CN102515147A - Method for preparing tri-metal tetra-oxide/graphene nanocomposite material - Google Patents
Method for preparing tri-metal tetra-oxide/graphene nanocomposite material Download PDFInfo
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- CN102515147A CN102515147A CN2011103742870A CN201110374287A CN102515147A CN 102515147 A CN102515147 A CN 102515147A CN 2011103742870 A CN2011103742870 A CN 2011103742870A CN 201110374287 A CN201110374287 A CN 201110374287A CN 102515147 A CN102515147 A CN 102515147A
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- salt
- water
- graphite oxide
- aqueous solution
- matrix material
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Abstract
The invention discloses a method for preparing a tri-metal tetra-oxide/graphene nanocomposite material. The method comprises the following steps: 1) ultrasonically oscillating, dissolving graphite oxide into water to prepare a graphite oxide aqueous solution, and continuously stirring at constant temperature of 90 DEG C; 2) dissolving a soluble bivalent M salt into the water to prepare an M-salt aqueous solution, dripping ammonia water after the M salt is totally dissolved to obtain a mixed solution; and mixing the mixed solution and the graphite oxide aqueous solution, preserving the heat at the constant temperature of 90 DEG C for 8 hours, repeatedly washing by distilled water, and drying. The manufacturing process is simple; the used equipment is simple; raw materials are low in cost; the production period is short; the specific surface area is large; and the sizes of particles are small, and the particles are uniformly distributed. The method is wide in application prospect in the fields of lithium batteries, super-capacitors, sensors, catalysts and the like.
Description
Technical field
The present invention relates to the preparation method of metal four oxidations three things/graphene nano matrix material, belong to the nano-functional material preparing technical field.
Background technology
In recent years; Nano material is a big focus of the research of field of materials, and especially 2004, two scientist An Delie Jim of Univ Manchester UK and the Ke Siteyanuowo Luo Fu that disappears had prepared in the world since the thinnest two dimensional surface material Graphene; The scientific circles that appear at of Graphene have evoked huge great waves; It is found that Graphene has excellent conductivity, heat conductivility, the intensity of superelevation and fabulous light transmission.
In field of compound material, Graphene is because great specific surface area, not only help second kind of material with the surface of Graphene as substrate, grow; And be convenient to the homodisperse of second kind of material; To obtain the matrix material of high-specific surface area; Such as being the Graphene/carbon nanotube composite materials of substrate grown carbon nanotube, with the Graphene Graphene/metal oxide composite of substrate grown metal oxide particle etc. with the Graphene.These are the matrix material of substrate with the Graphene, at the energy, and transmitter, fields such as catalyzer have demonstrated its powerful application prospect, become a big focus of current research.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of simple and general preparation metal four oxidations three things/graphene nano matrix material.
The preparation method of metal four oxidations three things of the present invention/graphene nano matrix material may further comprise the steps:
1) under the sonic oscillation, that graphite oxide is soluble in water, the preparation mass concentration is 0.1% ~ 0.2% the graphite oxide aqueous solution, in 90 ℃ of constant temperature, constantly stirs;
2) solubility divalence M salt is soluble in water, compound concentration is the M salt brine solution of 0.1 ~ 0.3mol/L, treat that M salt fully dissolves after; Dropping ammonia, the mol ratio of ammoniacal liquor and M salt is 6:1, obtains mixing solutions; After the graphite oxide aqueous solution with this mixing solutions and step 1),, use the zero(ppm) water repetitive scrubbing then 90 ℃ of constant temperature 8 hours; 80 ℃ of oven dry down obtain metal four oxidations three things/graphene nano matrix material.
Above-mentioned solubility divalence M salt can be Mn (NO
3)
2, Mn (Cl)
2, (CH
3COO)
2Mn, MnSO
4, Fe (NO
3)
2, Fe (Cl)
2, (CH
3COO)
2Fe, FeSO
4, Co (NO
3)
2, Co (Cl)
2, (CH
3COO)
2Co or CoSO
4
M of the present invention
3O
4/ graphene nano matrix material is substrate with the Graphene exactly, at Graphene surface growth M
3O
4Thereby nano particle obtains M
3O
4/ graphene nano matrix material.Its principle is: since the effect of electrostatic force, M
2+Be attracted near the graphite oxide functional group that has negative electricity, then M
2+Oxidized graphite oxidation is M
3O
4, and depend on the graphite oxide surface and grow, finally form M
3O
4Nano particle, in this process, graphite oxide also is reduced into simultaneously and is finally to obtain M by Graphene
3O
4/ graphene nano matrix material.
