CN103043729A - Cobalt molybdate-graphene nano compound and preparation method thereof - Google Patents
Cobalt molybdate-graphene nano compound and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a cobalt molybdate-graphene nano compound and a preparation method thereof. The method comprises steps of putting the oxidation graphite into water and ultrasonic dispersing; putting the cobalt salt into the system, stirring and dissolving; later putting the ammonium molybdate into the system and adjusting the pH; then transferring the mixture system into a water heating kettle to perform reaction; and when the reaction is ended, the product passes through separation, washing and dryness, and the cobalt molybdate-graphene nano compound is gained. The material is provided with broad application prospects in the field of energy and other electronic device fields.
Description
Technical field
The invention belongs to the Nano-composite materials field, specifically relate to a kind of take Graphene as propping material, and in the preparation method of finely dispersed cobalt molybdate nano particle, particularly cobalt molybdate-graphene nanometer composite of its surface deposition.This material has broad application prospects in the energy, sensing and other field of electronic devices.
Background technology
As the important member-cobalt molybdate of molybdate, because it has preferably chemical property, excellent stability has begun to be applied to the fields such as ultracapacitor, lithium ion battery.Up to the present, the research that cobalt molybdate is used for super capacitor also rarely has report.Wheat is vertical strong waits the method such as people's first passage " self-assembly-orientation overlap joint " at manganese molybdate nanometer rod grow cobalt molybdate and cobalt molybdate (Mai LiQiang, the Yang Fan of acquisition nano-scale, Zhao YunLong, Xu Xu, Xu Lin, Luo YanZhu, S Hierarchical MnMoO
4/ CoMoO
4Heterostructured nanowires with enhanced supercapacitor performance, Nature communications 2 (2011) 381).The method obtains the high area/volume ratio that material has, and is applied to electrical condenser, has obtained the electrode materials of the super capacitor of excellent performance.Graphene is SP
2The two-dimension graphite sheet that exists with an atomic thickness that the hydridization carbon atom forms according to honeycomb arrangement.Because its excellent electroconductibility (its electric transmission speed is than the fast decades of times of silicon), large specific surface area, thermal conductivity and mechanicalness etc. attract wide attention rapidly.Particularly owing to excellent conductivity and large specific surface area, Graphene is widely used in the research of ultracapacitor aspect.Both are compound to together, give full play to both advantages, thereby obtain the material of chemical property excellence, therefore prepare Graphene/cobalt molybdate matrix material very important, this material will be of great immediate significance and using value in ultracapacitor, lithium ion battery equal energy source field and other field of electronic devices.
Summary of the invention
The object of the present invention is to provide a kind of cobalt molybdate-graphene nanometer composite, and synthesis technique is simple, lower-cost hydrothermal method prepares the preparation method of cobalt molybdate-graphene nanocomposite material.
The technical solution that realizes the object of the invention is: a kind of cobalt molybdate-graphene nanometer composite, massfraction 5 ~ 50 wt% of Graphene in the described mixture.
A kind of preparation method of cobalt molybdate-graphene nanometer composite may further comprise the steps:
The first step gets graphene oxide solution with graphite oxide ultra-sonic dispersion in water;
Second step adds cobalt salt stirring and dissolving in the solution of the first step;
The 3rd step joined molybdate in the mixed solution of second step, and stirred, and regulated the pH value;
The 4th goes on foot, and the 3rd mixing solutions that goes on foot is transferred in the water heating kettle reacts;
In the 5th step, will obtain cobalt molybdate-graphene nanometer composite after the 4th also washing of step product filtering separation, the drying.
Ultrasonic time described in the step 1 is 60-120min, and described graphite oxide adopts the Hummer legal system standby.
Cobalt salt described in the step 2 is Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, Cobaltous diacetate, cobalt chloride or rose vitriol, and described churning time is 30-90min.
Molybdate described in the step 3 is ammonium paramolybdate, and the mol ratio of described molybdate and cobalt salt is 1:7, and churning time is 30-90min, described pH=6-11.
