CN106145179B - The cupric oxide nano-rod and its synthetic method of a kind of supported cobaltosic oxide - Google Patents

The cupric oxide nano-rod and its synthetic method of a kind of supported cobaltosic oxide Download PDF

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CN106145179B
CN106145179B CN201510163324.1A CN201510163324A CN106145179B CN 106145179 B CN106145179 B CN 106145179B CN 201510163324 A CN201510163324 A CN 201510163324A CN 106145179 B CN106145179 B CN 106145179B
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rod
heating
nanometer rods
cupric oxide
temperature
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CN106145179A (en
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陈瑞雪
梁砚琴
崔振铎
杨贤金
朱胜利
李朝阳
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Tianjin University
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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
    • 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
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C01G51/04—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • 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
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • 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
    • C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases

Abstract

The present invention discloses the cupric oxide nano-rod and its synthetic method of a kind of supported cobaltosic oxide, a diameter of 150 250nm of cupric oxide nano-rod, cobaltosic oxide is 10 15nm and is uniformly coated on the surface of cupric oxide nano-rod, cupric oxide nano-rod is prepared using thermally grown method, and carries out the load of cobaltosic oxide on cupric oxide nano-rod with hydrothermal chemistry method.Implementation cost of the present invention is low, easy to operate, and pollution is low, is a kind of synthetic method of high-efficiency and economic, while material structure of the invention is stable and has cathode electrocatalyst performance.

