CN109231284A - A kind of one-dimensional porous nano threadiness cobaltosic oxide electrode material and preparation method thereof - Google Patents

A kind of one-dimensional porous nano threadiness cobaltosic oxide electrode material and preparation method thereof Download PDF

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Publication number
CN109231284A
CN109231284A CN201811054174.0A CN201811054174A CN109231284A CN 109231284 A CN109231284 A CN 109231284A CN 201811054174 A CN201811054174 A CN 201811054174A CN 109231284 A CN109231284 A CN 109231284A
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dimensional porous
porous nano
cobaltosic oxide
oxide electrode
nano threadiness
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李丽
姜高学
孙馨愉
谢政军
曹丙强
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University of Jinan
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University of Jinan
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00Compounds of cobalt
    • C01G51/04Oxides; Hydroxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors [EDLCs]; Processes specially adapted for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their materials
    • H01G11/46Metal oxides, e.g. ruthenium oxide
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/04Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/10Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/16Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/16Pore diameter
    • C01P2006/17Pore diameter distribution
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/40Electric properties
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

Abstract

The invention belongs to the preparation fields of inorganic material, and in particular to a kind of one-dimensional porous nano threadiness cobaltosic oxide electrode material and preparation method thereof.The specific steps of this method are as follows: cobalt salt and nitrilotriacetic acid are dissolved in isopropanol and the mixed solution of deionized water, stirs, forms uniformly mixed solution;Above-mentioned uniformly mixed solution is placed in hydrothermal reaction kettle and is sealed, it is washed, be centrifugated out solid powder after hydro-thermal reaction, after vacuum drying, obtain predecessor;Obtained predecessor is subjected to high-temperature calcination in air atmosphere, is cooled to room temperature and one-dimensional porous nano threadiness cobaltosic oxide electrode material can be obtained.The one-dimensional porous nano threadiness cobaltosic oxide electrode material that this method is prepared has good continuity and shape is uniform, with high purity, when being used as electrode material for super capacitor, shows high specific capacitance and high rate performance.Preparation method of the present invention is simple, easily operated, reproducible.

