 300 ℃ for 180min in a nitrogen environment to obtain Cu2And (3) O nanotubes.
Example 13:
cu2The preparation method of the O nanotube comprises the following steps: step one, dissolving 0.0215g of copper chloride in 80ml of deionized water, and stirring for 30min to form a 2mmol/L copper chloride solution; dissolving 0.14ml of pyrrole in 20ml of deionized water, and stirring for 30min to form a dilute pyrrole solution; dropwise adding the prepared dilute pyrrole solution into the copper chloride solution, and stirring for 30min to obtain a precursor solution; step four, filling the precursor solution into a reaction kettle, putting the reaction kettle into a constant-temperature drying box, reacting for 16 hours at 160 ℃, step five, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Cu2The precursor of the O nano tube, step six, Cu2Placing the O nanotube precursor powder in a tube furnace, and annealing at 300 ℃ for 180min in a nitrogen environment to obtain Cu2And (3) O nanotubes.
Example 14:
cu2The preparation method of the O nanotube comprises the following steps: step one, dissolving 0.0215g of copper chloride and 0.0602g of copper nitrate in 80ml of deionized water, and stirring for 30min to form a 6mmol/L copper ion solution; dissolving 0.14ml of pyrrole in 20ml of deionized water, and stirring for 30min to form a dilute pyrrole solution; dropwise adding the prepared dilute pyrrole solution into the copper ion solution, and stirring for 30min to obtain a precursor solution; step four, filling the precursor solution into a reaction kettle, putting the reaction kettle into a constant-temperature drying box, reacting for 16 hours at 160 ℃, step five, taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing ethanol and deionized water for multiple times respectively, and drying to obtain Cu2The precursor of the O nano tube, step six, Cu2O nanotube precursorPutting the powder into a tube furnace, and annealing for 180min at 300 ℃ in a nitrogen environment to obtain Cu2And (3) O nanotubes.
Claims (6)
1. Cu2The preparation method of the O nanotube is characterized by comprising the following steps of:
step one, preparing a certain amount of copper source to be dissolved in certain deionized water, and stirring for a certain time to form a solution A, wherein the concentration of the solution A is 2-8 mmol/L;
step two, preparing a certain amount of pyrrole to be dissolved in a certain amount of deionized water, and stirring for a certain time to form a solution B, wherein the concentration of the solution B is 0.05-0.2 mol/L;
dropwise adding the solution B into the solution A, and stirring for a certain time to form a solution C;
step four, putting the solution C into a reaction kettle, putting the reaction kettle into a constant-temperature drying box, and reacting for 8-20 hours at the temperature of 120-;
taking out the reaction kettle, naturally cooling to room temperature, centrifuging, washing the reaction kettle with ethanol and deionized water for multiple times respectively, and drying to obtain Cu2An O nanotube precursor;
step six, adding Cu2Placing the O nanotube precursor powder in a tube furnace, annealing for 60-300 minutes in an inert gas environment at the temperature of 200-400 ℃ to obtain Cu2And (3) O nanotubes.
2. Cu according to claim 12The preparation method of the O nanotube is characterized by comprising the following steps: the copper source in the first step is one or a mixture of more of copper acetate, copper sulfate, copper nitrate or copper chloride.
3. Cu according to claim 12The preparation method of the O nanotube is characterized by comprising the following steps: the stirring time of the first step is 10-60 minutes.
4. Cu according to claim 12The preparation method of the O nanotube is characterized by comprising the following steps: the stirring time of the second step is 10-60 minutes.
5. Cu according to claim 12The preparation method of the O nanotube is characterized by comprising the following steps: the stirring time of the third step is 10-60 minutes.
6. Cu according to claim 12The preparation method of the O nanotube is characterized by comprising the following steps: the inert gas is nitrogen or argon.
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