CN112897567A - Preparation method of copper oxide with nanometer flower-like structure - Google Patents
Preparation method of copper oxide with nanometer flower-like structure Download PDFInfo
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- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 title claims abstract description 175
- 239000005751 Copper oxide Substances 0.000 title claims abstract description 175
- 229910000431 copper oxide Inorganic materials 0.000 title claims abstract description 175
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 132
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 86
- 239000010949 copper Substances 0.000 claims abstract description 54
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 53
- 229910052802 copper Inorganic materials 0.000 claims abstract description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 32
- 239000006260 foam Substances 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 17
- 239000011259 mixed solution Substances 0.000 claims abstract description 17
- 238000005406 washing Methods 0.000 claims abstract description 17
- 239000000243 solution Substances 0.000 claims abstract description 6
- 238000007146 photocatalysis Methods 0.000 claims abstract description 4
- 230000001699 photocatalysis Effects 0.000 claims abstract description 4
- 239000002057 nanoflower Substances 0.000 claims description 17
- 230000007613 environmental effect Effects 0.000 claims description 7
- 230000005693 optoelectronics Effects 0.000 claims description 2
- 230000001954 sterilising effect Effects 0.000 claims description 2
- 238000004659 sterilization and disinfection Methods 0.000 claims description 2
- 239000003344 environmental pollutant Substances 0.000 abstract description 13
- 231100000719 pollutant Toxicity 0.000 abstract description 10
- 230000000593 degrading effect Effects 0.000 abstract 1
- 238000005265 energy consumption Methods 0.000 abstract 1
- 239000008204 material by function Substances 0.000 abstract 1
- 238000004458 analytical method Methods 0.000 description 14
- 230000000877 morphologic effect Effects 0.000 description 14
- 238000001878 scanning electron micrograph Methods 0.000 description 14
- 238000002791 soaking Methods 0.000 description 14
- 230000003068 static effect Effects 0.000 description 14
- 239000000463 material Substances 0.000 description 10
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 239000002135 nanosheet Substances 0.000 description 6
- 239000002070 nanowire Substances 0.000 description 6
- 229940051841 polyoxyethylene ether Drugs 0.000 description 6
- 229920000056 polyoxyethylene ether Polymers 0.000 description 6
- 239000000356 contaminant Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000002073 nanorod Substances 0.000 description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- JJLJMEJHUUYSSY-UHFFFAOYSA-L Copper hydroxide Chemical compound [OH-].[OH-].[Cu+2] JJLJMEJHUUYSSY-UHFFFAOYSA-L 0.000 description 4
- 239000005750 Copper hydroxide Substances 0.000 description 4
- 229910001956 copper hydroxide Inorganic materials 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 230000001590 oxidative effect Effects 0.000 description 4
- 239000002585 base Substances 0.000 description 3
- 230000031700 light absorption Effects 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910016523 CuKa Inorganic materials 0.000 description 2
- 241000446313 Lamella Species 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 231100000956 nontoxicity Toxicity 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 235000005881 Calendula officinalis Nutrition 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 240000000785 Tagetes erecta Species 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000000970 chrono-amperometry Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- RDYMFSUJUZBWLH-UHFFFAOYSA-N endosulfan Chemical compound C12COS(=O)OCC2C2(Cl)C(Cl)=C(Cl)C1(Cl)C2(Cl)Cl RDYMFSUJUZBWLH-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 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
- 239000002120 nanofilm Substances 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- 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
Abstract
The invention discloses a preparation method of copper oxide with a nanometer flower-like structure, belonging to the technical field of functional materials. The preparation method of the nanometer flower-shaped copper oxide comprises the steps of adding the copper mesh/foam copper into a mixed solution of sodium hydroxide and ammonium persulfate, reacting the reaction solution at 20-50 ℃ for 10-60min, taking out, washing and drying to obtain the copper oxide with the nanometer flower-shaped structure. The nanometer flower-shaped copper oxide prepared by the method has the diameter of about 1-10 mu m, high purity, super-hydrophilic property and water contact angle of 0 degrees, and the preparation method disclosed by the invention is a one-step method, is simple and convenient, consumes short time, is low in energy consumption and is easy to scale. The nano flower-shaped copper oxide prepared by the method has excellent photoresponse characteristic and the function of degrading pollutants by photocatalysis.
Description
Technical Field
The invention relates to a preparation method of copper oxide with a nanometer flower-shaped structure, belonging to the technical field of nanometer materials.