Description

A kind of one-dimensional porous nano threadiness cobaltosic oxide electrode material and preparation method thereof
Technical field
The invention belongs to the preparation fields of inorganic material, and in particular to a kind of one-dimensional porous nano threadiness cobaltosic oxide electricity Pole material and preparation method thereof.
Background technique
Supercapacitor is excellent with its service life is long, charging rate is fast, power density is high etc. as a kind of important energy storage device Point causes the broad interest of people.Supercapacitor can be by carrying out ionic adsorption or reversible farad in surface of active material Redox reaction carrys out storage energy, power supply system, hybrid vehicle, commercial scale electric power and in terms of All there is very big application potential.From the angle of material, electrode material for super capacitor is broadly divided into three classes: carbon material, Metal oxide/hydroxide and conducting polymer.Wherein metal oxide or hydroxylcontaining materials are than conducting polymer and carbon substrate Expect that the specific capacitance generated is higher and is concerned.
In various transition metal oxides, Co3O4Because its is at low cost, redox active is good, theoretical specific capacitance is high (3560 F g−1) and be considered as most attraction one of material.However, in actual measurement, Co3O4Specific capacitance distance There are also a certain distance for theoretical specific capacitance.The pattern on nanoscale is controlled by different preparation methods, is reduced with reaching Size and the effect for increasing specific surface area, can effectively obtain more active sites, improve its specific capacitance and improve multiplying power Performance.In addition, one-dimensional porous material, can not only increase effective contact area, but also be conducive to electron-transport.Therefore, it develops A kind of novel one-dimensional porous nano threadiness cobaltosic oxide electrode material and its technology of preparing have important scientific meaning.
Summary of the invention
The purpose of the present invention is to provide a kind of one-dimensional porous nano threadiness cobaltosic oxide electrode material and its preparation sides Method, the preparation method is simple, easily operated, reproducible, and the prepared cobaltosic oxide for obtaining one-dimensional porous nano threadiness connects Excellent performance is shown in the application that continuous property is good, shape is uniform, with high purity and in supercapacitor.
Technical solution proposed by the present invention:
A kind of one-dimensional porous nano threadiness cobaltosic oxide electrode material and preparation method thereof, it is characterised in that use following step It is rapid:
(1) cobalt salt and nitrilotriacetic acid are dissolved in isopropanol and the mixed solution of deionized water, stir 30min, formed Uniformly mixed solution;Wherein, the concentration of cobalt salt in the solution is 0.05-0.2mol/L, and nitrilotriacetic acid is in the solution Concentration is 0.1-0.3mol/L;The volume ratio of isopropanol and deionized water is 1:4-4:1;
(2) the uniformly mixed solution that step (1) obtains is placed in hydrothermal reaction kettle and is sealed, react 12-at 150-200 DEG C 36h, after reaction, cooled to room temperature are centrifuged out solid powder, and washing after vacuum drying, obtains forerunner Object;
(3) predecessor that step (2) obtains is calcined in air atmosphere, is heated to the heating rate of 0.5-10 DEG C/min 300-500 DEG C, 0.2-4h is calcined, is cooled to room temperature up to one-dimensional porous nano threadiness cobaltosic oxide electrode material.
Preferably, cobalt salt as described in step (1) is cobalt chloride, cobalt nitrate, cobaltous sulfate or cobalt acetate.
Preferably, the concentration of cobalt salt as described in step (1) in the solution is 0.173mol/L, and nitrilotriacetic acid is molten Concentration in liquid is 0.118mol/L.
Preferably, isopropanol as described in step (1) and deionized water volume ratio are 3:1.
Preferably, mixed solution described in step (2), which is placed in hydrothermal reaction kettle, seals, hydrothermal condition 180 DEG C reaction for 24 hours.
Preferably, heating rate described in step (3) is 1 DEG C/min, and calcination temperature is 350 DEG C, and calcination time is 0.5h。
Beneficial effect
(1) present invention is prepared for a kind of one-dimensional porous nano threadiness cobaltosic oxide electrode material using hydro-thermal and calcination method, leads to The concentration of cobalt salt, nitrilotriacetic acid, isopropanol and deionized water volume ratio and hydrothermal temperature and time are overregulated, Make one-dimensional porous nano threadiness cobaltosic oxide electrode material it is continuous, uniformly, large specific surface area, to provide more active sites Point;
(2) preparation method simple process of the present invention, easily operated, reproducible, product purity height, in the application of supercapacitor In show excellent performance, specific capacitance is high, good rate capability.
Detailed description of the invention
Fig. 1 is one-dimensional porous nano threadiness Co prepared by the embodiment of the present invention 13O4Scanning electron microscope (SEM) shine Piece;
Fig. 2 is one-dimensional porous nano threadiness Co prepared by the embodiment of the present invention 13O4Transmission electron microscope (TEM) photo;
