CN108565436A - A kind of preparation method of spherical nickel molybdate/graphene composite material - Google Patents
A kind of preparation method of spherical nickel molybdate/graphene composite material Download PDFInfo
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- CN108565436A CN108565436A CN201810447452.2A CN201810447452A CN108565436A CN 108565436 A CN108565436 A CN 108565436A CN 201810447452 A CN201810447452 A CN 201810447452A CN 108565436 A CN108565436 A CN 108565436A
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- spherical nickel
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a kind of preparation methods of spherical nickel molybdate/graphene composite material.It is as follows：(1) by Ni (NO3)2·6H2O and MoCl5It is scattered in ethylene glycol solution simultaneously ultrasonic dissolution, obtains mixed solution；(2) ultrasonic disperse graphene oxide solution；(3) scattered graphene oxide solution is added in above-mentioned mixed solution and is uniformly mixed；(4) solution is placed in autoclave and is reacted；It filters and washs after reaction；(5) product after washing is freeze-dried；(6) the high-temperature sample calcination process after freeze-drying is obtained into spherical nickel molybdate/graphene composite material.The preparation method technological operation of the present invention is simple, and preparation efficiency is high, and raw material is relatively inexpensive.
Description
Technical field
Present invention relates particularly to field of material technology, more particularly to a kind of spherical nickel molybdate/graphene composite material
Preparation method.
Background technology
The energy and resource are the basic needs for driving human being's production life and pushing social development, in the 21st century, science
Technology development is swift and violent, however the rapid development of science and technology consumes many energy and resource, these usings energy source whiles brings
A series of problems, such as environmental pollution, and traditional energy is all non-renewable energy resources, by exploiting and consuming for a long time,
Through gradually starting exhaustion, cause traditional energy that cannot meet the needs of production and living, thus develop and utilize it is renewable, economical,
Environmental protection and clean energy resource (including wind energy, solar energy nuclear energy and tide energy etc.), improving energy utilization rate becomes energy industry urgently
It solves the problems, such as.Molybdic acid nickel material have high specific capacitance, abundance, cost is relatively low, advantages of environment protection, quilt it is believed that
It is very potential electrode material, gradually interested to researchers, foreground is very wide.
Molybdic acid nickel material is energy storage that is a kind of cheap and stablizing and energy converslon materials, but the electric conductivity of molybdic acid nickel material
Difference, and with magnetism so that serious agglomeration occurs for material.Current molybdic acid nickel electrode material there is also many problems,
If the actual specific capacitance of material is relatively low for theoretical value, be used as electrode material when service life cycle it is too short and times
Rate performance is not high.Nickel molybdate and graphene progress is compound, defect existing for single material can be made up, it is good to obtain pattern
Good, specific capacitance is big, the excellent electrode material of the uniform cycle performance of charge and discharge.Current nickel molybdate/graphene composite material is more
For sheet or rodlike.
Invention content
Preparation process in order to solve spherical nickel molybdate/graphene composite material in the prior art is high to equipment requirement, anti-
Answer the technical problems such as condition harshness, the purpose of the present invention is to provide a kind of spherical nickel molybdate that the pattern of simple possible is excellent/
The preparation method of graphene composite material.The preparation method avoids the use of strong acid and strong base, have it is environmental-friendly, it is easy to operate
Convenient, economic and practical is strong, and raw material is relatively inexpensive to be easy to get, and production cost is low, the advantages that can be applied to large-scale industrial production.
The technical proposal of the invention is realized in this way.
The present invention provides a kind of preparation method of spherical nickel molybdate/graphene composite material, is as follows：
(1) by Ni (NO3)2﹒ 6H2O、MoCl5It is scattered in ethylene glycol simultaneously ultrasonic dissolution with graphene oxide solution, is obtained
Mixed solution；
(2) mixed solution is placed in autoclave and is reacted, after reaction, be filtered successively, wash and
Freeze-drying；
(3) sample after freeze-drying is subjected to calcination process, obtains spherical nickel molybdate/graphene composite material.
In the present invention, in step (1), Ni (NO3)2﹒ 6H2O and MoCl5Molar ratio be 1:1~1:2；Ni(NO3)2﹒ 6H2O
Rate of charge with ethylene glycol is 1:3~1:10mol/L.
In the present invention, in step (1), a concentration of 0.8~2.2mg/ml of graphene oxide solution, graphene oxide solution
Volume ratio with ethylene glycol is 1:2~1:4.
In the present invention, in step (2), reaction temperature be 100~200 DEG C, the reaction time be 12~for 24 hours.
In the present invention, in step (3), calcination temperature is 400~1000 DEG C, and roasting time is 2~8h.
In the present invention, spherical nickel molybdate/graphene composite material obtained is spherical, grain size 0.5~2 μm it
Between.