Description

The cupric oxide nano-rod and its synthetic method of a kind of supported cobaltosic oxide
Technical field
The present invention relates to a kind of novel nano-material and its synthetic method, more particularly to a kind of oxygen of supported cobaltosic oxide Change copper nanometer rods and its synthetic method.
Background technology
It is that the sustainable solution of a cleaning is done to the energy problem of current getting worse that solar energy, which is converted into chemical fuel, Method.Driven by Solar Energy water decomposition based on semi-conducting material is artificial photosynthesis, by storage of solar energy in product H2 And O2Chemical bond in.Optical electro-chemistry (PEC) battery is widely used in solar energy electrolyzing water device.Because H2It is a kind of clean energy resource, Water is only produced during burning, so the evolving hydrogen reaction (HER) of negative electrode receives much concern.Optical electro-chemistry evolving hydrogen reaction in P-type semiconductor and The interface of electrolyte, to develop the photocathode of high energy, the small material of band gap is first choice, additionally nontoxic, inexpensive, resistance to Abrasion.
Cupric oxide is P-type semiconductor, due to synthetic method and the difference of condition, direct band gap scope be from 1.3eV to 1.8eV.Small band-gap energy allows CuO to absorb most of solar spectral, and direct band gap makes CuO compared with indirect band gap Material has bigger absorption coefficient.But single-phase structure C uO still has certain limitation, such as：(1) CuO surfaces Evolving hydrogen reaction overpotential is higher, and this is the FAQs of conductor oxidate.(2) CuO is unstable under cathode potential, CuO light The evolving hydrogen reaction photoelectric current of electric negative electrode quickly decays with the time.
Co3O4Crystallize as cubic system, there is normal AB2O4Spinel structure, it is a kind of important semiconductor function material Material, height ratio capacity, and also density is also larger, moreover it is possible to the discharge and recharge of relatively high power is born, it has stable chemical property and spy Fixed magnetic performance, therefore have extensively in many fields such as ultracapacitor, catalyst, gas sensor, lithium ion battery Application, primary disadvantage is that operating potential is higher.
The content of the invention
It is an object of the invention to provide a kind of cupric oxide nano-rod of supported cobaltosic oxide and its synthetic method, obtains one Kind specific surface area is big and has the nanorod structure of electrocatalysis characteristic, and the method has the characteristics of cost is low, preparation process is simple.
The purpose of the present invention is achieved by following technical proposals：
A kind of cupric oxide nano-rod of supported cobaltosic oxide, a diameter of 150-250nm of cupric oxide nano-rod, four oxidations Three cobalts are 10-15nm and are uniformly coated on the surface of cupric oxide nano-rod, and are carried out as steps described below：
Step 1, the preparation of CuO nanometer rods：Will be clear with deionized water after fine copper net surface hydrochloric acid or ethanol immersion ultrasound Wash clean, drying for standby；Fine copper net is placed in ceramic Noah's ark to be put into cabinet-type electric furnace and heated, heating-up temperature is 500-600 DEG C, Heat time is 5-8h, and the CuO nanometer rods being grown on copper mesh are made after furnace cooling.
Step 2, the copper mesh that obtained growth there are CuO nanometer rods in step 1 is placed in Co (NO3)2、NH4F, sodium potassium tartrate tetrahydrate (C4H4KNAaO6-4H2) and urea (CO (NH O2)2) water and ethylene glycol mixed solution in, carry out hydro-thermal reaction in a kettle.
Mixed solution reclaimed water described in step 2, ethylene glycol, Co (NO3)2、NH4F, sodium potassium tartrate tetrahydrate (C4H4KNAaO6- 4H2) and urea (CO (NH O2)2) the ratio between the amount of material be 8.4:2.7:(0.3-0.4):0.5:(0.1-0.3):(1.2- 1.6)；The packing ratio of mixed solution and reactor is 2:1；Heating-up temperature is 100 DEG C -150 DEG C；Heat time is 5-8h；
Step 3 cleans the reaction product in step 2 with deionized water, is heat-treated after drying in cabinet-type electric furnace, heats Temperature is 350-400 DEG C, heat time 2-3h, load C o is obtained after processing3O4CuO nanometer rods.
The present invention method cost it is low, it is easy to operate, take it is shorter, compared with traditional preparation methods, mainly have with Under several advantages：(1) solve the characteristics of particle agglomeration, make Co3O4It is evenly distributed in CuO nanometer rods (such as the institute of accompanying drawing 3 and 4 Show), cupric oxide has (002), (111), (- 202), (113) and (- 220) crystal face, cobaltosic oxide have (220), (311), And (511) crystal face (400)；(2) reaction time greatly shortens, and simple to operate；(3) electrochemical workstation Gamry is used Reference 600 is tested, and the solution for test is PH=7.25,0.25M Na for the solution for test2SO4It is molten Liquid, the speed for carrying out linear voltammetric scan are 50mV/s, load C o3O4CuO nanometer rods current density significantly increase it is (such as attached Shown in Fig. 7), show CuO-Co3O4The catalytic performance of compound greatly improves, and this material can be used as electrocatalyst for cathode.
Brief description of the drawings
Fig. 1 is 10K times of SEM patterns photo (FE-SEM, Hitachi S-4800) of CuO nanometer rods of the present invention；
Fig. 2 is CuO nanometer rods load C o of the present invention3O410K times of SEM patterns photo (FE-SEM, Hitachi S- 4800)；
Fig. 3 is CuO nanometer rods load C o of the present invention3O4500 times of SEM patterns photo (FE-SEM, Hitachi S- 4800)；
Fig. 4 is that CuO nanometer rods of the present invention loaded Co3O4Low power TEM patterns photo (TEM, Philips Tecnai afterwards G2F20)；
Fig. 5 is that CuO nanometer rods of the present invention loaded Co3O4High power TEM patterns photo (TEM, Philips Tecnai afterwards G2F20)
Fig. 6 is the XRD spectrum (XRD, RIGAKU/DMAX) of CuO-Co3O4 compounds of the present invention, and its orbicular spot represents CuO Crystal face, five-pointed star represents Co3O4 crystal face；
Fig. 7 is CuO nanometer rods of the present invention and CuO-Co3O4The linear voltammetric scan testing current figure line of compound, curve 1 For the test figure line of CuO nanometer rods, curve 2 is CuO-Co3O4The test figure line of compound.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, embodiment of the present invention is made below further It is described in detail on ground.
Embodiment 1
Fine copper net surface is cleaned up with after hydrochloric acid or ethanol immersion ultrasound with deionized water, drying for standby；By fine copper Net is placed in ceramic Noah's ark to be put into cabinet-type electric furnace and heated, and heating-up temperature is 500 DEG C, heat time 5h, is made after furnace cooling The CuO nanometer rods that must be grown on copper mesh.