Fig. 3 is one-dimensional porous nano threadiness Co prepared by the embodiment of the present invention 13O4X-ray diffraction (XRD) map;
Fig. 4 is one-dimensional porous nano threadiness Co prepared by the embodiment of the present invention 13O4N2 adsorption and pore size distribution curve;
Fig. 5 is one-dimensional porous nano threadiness Co prepared by the embodiment of the present invention 13O4The high rate performance figure of electrode.
Specific embodiment
It is set forth below that examples illustrate the present invention, but the invention is not limited to these embodiments.
Embodiment 1
6.9mmol cobalt chloride and 4.7mmol nitrilotriacetic acid are dissolved in the mixing of 30mL isopropanol and 10mL deionized water In solution, homogeneous solution is stirred to get.Above-mentioned homogeneous solution is put into hydrothermal reaction kettle and is sealed, in 180 DEG C of insulation reactions 24h.Obtained product is washed with 20mL deionized water, is centrifuged out solid, above-mentioned washing process is in triplicate;? To solid in be added 20mL dehydrated alcohol washing, after vacuum drying, obtain predecessor.By obtained predecessor in air atmosphere In 350 DEG C of calcining 0.5h, heating rate be 1 DEG C/min, one-dimensional porous nano threadiness cobaltosic oxide electrode material can be obtained. By one-dimensional porous nano threadiness cobaltosic oxide prepared by the present invention and acetylene black and polytetrafluoroethylene (PTFE) (PVDF) respectively according to 8: The ratio of 1:1 mixes, fully dispersed after dropwise addition 2 pyrrolidones of N-methyl-(NMP) solution to be ground, and is ground into and is homogenized It is coated in nickel foam after material, drying.Slurry is uniformly pressed into 1 × 1cm under 20 MPa pressure2Nickel foam in, in vacuum Under the conditions of 80 DEG C drying 10 hours.It is working electrode, bubble by the electrode material of preparation in the electrochemical measurement of three-electrode system Foam nickel is to electrode, and Hg/HgO electrode is reference electrode, has carried out electrochemistry in the three-electrode system of 2 M KOH aqueous solutions It can test.Fig. 1 is one-dimensional porous nano threadiness Co manufactured in the present embodiment3O4SEM photograph, as can be seen from the figure prepare Cobaltosic oxide is one-dimensional porous nano linear structure.Fig. 2 is one-dimensional porous nano threadiness Co manufactured in the present embodiment3O4TEM Photo, the about 100-200nm of cobaltosic oxide diameter of the porous nano threadiness as can be seen from the figure prepared, by little particle group At.X-ray diffraction pattern (Fig. 3) demonstrates synthesized Co3O4For pure phase (JCPDS:42-1467).Fig. 4 is the present embodiment preparation One-dimensional porous nano threadiness Co3O4N2 adsorption and pore size distribution curve, wherein specific surface area is about 117.9 m2 g-1, hole Diameter size is mainly 17.5 nm, this illustrates one-dimensional porous nano threadiness Co3O4Electrode material has big specific surface area, therefore More active sites can be provided.Fig. 5 is the one-dimensional porous nano threadiness Co of this implementation preparation3O4High rate performance figure, in electric current Density is 1,2,5,10 and 20 A g-1When, specific capacitance is respectively 2853,2035,1455,1217 and 765 F g-1.It shows Good high rate performance illustrates the one-dimensional porous nano threadiness Co of preparation3O4Electrode material has very big in supercapacitor Application prospect.
Embodiment 2
5mmol cobalt nitrate and 10mmol nitrilotriacetic acid are dissolved in the mixed solution of 8mL isopropanol and 32mL deionized water In, stir to get homogeneous solution.Homogeneous solution obtained is put into hydrothermal reaction kettle and is sealed, in 200 DEG C of insulation reaction 36h. Obtained product is washed with 20mL deionized water, is centrifuged out solid, above-mentioned washing process is in triplicate;What is obtained consolidates The washing of 20mL dehydrated alcohol is added in body, after vacuum drying, obtains predecessor.By obtained predecessor 500 DEG C in air atmosphere 0.2h is calcined, heating rate is 10 DEG C/min to get cobaltosic oxide material.
Embodiment 3
2mmol cobalt acetate and 4mmol nitrilotriacetic acid are dissolved in the mixed solution of 32mL isopropanol and 8mL deionized water In, stir to get homogeneous solution.Homogeneous solution obtained is put into hydrothermal reaction kettle and is sealed, in 150 DEG C of insulation reaction 12h. Obtained product is washed with 20mL deionized water, is centrifuged out solid, in triplicate, what is obtained consolidates above-mentioned washing process The washing of 20mL dehydrated alcohol is added in body, after vacuum drying, obtains predecessor.By obtained predecessor 300 DEG C in air atmosphere 4h is calcined, heating rate is 5 DEG C/min to get cobaltosic oxide material.
Embodiment 4
8mmol cobaltous sulfate and 12mmol nitrilotriacetic acid are dissolved in the mixed solution of 20mL isopropanol and 20mL deionized water In, stir to get homogeneous solution.Homogeneous solution obtained is put into hydrothermal reaction kettle and is sealed, 200 DEG C of insulation reactions for 24 hours. Obtained product is washed with 20mL deionized water, is centrifuged out solid, in triplicate, what is obtained consolidates above-mentioned washing process The washing of 20mL dehydrated alcohol is added in body, after vacuum drying, obtains predecessor.By obtained predecessor 500 DEG C in air atmosphere 4h is calcined, heating rate is 5 DEG C/min to get cobaltosic oxide material.