Advantage of the present invention is:
M of the present invention
3O
4/ graphene nano matrix material, at first with Graphene as substrate, it conducts electricity very well; Secondly the Graphene specific surface area is big, is convenient to a large amount of M
3O
4Nano particle is dispersed in its surface.Based on These characteristics, it is at lithium cell, ultracapacitor, and transmitter, fields such as catalyzer have application prospect.
Manufacture craft of the present invention is simple, and the equipment of use is simple, and the prices of raw and semifnished materials are cheap, and are with short production cycle, and specific surface area is big, and particle size is little and be evenly distributed.
Description of drawings
Fig. 1 is the SEM scanned photograph of metal four oxidations three things/graphene nano matrix material, and wherein a is Mn
3O
4/ graphene nano matrix material; B is Fe
3O
4/ graphene nano matrix material; C is Co
3O
4/ graphene nano matrix material.
Embodiment
Embodiment 1:
Take by weighing the 200mg graphite oxide, pour into and carried out supersound process in the beaker that fills 150ml zero(ppm) water 1 hour, it is dispersed in the aqueous solution, pour there-necked flask then into, it is heated to 90 ℃, and constantly stir with heating jacket.Take by weighing 1.225g (CH
3COOH)
2Mn4H
2O (0.005mol) pours in the beaker that fills 50ml zero(ppm) water, stirs and makes its dissolving, pours 10mlNH into
3H
2O (mass concentration 25%) is poured into mixing solutions in the above-mentioned there-necked flask then and handled 8 hours at 90 ℃ of constant temperature, and constantly stirs.At last gained solution is carried out a large amount of washings, vacuum drying obtains Mn at last
3O
4/ graphene nano matrix material, its SEM scanned photograph is seen Fig. 1 a.
Embodiment 2:
Take by weighing the 200mg graphite oxide, pour into and carried out supersound process in the beaker that fills 150ml zero(ppm) water 1 hour, it is dispersed in the aqueous solution, pour there-necked flask then into, it is heated to 90 ℃, and constantly stir with heating jacket.Take by weighing 4.17g FeSO
47H
2O (0.15mol) pours in the beaker that fills 50ml zero(ppm) water, stirs and makes its dissolving, pours 10mlNH into
3H
2O (concentration 25%) is poured into mixing solutions in the above-mentioned there-necked flask then and handled 8 hours at 90 ℃ of constant temperature, and constantly stirs.At last gained solution is carried out a large amount of washings, vacuum drying obtains Fe at last
3O
4/ graphene nano matrix material.Its SEM scanned photograph is seen Fig. 1 b.
Embodiment 3:
Take by weighing the 200mg graphite oxide, pour into and carried out supersound process in the beaker that fills 150ml zero(ppm) water 1 hour, it is dispersed in the aqueous solution, pour there-necked flask then into, it is heated to 90 ℃, and constantly stir with heating jacket.Take by weighing 2.91g Co (NO
3)
26H
2O (0.01mol) pours in the beaker that fills 50ml zero(ppm) water, stirs and makes its dissolving, pours 10mlNH into
3H
2O (concentration 25%) is poured into mixing solutions in the above-mentioned there-necked flask then and handled 8 hours at 90 ℃ of constant temperature, and constantly stirs.At last gained solution is carried out a large amount of washings, vacuum drying obtains Co at last
3O
4/ graphene nano matrix material, its SEM scanned photograph is seen Fig. 1 c.
