CN104801307A - Transition metal hydroxide-graphene oxide composite material as well as preparation and application thereof - Google Patents
Transition metal hydroxide-graphene oxide composite material as well as preparation and application thereof Download PDFInfo
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Abstract
The invention discloses a transition metal hydroxide-graphene oxide composite material. Transition metal hydroxide nano particles are loaded on a graphene oxide. The invention further discloses a preparation method of the composite material and application of the composite material to anodic oxygen evolution reaction of alkaline electrolyzed water. The preparation method comprises the following steps: (1) dispersing the graphene oxide in a solvent to form a suspension; (2) dissolving a transition metal source in the solvent to prepare a solution; (3) under the stirring condition, dropwise adding the solution obtained from the step (2) in the suspension obtained from the step (1); (4) dropwise adding an alkaline solution, reacting for 3-20 hours in stirring; (5) separating, washing and drying a sediment product obtained from the step (4) to obtain the composite material. The transition metal hydroxide nano particles which are uniform in size and are extremely small in grain size are loaded on the graphene oxide, so that the catalytic performance of the transition metal hydroxide is improved greatly.
Description
Technical field
The present invention relates to field of nanometer material technology, particularly relate to a kind of high capacity amount (material typically referring to more than 20% ratio disperses on another material), high dispersive transition metal hydroxide-graphene oxide composite and preparation method thereof and application.
Background technology
Graphene is a kind of by sp
2the carbon atom of hydridization forms the Two-dimensional Carbon material of periodic cellular shape with hexagonal array.The thickness of single-layer graphene is only 0.35nm.As novel nano material, Graphene to have under room temperature electron mobility (15000cm at a high speed
2/ (Vs)), its theoretical specific surface area is up to 2630m
2/ g, has good thermal conductivity (5000W/ (mK) and mechanical strength (130GPa).The character of these uniquenesses makes Graphene become electrochemical ideal material.Store and converting field at electrochemical energy, as: lithium battery, ultracapacitor and fuel cell, make remarkable progress.In the recent period, highly active transition metal oxide nano particle and Graphene Application of composite are become focus in electro-catalysis.This mainly make use of Graphene to advantage that is soft, extremely thin, high connductivity.Theoretical according to face-point cantact, based on it to soft feature, Graphene and active catalyst have very high contacting efficiency, based on it to thin high conductivity feature, every sheet Graphene all participates in forming conductive network, fast transmission electronic, compensate for the inferior position that metal oxide-type catalyst electrical conductivity is lower.Relative to traditional catalyst point-point cantact pattern, the conductive network of millet cake model construction, its carbon atom service efficiency, contacting efficiency and load capacity, all far above the point-dot pattern of traditional catalyst particle, therefore have very high electron transport efficiency.So in current report, graphene-supported nanoparticle catalyst has extraordinary performance.
On the other hand, along with the quantitative change of nanoparticle size, the qualitative change of particle properties can be caused under certain condition.The change diminishing Macroscopic physical character caused due to particle size is called small-size effect.For ultramicro powder, size diminishes, and its specific area also significantly increases simultaneously, thus produces the character of a series of novelty.Transition metal hydroxide has the activity of good catalytic electrolysis water anode reaction.Set up the preparation method of high capacity amount high dispersive transition metal hydroxide-graphene oxide composite, transition metal hydroxide nano particle catalytic performance may be made greatly to promote.
Summary of the invention
One of the technical problem to be solved in the present invention is to provide a kind of transition metal hydroxide-graphene oxide composite, and it can improve the activity of transition metal hydroxide nano particle catalytic electrolysis water anode reaction.
For solving the problems of the technologies described above, transition metal hydroxide of the present invention-graphene oxide composite, on its graphene oxide, load has transition metal hydroxide nano particle.
The average grain diameter of described transition metal hydroxide nano particle is no more than 3 nanometers.
Described transition metal hydroxide can be cobalt hydroxide, nickel hydroxide or manganous hydroxide.
Two of the technical problem to be solved in the present invention is to provide the preparation method of above-mentioned transition metal hydroxide-graphene oxide composite, and the method is simple to operate, and reaction condition is gentle.