Background
Copper oxide is a black oxide of copper, has excellent thermal stability and chemical stability at high temperature, has a band gap of about 1.2eV, has a high light absorption coefficient in an ultraviolet-visible-near infrared band, can convert absorbed light into heat through non-radiative recombination of electron-hole pairs generated by light absorption, and is an important sunlight photo-thermal absorption layer, photovoltaic, photoelectrocatalysis and light detection material; as an important p-type semiconductor, copper oxide has larger exciton confinement energy and has great application prospect in batteries, super capacitors, solar cells and optoelectronic devices. Besides, the copper oxide also shows excellent catalytic performance and has important application in the fields of photocatalysis, sterilization, environmental treatment and biochemical sensors; meanwhile, the copper oxide also has the obvious advantages of no toxicity, environmental protection, recyclability, low cost and the like, and is an important structural function (hydrophilic and hydrophobic) material, so that the copper oxide is more widely applied in various fields.
At present, many researchers have actively explored and synthesized nanoscale copper oxide structural materials with different morphologies, such as nanowires, nanoflowers, nanosheets, nanorods, nanofilms and the like. Among them, the flower-like copper oxide has a relatively high specific surface area, multiple active sites, low bulk density, etc., and thus has a wide application in environmental catalysis, and thus, the synthesis of the flower-like copper oxide is receiving much attention. The preparation method is also various, such as hydrothermal synthesis method, CVD method, electroplating method, film growth method, etc. However, these methods are cumbersome to operate and require a long treatment time. Xu et al reported a method for preparing a hydrophilic copper oxide nanowire lattice structure by a two-step process of alkaline oxidation and heating (ACS Sustainable Chemistry & Engineering 7(2019) 5476-5485). Researchers also grow thread-shaped copper hydroxide on the surface of the foam copper by in-situ chemical reaction for 5 hours at room temperature, and then calcinate the copper hydroxide at 180 ℃ for 2 hours, so that the copper hydroxide on the surface of the foam copper is dehydrated to form petal-shaped copper oxide (Lepolitong, Wangchengtongning. preparation of multi-scale Ag/Cu composite photothermal material and application in seawater desalination [ J ] inorganic chemistry report 2020,36(08):1457 and 1464 ]. The flower-like copper oxide can be obtained by the method, but the copper foam is firstly etched to generate copper hydroxide and then is oxidized at high temperature to generate copper oxide, so that the preparation is complicated and the time is long.
Disclosure of Invention
In order to solve the problems of complicated steps, long time consumption and the like of preparing the nanometer flower-shaped copper oxide, the invention provides a simple and convenient preparation method of the nanometer flower-shaped structure copper oxide.
The nanometer flower-shaped copper oxide prepared by the invention is prepared by co-oxidizing sodium hydroxide and ammonium persulfate. According to the invention, the shape of the copper oxide is regulated and controlled by regulating and controlling the concentrations of different sodium hydroxide and ammonium persulfate, and finally, a method for simply and rapidly preparing the nanometer flower-shaped copper oxide is explored. The method can obtain the copper oxide by one step, and the prepared nano flower-shaped copper oxide is observed by a scanning electron microscope, so that the nano flower-shaped copper oxide is uniformly distributed, has excellent super-hydrophilic performance, has a contact angle with water of about 0 degree, and also provides a method for preparing the nano flower-shaped copper oxide by the one-step strong base oxidation method, which has the advantages of simple process, short time consumption and easiness in scale production.
Specifically, the invention provides a preparation method of copper oxide with a nanometer flower-like structure, which comprises the following steps: adding the copper mesh/foam copper into a mixed solution of sodium hydroxide and ammonium persulfate, reacting the reaction solution at 20-50 ℃ for 10-60min, taking out, washing with water, and drying to obtain the copper oxide with the nanometer flower-shaped structure.
In one embodiment of the invention, the concentration of sodium hydroxide is 2.5-5.0 mol/L.
In one embodiment of the invention, the concentration of the ammonium persulfate is 0.2-0.4 mol/L.
In one embodiment of the invention, the area of the copper mesh/copper foam is 2cm2-16cm2。
The copper oxide with the nanometer flower-like structure prepared by the novel method is a three-dimensional structure material consisting of nanosheets/wires and micrometer/nanometer flowers with the uniform size of 1-10 mu m, and the special flower-like nanometer structure can be observed through a scanning electron microscope.
