CN107235504B - 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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- C01G3/00—Compounds of copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
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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, it is used in combination hydrothermal chemistry method to carry out the load of cobaltosic oxide on cupric oxide nano-rod, a diameter of 150-250nm of cupric oxide nano-rod, cobaltosic oxide are 10-15nm and are uniformly coated on the surface of cupric oxide nano-rod.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 the material structure of the present invention is stable and have cathode electrocatalyst performance.
Description
The present patent application is parent application " a kind of cupric oxide nano-rod and its synthetic method of supported cobaltosic oxide "
Divisional application, parent application application No. is 2015101633241, 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
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, and solar energy is stored in product H2
And O2Chemical bond in.Optical electro-chemistry (PEC) battery is widely used in solar energy electrolyzing water device.Because of H2It is a kind of clean energy resource,
Water is only generated when burning, so the evolving hydrogen reaction (HER) of cathode is concerned.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 preferred, additionally wants nontoxic, inexpensive, resistance to
Abrasion.
Copper oxide is P-type semiconductor, due to synthetic method and the difference of condition, direct band gap range 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 the absorption coefficient of bigger.However single-phase structure C uO still has certain limitation, such as：(1) CuO surfaces
Evolving hydrogen reaction overpotential is higher, this is the FAQs of conductor oxidate.(2) CuO is unstable under cathode potential, CuO light
The evolving hydrogen reaction photoelectric current of electric cathode quickly decays at any time.
Co3O4Crystallization is cubic system, has 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 charge and discharge of relatively high power are 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.
Invention content
The object of the present invention is to provide a kind of cupric oxide nano-rod of supported cobaltosic oxide and its synthetic methods, obtain one
Kind large specific surface area and the nanorod structure with electrocatalysis characteristic, the method have the characteristics that at low cost, 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：It will be clear with deionized water after fine copper net surface hydrochloric acid or ethyl alcohol 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 is heated, heating 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 of CuO nanometer rods is placed in Co (NO growth obtained in step 13)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.
Water, ethylene glycol, Co (NO in mixed solution described in step 23)2、NH4F, sodium potassium tartrate tetrahydrate (C4H4KNAaO6-
4H2) and urea (CO (NH O2)2) the ratio between the amount of substance 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 reaction kettle is 2:1；Heating temperature is 100 DEG C -150 DEG C；Heating time is 5-8h；
Step 3 cleans the reaction product in step 2 with deionized water, is heat-treated in cabinet-type electric furnace after dry, heats
Temperature is 350-400 DEG C, and heating time 2-3h obtains load C o 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) it solves the characteristics of particle agglomeration, makes Co3O4It is evenly distributed in CuO nanometer rods (such as attached drawing 3 and 4 institutes
Show), copper oxide have (002), (111), (- 202), (113) and (- 220) crystal face, cobaltosic oxide with (220), (311),
(400) and (511) crystal face；(2) reaction time greatly shortens, and easy to operate；(3) electrochemical workstation Gamry is used
Reference 600 is tested, and the solution for test is PH=7.25, the Na of 0.25M for the solution for test2SO4It is molten
Liquid, the rate 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.
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 orbicular spot represents CuO
Crystal face, five-pointed star represents the crystal face of Co3O4；
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.
Specific implementation mode
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
It will be cleaned up with deionized water after fine copper net surface hydrochloric acid or ethyl alcohol immersion ultrasound, drying for standby；By fine copper
Net is placed in ceramic Noah's ark to be put into cabinet-type electric furnace and heat, and heating temperature is 500 DEG C, and heating time 5h makes after furnace cooling
The CuO nanometer rods that must be grown on copper mesh.
There is the copper mesh of CuO nanometer rods to be placed in Co (NO growth obtained3)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.Wherein 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 substance be 8.4:
2.7:0.35:0.5:0.2:1.5 the packing ratio of mixed solution and reaction kettle is 2:1；Heating temperature is 110 DEG C；Heating time is
5h。
Above-mentioned reaction product is cleaned with deionized water, is heat-treated in cabinet-type electric furnace after dry, heating temperature 350
DEG C, heating time 2h obtains load C o after processing3O4CuO nanometer rods.
Embodiment 2
It will be cleaned up with deionized water after fine copper net surface hydrochloric acid or ethyl alcohol immersion ultrasound, drying for standby；By fine copper
Net is placed in ceramic Noah's ark to be put into cabinet-type electric furnace and heat, and heating temperature is 500 DEG C, and heating time 5h makes after furnace cooling
The CuO nanometer rods that must be grown on copper mesh.
There is the copper mesh of CuO nanometer rods to be placed in Co (NO growth obtained3)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.Wherein 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 substance be 8.4:
2.7:0.3:0.5:0.1:1.3, the packing ratio of mixed solution and reaction kettle is 2:1；Heating temperature is 110 DEG C；Heating time is
6h。
Above-mentioned reaction product is cleaned with deionized water, is heat-treated in cabinet-type electric furnace after dry, heating temperature 350
DEG C, heating time 2h obtains load C o after processing3O4CuO nanometer rods.
Embodiment 3
It will be cleaned up with deionized water after fine copper net surface hydrochloric acid or ethyl alcohol immersion ultrasound, drying for standby；By fine copper
Net is placed in ceramic Noah's ark to be put into cabinet-type electric furnace and heat, and heating temperature is 500 DEG C, and heating time 5h makes after furnace cooling
The CuO nanometer rods that must be grown on copper mesh.