For solving the problems of the technologies described above, the preparation method of transition metal hydroxide of the present invention-graphene oxide composite, step comprises:
1) by graphene oxide dispersion in a solvent, suspension is formed;
2) transition metal source is dissolved in solvent, is prepared into solution;
3) under agitation, by step 2) solution prepared is added drop-wise to step 1) in described suspension;
4) drip alkaline solution, under agitation react 3 ~ 20 hours;
5) by step 4) precipitated product that obtains is separated, washing, dry, obtain the composite of transition metal hydroxide nano particle load on graphene oxide.
Step 1) described solvent is ethanol.
Step 2) described transition metal source comprise nickeliferous salt, containing cobalt salt or containing manganese salt in one or more.Preferably, described nickeliferous salt is divalent nickel salt, and the salt containing cobalt is divalent cobalt, and the salt containing manganese is manganous salt.Described divalent nickel salt comprise in nickel acetate or nickel nitrate one or more, divalent cobalt comprise in cobalt acetate or cobalt nitrate one or more, manganous salt comprise in manganese acetate or manganese nitrate one or more.
Step 2) described solvent is deionized water.
Step 3) and 4) temperature be 0 ~ 80 DEG C.
Step 4) described alkaline solution comprise in concentrated ammonia liquor or sodium hydroxide solution one or more.
Three of the technical problem to be solved in the present invention is to provide the application of above-mentioned transition metal hydroxide-graphene oxide composite.Can the powder of this transition metal hydroxide-graphene oxide composite be supported on anode by Nafion perfluorinated resin solution, after oven dry, react for catalysis electrolyzed alkaline water Oxygen anodic evolution.
The reaction condition of electro-catalysis is generally: reaction temperature is 0 ~ 60 DEG C, and voltage is 0 ~ 1.5V, and electrolyte adopts concentration to be the KOH of 1mol/L.
The present invention is carried on graphene oxide by granular size is homogeneous and that particle diameter is minimum (average grain diameter is less than 3 nanometers) transition metal hydroxide nano particle, greatly improves the catalytic performance of transition metal hydroxide.In addition, the method that the present invention prepares composite is simple to operate, and reaction condition is gentle, is applicable to commercial Application.
Accompanying drawing explanation
Fig. 1 is XRD (X-ray diffraction) collection of illustrative plates of composite prepared by the embodiment of the present invention 1;
Fig. 2 is FTIR (Fourier transform infrared spectroscopy) collection of illustrative plates of composite prepared by the embodiment of the present invention 1;
Fig. 3 is high-resolution XPS (x-ray photoelectron power spectrum) the Co 2p peak collection of illustrative plates of composite prepared by the embodiment of the present invention 1;
Fig. 4 is TEM (transmission electron microscope) photo of composite prepared by the embodiment of the present invention 1;
Fig. 5 is the grain size distribution of composite prepared by the embodiment of the present invention 1;
Fig. 6 is the performance map of composite catalytic electrolysis water Oxygen anodic evolution reaction prepared by the embodiment of the present invention 1.
Detailed description of the invention
Embodiment 1
Take graphene oxide 60mg to mix with 180ml absolute ethyl alcohol, ultrasonic 1 hour, form suspension.Take 79mgCo (Ac)
24H
2o is made into the 9ml aqueous solution.At 0 DEG C and stir under, the cobalt acetate aqueous solution is added dropwise to above-mentioned suspension, subsequently drip 4ml ammoniacal liquor (concentration is 25%).Reactant mixture stirs 10 hours at 0 DEG C.Isolated by filtration obtains solid, with deionized water and absolute ethanol washing 3 times, and vacuum drying 12 hours at 40 DEG C.Obtain the composite that ultra-fine cobalt hydroxide nano particle is carried on graphene oxide.
The XRD collection of illustrative plates of this composite as shown in Figure 1.By analyzing this figure, can find the cobalt species of load on graphene oxide be unformed or particle diameter quite little.The FTIR collection of illustrative plates of this composite as shown in Figure 2.The XPS collection of illustrative plates at the Co 2p peak of this composite as shown in Figure 3.Can find in this composite by analysis chart 2 and Fig. 3, cobalt species exist with cobalt hydroxide form.Respectively as shown in Figure 4,5, visible cobalt hydroxide nano particle is evenly dispersed in graphene oxide surface, and the average grain diameter of cobalt hydroxide nano particle is 2.2nm for the TEM photo of this composite and grain size distribution.