Temperature of reaction described in the step 4 is 140-200 ℃, and the described reaction times is 6-16h.
Massfraction 5 ~ 50 wt% of Graphene in cobalt molybdate-graphene nanocomposite material described in the step 5.
The present invention compared with prior art, its advantage is: (1) adopts Graphene is propping material, at the finely dispersed cobalt molybdate nano particle of its surface deposition, provides larger surface-area; (2) by hydro-thermal reaction, graphite oxide is reduced into Graphene, has avoided using other reductive agents, environmentally safe; (3) use the cobalt molybdate-Graphene of the present invention's preparation, combine the characteristic of Graphene and cobalt molybdate, can be at ultracapacitor, lithium ion battery equal energy source material, and there are preferably application prospect and economic benefit in the fields such as environment, life science.
Description of drawings
Accompanying drawing 2 is TEM photos (a-embodiment 1, b-embodiment 2, c-embodiment 3, d-embodiment 4, e-embodiment 5) of example 1-5 gained cobalt molybdate-graphene nanocomposite material of the present invention.
Accompanying drawing 3 is example 3 gained cobalt molybdate-Graphenes of the present invention (27 wt%) nano-complex (G/CoMoO
4-1) with pure CoMoO
4Cyclic voltammetric (a), alternating-current impedance (b), 0.5A/g constant current charge-discharge (c) and specific storage and sweep the graph of a relation (d) of speed.
Embodiment
By reference to the accompanying drawings 1, cobalt molybdate-Graphene (5 ~ 50 wt%) nano-complex, by the following steps preparation and get:
The first step with ultrasonic minute 60 ~ 120min during graphite oxide is in water, gets graphene oxide solution;
Second step adds Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES stirring and dissolving in the solution of the first step, churning time 30 ~ 90min;
The 3rd step joined ammonium paramolybdate (mol ratio of paramolybdate and cobalt salt is 1:7) in the mixed solution of second step, and stirs 30 ~ 90min, regulated pH(6-11) value;
The 4th goes on foot, and the 3rd mixing solutions that goes on foot is transferred in the water heating kettle reacts, and temperature of reaction is 140 ~ 200 ℃, reaction times 6 ~ 16h;
In the 5th step, will obtain cobalt molybdate-Graphene (5 ~ 50 wt%) nano-complex after the 4th also washing of step product filtering separation, the drying.
Embodiment 1:The preparation method of cobalt molybdate-Graphene of the present invention (50 wt%) nano-complex may further comprise the steps:
The first step adopts the standby graphite oxide of Hummer legal system.10 g Graphite Powder 99s are joined 80 ℃ Potassium Persulphate (5 g), in the concentrated sulfuric acid solution (15mL) of Vanadium Pentoxide in FLAKES (5g), preoxidation 6 hours, cool to room temperature filters afterwards, and washing is to neutral.The Graphite Powder 99 (10 g) of preoxidation joined in 0 ℃ the 230 mL concentrated sulfuric acid solutions, the potassium permanganate of careful adding 30g afterwards, afterwards in 35 ℃ of reaction 2h, 30% of adding 1L deionized water and 25mL hydrogen peroxide makes reaction terminating in the most backward reaction solution, filter, washing, dialysis makes graphite oxide; The graphite oxide of 80 mg is placed 80mL water ultra-sonic dispersion 120min;
Second step with stirring and dissolving in the solution of the 0.366mmol Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES adding the first step, stirs 50min;
The 3rd step joined the 0.052mmol ammonium paramolybdate in the mixed solution of second step, and stirred 90min, regulated pH=11 values;
The 4th goes on foot, and the 3rd mixing solutions that goes on foot is transferred in the water heating kettle reacts, and temperature of reaction is 160 ℃, reaction times 12h;
In the 5th step, will obtain cobalt molybdate-Graphene (50 wt%) nano-complex after the 4th also washing of step product filtering separation, the drying.Its TEM photo such as Fig. 2 a.
