CN107235504A - The synthetic method of the cupric oxide nano-rod of supported cobaltosic oxide - Google Patents
The synthetic method of the cupric oxide nano-rod of supported cobaltosic oxide Download PDFInfo
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Abstract
The present invention discloses the synthetic method of the cupric oxide nano-rod of supported cobaltosic oxide, cupric oxide nano-rod is prepared using thermally grown method, and the load of cobaltosic oxide is carried out on cupric oxide nano-rod with hydrothermal chemistry method, 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.Implementation cost of the present invention is low, easy to operate, pollutes low, is a kind of synthetic method of high-efficiency and economic, while the material structure of the present invention is stable and with cathode electrocatalyst performance.
Description
The present patent application is parent application " cupric oxide nano-rod and its synthetic method of a kind of supported cobaltosic oxide "
Divisional application, the Application No. 2015101633241 of parent application, the applying date is on April 8th, 2015.
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
Solar energy is converted into chemical fuel to increasingly serious energy problem is that the sustainable solution of a cleaning is done now
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, with normal AB2O4Spinel structure, 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 chemical property and the spy of stabilization
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, one is obtained
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, hydro-thermal reaction is carried out 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, heating
Temperature is 350-400 DEG C, and the heat time is to obtain load C o after 2-3h, 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) the characteristics of solving particle agglomeration, makes Co3O4It is evenly distributed in CuO nanometer rods (such as the institute of accompanying drawing 3 and 4
Show), cupric oxide have (002), (111), (- 202), (113) and (- 220) crystal face, cobaltosic oxide with (220), (311),
And (511) crystal face (400)；(2) reaction time greatly shortens, and simple to operate；(3) using electrochemical workstation Gamry
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 is 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 is greatly improved, 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, HitachiS-4800)；
Fig. 3 is CuO nanometer rods load C o of the present invention3O4500 times of SEM patterns photos (FE-SEM, HitachiS-4800)；
Fig. 4 is that CuO nanometer rods of the present invention loaded Co3O4Low power TEM pattern photos (TEM, Philips afterwards
TecnaiG2F20)；
Fig. 5 is that CuO nanometer rods of the present invention loaded Co3O4High power TEM pattern photos (TEM, Philips afterwards
TecnaiG2F20)
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, further is made to embodiment of the present invention below
It is described in detail on ground.
Embodiment 1
Cleaned up after fine copper net surface is soaked into ultrasound with hydrochloric acid or ethanol 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, and the heat time is 5h, is made after furnace cooling
The CuO nanometer rods on copper mesh must be grown in.
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, hydro-thermal reaction is carried out 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 is 350
DEG C, the heat time is to obtain load C o after 2h, processing3O4CuO nanometer rods.
Embodiment 2
Cleaned up after fine copper net surface is soaked into ultrasound with hydrochloric acid or ethanol 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, and the heat time is 5h, is made after furnace cooling
The CuO nanometer rods on copper mesh must be grown in.
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, hydro-thermal reaction is carried out 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 is 350
DEG C, the heat time is to obtain load C o after 2h, processing3O4CuO nanometer rods.
Embodiment 3
Cleaned up after fine copper net surface is soaked into ultrasound with hydrochloric acid or ethanol 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, and the heat time is 5h, is made after furnace cooling
The CuO nanometer rods on copper mesh must be grown in.
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, hydro-thermal reaction is carried out 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 is 350
DEG C, the heat time is to obtain load C o after 2h, processing3O4CuO nanometer rods.
Embodiment 4
Cleaned up after fine copper net surface is soaked into ultrasound with hydrochloric acid or ethanol 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, and the heat time is 6h, is made after furnace cooling
The CuO nanometer rods on copper mesh must be grown in.
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, hydro-thermal reaction is carried out 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 is 380
DEG C, the heat time is to obtain load C o after 2h, processing3O4CuO nanometer rods.
Embodiment 5
Cleaned up after fine copper net surface is soaked into ultrasound with hydrochloric acid or ethanol 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, and the heat time is 5h, is made after furnace cooling
The CuO nanometer rods on copper mesh must be grown in.
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, hydro-thermal reaction is carried out 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 is 400
DEG C, the heat time is to obtain load C o after 1h, processing3O4CuO nanometer rods.
Embodiment 6
Cleaned up after fine copper net surface is soaked into ultrasound with hydrochloric acid or ethanol 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, and the heat time is 5h, is made after furnace cooling
The CuO nanometer rods on copper mesh must be grown in.
