CN104971747A - Production method of high stability CoSe2 / graphene composite electrode material - Google Patents
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Abstract
The invention discloses a production method of a high stability CoSe2 / graphene composite electrode material. The method comprises the steps: (1), synthesis of graphene oxide; (2) preparation of a cobalt hydroxide and graphene oxide mixed sol; (3) constant temperature vacuum aging; and (4) preparation of a CoSe2 / graphene composite electrode material. The present invention has the advantages of: (1), according to the above preparation method, CoSe2 is uniformly loaded on the graphene surface to achieve synthesis of a high stability CoSe2 / graphene composite electrode material; (2) the synthesis process is simple and easy to operate, and has mild conditions and low cost of raw materials; (3) compared with the existing non-noble metal electrode material, the CoSe2 / graphene composite electrode material prepared by the present invention has high efficiency electro-catalytic activity; and (4), the CoSe2 / graphene composite electrode material prepared by the present invention has good crystallinity, high stability and strong resistance to poison. The high stability CoSe2 / graphene composite electrode material can be used as a cathode catalyst for a polymer electrolyte membrane (PEMFC) fuel cell, has significantly increased catalytic activity in acid medium, reduces catalyst costs, and significantly enhances battery performance.
Description
Technical field
The present invention relates to field of composite material preparation, be specifically related to a kind of high stability CoSe
2the preparation method of/graphene combination electrode material.
Background technology
Graphene is the lattice structure new material be made up of planar monolayer carbon atom, is to be rolled into fullerene, to be curled into CNT and to be piled into the elementary cell of other carbon allotropes such as graphite.Graphene has that specific area is large, conductive capability is strong and stability advantages of higher, and as Pt/ graphen catalyst prepared by carrier, resistance to corrosion is strong, electrical conductivity performance is good, electro catalytic activity is high, is excellent fuel battery cathod catalyst.But, Pt metal resource scarcity, expensive, become the bottleneck of restriction PEMFC large-scale production.Therefore, study cheap, that catalytic activity is high non-precious metal catalyst and become the important goal promoting PEMFC development.In numerous non-precious metal catalyst, high, selective strong, the good stability of Transition-metal dichalcogenide oxygen reduction catalytic activity in acid medium, and cheap, be expected to the alternative materials becoming Pt catalyst.Co-Se compound is as a kind of Transition-metal dichalcogenide, and the price cheap with it and good catalytic performance, become the study hotspot that cathodic oxygen reduction catalyst one is new, is the up-and-coming PEMFC cathode catalyst material of a class.The Co-Se with premium properties of exploration synthesizing new and graphene composite material are the hot fields of Chinese scholars research always.
The synthetic method of Co-Se and graphene composite material mainly contains solid phase method, solvent-thermal method, low temperature reflux method, and each method has different features, can adopt different synthetic methods according to the requirement of product property.At present adopt solvent structure Co-Se and graphene composite material more, first utilize reducing agent that graphite oxide is reduced to Graphene, subsequently selenium and cobalt compound and Graphene are added solvent, solvent-thermal process Co-Se and graphene composite material.Co-Se and the graphene composite material of the synthesis of this method have good performance, but technique relative complex, and Co-Se particle crystallization is bad, as electrode material poor stability and catalytic activity not high, be unfavorable for large-scale production and application.Comprehensive above analysis, by the simple method of one, obtaining having good crystallinity, the Co-Se of high stability and high catalytic activity and graphene combination electrode material, is the work having important scientific meaning.
Summary of the invention
The object of the invention is to provide a kind of high stability CoSe
2the preparation method of/graphene combination electrode material, solves prior art and prepares CoSe
2the expensive catalyst existed with graphene combination electrode material, poor stability and catalytic activity are not high, particle crystallization is bad, the inconvenient control of reaction ratio and complex process problem.