Embodiment 2:The preparation method of cobalt molybdate-Graphene of the present invention (42 wt%) nano-complex may further comprise the steps:
The first step, graphite oxide prepares with embodiment 1, and the graphite oxide of 80 mg is placed 80mL water ultra-sonic dispersion 60min;
Second step with stirring and dissolving in the solution of the 0.5mmol Cobaltous diacetate adding the first step, stirs 90min;
The 3rd step joined the 0.071mmol ammonium paramolybdate in the mixed solution of second step, and stirred 30min, regulated the pH=7 value;
The 4th goes on foot, and the 3rd mixing solutions that goes on foot is transferred in the water heating kettle reacts, and temperature of reaction is 140 ℃, reaction times 16h;
In the 5th step, will obtain cobalt molybdate-Graphene (42 wt%) nano-complex after the 4th also washing of step product filtering separation, the drying.Its TEM photo such as Fig. 2 b.
Embodiment 3:The preparation method of cobalt molybdate-Graphene of the present invention (27 wt%) nano-complex may further comprise the steps:
The first step, graphite oxide prepares with embodiment 1, and the graphite oxide of 80 mg is placed 80mL water ultra-sonic dispersion 90min;
Second step with stirring and dissolving in the solution of the 1mmol Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES adding the first step, stirs 40min;
The 3rd step joined the 0.142mmol ammonium paramolybdate in the mixed solution of second step, and stirred 60min, regulated the pH=7 value;
The 4th goes on foot, and the 3rd mixing solutions that goes on foot is transferred in the water heating kettle reacts, and temperature of reaction is 180 ℃, reaction times 12h;
In the 5th step, will obtain cobalt molybdate-Graphene (27 wt%) nano-complex after the 4th also washing of step product filtering separation, the drying.Its TEM photo such as Fig. 2 c.
The gained matrix material is labeled as G/CoMoO
4-1, as electrode materials, under the same test condition, the performance (accompanying drawing 3-c) of its electrochemistry cyclic voltammetric (accompanying drawing 3-a), alternating-current impedance (accompanying drawing 3-b), constant current charge-discharge and pure CoMoO
4Compare, higher ratio electric capacity, less internal resistance, longer discharge performance are arranged; The relation of its specific storage and scanning speed is shown in accompanying drawing 3-d.
Embodiment 4:The preparation method of cobalt molybdate-Graphene of the present invention (8 wt%) nano-complex may further comprise the steps:
The first step, graphite oxide prepares with embodiment 1, and the graphite oxide of 80 mg is placed 80mL water ultra-sonic dispersion 90min;
Second step with stirring and dissolving in the solution of the 4.203mmol rose vitriol adding the first step, stirs 90min;
The 3rd step joined the 0.6mmol ammonium paramolybdate in the mixed solution of second step, and stirred 70min, regulated the pH=9 value;
The 4th goes on foot, and the 3rd mixing solutions that goes on foot is transferred in the water heating kettle reacts, and temperature of reaction is 160 ℃, reaction times 14h;
In the 5th step, will obtain cobalt molybdate-Graphene (8 wt%) nano-complex after the 4th also washing of step product filtering separation, the drying.Its TEM photo such as Fig. 2 d.
Embodiment 5:The preparation method of cobalt molybdate-Graphene of the present invention (5 wt%) nano-complex may further comprise the steps:
The first step, graphite oxide prepares with embodiment 1, and the graphite oxide of 80 mg is placed 80mL water ultra-sonic dispersion 100min;
Second step with stirring and dissolving in the solution of the 6.945mmol cobalt chloride adding the first step, stirs 30min;
The 3rd step joined the 0.992mmol ammonium paramolybdate in the mixed solution of second step, and stirred 90min, regulated pH(pH=6) value;
The 4th goes on foot, and the 3rd mixing solutions that goes on foot is transferred in the water heating kettle reacts, and temperature of reaction is 200 ℃, reaction times 6h;
In the 5th step, will obtain cobalt molybdate-Graphene (5 wt%) nano-complex after the 4th also washing of step product filtering separation, the drying.Its TEM photo such as Fig. 2 d.
