CN103084194A - Tungsten carbide/graphene nano composite material and preparation method thereof - Google Patents
Tungsten carbide/graphene nano composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a tungsten carbide/graphene nano composite material. The preparation method comprises the following steps of: (1) firstly dissolving tungsten-containing substances into a solvent, adding a right amount of dispersing agent, then adding graphene powder, and carrying out ultrasonic dispersion to obtain homogeneously dispersed printing-ink-like mixed liquor; (2) then transferring the homogeneously dispersed printing-ink-like mixed liquor into a microwave oven, and intermittently heating until a powdery product is obtained; and (3) calcining the powdery product for 3-5 hours at a high temperature in reducing atmosphere, and cooling, so that the tungsten carbide/graphene nano composite material is obtained. The preparation method of the tungsten carbide/graphene nano composite material disclosed by the invention is simple in process, quick and time-saving, and the prepared tungsten carbide/graphene nano composite material has the characteristics of small tungsten carbide particles, uniform distribution and singe phase. The nano composite material prepared by adopting the preparation method disclosed by the invention can serve as a catalyst or a catalyst carrier and is hopeful to being applied to the fields of electrochemical catalysis, sensors and organic synthesis, so that the aim of saving a noble metal catalyst is achieved.
Description
Technical field
The present invention relates to a kind of tungsten carbide/graphene nanocomposite material, it can be used as catalyst or catalyst carrier in electrochemistry and organic synthesis.The invention still further relates to the preparation method of this tungsten carbide/graphene nanocomposite material.
Background technology
Tungsten carbide (WC) is a kind of material with unique physical and chemical characteristic.On the one hand, tungsten carbide has high rigidity, high-wearing feature, high-melting-point, the characteristics such as corrosion-resistant and is widely used in cutting element, wear resistant tools, accurate grinding tool and drill bit.On the other hand, tungsten carbide have similar platinum catalytic activity (R. B. Levy, M. Boudart,
Science, 1973,181:547.), the physics and chemistry stable performance, and cheap, show unique catalytic activity in some fields as catalyst.Along with the attention of people to clean energy resource, tungsten carbide is at catalytic field, and the application of aspects such as DMFC, lithium ion battery, catalytic hydrogen evolution, super-capacitor and catalytic hydrogenation and dechlorination has caused scientist's extensive concern.In electrochemical field, tungsten carbide is that as the advantage of anode catalyst it not only has catalytic performance and can replace the precious metals such as platinum, palladium, and be difficult for being poisoned by carbon monoxide (Y. Wang, S. Q. Song, P. K. Shen, et al.,
J .Mater. Chem., 2009,19:6149.).Thereby tungsten carbide catalyst can Partial Replacement or is saved to a certain extent the precious metals such as platinum, palladium, and it has a extensive future.
Traditional preparation technology of tungsten carbide acts in metallurgical industry, and it gets in the pyroreaction more than 1500 ℃ by tungsten powder and powdered carbon.But the tungsten carbide product that makes is in this way reunited seriously, specific area is little, purity is low, can only satisfy the metallurgical industry needs, can not effectively bring into play its catalytic action.In order to adapt to tungsten carbide in the application aspect catalysis and absorption, the scientific research personnel has developed some and has prepared the method for high specific surface area tungsten carbide.For example, the reaction of vapor-phase reactant and solid metallic compound, the gas-phase reaction of volatile metal compounds and vapour deposition process etc.Usually, adopt compound catalytic activity and the stability for improving tungsten carbide of high specific surface carrier and tungsten carbide to play an important role, this high-specific surface area mainly due to carrier is conducive to the high degree of dispersion of tungsten carbide.Graphene (Graphene) is with sp by carbon atom
2A kind of carbonaceous new material of the tightly packed one-tenth bi-dimensional cellular of the monolayer carbon atom shape lattice structure that hydridization connects, its theoretic throat only has 0.355nm, is the thinnest known two-dimensional material at present in the world.Thereby Graphene has good electric conductivity, (single-layer graphene has the specific area of super large to high specific area, and its theoretical value is up to 2600m
2/ g), having simultaneously good adsorption capacity, these characteristics all provide obvious advantage for Graphene as catalytic carrier.Therefore, how to adopt simple method to prepare that specific area is high, tungsten carbide particle is little and finely dispersed tungsten carbide/graphene nanocomposite material, have important scientific meaning for the development and application that promotes tungsten carbide catalyst.
