CN103811189B - A kind of cobalt molybdate and the preparation method of graphene nanocomposite material - Google Patents

A kind of cobalt molybdate and the preparation method of graphene nanocomposite material Download PDF

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Publication number
CN103811189B
CN103811189B CN201410048904.1A CN201410048904A CN103811189B CN 103811189 B CN103811189 B CN 103811189B CN 201410048904 A CN201410048904 A CN 201410048904A CN 103811189 B CN103811189 B CN 103811189B
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China
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deionized water
graphene
cobalt molybdate
graphene nanocomposite
nanocomposite
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CN201410048904.1A
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CN103811189A (en
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胡俊青
朝洁
徐开兵
刘倩
安磊
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东华大学
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Abstract

The present invention relates to the preparation method of a kind of cobalt molybdate and graphene nanocomposite material, including: (1) graphene oxide is scattered in deionized water, ultrasonic;(2) graphene oxide solution after ultrasonic completing adds CoCl2·6H2O and deionized water, stirring;(3) in above-mentioned solution, Na is added2MoO4·2H2O, continues stirring, is subsequently adding 120 180 DEG C of reaction 8 15h in reactor;(4), after reaction terminates, it is cooled to room temperature, centrifugal obtained product, respectively with deionized water and alcohol solvent washing, and it is dried, obtains cobalt molybdate and graphene nanocomposite material.The experimental technique of the present invention is simple to operation, environmentally safe, and cost is relatively low, is suitable to large-scale production.

Description

A kind of cobalt molybdate and the preparation method of graphene nanocomposite material

Technical field

The invention belongs to electrode material for super capacitor field, particularly to the system of a kind of cobalt molybdate Yu graphene nanocomposite material Preparation Method.

Background technology

In recent years, because of the ecological threat that minimizing and global warming bring day by day of the fossil energy deposits such as oil, people are devoted to Seek fungible energy source storage and conversion system.Big along with portable type electronic product (such as mobile phone, notebook computer etc.) Amount is emerged in large numbers and people's urgent needs to electric powered motor power supply, and the research and development of novel high-energy electrochmical power source was in recent years Developed rapidly.For portable type electronic product correlation technique and power system of electric automobile, there is high-energy-density, height The high energy storage system of safety and low cost becomes the most important thing.Therefore, it can be provided simultaneously with the super electricity of these excellent properties Container causes the extensive concern of researcher.

The electrode material being currently used for ultracapacitor mainly includes material with carbon element, conducting polymer and transition metal oxide three major types. CoMoO4Zeng Zuowei negative material is assembled into Study on Li-ion batteries and crosses its chemical property, it turned out that, its performance is original, But as being studied little for the electrode material of ultracapacitor.Research shows CoMoO4Though capacity less than MnMoO4, But its crystal structure compares MnMoO4Stable, good cyclical stability can be shown.Between the electrochemical behavior that it is outstanding, will It makes nano material can increase the contact area of electrode material and electrolyte, increases fast charging and discharging ability, can shorten simultaneously Ion deinsertion distance, can be effectively improved ultracapacitor cycle life.

As a kind of emerging material with carbon element, Graphene is because of the chemical property of its excellence, at energy field by researcher Extensive concern.Graphene has monoatomic layer thickness, and pole is beneficial to growth function nano material.By Graphene and oxo transition metal The compound cooperative effect that can produce of compound, improves the chemical property of composite, can significantly improve simple metal-oxide or Hydroxide is as the problem of electrode material cyclical stability difference.Currently, with respect to Graphene and CoMoO4Complex preparation method Research the most fewer.

Summary of the invention

The technical problem to be solved is to provide the preparation method of a kind of cobalt molybdate and graphene nanocomposite material, the party Method is simple to operation, environmentally safe, and cost is relatively low, is suitable to large-scale production.

A kind of cobalt molybdate of the present invention and the preparation method of graphene nanocomposite material, including:

(1) during graphene oxide is scattered in deionized water, ultrasonic;

(2) graphene oxide solution after ultrasonic completing adds CoCl2·6H2O and deionized water, stirring;

(3) in above-mentioned solution, Na is added2MoO4·2H2O, continues stirring, is subsequently adding 120-180 DEG C of reaction 8-15h in reactor;

(4), after reaction terminates, it is cooled to room temperature, centrifugal obtained product, respectively with deionized water and alcohol solvent washing, and do Dry, obtain cobalt molybdate and graphene nanocomposite material.

Graphene oxide and the amount ratio of deionized water in described step (1) are 10-30mg:5ml.

Ultrasonic time in described step (1) is 4-10h.

CoCl in described step (2)2·6H2The amount ratio of O, graphene oxide solution and deionized water is 1-4mmol:5ml: 40ml。

Na in described step (3)2MoO4·2H2O and CoCl2·6H2The amount ratio of O is 1-4mmol:1-4mmol.

Cobalt molybdate in described step (4) and graphene nanocomposite material are nanometer rods packed structures.

The present invention is (template) with Graphene as substrate, prepares this electrode material by hydro-thermal method simple, green, low cost.

Beneficial effect

(1) nano composite material that the present invention prepares is club shaped structure, can effectively suppress reunion and the improvement of graphene sheet layer CoMoO4Make the problem of cyclical stability difference during electrode material.

(2) the inventive method is simple to operation, environmental protection, low cost, solve graphene nanocomposite material at ultracapacitor The problem being difficult to scale application in industry.