The copper mesh that obtained growth there are CuO nanometer rods is placed in Co (NO3)2、NH4F, sodium potassium tartrate tetrahydrate (C4H4KNAaO6- 4H2) and urea (CO (NH O2)2) water and ethylene glycol mixed solution in, carry out hydro-thermal reaction in a kettle.Its reclaimed water, second two Alcohol, Co (NO3)2、NH4F, sodium potassium tartrate tetrahydrate (C4H4KNAaO6-4H2) and urea (CO (NH O2)2) the ratio between the amount of material be 8.4: 2.7:0.35:0.5:0.2:1.5, the packing ratio of mixed solution and reactor is 2:1；Heating-up temperature is 110 DEG C；Heat time is 5h。
Above-mentioned reaction product is cleaned with deionized water, is heat-treated after drying in cabinet-type electric furnace, heating-up temperature 350 DEG C, heat time 2h, load C o is obtained after processing3O4CuO nanometer rods.
Embodiment 2
Fine copper net surface is cleaned up with after hydrochloric acid or ethanol immersion ultrasound with deionized water, drying for standby；By fine copper Net is placed in ceramic Noah's ark to be put into cabinet-type electric furnace and heated, and heating-up temperature is 500 DEG C, heat time 5h, is made after furnace cooling The CuO nanometer rods that must be grown on copper mesh.
The copper mesh that obtained growth there are CuO nanometer rods is placed in Co (NO3)2、NH4F, sodium potassium tartrate tetrahydrate (C4H4KNAaO6- 4H2) and urea (CO (NH O2)2) water and ethylene glycol mixed solution in, carry out hydro-thermal reaction in a kettle.Its reclaimed water, second two Alcohol, Co (NO3)2、NH4F, sodium potassium tartrate tetrahydrate (C4H4KNAaO6-4H2) and urea (CO (NH O2)2) the ratio between the amount of material be 8.4: 2.7:0.3:0.5:0.1:1.3, the packing ratio of mixed solution and reactor is 2:1；Heating-up temperature is 110 DEG C；Heat time is 6h。
Above-mentioned reaction product is cleaned with deionized water, is heat-treated after drying in cabinet-type electric furnace, heating-up temperature 350 DEG C, heat time 2h, load C o is obtained after processing3O4CuO nanometer rods.
Embodiment 3
Fine copper net surface is cleaned up with after hydrochloric acid or ethanol immersion ultrasound with deionized water, drying for standby；By fine copper Net is placed in ceramic Noah's ark to be put into cabinet-type electric furnace and heated, and heating-up temperature is 500 DEG C, heat time 5h, is made after furnace cooling The CuO nanometer rods that must be grown on copper mesh.
The copper mesh that obtained growth there are CuO nanometer rods is placed in Co (NO3)2、NH4F, sodium potassium tartrate tetrahydrate (C4H4KNAaO6- 4H2) and urea (CO (NH O2)2) water and ethylene glycol mixed solution in, carry out hydro-thermal reaction in a kettle.Its reclaimed water, second two Alcohol, Co (NO3)2、NH4F, sodium potassium tartrate tetrahydrate (C4H4KNAaO6-4H2) and urea (CO (NH O2)2) the ratio between the amount of material be 8.4: 2.7:0.4:0.5:0.3:1.4, the packing ratio of mixed solution and reactor is 2:1；Heating-up temperature is 100 DEG C；Heat time is 5h。
Above-mentioned reaction product is cleaned with deionized water, is heat-treated after drying in cabinet-type electric furnace, heating-up temperature 350 DEG C, heat time 2h, load C o is obtained after processing3O4CuO nanometer rods.
Embodiment 4
Fine copper net surface is cleaned up with after hydrochloric acid or ethanol immersion ultrasound with deionized water, drying for standby；By fine copper Net is placed in ceramic Noah's ark to be put into cabinet-type electric furnace and heated, and heating-up temperature is 600 DEG C, heat time 6h, is made after furnace cooling The CuO nanometer rods that must be grown on copper mesh.
The copper mesh that obtained growth there are CuO nanometer rods is placed in Co (NO3)2、NH4F, sodium potassium tartrate tetrahydrate (C4H4KNAaO6- 4H2) and urea (CO (NH O2)2) water and ethylene glycol mixed solution in, carry out hydro-thermal reaction in a kettle.Its reclaimed water, second two Alcohol, Co (NO3)2、NH4F, sodium potassium tartrate tetrahydrate (C4H4KNAaO6-4H2) and urea (CO (NH O2)2) the ratio between the amount of material be 8.4: 2.7:0.38:0.5:0.2:1.6, the packing ratio of mixed solution and reactor is 2:1；Heating-up temperature is 120 DEG C；Heat time is 6h。
Above-mentioned reaction product is cleaned with deionized water, is heat-treated after drying in cabinet-type electric furnace, heating-up temperature 380 DEG C, heat time 2h, load C o is obtained after processing3O4CuO nanometer rods.
Embodiment 5
Fine copper net surface is cleaned up with after hydrochloric acid or ethanol immersion ultrasound with deionized water, drying for standby；By fine copper Net is placed in ceramic Noah's ark to be put into cabinet-type electric furnace and heated, and heating-up temperature is 500 DEG C, heat time 5h, is made after furnace cooling The CuO nanometer rods that must be grown on copper mesh.
The copper mesh that obtained growth there are CuO nanometer rods is placed in Co (NO3)2、NH4F, sodium potassium tartrate tetrahydrate (C4H4KNAaO6- 4H2) and urea (CO (NH O2)2) water and ethylene glycol mixed solution in, carry out hydro-thermal reaction in a kettle.Its reclaimed water, second two Alcohol, Co (NO3)2、NH4F, sodium potassium tartrate tetrahydrate (C4H4KNAaO6-4H2) and urea (CO (NH O2)2) the ratio between the amount of material be 8.4: 2.7:0.36:0.5:0.3:1.3, the packing ratio of mixed solution and reactor is 2:1；Heating-up temperature is 150 DEG C；Heat time is 6h。
Above-mentioned reaction product is cleaned with deionized water, is heat-treated after drying in cabinet-type electric furnace, heating-up temperature 400 DEG C, heat time 1h, load C o is obtained after processing3O4CuO nanometer rods.
Embodiment 6
Fine copper net surface is cleaned up with after hydrochloric acid or ethanol immersion ultrasound with deionized water, drying for standby；By fine copper Net is placed in ceramic Noah's ark to be put into cabinet-type electric furnace and heated, and heating-up temperature is 500 DEG C, heat time 5h, is made after furnace cooling The CuO nanometer rods that must be grown on copper mesh.
The copper mesh that obtained growth there are CuO nanometer rods is placed in Co (NO3)2、NH4F, sodium potassium tartrate tetrahydrate (C4H4KNAaO6- 4H2) and urea (CO (NH O2)2) water and ethylene glycol mixed solution in, carry out hydro-thermal reaction in a kettle.Its reclaimed water, second two Alcohol, Co (NO3)2、NH4F, sodium potassium tartrate tetrahydrate (C4H4KNAaO6-4H2) and urea (CO (NH O2)2) the ratio between the amount of material be 8.4: 2.7:0.4:0.5:0.0.3:1.5, the packing ratio of mixed solution and reactor is 2:1；Heating-up temperature is 100 DEG C；Heat time For 8h.
Above-mentioned reaction product is cleaned with deionized water, is heat-treated after drying in cabinet-type electric furnace, heating-up temperature 350 DEG C, heat time 2h, load C o is obtained after processing3O4CuO nanometer rods.
Exemplary description has been done to the present invention above, it should explanation, in the situation for the core for not departing from the present invention Under, any simple deformation, modification or other skilled in the art can not spend the equivalent substitution of creative work equal Fall into protection scope of the present invention.