The copper oxide with a nano flower-like structure prepared by the novel method developed by the invention can obtain diffraction peaks at 32.4 degrees, 35.4 degrees, 38.7 degrees, 43.3 degrees, 48.7 degrees, 50.43 degrees, 58.3 degrees, 61.5 degrees, 65.7 degrees, 68.0 degrees and 74.1 degrees by an X-ray diffractometer, and the diffraction peaks respectively correspond to (110), (002), (111), (202), (200), (202), (113), (022), (220) and (220) crystal planes. These peaks align well with the face centered cubic phase of copper oxide (PDF card JCPDS No.45-0937), further confirming the high purity of the synthesized copper oxide.
The copper oxide with the nano flower-like structure prepared by the method disclosed by the invention shows an excellent hydrophilic effect, the contact angle of the copper oxide with water is approximately equal to 0 degree, and the copper oxide can be developed and utilized as a base material of a structural functional material.
The invention has the beneficial effects that:
(1) the invention develops a one-step strong alkali oxidation method for preparing the copper oxide with the nanometer flower shape, and the method has the advantages of simple process, easy operation, short time consumption and capability of expanding to large-scale preparation.
(2) The nano flower-shaped copper oxide prepared by the method has good hydrophilic performance, the water contact angle of the nano flower-shaped copper oxide is higher than or equal to 0 degree, and the nano flower-shaped copper oxide can be used as a base material of a structural functional material.
(3) The nano flower-shaped copper oxide prepared by the method disclosed by the invention has a multi-scale three-dimensional structure (comprising a millimeter-scale hole structure and a micro-nano-scale linear and sheet structure) on the surface, can effectively capture incident visible light, and has a flower-shaped sphere-like structure formed by tightly embedding layered nano sheets, so that light capture sites are greatly increased, the absorption capacity of the nano flower-shaped copper oxide on visible light is remarkably enhanced, and the nano flower-shaped copper oxide can be applied to photocatalysis.
(4) The nano flower-shaped copper oxide prepared by the method has a pore structure and a layered petal-shaped structure on the surface, so that the specific surface area of the copper oxide is increased, the adsorption capacity of the copper oxide on pollutants is obviously enhanced, and the method can be applied to the aspect of environmental pollutant treatment.
Drawings
FIG. 1 is a scanning electron micrograph of copper oxide oxidized in 2.5mol/l sodium hydroxide and 0.2mol/l ammonium persulfate for 10 minutes.
FIG. 2 is a scanning electron micrograph of copper oxide oxidized in 2.5mol/l sodium hydroxide and 0.2mol/l ammonium persulfate for 20 minutes.
FIG. 3 is a scanning electron micrograph of copper oxide oxidized in 2.5mol/l sodium hydroxide and 0.2mol/l ammonium persulfate for 30 minutes.
FIG. 4 is a scanning electron micrograph of copper oxide oxidized in 2.5mol/l sodium hydroxide and 0.2mol/l ammonium persulfate for 40 minutes.
FIG. 5 is a scanning electron micrograph of copper oxide oxidized in 5.0mol/l sodium hydroxide and 0.4mol/l ammonium persulfate for 10 minutes.
FIG. 6 is a scanning electron micrograph of copper oxide oxidized in 5.0mol/l sodium hydroxide and 0.4mol/l ammonium persulfate for 20 minutes.
FIG. 7 is a scanning electron micrograph of copper oxide oxidized in 5.0mol/l sodium hydroxide and 0.4mol/l ammonium persulfate for 30 minutes.
FIG. 8 is a contact angle image of copper oxide after copper foam has been oxidized in 5.0mol/l sodium hydroxide and 0.4mol/l ammonium persulfate for 30 minutes.
FIG. 9 is an X-ray diffraction pattern of copper oxide from copper foam oxidized for 30 minutes in 5.0mol/l sodium hydroxide and 0.4mol/l ammonium persulfate.
FIG. 10 is a photo current response curve of nano flower-like copper oxide prepared by oxidizing copper foam in 5.0mol/l sodium hydroxide and 0.4mol/l ammonium persulfate for 30 minutes.
FIG. 11 is a graph showing the effect of photocatalytic degradation of octylphenol polyoxyethylene ether by nano flower-like copper oxide, prepared by oxidizing copper foam in 5.0mol/l sodium hydroxide and 0.4mol/l ammonium persulfate for 30 minutes.
FIG. 12 is a scanning electron micrograph of copper oxide oxidized from copper foam in 5.0mol/l sodium hydroxide and 0.4mol/l ammonium persulfate for 40 minutes.