Accompanying drawing explanation

Fig. 1 is cobalt molybdate and the graphene nanocomposite material SEM picture of embodiment 3 preparation in the present invention;

Fig. 2 is cobalt molybdate and the graphene nanocomposite material TEM picture of embodiment 3 preparation in the present invention;

Fig. 3 is cobalt molybdate and the graphene nanocomposite material XRD figure sheet of embodiment 3 preparation in the present invention.

Detailed description of the invention

Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments be merely to illustrate the present invention and not For limiting the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, those skilled in the art can To make various changes or modifications the present invention, these equivalent form of values fall within the application appended claims limited range equally.

Embodiment 1

(1) during 10mg graphene oxide is scattered in 5ml deionized water, ultrasonic 4h;

(2) graphene oxide solution after ultrasonic completing adds CoCl2·6H2O2mmol and deionized water 40ml, stirring 30min;

(3) in above-mentioned solution, Na is added2MoO4·2H2O2mmol, continues stirring 5h;Then move into 50ml politef anti- Answer in still, at 120 DEG C, react 15h;

(4), after reaction terminates, it is cooled to room temperature, centrifugal obtained product, respectively with deionized water and alcohol solvent washing, and do Dry.

Embodiment 2

(1) during 10mg graphene oxide is scattered in 5ml deionized water, ultrasonic 4h;

(2) graphene oxide solution after ultrasonic completing adds CoCl2·6H2O2mmol and deionized water 40ml, stirring 30min;

(3) in above-mentioned solution, Na is added2MoO4·2H2O2mmol, continues stirring 5h;Then move into 50ml politef anti- Answer in still, at 180 DEG C, react 15h;

(4), after reaction terminates, it is cooled to room temperature, centrifugal obtained product, respectively with deionized water and alcohol solvent washing, and do Dry.

Embodiment 3

(1) during 30mg graphene oxide is scattered in 5ml deionized water, ultrasonic 4h;

(2) graphene oxide solution after ultrasonic completing adds CoCl2·6H2O2mmol and deionized water 40ml, stirring 30min;

(3) in above-mentioned solution, Na is added2MoO4·2H2O2mmol, continues stirring 5h;Then move into 50ml politef anti- Answer in still, at 180 DEG C, react 15h.

(4), after reaction terminates, it is cooled to room temperature, centrifugal obtained product, respectively with deionized water and alcohol solvent washing, and do Dry.

Claims (5)

1. cobalt molybdate and a preparation method for graphene nanocomposite material, including:
(1) during graphene oxide is scattered in deionized water, ultrasonic;
(2) graphene oxide solution after ultrasonic completing adds CoCl2·6H2O and deionized water, stirring;
(3) in above-mentioned solution, Na is added2MoO4·2H2O, continues stirring, is subsequently adding 120-180 DEG C of reaction 8-15h in reactor;
(4), after reaction terminates, it is cooled to room temperature, centrifugal obtained product, respectively with deionized water and alcohol solvent washing, and do Dry, obtain cobalt molybdate and graphene nanocomposite material;Wherein, cobalt molybdate and graphene nanocomposite material are that nanometer rods is piled up Structure.
A kind of cobalt molybdate the most according to claim 1 and the preparation method of graphene nanocomposite material, it is characterised in that: described Graphene oxide and the amount ratio of deionized water in step (1) are 10-30mg:5ml.
A kind of cobalt molybdate the most according to claim 1 and the preparation method of graphene nanocomposite material, it is characterised in that: described Ultrasonic time in step (1) is 4-10h.
A kind of cobalt molybdate the most according to claim 1 and the preparation method of graphene nanocomposite material, it is characterised in that: described CoCl in step (2)2·6H2The amount ratio of O, graphene oxide solution and deionized water is 1-4mmol:5ml:40ml.
A kind of cobalt molybdate the most according to claim 1 and the preparation method of graphene nanocomposite material, it is characterised in that: described Na in step (3)2MoO4·2H2O and CoCl2·6H2The amount ratio of O is 1-4mmol:1-4mmol.
CN201410048904.1A 2014-02-12 2014-02-12 A kind of cobalt molybdate and the preparation method of graphene nanocomposite material CN103811189B (en)

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CN105810450A (en) * 2016-03-10 2016-07-27 同济大学 Method for synthesizing CoMoO4 loaded on foamed nickel electrode material through solvothermal method
CN106449143A (en) * 2016-10-31 2017-02-22 安徽工业大学 Preparing method of nickel-based lamellar double hydroxide/reduced graphene oxide supercapacitor electrode material
CN107195482A (en) * 2017-05-04 2017-09-22 华侨大学 A kind of nanometer rods array composite and its preparation method and application
CN107834045A (en) * 2017-11-02 2018-03-23 济南大学 A kind of preparation method of bar-shaped carbon coating cobalt molybdate and its application in lithium ion battery
CN108063258B (en) * 2017-12-26 2020-02-18 成都新柯力化工科技有限公司 Preparation method of binder for improving cycle stability of lithium battery silicon electrode
CN108314092B (en) * 2017-12-29 2020-10-23 安泰科技股份有限公司 Foam nickel loaded nano rod-shaped cobalt molybdate and preparation method and application thereof
CN108232157A (en) * 2018-01-04 2018-06-29 济南大学 A kind of carbon coating molybdic acid nickel electrode material and preparation method thereof
CN108380229B (en) * 2018-04-25 2019-03-22 华中农业大学 A kind of preparation method and products thereof of phosphorus doping cobalt molybdate Electrocatalytic Activity for Hydrogen Evolution Reaction agent
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