Summary of the invention
Technical problem solved by the invention is to provide a kind of tungsten carbide/graphene nanocomposite material, this material have tungsten carbide particle little, be uniformly dispersed and the characteristics such as phase is single.This composite is expected to be widely used in various electrochemical catalysis, sensor and organic synthesis etc., especially can be directly as catalyst or the carrier of methanol fuel cell, to reach the purpose of saving noble metal catalyst, the present invention also provides the method for preparing described tungsten carbide/graphene nanocomposite material, to solve the shortcoming in the above-mentioned background technology.
Technical problem solved by the invention realizes by the following technical solutions:
A kind of preparation method of tungsten carbide/graphene nanocomposite material comprises the steps:
(1) with the tungstenic substance dissolves in solvent, add appropriate dispersant, then add the Graphene powder, ultrasonic dispersion obtains homodisperse ink-like mixed solution;
(2) the ink-like mixed solution with step (1) gained is placed in micro-wave oven, adopts the batch (-type) heating, until obtain powdery product;
(3) under reducing atmosphere, the product of step (2) gained was at high temperature calcined 3-5 hour, then cooling, namely obtain tungsten carbide/graphene nanocomposite material.
Preferably, (1) in step, described tungstenic material is one or more the mixture in wolframic acid, tungstates, metatungstate, and in solution, the quality percentage composition of tungstenic material is 3-10%, described dispersant is 1-METHYLPYRROLIDONE, N, one or more kinds of mixtures in dinethylformamide and polyvinylpyrrolidone, and the quality percentage composition of dispersant is 5-50%, the mass ratio of described tungstenic material and Graphene powder is 1:1-15.
Preferably, in step (2), described intermittent type microwave heat time heating time is 5-30 minute, and in described step (3), described hot conditions is preferably 700~1200 ℃.
In described step (3), optimum condition is, described high-temperature temperature is 900 ℃, and calcination time is 4 hours.
Preferably, described reducing atmosphere is the gaseous mixture of hydrogen or methane and inert gas, and its throughput is 30~80mL/min, and volume ratio is 1:1~6, and preferred volume ratio is 1:4.
Can make tungsten carbide/graphene nanocomposite material of the present invention according to above any one preparation method.
Beneficial effect
The present invention has following advantage with respect to prior art:
(1) adopt microwave preheating to process, tungstenic material speed of separating out is fast, and the crystallite dimension of generation is little, is conducive to the tungstenic material in dispersion and the load of Graphene carrier.
(2) the tungstenic material does not need to separate with graphene powder, is convenient to regulate the Theoretical Mass ratio of tungsten source (tungstenic material) and carbon source (Graphene).
(3) Graphene has high specific area and high absorption property, is conducive to load and the dispersion of tungstenic material on the Graphene carrier.
(4) Graphene is carrier, is also the reactant carbon source, does not need to introduce other impurity, and the product purity that reaction obtains is high, phase is single.
Compared with prior art, the present invention obtain tungsten carbide/the graphene nanocomposite material phase is single, tungsten carbide particle is little and be uniformly dispersed.This composite can be widely used in various electrochemical catalysis, sensor and organic synthesis etc., especially can be used as catalyst or the carrier of DMFC, to reach the target of saving noble metal catalyst.
Description of drawings
Fig. 1 is the wide-angle x-ray diffraction figure of tungsten carbide/graphene nanocomposite material.
Fig. 2 is the transmission electron microscope picture of tungsten carbide/graphene nanocomposite material.
The specific embodiment
Below in conjunction with embodiment, technical scheme of the present invention is further described, but is not subject to these embodiment.