Above-mentioned for 5mg cobalt hydroxide-graphene oxide composite powder is dispersed in the mixed liquor be made up of 0.75ml water and 0.25ml isopropyl alcohol, adds 0.016ml 5wt%Nafion solution wherein.Ultrasonic 30 minutes of this mixture is to obtain the finely dispersed suspension of catalyst solid.From then on getting 0.02ml in suspension drips on carbon paper, dries 30 minutes at 60 DEG C, and obtained catalyst loading area is 1cm
2working electrode.
Above-mentioned working electrode is used for anode of electrolytic water catalysis oxygen evolution reaction, the reaction condition of electro-catalysis is: reaction temperature 25 DEG C, voltage 0 ~ 1.5V, and electrolyte adopts concentration to be the KOH of 1mol/L.As shown in Figure 6, catalytic activity is better than yittrium oxide catalyst to the catalytic performance of this composite in anode of electrolytic water oxygen evolution reaction.
Embodiment 2
Take graphene oxide 60mg to mix with 180ml absolute ethyl alcohol, ultrasonic 1 hour, form suspension.Take 169mgNi (NO
3)
26H
2o is made into the 9ml aqueous solution.At 0 DEG C and stir under, nickel nitrate aqueous solution is added dropwise to above-mentioned suspension, subsequently drip 4ml ammoniacal liquor (concentration is 25%).Reactant mixture stirs 10 hours at 0 DEG C.Isolated by filtration obtains solid, with deionized water and absolute ethanol washing 3 times, and vacuum drying 12 hours at 40 DEG C.Obtain ultra-fine nickel hydroxide nano particulate load in the composite of graphene oxide.
Above-mentioned for 5mg nickel hydroxide-graphene oxide composite powder is dispersed in the mixed liquor be made up of 0.75ml water and 0.25ml isopropyl alcohol, adds 0.016ml 5wt%Nafion solution wherein.Ultrasonic 30 minutes of this mixture is to obtain the finely dispersed suspension of catalyst solid.From then on getting 0.02ml in suspension drips on carbon paper, dries 30 minutes at 60 DEG C, and obtained catalyst loading area is 1cm
2working electrode.
Above-mentioned working electrode is used for anode of electrolytic water catalysis oxygen evolution reaction, the reaction condition of electro-catalysis is: reaction temperature 25 DEG C, voltage 0 ~ 1.5V, and electrolyte adopts concentration to be the KOH of 1mol/L.
Embodiment 3
Take graphene oxide 60mg to mix with 180ml absolute ethyl alcohol, ultrasonic 1 hour, form suspension.Take 193mgMn (Ac)
24H
2o is made into the 9ml aqueous solution.At 0 DEG C and stir under, the manganese acetate aqueous solution is added dropwise to above-mentioned suspension, subsequently drip 4ml sodium hydroxide solution (concentration is 2mol/L).Reactant mixture stirs 10 hours at 0 DEG C.Isolated by filtration obtains solid, and with deionized water and absolute ethanol washing 3 times, vacuum drying 12 hours at 40 DEG C, obtains the composite that ultra-fine manganous hydroxide nano particle is carried on graphene oxide.
Above-mentioned for 5mg manganous hydroxide-graphene oxide composite powder is dispersed in the mixed liquor be made up of 0.75ml water and 0.25ml isopropyl alcohol, adds 0.016ml 5wt%Nafion solution wherein.Ultrasonic 30 minutes of this mixture is to obtain the finely dispersed suspension of catalyst solid.From then on getting 0.02ml in suspension drips on carbon paper, dries 30 minutes at 60 DEG C, and obtained catalyst loading area is 1cm
2working electrode.
Above-mentioned working electrode is used for anode of electrolytic water catalysis oxygen evolution reaction, the reaction condition of electro-catalysis is: reaction temperature 25 DEG C, voltage 0 ~ 1.5V, and electrolyte adopts concentration to be the KOH of 1mol/L.