Technical scheme of the present invention is for achieving the above object, a kind of high stability CoSe
2the preparation method of/graphene combination electrode material, comprises the following steps:
One, the synthesis of graphene oxide: precise 200mg graphite oxide, is scattered in 100mL glucose solution, and through ultrasonic, centrifugation, collects supernatant liquor, i.e. obtained graphene oxide solution;
Two, the mixed sols of cobalt hydroxide and graphene oxide is prepared: measure 10 ~ 15mL ethylene glycol, drip 1.0 ~ 2.5mL low concentration ammoniacal liquor, at the uniform velocity stir, after a certain amount of cobalt acetate is dissolved in graphene oxide solution, dropwise join in ethylene glycol, control temperature is at 60 ~ 75 DEG C, and continuous gradient at the uniform velocity stirs 0.5 ~ 1.5 hour, namely forms uniform cobalt hydroxide and graphene oxide mixed sols;
Three, constant-temperature vacuum ageing: vacuum ageing 5 ~ 10h, control temperature is at 30 ~ 60 DEG C, and vacuum is 70Pa;
Four, CoSe is prepared
2/ graphene combination electrode material: the mixed sols obtained in step 3 is joined in hydrothermal reaction kettle, add a certain amount of selenium powder again, drip the sodium hydroxide solution of 4 ~ 6mL, control cobalt acetate and selenium powder amount of substance are than being 1:2, and after being sealed by reactor, temperature control was 160 ~ 180 DEG C of reactions 12 hours, filtration under diminished pressure, washing, vacuum drying, namely obtains high stability CoSe
2/ graphene combination electrode material.
The concentration of described glucose solution is 1.0 ~ 2.0mol/L, under 40 ~ 50kHz frequency ultrasonic 20 minutes; Centrifugation rate controls at 7000r/min.
Described concentration of sodium hydroxide solution is 4mol/L.
The speed that described continuous gradient at the uniform velocity stirs is 100 ~ 250r/min.
Advantage of the present invention: one, adopt above-mentioned preparation method, CoSe
2uniform load, at graphenic surface, achieves high stability CoSe
2the synthesis of/graphene combination electrode material; Two, synthesis technique is simple to operation, mild condition, and cost of material is low; Three, the CoSe for preparing of the present invention
2/ graphene combination electrode material, compared with existing base metal electrode material, has efficient electric catalytic activity; Four, the CoSe for preparing of the present invention
2/ graphene combination electrode material, good crystallinity, stability is high, and the resistance to ability of poisoning is strong.High stability CoSe prepared by the present invention
2/ graphene combination electrode material, be applicable to the cathod catalyst as polymer dielectric film (PEMFC) fuel cell, in acid medium, catalytic activity significantly improves, and catalyst cost reduces, and battery performance obviously strengthens.
Accompanying drawing explanation
A kind of high stability CoSe that Fig. 1, Fig. 2, Fig. 3 are embodiment 1 respectively, embodiment 2 and embodiment 3 obtain
2/ graphene combination electrode material XRD figure.
Detailed description of the invention
For a better understanding of the present invention, below by accompanying drawing and specific embodiment, technical scheme of the present invention is described.