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, hydro-thermal reaction is carried out 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 is 350
DEG C, the heat time is to obtain load C o after 2h, processing3O4CuO nanometer rods.
Exemplary description is 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. the synthetic method of the cupric oxide nano-rod of supported cobaltosic oxide, it is characterised in that carry out as steps described below：
Step 1, the preparation of CuO nanometer rods：Fine copper net surface is soaked with hydrochloric acid or ethanol and cleans dry after 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
Element (CO (NH2)2) water and ethylene glycol mixed solution in, hydro-thermal reaction is carried out in a kettle.；
Mixed solution reclaimed water described in step 2, ethylene glycol, Co (NO3)2、NH4F, sodium potassium tartrate tetrahydrate and urea (CO (NH2)2) thing
The ratio between amount of matter is 8.4:2.7:(0.3-0.4):0.5:(0.1-0.3):(1.2-1.6)；The filling of mixed solution and reactor
Than for 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, the heat time is to obtain load C o after 2-3h, processing3O4CuO nanometer rods.
2. the synthetic method of the cupric oxide nano-rod of supported cobaltosic oxide according to claim 1, it is characterised in that institute
State in step (1), heating-up temperature is 500 DEG C, and the heat time is 5h, a diameter of 200nm of gained CuO nanometer rods.
3. the synthetic method of the cupric oxide nano-rod of supported cobaltosic oxide according to claim 1, it is characterised in that institute
The heating-up temperature for stating hydro-thermal reaction in step (2) is 100 DEG C -110 DEG C；Heat time is 5-6h.
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| CN201710364560.9A CN107235504B (en) | 2015-04-08 | 2015-04-08 | The synthetic method of the cupric oxide nano-rod of supported cobaltosic oxide |
| CN201510163324.1A CN106145179B (en) | 2015-04-08 | 2015-04-08 | The cupric oxide nano-rod and its synthetic method of a kind of supported cobaltosic oxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110514700A (en) * | 2019-09-27 | 2019-11-29 | 西安电子科技大学 | A kind of copper oxide and cobaltosic oxide heterogeneous structural nano line composite sensitive material, ethylene glycol sensor and preparation method |
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| CN101311363A (en) * | 2008-04-22 | 2008-11-26 | 华东师范大学 | Bar-shaped CuO nano-material and method for preparing same |
| CN101508528A (en) * | 2009-02-24 | 2009-08-19 | 北京科技大学 | Nano-copper particle dispersion cobalt oxide complex optical film and preparation method |
| CN102320646A (en) * | 2011-09-09 | 2012-01-18 | 樊余杰 | Method for preparing copper oxide and cuprous oxide with waste copper foil |
| CN104009208A (en) * | 2014-05-29 | 2014-08-27 | 中国科学院过程工程研究所 | Method for synthesizing nanometer Ni2O3/Co3O4 cathode material on copper sheet current collector through two-step method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP4174887B2 (en) * | 1998-05-21 | 2008-11-05 | 堺化学工業株式会社 | Method for producing fine spherical particles of nickel, cobalt or copper carbonate or hydroxide |
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- 2015-04-08 CN CN201710364560.9A patent/CN107235504B/en not_active Expired - Fee Related
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101311363A (en) * | 2008-04-22 | 2008-11-26 | 华东师范大学 | Bar-shaped CuO nano-material and method for preparing same |
| CN101508528A (en) * | 2009-02-24 | 2009-08-19 | 北京科技大学 | Nano-copper particle dispersion cobalt oxide complex optical film and preparation method |
| CN102320646A (en) * | 2011-09-09 | 2012-01-18 | 樊余杰 | Method for preparing copper oxide and cuprous oxide with waste copper foil |
| CN104009208A (en) * | 2014-05-29 | 2014-08-27 | 中国科学院过程工程研究所 | Method for synthesizing nanometer Ni2O3/Co3O4 cathode material on copper sheet current collector through two-step method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110514700A (en) * | 2019-09-27 | 2019-11-29 | 西安电子科技大学 | A kind of copper oxide and cobaltosic oxide heterogeneous structural nano line composite sensitive material, ethylene glycol sensor and preparation method |
| CN110514700B (en) * | 2019-09-27 | 2021-09-07 | 西安电子科技大学 | Copper oxide and cobaltosic oxide heterostructure nanowire composite sensitive material, ethylene glycol sensor and preparation method |
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| CN106145179B (en) | 2018-02-27 |
| CN107235504B (en) | 2018-10-26 |
| CN106145179A (en) | 2016-11-23 |
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