FIG. 13 is a scanning electron micrograph of copper oxide where the copper mesh was oxidized in 2.5mol/l sodium hydroxide and 0.2mol/l ammonium persulfate for 10 minutes.
FIG. 14 is a scanning electron micrograph of copper oxide from a copper mesh oxidized in 2.5mol/l sodium hydroxide and 0.2mol/l ammonium persulfate for 20 minutes.
FIG. 15 is a scanning electron micrograph of copper oxide where the copper mesh was oxidized in 2.5mol/l sodium hydroxide and 0.2mol/l ammonium persulfate for 30 minutes.
FIG. 16 is a scanning electron micrograph of copper oxide where the copper mesh was oxidized in 5.0mol/l sodium hydroxide and 0.4mol/l ammonium persulfate for 10 minutes.
FIG. 17 is a scanning electron micrograph of copper oxide from a copper mesh oxidized for 20 minutes in 5.0mol/l sodium hydroxide and 0.4mol/l ammonium persulfate.
FIG. 18 is a scanning electron micrograph of copper oxide where the copper mesh was oxidized in 5.0mol/l sodium hydroxide and 0.4mol/l ammonium persulfate for 30 minutes.
FIG. 19 is a contact angle image of copper oxide with a copper mesh oxidized for 30 minutes in 5.0mol/l sodium hydroxide and 0.4mol/l ammonium persulfate.
FIG. 20 is an X-ray diffraction pattern of copper oxide from a copper mesh oxidized for 30 minutes in 5.0mol/l sodium hydroxide and 0.4mol/l ammonium persulfate.
FIG. 21 is a photo current response curve of nano flower-like copper oxide prepared by oxidizing a copper mesh in 5.0mol/l sodium hydroxide and 0.4mol/l ammonium persulfate for 30 minutes.
FIG. 22 is a graph showing the effect of photocatalytic degradation of octylphenol polyoxyethylene ether of nano flower-like copper oxide prepared by oxidizing a copper mesh in 5.0mol/l sodium hydroxide and 0.4mol/l ammonium persulfate for 30 minutes.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of better illustrating the invention and is not intended to limit the invention thereto.
The test method comprises the following steps:
1. and (4) SEM test: the morphology of the synthesized copper oxide at different sodium hydroxide and ammonium persulfate concentrations was observed by scanning electron microscopy (hitachi su 1510).
2. And (3) testing the hydrophilic performance: the water contact angle was obtained by measuring 5. mu.L of water at five positions of each sample with a contact angle measuring instrument (Powereach JC2000D1) at room temperature, and calculating the average value.
3. And (3) crystal form testing: the crystalline form of the synthesized copper oxide was analyzed by X-ray diffractometry (bruke D2 PHASER) at room temperature.
4. Photocurrent response test: the photocurrent response of the synthesized copper oxide was analyzed at room temperature using a Huachen electrochemical workstation (CHI 660B), with the sample directly as the working electrode, platinum as the counter electrode, and silver/silver chloride as the reference electrode. The photoelectric characteristics were measured by chronoamperometry under a xenon lamp light source.
5. And (3) pollutant concentration test: the concentration of the contaminant in the reaction solution was quantitatively measured by using a high performance liquid chromatograph (Waters e 2695).
Example 1
A preparation method of copper oxide with a nanometer flower-like structure comprises the following steps:
soaking the foamy copper with the area size of 2cm multiplied by 2cm in 20ml of mixed solution containing 2.5mol/l of sodium hydroxide and 0.2mol/l of ammonium persulfate, reacting for 10 minutes, repeatedly washing with water after the reaction is finished, and drying in an oven at 60 ℃ to obtain the copper oxide.
FIG. 1 is a morphological analysis of copper oxide as in example 1 by a scanning electron microscope of Japanese Hitachi su 1510. As shown in FIG. 1, the copper oxide nanowires are formed, and have a length of 1 μm to 5 μm and a diameter of about 100 nm to 500 nm.
To the surface of the copper oxide prepared in example 1, 5. mu.L of a water droplet was dropped by a contact angle measuring instrument, and the static water contact angle thereof was 0 °.
Example 2
A preparation method of copper oxide with a nanometer flower-like structure comprises the following steps:
soaking the foamy copper with the area size of 2cm multiplied by 2cm in 20ml of mixed solution containing 2.5mol/l of sodium hydroxide and 0.2mol/l of ammonium persulfate, reacting for 20 minutes, repeatedly washing with water after the reaction is finished, and drying in an oven at 60 ℃ to obtain the copper oxide.