Above embodiment four water cobalt acetates (Co (Ac) used
24H
2o), six water nickel nitrate (Ni (NO
3)
26H
2o), four water manganese acetates (Mn (Ac)
24H
2o), ethanol (C
2h
5oH), isopropyl alcohol ((CH
3)
2cHOH), NaOH (NaOH), potassium hydroxide (KOH) and ammoniacal liquor purchased from chemical reagents corporation of traditional Chinese medicines group, Nafion perfluorinated resin solution, purchased from Sigma-Aldrich group, not purifiedly can to use.Graphene oxide adopts the concentrated sulfuric acid and potassium permanganate and powdered graphite to obtain through oxidation reaction by hummers method.
Claims (12)
1. transition metal hydroxide-graphene oxide composite, is characterized in that, on described graphene oxide, load has transition metal hydroxide nano particle.
2. transition metal hydroxide according to claim 1-graphene oxide composite, is characterized in that, the average grain diameter of described transition metal hydroxide nano particle is no more than 3 nanometers.
3. transition metal hydroxide according to claim 1 and 2-graphene oxide composite, is characterized in that, described transition metal hydroxide comprises cobalt hydroxide, nickel hydroxide or manganous hydroxide.
4. the preparation method of the transition metal hydroxide-graphene oxide composite of claim 1-3 described in any one, it is characterized in that, step comprises:
1) by graphene oxide dispersion in a solvent, suspension is formed;
2) transition metal source is dissolved in solvent, is prepared into solution;
3) under agitation, by step 2) solution prepared is added drop-wise to step 1) in described suspension;
4) drip alkaline solution, under agitation react 3 ~ 20 hours;
5) by step 4) precipitated product that obtains is separated, washing, dry, obtain the composite of transition metal hydroxide nano particle load on graphene oxide.
5. method according to claim 4, is characterized in that, step 1) described solvent is ethanol.
6. method according to claim 4, is characterized in that, step 2) described transition metal source comprise nickeliferous salt, containing cobalt salt or containing manganese salt in one or more.
7. method according to claim 6, is characterized in that, described nickeliferous salt is divalent nickel salt, and the salt containing cobalt is divalent cobalt, and the salt containing manganese is manganous salt.
8. method according to claim 7, it is characterized in that, described divalent nickel salt comprise in nickel acetate or nickel nitrate one or more, divalent cobalt comprise in cobalt acetate or cobalt nitrate one or more, manganous salt comprise in manganese acetate or manganese nitrate one or more.
9. method according to claim 4, is characterized in that, step 2) described solvent is deionized water.
10. method according to claim 4, is characterized in that, step 3) and 4) temperature be 0 ~ 80 DEG C.
11. methods according to claim 4, is characterized in that, step 4) described alkaline solution comprise in concentrated ammonia liquor or sodium hydroxide solution one or more.
The application of transition metal hydroxide described in 12. claims 1 or 2-graphene oxide composite, is characterized in that, is supported on anode, reacts for catalysis electrolyzed alkaline water Oxygen anodic evolution.
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| CN105118693A (en) * | 2015-09-14 | 2015-12-02 | 南京大学 | Preparation method for three-dimensional reticular nitrogen-doped graphene composite cobalt hydroxide hexagonal nano-sheet electrode material |
| CN105374574A (en) * | 2015-12-25 | 2016-03-02 | 哈尔滨工业大学 | Preparation method and application of cobalt hydroxide/graphene flexible electrode material |
| CN105513835A (en) * | 2015-12-25 | 2016-04-20 | 哈尔滨工业大学 | Preparation method and application of nickel hydroxide/graphene flexible electrode material |
| CN106011926A (en) * | 2016-07-07 | 2016-10-12 | 江苏大学 | Electrocatalyst with cobalt-based multi-stage nano-composite structure for oxygen production by electrolysis of water and preparation method of electrocatalyst |
| CN106543534A (en) * | 2016-11-02 | 2017-03-29 | 北京圣盟丰联科贸有限公司 | Multifunctional graphite vinyl/polymer masterbatch and preparation method thereof |
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| CN110075847A (en) * | 2019-03-15 | 2019-08-02 | 浙江师范大学 | A kind of graphene ribbon/cobalt hydroxide composite nano materials and preparation method thereof |
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