Embodiment 1
Get 2 g graphite powders and join in the 50 mL concentrated sulfuric acids, be placed in ice bath and be cooled to 0 ℃, dropwise add the KMnO of 5.0 g
4, be warming up to 30 ℃, stir 2 h.Then, slowly add respectively 400 mL water and 4 mL hydrogen peroxide, centrifugal (800 rpm) removes impurity, continues ultrasonic 1 h, and microwave thermal is processed 1 h then, namely obtains graphene oxide.
Under room temperature, get 1.0 g ammonium metatungstates and 4.0g 1-METHYLPYRROLIDONE, join respectively in 30.0 g deionized waters, stir, until the solution clear.Then add the 2g graphene oxide, ultrasonic in ice-water bath (400 W, 50 Hz) disperseed 30 minutes, namely obtained homodisperse ink-like mixed liquor.
Above-mentioned ink-like mixed solution is placed in micro-wave oven, adopts the batch (-type) mode of heating, microwave (800 W, 2450 Hz) was processed 30 minutes, obtained the black solid powder.Then be placed in tube furnace, passing into throughput is that 30 mL/min, volume ratio are the nitrogen of 6:1 and the gaseous mixture of hydrogen, is warming up to gradually 700 ℃, calcines 4 hours, and temperature programming speed is 3 ℃/min.Then naturally cooling, grind, namely obtain tungsten carbide/graphene nanocomposite material.
Fig. 1 is the XRD figure of the prepared tungsten carbide/graphene nanocomposite material of this embodiment.Can find out, in figure, all characteristic diffraction peak all fits like a glove with the phase (standard card PDF#51-0939) of WC, shows that this composite is single WC phase.2 θ are 26
oThe weak diffraction maximum of left and right is the characteristic peak of Graphene.
Fig. 2 is the TEM transmission electron microscope picture of the prepared tungsten carbide/graphene nanocomposite material of this embodiment, can find out, the WC nano particle is dispersed on the lamella of Graphene, the particle diameter of nanometer WC has proved in the tungsten carbide/graphene nanocomposite material of the present invention's preparation that tungsten carbide particle is little, has been evenly distributed between 10 ~ 30 nm.
Get the 2g graphite powder and join in the 50 mL concentrated sulfuric acids, be placed in ice bath and be cooled to 0 ℃, dropwise add the KMnO of 5.5 g
4, be warming up to 30 ℃, stir 2 h.Then, slowly add respectively 400 mL water and 5 mL hydrogen peroxide, centrifugal (800 rpm) removes impurity, continues ultrasonic 1 h, and microwave thermal is processed 1 h then, namely obtains graphene oxide.
Under room temperature, get 1.0 g ammonium metatungstates and 2.4g polyvinylpyrrolidone, join respectively in 30.0 g deionized waters, stir, until the solution clear.Then add the 1.2g graphene oxide, ultrasonic in ice-water bath (400 W, 50 Hz) disperseed 30 minutes, namely obtained homodisperse ink-like mixed liquor.
Above-mentioned ink-like mixed solution is placed in micro-wave oven, adopts the batch (-type) mode of heating, microwave (800 W, 2450 Hz) was processed 20 minutes, obtained the black solid powder.Then be placed in tube furnace, passing into throughput is that 60 mL/min, volume ratio are the nitrogen of 4:1 and the gaseous mixture of hydrogen, is warming up to gradually 900 ℃, calcines 4 hours, and temperature programming speed is 3 ℃/min.Then naturally cooling, grind, namely obtain tungsten carbide/graphene nanocomposite material.
Embodiment 3
Get the 2g graphite powder and join in the 50 mL concentrated sulfuric acids, be placed in ice bath and be cooled to 0 ℃, dropwise add the KMnO of 5.0 g
4, be warming up to 30 ℃, stir 2 h.Then, slowly add respectively 400 mL water and 4 mL hydrogen peroxide, centrifugal (800 rpm) removes impurity, continues ultrasonic 1 h, and microwave thermal is processed 1 h then, namely obtains graphene oxide.