Claims (2)
1. the preparation method of metal four oxidations three things/graphene nano matrix material is characterized in that may further comprise the steps:
1) under the sonic oscillation, that graphite oxide is soluble in water, the preparation mass concentration is 0.1% ~ 0.2% the graphite oxide aqueous solution, in 90 ℃ of constant temperature, constantly stirs;
2) solubility divalence M salt is soluble in water, compound concentration is the M salt brine solution of 0.1 ~ 0.3mol/L, treat that M salt fully dissolves after; Dropping ammonia, the mol ratio of ammoniacal liquor and M salt is 6:1, obtains mixing solutions; After the graphite oxide aqueous solution with this mixing solutions and step 1),, use the zero(ppm) water repetitive scrubbing then 90 ℃ of constant temperature 8 hours; 80 ℃ of oven dry down obtain metal four oxidations three things/graphene nano matrix material.
2. by the preparation method of described metal four oxidations of right 1 requirement three things/graphene nano matrix material, it is characterized in that described solubility divalence M salt is Mn (NO
3)
2, Mn (Cl)
2, (CH
3COO)
2Mn, MnSO
4, Fe (NO
3)
2, Fe (Cl)
2, (CH
3COO)
2Fe, FeSO
4, Co (NO
3)
2, Co (Cl)
2, (CH
3COO)
2Co or CoSO
4
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|---|---|---|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103022463A (en) * | 2012-12-20 | 2013-04-03 | 中国东方电气集团有限公司 | Manganese-based compound cathode material of lithium battery and preparation method of material |
| CN103450463A (en) * | 2013-08-28 | 2013-12-18 | 西北工业大学 | Preparation method of poly(3,4-ethylenedioxythiophene)/reduced graphene oxide/Co3O4 (PEDOT-RGO-Co3O4) nano wave-absorbing material |
| CN104036878A (en) * | 2014-06-24 | 2014-09-10 | 国家纳米科学中心 | Preparation method of graphene-carbon nanotube three-dimensional structure material |
| CN105244483A (en) * | 2015-09-16 | 2016-01-13 | 常州大学 | Preparation method modified manganese-based composite material used for lithium ion battery |
| CN109354073A (en) * | 2018-11-01 | 2019-02-19 | 黄爱强 | A kind of graphene paramagnetic resonance probe |
| CN109378455A (en) * | 2018-10-08 | 2019-02-22 | 西安交通大学 | A kind of classifying porous cobalt oxide nanosphere/graphene composite material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811696A (en) * | 2010-04-28 | 2010-08-25 | 东南大学 | Graphene-supported cobaltosic oxide nano composite material and preparation method thereof |
| CN101941842A (en) * | 2010-10-11 | 2011-01-12 | 东华大学 | Method for preparing graphene loaded ferroferric oxide magnetic nanometer particle composite material |
-
2011
- 2011-11-23 CN CN2011103742870A patent/CN102515147A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811696A (en) * | 2010-04-28 | 2010-08-25 | 东南大学 | Graphene-supported cobaltosic oxide nano composite material and preparation method thereof |
| CN101941842A (en) * | 2010-10-11 | 2011-01-12 | 东华大学 | Method for preparing graphene loaded ferroferric oxide magnetic nanometer particle composite material |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103022463A (en) * | 2012-12-20 | 2013-04-03 | 中国东方电气集团有限公司 | Manganese-based compound cathode material of lithium battery and preparation method of material |
| CN103450463A (en) * | 2013-08-28 | 2013-12-18 | 西北工业大学 | Preparation method of poly(3,4-ethylenedioxythiophene)/reduced graphene oxide/Co3O4 (PEDOT-RGO-Co3O4) nano wave-absorbing material |
| CN104036878A (en) * | 2014-06-24 | 2014-09-10 | 国家纳米科学中心 | Preparation method of graphene-carbon nanotube three-dimensional structure material |
| CN104036878B (en) * | 2014-06-24 | 2018-02-27 | 国家纳米科学中心 | A kind of preparation method of graphene and CNT three-dimensional structure material |
| CN105244483A (en) * | 2015-09-16 | 2016-01-13 | 常州大学 | Preparation method modified manganese-based composite material used for lithium ion battery |
| CN109378455A (en) * | 2018-10-08 | 2019-02-22 | 西安交通大学 | A kind of classifying porous cobalt oxide nanosphere/graphene composite material and preparation method thereof |
| CN109354073A (en) * | 2018-11-01 | 2019-02-19 | 黄爱强 | A kind of graphene paramagnetic resonance probe |
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Application publication date: 20120627 |