embodiment 1:a kind of high stability CoSe
2the preparation method of/graphene combination electrode material, specifically completes according to the following steps:
One, the synthesis of graphene oxide: precise 200mg graphite oxide, is scattered in 100mL glucose solution, and through ultrasonic, centrifugation, collects supernatant liquor, i.e. obtained graphene oxide solution;
Two, the mixed sols of cobalt hydroxide and graphene oxide is prepared: measure 10mL ethylene glycol, drip 1.0mL low concentration ammoniacal liquor, at the uniform velocity stir, after a certain amount of cobalt acetate is dissolved in graphene oxide solution, dropwise join in ethylene glycol, at 75 DEG C, continuous gradient at the uniform velocity stirs 1.5 hours, namely forms uniform cobalt hydroxide and graphene oxide mixed sols;
Three, constant-temperature vacuum ageing: vacuum ageing 5h, control temperature 30 DEG C, vacuum is 70Pa;
Four, CoSe is prepared
2/ graphene combination electrode material: the mixed sols obtained in step 3 is joined in hydrothermal reaction kettle, add a certain amount of selenium powder again, drip the sodium hydroxide solution of 4mL, control cobalt acetate and selenium powder amount of substance are than being 1:2, and after being sealed by reactor, temperature control was 160 DEG C of reactions 12 hours, filtration under diminished pressure, washing, vacuum drying, namely obtains high stability CoSe
2/ graphene combination electrode material;
The cobalt acetate quality added in the present embodiment is 0.5g, and selenium powder is 0.32g;
In the present embodiment, continuous gradient at the uniform velocity stirs and is: first 100r/min stirs 30min, then 150r/min stirs 60min;
To the CoSe that the present embodiment obtains
2/ graphene composite material carries out XRD test, obtains XRD as shown in Figure 1, CoSe
2diffraction maximum obvious, by the known CoSe of diffraction peak intensity
2good crystallinity.
embodiment2: a kind of high stability CoSe
2the preparation method of/graphene combination electrode material, specifically completes according to the following steps:
One, the synthesis of graphene oxide: precise 200mg graphite oxide, is scattered in 100mL glucose solution, and through ultrasonic, centrifugation, collects supernatant liquor, i.e. obtained graphene oxide solution;
Two, the mixed sols of cobalt hydroxide and graphene oxide is prepared: measure 12mL ethylene glycol, drip 1.2mL low concentration ammoniacal liquor, at the uniform velocity stir, after a certain amount of cobalt acetate is dissolved in graphene oxide solution, dropwise join in ethylene glycol, at 75 DEG C, continuous gradient at the uniform velocity stirs 1.0 hours, namely forms uniform cobalt hydroxide and graphene oxide mixed sols;
Three, constant-temperature vacuum ageing: vacuum ageing 8h, control temperature 45 DEG C, vacuum is 70Pa;
Four, CoSe is prepared
2/ graphene combination electrode material: join in hydrothermal reaction kettle by the mixed sols obtained in step 3, add a certain amount of selenium powder again, drip the strong caustic of 5mL, control cobalt acetate and selenium powder amount of substance are than being 1:2, and after being sealed by reactor, temperature control was 170 DEG C of reactions 12 hours, filtration under diminished pressure, washing, vacuum drying, namely obtains high stability CoSe
2/ graphene combination electrode material.
The cobalt acetate quality added in the present embodiment is 1.0g, and selenium powder is 0.64g.
In the present embodiment, continuous gradient at the uniform velocity stirs and is: first 120r/min stirs 20min, then 180r/min stirs 40min.
To the CoSe that the present embodiment obtains
2carry out XRD test with graphene composite material, obtain XRD as shown in Figure 2, CoSe
2diffraction maximum obvious, by the known CoSe of diffraction peak intensity
2good crystallinity.
embodiment3: a kind of high stability CoSe
2the preparation method of/graphene combination electrode material, specifically completes according to the following steps:
One, the synthesis of graphene oxide: precise 200mg graphite oxide, is scattered in 100mL glucose solution, and through ultrasonic, centrifugation, collects supernatant liquor, i.e. obtained graphene oxide solution;
Two, the mixed sols of cobalt hydroxide and graphene oxide is prepared: measure 15mL ethylene glycol, drip 2.5mL low concentration ammoniacal liquor, at the uniform velocity stir, after a certain amount of cobalt acetate is dissolved in graphene oxide solution, dropwise join in ethylene glycol, at 72 DEG C, continuous gradient at the uniform velocity stirs 0.5 hour, namely forms uniform cobalt hydroxide and graphene oxide mixed sols;
Three, constant-temperature vacuum ageing: vacuum ageing 9h, control temperature 60 DEG C, vacuum is 70Pa;
Four, CoSe is prepared
2/ graphene combination electrode material: the mixed sols obtained in step 3 is joined in hydrothermal reaction kettle, add a certain amount of selenium powder again, drip the sodium hydroxide solution of 6mL, control cobalt acetate and selenium powder amount of substance are than being 1:2, and after being sealed by reactor, temperature control was 180 DEG C of reactions 12 hours, filtration under diminished pressure, washing, vacuum drying, namely obtains high stability CoSe
2/ graphene combination electrode material.