Claims (3)

  1. A kind of 1. cupric oxide nano-rod of supported cobaltosic oxide, it is characterised in that a diameter of 150- of cupric oxide nano-rod 250nm, cobaltosic oxide is 10-15nm and is uniformly coated on the surface of cupric oxide nano-rod, and is entered as steps described below OK：
    Step 1, the preparation of CuO nanometer rods：Fine copper net surface is dry with being cleaned after hydrochloric acid or ethanol immersion ultrasound with deionized water Only, drying for standby；Fine copper net is placed in ceramic Noah's ark to be put into cabinet-type electric furnace and heated, heating-up temperature is 500-600 DEG C, heating Time is 5-8h, and the CuO nanometer rods being grown on copper mesh are made after furnace cooling；
    Step 2, the copper mesh that obtained growth there are CuO nanometer rods in step 1 is placed in Co (NO3)2、NH4F, sodium potassium tartrate tetrahydrate and urine The water of element with ethylene glycol mixed solution, carrying out hydro-thermal reaction in a kettle；Mixed solution reclaimed water described in step 2, second two Alcohol, Co (NO3)2、NH4F, the ratio between amount of material of sodium potassium tartrate tetrahydrate and urea is 8.4:2.7:(0.3-0.4):0.5:(0.1- 0.3):(1.2-1.6)；The packing ratio of mixed solution and reactor is 2:1；Heating-up temperature is 100 DEG C -150 DEG C；Heat time is 5-8h；
    Step 3 cleans the reaction product in step 2 with deionized water, is heat-treated after drying in cabinet-type electric furnace, heating-up temperature For 350-400 DEG C, heat time 2-3h, load C o is obtained after processing3O4CuO nanometer rods.
  2. 2. the cupric oxide nano-rod of supported cobaltosic oxide according to claim 1, it is characterised in that in the step 1, Heating-up temperature is 500 DEG C, heat time 5h, a diameter of 200nm of gained CuO nanometer rods.
  3. 3. the cupric oxide nano-rod of supported cobaltosic oxide according to claim 1, it is characterised in that in the step 2 The heating-up temperature of hydro-thermal reaction is 100 DEG C -110 DEG C；Heat time is 5-6h.
CN201510163324.1A 2015-04-08 2015-04-08 The cupric oxide nano-rod and its synthetic method of a kind of supported cobaltosic oxide Expired - Fee Related CN106145179B (en)

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CN102320646A (en) * 2011-09-09 2012-01-18 樊余杰 Method for preparing copper oxide and cuprous oxide with waste copper foil
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一维纳米Co3O4，Ag/Co3O4及CuO/Co3O4的合成与电催化性能;潘路 等;《无机化学学报》;20100430;第26卷(第4期);第573-580页 *

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