There is the copper mesh of CuO nanometer rods to be placed in Co (NO growth obtained3)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.Wherein 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 substance be 8.4:
2.7:0.4:0.5:0.3:1.4, the packing ratio of mixed solution and reaction kettle is 2:1；Heating temperature is 100 DEG C；Heating time is
5h。
Above-mentioned reaction product is cleaned with deionized water, is heat-treated in cabinet-type electric furnace after dry, heating temperature 350
DEG C, heating time 2h obtains load C o after processing3O4CuO nanometer rods.
Embodiment 4
It will be cleaned up with deionized water after fine copper net surface hydrochloric acid or ethyl alcohol immersion ultrasound, drying for standby；By fine copper
Net is placed in ceramic Noah's ark to be put into cabinet-type electric furnace and heat, and heating temperature is 600 DEG C, and heating time 6h makes after furnace cooling
The CuO nanometer rods that must be grown on copper mesh.
There is the copper mesh of CuO nanometer rods to be placed in Co (NO growth obtained3)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.Wherein 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 substance be 8.4:
2.7:0.38:0.5:0.2:1.6, the packing ratio of mixed solution and reaction kettle is 2:1；Heating temperature is 120 DEG C；Heating time is
6h。
Above-mentioned reaction product is cleaned with deionized water, is heat-treated in cabinet-type electric furnace after dry, heating temperature 380
DEG C, heating time 2h obtains load C o after processing3O4CuO nanometer rods.
Embodiment 5
It will be cleaned up with deionized water after fine copper net surface hydrochloric acid or ethyl alcohol immersion ultrasound, drying for standby；By fine copper
Net is placed in ceramic Noah's ark to be put into cabinet-type electric furnace and heat, and heating temperature is 500 DEG C, and heating time 5h makes after furnace cooling
The CuO nanometer rods that must be grown on copper mesh.
There is the copper mesh of CuO nanometer rods to be placed in Co (NO growth obtained3)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.Wherein 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 substance be 8.4:
2.7:0.36:0.5:0.3:1.3, the packing ratio of mixed solution and reaction kettle is 2:1；Heating temperature is 150 DEG C；Heating time is
6h。
Above-mentioned reaction product is cleaned with deionized water, is heat-treated in cabinet-type electric furnace after dry, heating temperature 400
DEG C, heating time 1h obtains load C o after processing3O4CuO nanometer rods.
Embodiment 6
It will be cleaned up with deionized water after fine copper net surface hydrochloric acid or ethyl alcohol immersion ultrasound, drying for standby；By fine copper
Net is placed in ceramic Noah's ark to be put into cabinet-type electric furnace and heat, and heating temperature is 500 DEG C, and heating time 5h makes after furnace cooling
The CuO nanometer rods that must be grown on copper mesh.
There is the copper mesh of CuO nanometer rods to be placed in Co (NO growth obtained3)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.Wherein 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 substance be 8.4:
2.7:0.4:0.5:0.0.3:1.5, the packing ratio of mixed solution and reaction kettle is 2:1；Heating temperature is 100 DEG C；Heating time
For 8h.
Above-mentioned reaction product is cleaned with deionized water, is heat-treated in cabinet-type electric furnace after dry, heating temperature 350
DEG C, heating time 2h obtains load C o after processing3O4CuO nanometer rods.
Illustrative description has been done to the present invention above, it should explanation, the case where not departing from core of the invention
Under, any simple deformation, modification or other skilled in the art can not spend the equivalent replacement 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, which is characterized in that carry out as steps described below：
Step 1, the preparation of CuO nanometer rods：It is dry by being cleaned with deionized water after fine copper net surface hydrochloric acid or ethyl alcohol immersion ultrasound
Only, drying for standby；Fine copper net is placed in ceramic Noah's ark to be put into cabinet-type electric furnace and is heated, heating 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 of CuO nanometer rods is placed in Co (NO growth obtained in step 13)2、NH4F, sodium potassium tartrate tetrahydrate and urine
The water of element carries out hydro-thermal reaction in a kettle with ethylene glycol mixed solution；
Water, ethylene glycol, Co (NO in mixed solution described in step 23)2、NH4F, the amount of the substance of sodium potassium tartrate tetrahydrate and urea it
Than being 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 reaction kettle is 2:1；
Heating temperature is 100 DEG C -150 DEG C；Heating time is 5-8h；
Step 3 cleans the reaction product in step 2 with deionized water, is heat-treated in cabinet-type electric furnace after dry, heating temperature
It it is 350-400 DEG C, heating time 2-3h obtains load C o after processing3O4CuO nanometer rods.
2. the synthetic method of the cupric oxide nano-rod of supported cobaltosic oxide according to claim 1, which is characterized in that institute
It states in step 1, heating temperature is 500 DEG C, heating time 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, which is characterized in that institute
The heating temperature for stating hydro-thermal reaction in step 2 is 100 DEG C -110 DEG C；Heating 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 |
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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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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 |
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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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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 |
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| CN106145179B (en) | 2018-02-27 |
| CN107235504A (en) | 2017-10-10 |
| CN106145179A (en) | 2016-11-23 |
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