Compared with existing scheme, the beneficial effects of the present invention are：Preparation process of the present invention is avoided using strong acid and strong base
It uses, has the characteristics that environmentally friendly, prepared spherical nickel molybdate/graphene composite material size is more uniform, operation letter
Just, economic and practical is strong for folk prescription, and raw material is relatively inexpensive to be easy to get, and production cost is low, has broad application prospects and market potential.
Description of the drawings
Fig. 1 is the SEM figures before spherical nickel molybdate/graphene composite material roasting prepared by embodiment 1.
Fig. 2 is the SEM figures after spherical nickel molybdate/graphene composite material roasting prepared by embodiment 2.
Specific implementation mode
Technical scheme of the present invention is further described with reference to specific embodiment, but the present invention is not limited to
Following embodiments.
Embodiment 1
A kind of preparation method of spherical nickel molybdate/graphene composite material, specifically includes following steps：
(1) 2mmol Ni (NO are weighed3)2﹒ 6H2O and 2mmol MoCl5It is added in beaker.
(2) graphene solution that 15ml ethylene glycol and a concentration of 1.0mg/ml of 5ml are measured with graduated cylinder is added to above-mentioned beaker
In.
(3) 30ml autoclaves are moved into after being dissolved with ultrasonic disperse, thermostatic drying chamber are then placed in, in 180 DEG C of conditions
Lower reaction is for 24 hours.
(4) after reaction, then cooled to room temperature removes product in centrifuge tube from autoclave, centrifugation
It is used in combination ethyl alcohol to wash 2-3 times.
(5) the good product of centrifugal treating is put in freeze drying box again and is freeze-dried.
(6) dried sample is finally transferred to tube furnace, under nitrogen atmosphere, 500 DEG C of roasting 2h obtain molybdic acid
Nickel/graphene composite material.Fig. 1 is the SEM figures before the spherical nickel molybdate/graphene composite material roasting prepared.The results show that
It is in spherical, and grain size is at 1~1.6 μm or so.
Embodiment 2
A kind of preparation method of spherical nickel molybdate/graphene composite material, specifically includes following steps：
(1) 1mmol Ni (NO are weighed3)2﹒ 6H2O and 2mmol MoCl5It is added in beaker.
(2) it is added to the graphene solution of graduated cylinder measurement 15ml ethylene glycol solutions and a concentration of 1.5mg/ml of 5ml above-mentioned
In beaker.
(3) 30ml autoclaves are moved into after being dissolved with ultrasonic disperse, thermostatic drying chamber are then placed in, in 160 DEG C of conditions
Lower reaction 18h.
(4) after reaction, then cooled to room temperature removes product in centrifuge tube from autoclave, centrifugation
It is used in combination ethyl alcohol to wash 2-3 times.
(5) the good product of centrifugal treating is put in freeze drying box again and is freeze-dried.
(6) dried sample is finally transferred to tube furnace, under nitrogen atmosphere, 600 DEG C of roasting 2h obtain molybdic acid
Nickel/graphene composite material.The results show that it is in spherical, grain size is at 0.8~1.4 μm or so.
Embodiment 3
A kind of preparation method of spherical nickel molybdate/graphene composite material, specifically includes following steps：
(1) 2mmol Ni (NO are weighed3)2﹒ 6H2O and 2mmol MoCl5It is added in beaker.
(2) it is added to the graphene solution of graduated cylinder measurement 15ml ethylene glycol solutions and a concentration of 1.2mg/ml of 5ml above-mentioned
In beaker.
(3) 30ml autoclaves are moved into after being dissolved with ultrasonic disperse, thermostatic drying chamber are then placed in, in 200 DEG C of conditions
Lower reaction 12h.
(4) after reaction, then cooled to room temperature removes product in centrifuge tube from autoclave, centrifugation
It is used in combination ethyl alcohol to wash 2-3 times.
(5) the good product of centrifugal treating is put in freeze drying box again and is freeze-dried.
(6) dried sample is finally transferred to tube furnace, under nitrogen atmosphere, 500 DEG C of roasting 4h obtain molybdic acid
Nickel/graphene composite material.The results show that it is in spherical, grain size is at 0.8~1.2 μm or so.
Embodiment 4
A kind of preparation method of spherical nickel molybdate/graphene composite material, specifically includes following steps：
(1) 1mmol Ni (NO are weighed3)2﹒ 6H2O and 2mmol MoCl5It is added in beaker.
(2) it is added to the graphene solution of graduated cylinder measurement 15ml ethylene glycol solutions and a concentration of 0.8mg/ml of 5ml above-mentioned
In beaker.
(3) 30ml autoclaves are moved into after being dissolved with ultrasonic disperse, thermostatic drying chamber are then placed in, in 140 DEG C of conditions
Lower reaction 20h.
(4) after reaction, then cooled to room temperature removes product in centrifuge tube from autoclave, centrifugation
It is used in combination ethyl alcohol to wash 2-3 times.
(5) the good product of centrifugal treating is put in freeze drying box again and is freeze-dried.