FIG. 2 is a morphological analysis of copper oxide as in example 2 by a scanning electron microscope of Japanese Hitachi su 1510. As shown in FIG. 2, a nanowire-nanosheet copper oxide is formed, wherein the nanowire has a length of 1-5 μm, a diameter of about 100-500 nm, and a diameter of 1-3 μm.
To the surface of the copper oxide prepared in example 2, 5. mu.L of a water droplet was dropped by a contact angle measuring instrument, and the static water contact angle thereof was 0 °.
Example 3
A preparation method of copper oxide with a nanometer flower-like structure comprises the following steps:
soaking the foamy copper with the area size of 2cm multiplied by 2cm in 20ml of mixed solution containing 2.5mol/l of sodium hydroxide and 0.2mol/l of ammonium persulfate, reacting for 30 minutes, repeatedly washing with water after the reaction is finished, and drying in an oven at 60 ℃ to obtain the copper oxide.
FIG. 3 is a morphological analysis of copper oxide as in example 3 by a scanning electron microscope of Japanese Hitachi su 1510. As shown in FIG. 3, a nano flower-like copper oxide is formed, wherein the nano flower diameter is about 1 μm to 5 μm.
To the surface of the copper oxide prepared in example 3, 5. mu.L of a water droplet was dropped by a contact angle meter, and the static water contact angle thereof was 0 °.
Example 4
A preparation method of copper oxide with a nanometer flower-like structure comprises the following steps:
soaking the foamy copper with the area size of 2cm multiplied by 2cm in 20ml of mixed solution containing 2.5mol/l of sodium hydroxide and 0.2mol/l of ammonium persulfate, reacting for 40 minutes, repeatedly washing with water after the reaction is finished, and drying in an oven at 60 ℃ to obtain the copper oxide.
FIG. 4 is a morphological analysis of copper oxide as in example 4 by a scanning electron microscope of Japanese Hitachi su 1510. As shown in fig. 4, the middle layer of the nanoflower shrinks to form a micrometer flower shape with a grid structure inside. Wherein the diameter of the sphere is about 1-10 μm.
To the surface of the copper oxide prepared in example 4, 5. mu.L of a water droplet was dropped by a contact angle meter, and the static water contact angle thereof was 0 °.
Example 5
A preparation method of copper oxide with a nanometer flower-like structure comprises the following steps:
soaking the copper foam with the area size of 4cm multiplied by 4cm in 20ml of mixed solution containing 5.0mol/l of sodium hydroxide and 0.4mol/l of ammonium persulfate, reacting for 10 minutes, repeatedly washing with water after the reaction is finished, and drying in an oven at 60 ℃ to obtain the copper oxide.
FIG. 5 is a morphological analysis of copper oxide as in example 5 by a scanning electron microscope of Japanese Hitachi su 1510. As shown in FIG. 5, the nano-rod copper oxide is formed, and has a length of 1 μm to 10 μm and a diameter of about 100 nm to 1000 nm.
To the surface of the copper oxide prepared in example 5, 5. mu.L of a water droplet was dropped by a contact angle meter, and the static water contact angle thereof was 0 °.
Example 6
A preparation method of copper oxide with a nanometer flower-like structure comprises the following steps:
soaking the copper foam with the area of 4cm multiplied by 4cm in 20ml of mixed solution containing 5.0mol/l of sodium hydroxide and 0.4mol/l of ammonium persulfate, reacting for 20 minutes, repeatedly washing with water after the reaction is finished, and drying in an oven at 60 ℃ to obtain the copper oxide.
FIG. 6 is a morphological analysis of copper oxide as in example 6 by a scanning electron microscope of Japanese Hitachi su 1510. As shown in fig. 6, the nanorod-nanoflower copper oxide is formed at this time, but the nanoflower here is just a sphere formed by stacking of nanosheets, and the lamella is not yet completely opened and is not formed in a flower shape. Wherein, the length of the nano rod is between 1 and 10 mu m, the diameter is between 100 and 1000nm, and the diameter of the nano flower is between 1 and 5 mu m.
To the surface of the copper oxide prepared in example 6, 5. mu.L of a water droplet was dropped by a contact angle meter, and the static water contact angle thereof was 0 °.