The cobalt acetate quality added in the present embodiment is 1.5g, and selenium powder is 0.96g.
In the present embodiment, continuous gradient at the uniform velocity stirs and is: first 130r/min stirs 10min, then 250r/min stirs 20min.
To the CoSe that the present embodiment obtains
2carry out XRD test with graphene composite material, obtain XRD as shown in Figure 3, CoSe
2xRD diffraction maximum obvious, by the known CoSe of diffraction peak intensity
2good crystallinity.
Claims (4)
1. a high stability CoSe
2the preparation method of/graphene combination electrode material, is characterized in that: described preparation method comprises the steps:
One, the synthesis of graphene oxide: precise 200mg graphite oxide, is scattered in 100mL glucose solution, and through ultrasonic, centrifugation, collects supernatant liquor, i.e. obtained graphene oxide solution;
Two, the mixed sols of cobalt hydroxide and graphene oxide is prepared: measure 10 ~ 15mL ethylene glycol, drip 1.0 ~ 2.5mL low concentration ammoniacal liquor, at the uniform velocity stir, after a certain amount of cobalt acetate is dissolved in graphene oxide solution, dropwise join in ethylene glycol, at 60 ~ 75 DEG C, continuous gradient at the uniform velocity stirs 0.5 ~ 1.5 hour, namely forms uniform cobalt hydroxide and graphene oxide mixed sols;
Three, constant-temperature vacuum ageing: vacuum ageing 5 ~ 10h, control temperature 30 ~ 60 DEG C, vacuum is 70Pa;
Four, CoSe is prepared
2/ graphene combination electrode material: the mixed sols obtained in step 3 is joined in hydrothermal reaction kettle, add a certain amount of selenium powder again, drip 4 ~ 6mL sodium hydroxide solution, control cobalt acetate and selenium powder amount of substance are than being 1:2, and after being sealed by reactor, temperature control was 160 ~ 180 DEG C of reactions 12 hours, filtration under diminished pressure, washing, vacuum drying, namely obtains high stability CoSe
2/ graphene combination electrode material.
2. a kind of high stability CoSe according to claim 1
2the preparation method of/graphene combination electrode material, is characterized in that: the concentration of glucose solution is 1.0 ~ 2.0mol/L, under 40 ~ 50kHz frequency ultrasonic 20 minutes; Centrifugation rate controls at 7000r/min.
3. a kind of high stability CoSe according to claim 1
2the preparation method of/graphene combination electrode material, is characterized in that: concentration of sodium hydroxide solution is 4mol/L.
4. a kind of high stability CoSe according to claim 1
2the preparation method of/graphene combination electrode material, is characterized in that: the speed that continuous gradient at the uniform velocity stirs is 100 ~ 250r/min.