(6) dried sample is finally transferred to tube furnace, under nitrogen atmosphere, 600 DEG C of roasting 4h obtain molybdic acid
Nickel/graphene composite material.The results show that it is in spherical, grain size is at 1~1.8 μm or so.
Embodiment 5
A kind of preparation method of spherical nickel molybdate/graphene composite material, specifically includes following steps：
(1) 2mmol Ni (NO are weighed3)2﹒ 6H2O and 2mmol MoCl5It is added in beaker.
(2) graphene solution that 15ml ethylene glycol solutions and a concentration of 2mg/ml of 5ml are measured with graduated cylinder is added to above-mentioned burning
In cup.
(3) 30ml autoclaves are moved into after being dissolved with ultrasonic disperse, thermostatic drying chamber are then placed in, in 120 DEG C of conditions
Lower reaction 22h.
(4) after reaction, then cooled to room temperature removes product in centrifuge tube from autoclave, centrifugation
It is used in combination ethyl alcohol to wash 2-3 times.
(5) the good product of centrifugal treating is put in freeze drying box again and is freeze-dried.
(6) dried sample is finally transferred to tube furnace, under nitrogen atmosphere, 500 DEG C of roasting 4h obtain molybdic acid
Nickel/graphene composite material.The results show that it is in spherical, grain size is at 1.2~1.5 μm or so.
Being compared with traditional nickel molybdate/graphene composite material has more regular structure, and pattern can from SEM figures
Find out.Spherical nickel molybdate/graphene composite material size is more uniform, it can be seen that material is at uniform from scanning electron microscope (SEM) photograph
Chondritic, diameter are about 0.5~2 μm.The present invention is simple to operate, and economic and practical is strong, and raw material is relatively inexpensive to be easy to get, raw
It produces at low cost, has broad application prospects and market potential.
The above is only the basic explanation under present inventive concept, and that technical solution according to the present invention is done is any etc.
Effect transformation, is within the scope of protection of the invention.
Claims (6)
1. a kind of preparation method of spherical nickel molybdate/graphene composite material, which is characterized in that be as follows：
(1) by Ni (NO3)2﹒ 6H2O、MoCl5It is scattered in ethylene glycol simultaneously ultrasonic dissolution with graphene oxide solution, obtains mixing molten
Liquid；
(2) mixed solution is placed in autoclave and is reacted, after reaction, be filtered, wash and freeze successively
It is dry；
(3) sample after freeze-drying is subjected to calcination process, obtains spherical nickel molybdate/graphene composite material.
2. preparation method according to claim 1, which is characterized in that in step (1), Ni (NO3)2﹒ 6H2O and MoCl5Rub
You are than being 1:1~1:2；Ni(NO3)2﹒ 6H2O and the rate of charge of ethylene glycol are 1:3~1:10mol/L.
3. preparation method according to claim 1, which is characterized in that in step (1), graphene oxide solution it is a concentration of
The volume ratio of 0.8~2.2mg/ml, graphene oxide solution and ethylene glycol is 1:2~1:4.
4. preparation method according to claim 1, which is characterized in that in step (2), reaction temperature is 100~200 DEG C,
Reaction time be 12~for 24 hours.
5. preparation method according to claim 1, which is characterized in that in step (3), calcination temperature is 400~1000 DEG C,
Roasting time is 2~8h.
6. preparation method according to claim 1, which is characterized in that spherical nickel molybdate/graphene composite material obtained
It is spherical, grain size is between 0.5~2 μm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109243847A (en) * | 2018-10-25 | 2019-01-18 | 上海应用技术大学 | Three-dimensional ordered macroporous carbon-coated NiMoO4/ redox graphene nanocomposite of one kind and preparation method thereof |
| CN110428977A (en) * | 2019-07-16 | 2019-11-08 | 上海应用技术大学 | A kind of flower-shape Ni MoO4The preparation method and applications of graphene three-dimensional composite material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104752067A (en) * | 2015-03-27 | 2015-07-01 | 新疆大学 | Microwave-assisted method of nickel molybdate graphene composite material used for capacitor |
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2018
- 2018-05-11 CN CN201810447452.2A patent/CN108565436A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104752067A (en) * | 2015-03-27 | 2015-07-01 | 新疆大学 | Microwave-assisted method of nickel molybdate graphene composite material used for capacitor |
Non-Patent Citations (1)
| Title |
|---|
| LV JINLONG等: "A novel mesoporous NiMoO4@rGO nanostructure for supercapacitor applications", 《MATERIALS LETTERS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109243847A (en) * | 2018-10-25 | 2019-01-18 | 上海应用技术大学 | Three-dimensional ordered macroporous carbon-coated NiMoO4/ redox graphene nanocomposite of one kind and preparation method thereof |
| CN110428977A (en) * | 2019-07-16 | 2019-11-08 | 上海应用技术大学 | A kind of flower-shape Ni MoO4The preparation method and applications of graphene three-dimensional composite material |
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Application publication date: 20180921 |