Example 7
A preparation method of copper oxide with a nanometer flower-like structure comprises the following steps:
soaking a copper foam having an area of 4cm × 4cm in 20ml of a mixed solution containing 5.0mol/l sodium hydroxide and 0.4mol/l ammonium persulfateIn the course of 30 minutes, OH-And Cu2+Ions coordinate to nucleate under alkaline conditions, resulting in the growth of copper oxide nanoplatelet structures that form networks with each other through van der waals forces and hydrogen bonding, thereby forming a larger observable nanoflower copper oxide geometry. And after the reaction is finished, repeatedly washing with water, and drying in a 60 ℃ oven to obtain the nano flower-shaped copper oxide.
FIG. 7 is a morphological analysis of copper oxide as in example 7 by a scanning electron microscope of Japanese Hitachi su 1510. As shown in FIG. 7, the single-layered flower-like branches grow in different directions and exist in the copper-based foam structure, and the sizes are almost uniform, the entire nanoflower is assembled in multiple layers, the roots of the petals thereof are connected with each other and fixed at one center, and finally, a circular flower-like shape similar to marigold is formed. The length of the single petal is about 300-500 nm, and the diameter range of the complete single petal is about 1-5 μm.
5. mu.L of a water droplet was dropped on the surface of the copper oxide prepared in example 7 by a contact angle measuring instrument, and the static water contact angle was 0 ℃ as shown in FIG. 8.
The graph in FIG. 9 is an X-ray diffraction (XRD) pattern of the flower-like copper oxide prepared in example 7, and X-ray diffraction analysis was performed at room temperature using a DX-27000X-ray diffractometer using CuKa rays (wavelength. lambda.: 0.15405nm, scanning mode: continuous scanning, scanning speed: 0.1 °/s, scanning angle: 5 to 90 °, tube voltage: 35kV, tube current: 35mA) as a diffraction light source. As shown in fig. 9, the diffraction peaks of copper oxide at 2-fold diffraction angles of 32.4 °, 35.4 °, 38.7 °, 43.3 °, 48.7 °, 50.43 °, 58.3 °, 61.5 °, 65.7 °, 68.0 ° and 74.1 ° respectively correspond to the (110), (002), (111), (202), (200), (202), (113), (022), (220) and (220) crystal planes. These peaks align well with the face centered cubic phase of copper oxide (PDF card JCPDS No.45-0937), further confirming the high purity of the synthesized copper oxide.
As shown in fig. 10, the current density of the copper oxide sample prepared from the copper foam sharply increased or decreased with the light source on and off, which is a sufficient indication that the copper oxide has good photoresponse characteristics.
FIG. 11 is a graph showing the photocatalytic degradation of copper oxide prepared from copper foam to the environmental pollutant octylphenol polyoxyethylene ether. In the experimental procedure, 1cm × 1cm copper oxide (0.08g) was first placed in 10 ml of a contaminant solution with a concentration of 25ppm (total amount of contaminants is 0.25mg), and placed in the dark for a certain period of time to allow equilibrium adsorption. Subsequently, the samples were exposed to visible light to evaluate the ability of the copper oxide to photocatalytically degrade contaminants. As shown in FIG. 11, the nano flower-like copper oxide prepared from the copper foam has good visible light degradation capability on octylphenol polyoxyethylene ether pollutants, and can be further applied to environmental treatment of other pollutants.
Example 8
A preparation method of copper oxide with a nanometer flower-like structure comprises the following steps:
soaking the copper foam with the area of 4cm multiplied by 4cm in 20ml of mixed solution containing 5.0mol/l of sodium hydroxide and 0.4mol/l of ammonium persulfate, reacting for 40 minutes, repeatedly washing with water after the reaction is finished, and drying in an oven at 60 ℃ to obtain the copper oxide.
FIG. 12 is a morphological analysis of copper oxide as in example 8 by a scanning electron microscope of Japanese Hitachi su 1510. As shown in fig. 12, the nanoflower was peeled off from the copper oxide to form a flat sheet structure. Wherein the length of the lamella is about 1-3 μm.
To the surface of the copper oxide prepared in example 8, 5. mu.L of a water droplet was dropped by a contact angle meter, and the static water contact angle thereof was 0 °.
Example 9
A preparation method of copper oxide with a nanometer flower-like structure comprises the following steps:
and (3) soaking a copper net with the area of 2cm multiplied by 2cm in 20ml of mixed solution containing 2.5mol/l of sodium hydroxide and 0.2mol/l of ammonium persulfate, reacting for 10 minutes, repeatedly washing with water after the reaction is finished, and drying in an oven at 60 ℃ to obtain the copper oxide.