Claims (6)

1. a kind of one-dimensional porous nano threadiness cobaltosic oxide electrode material and preparation method thereof, it is characterised in that use following step It is rapid:
(1) cobalt salt and nitrilotriacetic acid are dissolved in isopropanol and the mixed solution of deionized water, are stirred, it is equal to form mixing Even solution;Wherein, the concentration of cobalt salt in the solution is 0.05-0.2mol/L, and the concentration of nitrilotriacetic acid in the solution is 0.1—0.3mol/L;Isopropanol and deionized water volume ratio are 1:4-4:1;
(2) the uniformly mixed solution that step (1) obtains is placed in hydrothermal reaction kettle and is sealed, react 12-at 150-200 DEG C 36h, after reaction, cooled to room temperature are centrifuged out solid powder, washing, after vacuum drying, before can be obtained Drive object;
(3) predecessor that step (2) obtains is calcined in air atmosphere, is heated to the heating rate of 0.5-10 DEG C/min 300-500 DEG C, calcination time is 0.2-4h, is cooled to room temperature up to one-dimensional porous nano threadiness cobaltosic oxide electrode material Material.
2. a kind of one-dimensional porous nano threadiness cobaltosic oxide electrode material according to claim 1 and preparation method thereof, It is characterized in that cobalt salt as described in step (1) is selected from cobalt chloride, cobalt nitrate, cobaltous sulfate or cobalt acetate.
3. a kind of one-dimensional porous nano threadiness cobaltosic oxide electrode material according to claim 1 and preparation method thereof, It is characterized in that the volume ratio of isopropanol as described in step (1) and deionized water is 3:1.
4. a kind of one-dimensional porous nano threadiness cobaltosic oxide electrode material according to claim 1 and preparation method thereof, It is characterized in that the concentration of cobalt salt in the solution described in step (1) is 0.173mol/L, nitrilotriacetic acid is in the solution Concentration is 0.118mol/L.
5. a kind of one-dimensional porous nano threadiness cobaltosic oxide electrode material according to claim 1 and preparation method thereof, It is characterized in that solution uniformly mixed described in step (2) is placed in hydrothermal reaction kettle and seals, hydrothermal condition is 180 DEG C Reaction is for 24 hours.
6. a kind of one-dimensional porous nano threadiness cobaltosic oxide electrode material according to claim 1 and preparation method thereof, It is characterized in that heating rate described in step (3) is 1 DEG C/min, calcination temperature is 350 DEG C, calcination time 0.5h.
CN201811054174.0A 2018-09-11 2018-09-11 A kind of one-dimensional porous nano threadiness cobaltosic oxide electrode material and preparation method thereof Pending CN109231284A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109904001A (en) * 2019-04-10 2019-06-18 蚌埠学院 A kind of nano combined electrode material for super capacitor of nickel oxide/nickel and preparation method thereof
CN109904000A (en) * 2019-04-10 2019-06-18 蚌埠学院 A kind of preparation method and applications of the Ni-based complex electrode material of nanometer of threadiness

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CN105870440A (en) * 2016-04-22 2016-08-17 济南大学 Preparation method and application for bowknot-shaped cobaltosic oxide
CN106450288A (en) * 2016-11-04 2017-02-22 济南大学 Preparation method and application of porous cobalt oxide
CN107819125A (en) * 2017-11-02 2018-03-20 济南大学 A kind of preparation method of straw bundle shape cobaltosic oxide and its application in lithium ion battery
CN108110256A (en) * 2017-12-07 2018-06-01 成都新柯力化工科技有限公司 A kind of metal-nitrilotriacetic acid the composite negative pole material and preparation method of electricity lithium battery

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109904001A (en) * 2019-04-10 2019-06-18 蚌埠学院 A kind of nano combined electrode material for super capacitor of nickel oxide/nickel and preparation method thereof
CN109904000A (en) * 2019-04-10 2019-06-18 蚌埠学院 A kind of preparation method and applications of the Ni-based complex electrode material of nanometer of threadiness

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Application publication date: 20190118