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Cited By (18)
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| CN105428647A (en) * | 2015-11-14 | 2016-03-23 | 华中科技大学 | Cobalt diselenide/carbon nanomaterial, preparation method therefor and application thereof |
| CN105552392A (en) * | 2016-01-06 | 2016-05-04 | 复旦大学 | Cobalt diselenide/graphite carbon composite material, namely oxygen reduction catalyst, and preparation method thereof |
| CN105789584A (en) * | 2016-03-27 | 2016-07-20 | 华南理工大学 | Cobalt selenide/carbon sodium ion battery composite negative electrode material as well as preparation method and application of cobalt selenide/carbon-sodium ion battery composite negative electrode material |
| CN106237791A (en) * | 2016-09-06 | 2016-12-21 | 中南大学 | The method that nitrogen resource is reclaimed in the efficient complexed absorption of a kind of NO/electro-catalysis reduction |
| CN106492846A (en) * | 2016-10-12 | 2017-03-15 | 吉林大学 | One kind efficiently cracks low overpotential elctro-catalyst of Aquatic product hydrogen and preparation method thereof |
| CN106710888A (en) * | 2017-02-14 | 2017-05-24 | 安聪聪 | Cobalt selenide/graphene composite nanometer material, preparation of nanometer material and supercapacitor |
| CN108374179A (en) * | 2018-02-07 | 2018-08-07 | 浙江大学 | A kind of preparation method and application of the compound nitrogen-doped carbon material of two cobaltous selenide of Fe2O3 doping |
| CN108588751A (en) * | 2018-04-23 | 2018-09-28 | 山东大学 | Oxygen application is analysed in chalcogen cobalt-base catalyst, preparation method and electro-catalysis |
| CN108821247A (en) * | 2018-05-24 | 2018-11-16 | 北京科技大学 | A kind of kalium ion battery negative electrode material three-dimensional framework shape CoSe2The preparation method of electrode |
| CN109473643A (en) * | 2018-10-17 | 2019-03-15 | 长沙学院 | A kind of CoSe2/ graphene composite material preparation method and purposes |
| CN109962229A (en) * | 2019-04-16 | 2019-07-02 | 福州大学 | A kind of two cobaltous selenides of molybdenum doping sheet/graphene combination electrode material preparation method |
| CN110479320A (en) * | 2019-08-22 | 2019-11-22 | 内蒙古民族大学 | A kind of efficiently difunctional decomposition water power catalyst and preparation method thereof |
| CN110508298A (en) * | 2019-09-04 | 2019-11-29 | 温州涂屋信息科技有限公司 | A kind of AlOOH-CoSe2O compoiste material and its preparation method are analysed in electro-catalysis |
| CN111054418A (en) * | 2019-12-19 | 2020-04-24 | 中南大学 | Oxygen/hydrogen evolution two-dimensional cobalt monoxide @ cobalt diselenide @ nitrogen doped carbon nanotube/graphene dual-functional composite catalyst |
| CN111349915A (en) * | 2020-02-20 | 2020-06-30 | 齐鲁工业大学 | CoSe with controllable appearance2/Ti composite material and preparation method thereof |
| CN112018361A (en) * | 2020-08-31 | 2020-12-01 | 华中科技大学 | Carbon cloth loaded carbon coated cobalt selenide nanosheet battery cathode material and preparation thereof |
| CN113443663A (en) * | 2021-07-19 | 2021-09-28 | 黑龙江工程学院 | Preparation method of cobalt oxide/cobalt diselenide heterostructure loaded carbon-nitrogen-carbon four-composite material |
| CN114449695A (en) * | 2022-02-16 | 2022-05-06 | 鞍山炭素有限公司 | Ultrahigh-power graphite electrode |
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| CN105428647A (en) * | 2015-11-14 | 2016-03-23 | 华中科技大学 | Cobalt diselenide/carbon nanomaterial, preparation method therefor and application thereof |
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| CN105789584B (en) * | 2016-03-27 | 2019-05-14 | 华南理工大学 | A kind of cobaltous selenide/carbon sodium-ion battery composite negative pole material and the preparation method and application thereof |
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| CN109473643B (en) * | 2018-10-17 | 2021-06-25 | 长沙学院 | CoSe2Preparation method and application of graphene composite material |
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| CN112018361A (en) * | 2020-08-31 | 2020-12-01 | 华中科技大学 | Carbon cloth loaded carbon coated cobalt selenide nanosheet battery cathode material and preparation thereof |
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Application publication date: 20151014 |