FIG. 13 is a morphological analysis of copper oxide as in example 9 by a scanning electron microscope of Japanese Hitachi su 1510. As shown in fig. 13, this is nanowire-shaped copper oxide. Wherein the length of the nanowire is between about 1 μm and 5 μm.
To the surface of the copper oxide prepared in example 9, 5. mu.L of a water droplet was dropped by a contact angle meter, and the static water contact angle thereof was 0 °.
Example 10
A preparation method of copper oxide with a nanometer flower-like structure comprises the following steps:
and (3) soaking a copper net with the area of 2cm multiplied by 2cm in 20ml of mixed solution containing 2.5mol/l of sodium hydroxide and 0.2mol/l of ammonium persulfate, reacting for 20 minutes, repeatedly washing with water after the reaction is finished, and drying in an oven at 60 ℃ to obtain the copper oxide.
FIG. 14 is a morphological analysis of copper oxide as in example 10 by a scanning electron microscope of Japanese Hitachi su 1510. As shown in fig. 14, a nanowire-nanoflower-shaped copper oxide in which the nanowire length is between 1 μm and 5 μm and the nanoflower diameter is between 1 μm and 6 μm was formed at this time.
To the surface of the copper oxide prepared in example 10, 5. mu.L of a water droplet was dropped by a contact angle meter, and the static water contact angle thereof was 0 °.
Example 11
A preparation method of copper oxide with a nanometer flower-like structure comprises the following steps:
and (3) soaking a copper net with the area of 2cm multiplied by 2cm in 20ml of mixed solution containing 2.5mol/l of sodium hydroxide and 0.2mol/l of ammonium persulfate, reacting for 30 minutes, repeatedly washing with water after the reaction is finished, and drying in an oven at 60 ℃ to obtain the copper oxide.
FIG. 15 is a morphological analysis of copper oxide as in example 11 by a scanning electron microscope of Japanese Hitachi su 1510. As shown in FIG. 15, a rosette of copper oxide was formed. Wherein the diameter of the nanoflower is between 1 and 5 microns.
To the surface of the copper oxide prepared in example 11, 5. mu.L of a water droplet was dropped by a contact angle meter, and the static water contact angle thereof was 0 °.
Example 12
A preparation method of copper oxide with a nanometer flower-like structure comprises the following steps:
and (3) soaking a copper net with the area of 4cm multiplied by 4cm in 20ml of mixed solution containing 5.0mol/l of sodium hydroxide and 0.4mol/l of ammonium persulfate, reacting for 10 minutes, repeatedly washing with water after the reaction is finished, and drying in an oven at 60 ℃ to obtain the copper oxide.
FIG. 16 is a morphological analysis of copper oxide as in example 12 by a scanning electron microscope of Japanese Hitachi su 1510. As shown in FIG. 16, the nano-rod copper oxide is formed, and has a length of 1 μm to 10 μm and a diameter of about 100 nm to 1000 nm.
To the surface of the copper oxide prepared in example 12, 5. mu.L of a water droplet was dropped by a contact angle meter, and the static water contact angle thereof was 0 °.
Example 13
A preparation method of copper oxide with a nanometer flower-like structure comprises the following steps:
and (3) soaking a copper net with the area of 4cm multiplied by 4cm in 20ml of mixed solution containing 5.0mol/l of sodium hydroxide and 0.4mol/l of ammonium persulfate, reacting for 20 minutes, repeatedly washing with water after the reaction is finished, and drying in an oven at 60 ℃ to obtain the copper oxide.
FIG. 17 is a morphological analysis of copper oxide as in example 6 by a scanning electron microscope of Japanese Hitachi su 1510. As shown in fig. 17, nanorod-nanoflower copper oxide is formed at this time. Wherein, the length of the nano rod is between 1 and 10 mu m, the diameter is between 100 and 1000nm, and the diameter of the nano flower is between 1 and 5 mu m.
To the surface of the copper oxide prepared in example 13, 5. mu.L of a water droplet was dropped by a contact angle meter, and the static water contact angle thereof was 0 °.
Example 14
A preparation method of copper oxide with a nanometer flower-like structure comprises the following steps:
soaking a copper net with the area of 4cm multiplied by 4cm in 20ml of mixed solution containing 5.0mol/l of sodium hydroxide and 0.4mol/l of ammonium persulfate, reacting for 30 minutes, wherein a large number of nano lamellar structures appear on the surface of the copper net and rapidly aggregate to form a flower-shaped structure, repeatedly washing with water after the reaction is finished, and drying in a 60 ℃ oven to obtain the nano flower-shaped copper oxide.