Under room temperature, get 1.0 g ammonium metatungstates and 3.6g DMF, join respectively in 30.0 g deionized waters, stir, until the solution clear.Then add the 2.0g graphene oxide, ultrasonic in ice-water bath (400 W, 50 Hz) disperseed 30 minutes, namely obtained homodisperse ink-like mixed liquor.
Above-mentioned ink-like mixed solution is placed in micro-wave oven, adopts the batch (-type) mode of heating, microwave (800 W, 2450 Hz) was processed 5 minutes, obtained the black solid powder.Then be placed in tube furnace, passing into throughput is that 60 mL/min, volume ratio are the nitrogen of 3:1 and the gaseous mixture of hydrogen, is warming up to gradually 1200 ℃, calcines 4 hours, and temperature programming speed is 3 ℃/min.Then naturally cooling, grind, namely obtain tungsten carbide/graphene nanocomposite material.
Embodiment 4
Get the 2g graphite powder and join in the 50 mL concentrated sulfuric acids, be placed in ice bath and be cooled to 0 ℃, dropwise add the KMnO of 5.5 g
4, be warming up to 30 ℃, stir 2 h.Then, slowly add respectively 400 mL water and 5 mL hydrogen peroxide, centrifugal (800 rpm) removes impurity, continues ultrasonic 1 h, and microwave thermal is processed 1 h then, namely obtains graphene oxide.
Under room temperature, get 1.0 g ammonium metatungstates and 4.0g 1-METHYLPYRROLIDONE, join respectively in 30.0 g deionized waters, stir, until the solution clear.Then add the 3g graphene oxide, ultrasonic in ice-water bath (400 W, 50 Hz) disperseed 30 minutes, namely obtained homodisperse ink-like mixed liquor.
Above-mentioned ink-like mixed solution is placed in micro-wave oven, adopts the batch (-type) mode of heating, microwave (800 W, 2450 Hz) was processed 30 minutes, obtained the black solid powder.Then be placed in tube furnace, passing into throughput is that 80 mL/min, volume ratio are the nitrogen of 1:1 and the gaseous mixture of hydrogen, is warming up to gradually 900 ℃, calcines 4 hours, and temperature programming speed is 3 ℃/min.Then naturally cooling, grind, namely obtain tungsten carbide/graphene nanocomposite material.
Above demonstration and described basic principle of the present invention and principal character and advantage of the present invention; the technical staff of the industry should understand; the present invention is not restricted to the described embodiments; that describes in above-described embodiment and specification just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications; these changes and improvements all fall in the claimed scope of the invention, and the claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (10)
1. the preparation method of a tungsten carbide/graphene nanocomposite material, is characterized in that, comprises the steps:
(1) with the tungstenic substance dissolves in solvent, add appropriate dispersant, then add the Graphene powder, ultrasonic dispersion obtains homodisperse ink-like mixed solution;
(2) the ink-like mixed solution with step (1) gained is placed in micro-wave oven, adopts the batch (-type) heating, until obtain powdery product;
(3) under reducing atmosphere, the product of step (2) gained was at high temperature calcined 3-5 hour, then cooling, namely obtain tungsten carbide/graphene nanocomposite material.
2. the preparation method of a kind of tungsten carbide/graphene nanocomposite material according to claim 1, it is characterized in that, described tungstenic material is one or more the mixture in wolframic acid, tungstates, metatungstate, and in solution, the quality percentage composition of tungstenic material is 3-10%.
3. the preparation method of a kind of tungsten carbide/graphene nanocomposite material according to claim 1, it is characterized in that, described dispersant is 1-METHYLPYRROLIDONE, N, one or more kinds of mixtures in dinethylformamide and polyvinylpyrrolidone, and the quality percentage composition of dispersant is 5-50%.
4. the preparation method of a kind of tungsten carbide/graphene nanocomposite material according to claim 1, is characterized in that, the mass ratio of described tungstenic material and Graphene powder is 1:1-15.
5. the preparation method of a kind of tungsten carbide/graphene nanocomposite material according to claim 1, is characterized in that, in described step (2), described intermittent type microwave heat time heating time is 5-30 minute.