Claims (10)
1. cobalt molybdate-graphene nanometer composite is characterized in that massfraction 5 ~ 50 wt% of Graphene in the described mixture.
2. cobalt molybdate-graphene nanometer composite according to claim 1 is characterized in that described mixture prepares according to the following steps:
In the 1st step, graphite oxide ultra-sonic dispersion in water is got graphene oxide solution;
In the 2nd step, cobalt salt is added stirring and dissolving in the 1st solution that goes on foot;
The 3rd step joined molybdate in the mixed solution in the 2nd step, and stirred, and regulated the pH value;
The 4th goes on foot, and the 3rd mixing solutions that goes on foot is transferred in the water heating kettle reacts;
In the 5th step, will obtain cobalt molybdate-graphene nanometer composite after the 4th also washing of step product filtering separation, the drying.
3. described cobalt molybdate-graphene nanometer composite according to claim 2 is characterized in that the ultrasonic time described in the step 1 is 60-120min, and described graphite oxide adopts the Hummer legal system standby.
4. described cobalt molybdate-graphene nanometer composite according to claim 2 is characterized in that cobalt salt described in the step 2 is Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, Cobaltous diacetate, cobalt chloride or rose vitriol, and described churning time is 30-90min.
5. described cobalt molybdate-graphene nanometer composite according to claim 2 is characterized in that the molybdate described in the step 3 is ammonium paramolybdate, and the mol ratio of described molybdate and cobalt salt is 1:7, and churning time is 30-90min, described pH=6-11.
6. described cobalt molybdate-graphene nanometer composite according to claim 2 is characterized in that the temperature of reaction described in the step 4 is 140-200 ℃, and the described reaction times is 6-16h.
7. the preparation method of a cobalt molybdate-graphene nanometer composite is characterized in that said method comprising the steps of:
The first step gets graphene oxide solution with ultra-sonic dispersion during graphite oxide is in water;
Second step adds cobalt salt stirring and dissolving in the solution of the first step;
The 3rd step joined molybdate in the mixed solution of second step, and stirred, and regulated the pH value;
The 4th goes on foot, and the 3rd mixing solutions that goes on foot is transferred in the water heating kettle reacts;
In the 5th step, will obtain cobalt molybdate-graphene nanometer composite after the 4th also washing of step product filtering separation, the drying.
8. the preparation method of cobalt molybdate-graphene nanometer composite according to claim 7 is characterized in that the ultrasonic time described in the step 1 is 60-120min, and described graphite oxide adopts the Hummer legal system standby.
9. the preparation method of cobalt molybdate-graphene nanometer composite according to claim 7 is characterized in that cobalt salt described in the step 2 is Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, Cobaltous diacetate, cobalt chloride or rose vitriol, and described churning time is 30-90min; Molybdate described in the step 3 is ammonium paramolybdate, and the mol ratio of described molybdate and cobalt salt is 1:7, and churning time is 30-90min, described pH=6-11; Temperature of reaction described in the step 4 is 140-200 ℃, and the described reaction times is 6-16h.
10. the preparation method of cobalt molybdate-graphene nanometer composite according to claim 7 is characterized in that massfraction 5 ~ 50 wt% of Graphene in the cobalt molybdate-graphene nanocomposite material described in the step 5.
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| CN103539210A (en) * | 2013-10-30 | 2014-01-29 | 渤海大学 | Preparation method of cobalt molybdate microcrystals |
| CN103779105A (en) * | 2014-02-12 | 2014-05-07 | 东华大学 | Method for preparing nickel molybdate and graphene nanocomposite |
| CN103811189A (en) * | 2014-02-12 | 2014-05-21 | 东华大学 | Preparation method of cobalt molybdate and graphene nanocomposite |
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