FIG. 18 is a morphological analysis of copper oxide as in example 14 by a scanning electron microscope of Japanese Hitachi su 1510. As shown in FIG. 18, the close mosaic of the nano-sheets with layered petal-shaped structure forms a rose-like shape, and the diameter of the flower-shaped structure is about 1 μm to 5 μm.
To the surface of the copper oxide prepared in example 14, 5. mu.L of a water droplet was dropped by a contact angle measuring instrument, and as shown in FIG. 19, the static water contact angle was 0 °.
The graph in FIG. 20 is an X-ray diffraction (XRD) pattern of the flower-like copper oxide prepared in example 14, and X-ray diffraction analysis was performed at room temperature using a DX-27000X-ray diffractometer using CuKa rays (wavelength. lambda.: 0.15405nm, scanning mode: continuous scanning, scanning speed: 0.1 °/s, scanning angle: 5 to 90 °, tube voltage: 35kV, tube current: 35mA) as a diffraction light source. As shown in fig. 20, the diffraction peaks of copper oxide at 2-fold diffraction angles of 32.4 °, 35.4 °, 38.7 °, 43.3 °, 48.7 °, 50.43 °, 58.3 °, 61.5 °, 65.7 °, 68.0 ° and 74.1 ° respectively correspond to the (110), (002), (111), (202), (200), (202), (113), (022), (220) and (220) crystal planes. These peaks align well with the face centered cubic phase of copper oxide (PDF card JCPDS No.45-0937), further confirming the high purity of the synthesized copper oxide.
As shown in fig. 21, the current density of the copper oxide sample made from the copper mesh sharply increased or decreased with the light source on and off, indicating that it had good photoresponse characteristics.
FIG. 22 is a graph showing the photocatalytic degradation of environmental pollutants octylphenol polyoxyethylene ether by copper oxide prepared using a copper mesh. In the experimental process, the prepared copper oxide with the size of 1cm multiplied by 1cm (0.08g) is firstly put into 10 ml of pollutant solution with the concentration of 25ppm (the total amount of pollutants is 0.25mg), and is put in the dark for a certain time to reach equilibrium adsorption. Subsequently, the samples were exposed to visible light to evaluate the ability of the copper oxide to photocatalytically degrade contaminants. As shown in fig. 22, the nano flower-like copper oxide prepared from the copper mesh has good visible light degradation capability on octylphenol polyoxyethylene ether pollutants, and can be further applied to environmental treatment of other pollutants.
TABLE 1 morphology of copper oxide prepared in examples 1-14
Most of the copper oxide shows special physical and chemical properties in the aspects of light absorption, chemical activity, thermal resistance and the like, and has the remarkable characteristics of no toxicity, environmental protection, high stability, recyclability and the like, so that the copper oxide has wide application in industrial production. The novel method for preparing the copper oxide is simple and convenient, the nano-popcorn-shaped copper oxide can be quickly prepared, and the obtained copper oxide has high purity, good hydrophilicity, good photoresponse characteristic and excellent effect on the aspect of photocatalytic degradation of pollutants.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (6)
1. A preparation method of copper oxide with a nanometer flower-like structure is characterized by comprising the following steps: adding the copper mesh/foam copper into a mixed solution of sodium hydroxide and ammonium persulfate, reacting the reaction solution at 20-50 ℃ for 10-60min, taking out, washing with water, and drying to obtain the copper oxide with the nanometer flower-shaped structure.
2. The method for preparing copper oxide with a nanoflower structure according to claim 1, wherein the concentration of sodium hydroxide is 2.5-5.0 mol/L.
3. The method for preparing copper oxide with a nanoflower structure according to claim 1, wherein the concentration of ammonium persulfate is 0.2-0.4 mol/L.
4. The method for preparing copper oxide with nanoflower structure according to claim 1, wherein the copper oxide is prepared by the method of the following stepsThen, the area of the copper mesh/copper foam is 2cm2-16 cm2。
5. The method for preparing copper oxide with nanometer flower-like structure as claimed in claim 4, wherein the size of the copper mesh/copper foam is 2cm x 2 cm.
6. The application of the preparation method of copper oxide with a nanoflower structure in the fields of batteries, supercapacitors, solar cells, optoelectronic devices, photocatalysis, sterilization, environmental treatment or biochemical sensors according to any one of claims 1 to 5.
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