6. the preparation method of a kind of tungsten carbide/graphene nanocomposite material according to claim 1, is characterized in that, in described step (3), described hot conditions is 700~1200 ℃.
7. the preparation method of a kind of tungsten carbide/graphene nanocomposite material according to claim 1, is characterized in that, in described step (3), described high-temperature temperature is 900 ℃, and calcination time is 4 hours.
8. the preparation method of a kind of tungsten carbide/graphene nanocomposite material according to claim 1, is characterized in that, described reducing atmosphere is the gaseous mixture of hydrogen or methane and inert gas, and its throughput is 30~80mL/min, and volume ratio is 1:1~6.
9. the preparation method of a kind of tungsten carbide/graphene nanocomposite material according to claim 8, is characterized in that, described reducing atmosphere is the gaseous mixture of hydrogen or methane and inert gas, and its throughput is 30~80mL/min, and volume ratio is 1:4.
10. tungsten carbide/graphene nanocomposite material of making of according to claim 1-9 described preparation methods of any one.
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Cited By (8)
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CN103638929A (en) * | 2013-12-13 | 2014-03-19 | 江苏大学 | Graphene-silver tungstate composite photocatalytic material as well as preparation method thereof |
CN103977841A (en) * | 2014-06-04 | 2014-08-13 | 黑龙江大学 | Method for preparing nitride/carbon nano tube-graphene ternary complex |
CN105521804A (en) * | 2015-12-08 | 2016-04-27 | 广东石油化工学院 | Preparation method of honeycombed graphene/tungsten carbide/platinum composite electrocatalyst and application thereof |
CN107311175A (en) * | 2017-06-28 | 2017-11-03 | 中国航发北京航空材料研究院 | A kind of graphene is modified the preparation method of tungsten carbide self-lubricating abrasion-resistant additive |
CN107352534A (en) * | 2017-06-28 | 2017-11-17 | 中国航发北京航空材料研究院 | The graphene oxide that a kind of nanometer tungsten carbide is modified |
CN109987954A (en) * | 2019-03-15 | 2019-07-09 | 西安交通大学 | A kind of tungsten carbide enhancing graphite-base composite material and preparation method |
CN110453107A (en) * | 2019-08-01 | 2019-11-15 | 天津大学 | Graphene-tungsten carbide collaboration enhancing Cu-base composites preparation method |
CN114988716A (en) * | 2022-06-15 | 2022-09-02 | 中国科学院合肥物质科学研究院 | Tungsten carbide/graphene composite material and preparation method thereof |
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CN103977841B (en) * | 2014-06-04 | 2016-02-17 | 黑龙江大学 | A kind of method preparing nitride/CNT-Graphene ternary complex |
CN105521804A (en) * | 2015-12-08 | 2016-04-27 | 广东石油化工学院 | Preparation method of honeycombed graphene/tungsten carbide/platinum composite electrocatalyst and application thereof |
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CN107352534A (en) * | 2017-06-28 | 2017-11-17 | 中国航发北京航空材料研究院 | The graphene oxide that a kind of nanometer tungsten carbide is modified |
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CN109987954A (en) * | 2019-03-15 | 2019-07-09 | 西安交通大学 | A kind of tungsten carbide enhancing graphite-base composite material and preparation method |
CN109987954B (en) * | 2019-03-15 | 2020-10-27 | 西安交通大学 | Tungsten carbide reinforced graphite-based composite material and preparation method thereof |
CN110453107A (en) * | 2019-08-01 | 2019-11-15 | 天津大学 | Graphene-tungsten carbide collaboration enhancing Cu-base composites preparation method |
CN114988716A (en) * | 2022-06-15 | 2022-09-02 | 中国科学院合肥物质科学研究院 | Tungsten carbide/graphene composite material and preparation method thereof |
CN114988716B (en) * | 2022-06-15 | 2023-11-07 | 中国科学院合肥物质科学研究院 | Tungsten carbide/graphene composite material and preparation method thereof |
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