CN104772156A - Preparation method for graphene loaded cobalt nickel phosphide composite material - Google Patents
Preparation method for graphene loaded cobalt nickel phosphide composite material Download PDFInfo
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- CN104772156A CN104772156A CN201510127700.1A CN201510127700A CN104772156A CN 104772156 A CN104772156 A CN 104772156A CN 201510127700 A CN201510127700 A CN 201510127700A CN 104772156 A CN104772156 A CN 104772156A
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Abstract
The invention relates to a preparation method for a graphene loaded cobalt nickel phosphide composite material. The method includes: dissolving a nickel salt and a cobalt salt in deionized water, putting graphene oxide in deionized water to conduct ultrasonic treatment into a homogeneous solution, mixing the two fully, then transferring the mixture into a polytetrafluoroethylene lining, then adding red phosphorus, finally performing water hydro-thermal treatment, and subjecting the obtained product to vacuum drying, thus obtaining the graphene loaded cobalt nickel phosphide composite material. The method provided by the invention has the advantages of environment friendliness, simple and safe operation and the like.
Description
Technical field
The present invention relates to graphene-supported technical field of nanometer material preparation, particularly a kind of preparation method of graphene-supported nickel phosphide cobalt composite material.
Background technology
Due to compared with independent nano material, mixing nano composite material, in all many-sides, as optics, electricity, calorifics, mechanics and catalytic field all show excellent character, has attracted a large amount of researcher to study this material.And Graphene, be that one passes through sp by carbon atom
2hydridization covalent bond combines the two-dimentional honeycomb lattice nano material formed, in addition, and very large specific area (about 2600m
2/ g), well chemical stability and excellent electricity, mechanical performance etc., become a kind of carrier of being potential very much.At present, have in a large number about with graphene oxide or the reduced graphene report as carrier loaded nano material, these results of study all show the compound by Graphene and nano material, make raw material in photoelectrochemical behaviour, catalytic performance etc., have the improvement of highly significant, research also proposed and thisly improves the reason occurred, may be that the increase of the effective electron transfer number provided due to increase and the Graphene of material surface avtive spot quantity after compound causes.But in these researchs, graphene-supported metal ion and metal oxide composite are by large quantifier elimination, and studied less of graphene-supported metal phosphide.Due to the new catalytic material that phosphide is a class high activity, high stability, and in its structure, expose the unsaturated surface atom number of more coordination, therefore have than oxide, catalytic activity that sulfide is higher.
In addition, graphene oxide (GO) reduction process many employings chemical reduction method, the method needs to use the poisonous chemical reducing agent such as hydrazine hydrate, is unfavorable for very much environmental protection and experiment safety operation.But graphene oxide can cause its performance greatly to reduce with more oxy radical due to surface, therefore invent and a kind ofly fast and convenient for graphene oxide can be reduced to Graphene, and the preparation method simultaneously completing nanomaterial loadings there are very important meaning and wide application prospect.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide a kind of preparation method of graphene-supported nickel phosphide cobalt composite material, the advantages such as this method has environmental friendliness, easy to operate and safe.
For achieving the above object, the present invention takes technical scheme to be:
A preparation method for graphene-supported nickel phosphide cobalt composite material, comprises the following steps:
1) in beaker, add the deionized water that volume is 10 ~ 20mL, in every ml deionized water, add the nickel salt of 0.006g ~ 0.015g, 0.006g ~ 0.015g cobalt salt, stir until dissolve completely, form clear transparent solutions;
2) by standby by Hummers legal system and be dissolved in the conical flask that 15 ~ 25mL deionized water is housed by the graphene oxide that freeze drying obtains, ultrasonic until form homogeneous graphene oxide solution, graphene oxide concentration is 0.2 ~ 0.8g/L;
3) by step 2) gained solution joins step 1) beaker in continue to stir, then homogeneous liquid rotating is moved on in polytetrafluoroethyllining lining;
4) to step 3) liquid in add red phosphorus, 0.005 ~ 0.010g is added in every milliliter of clear solution, being stirred to solution surface has suspension to occur, polytetrafluoroethyllining lining is sealed in stainless steel mould, heats by room temperature in confined conditions and add thermal response 8 ~ 16h at 180 ~ 220 DEG C;
5) after having reacted, with stove cool to room temperature, then use fast quantification Filter paper filtering, obtain crude product;
6) wash crude product with deionized water and absolute ethyl alcohol respectively successively, insert in vacuum drying chamber by the product after washing, vacuum drying 4h at 50 ~ 60 DEG C, obtains graphene-supported nickel phosphide cobalt composite material.
Described nickel salt is Nickel dichloride hexahydrate, four hydration nickel acetates.
Described cobalt salt is four hydration cobalt acetates, cobalt sulfate and cobalt chloride hexahydrate.
Described polytetrafluoroethyllining lining is 50mL, and compactedness is 60 ~ 80%.
The present invention has following beneficial effect:
(1) adopt method step while load NiCoP nano particle of reducing under autoclave hot conditions to complete the reduction of graphene oxide, avoid using highly toxic electronation reagent, convenient experimental operation, safety.
(2) electrology characteristic of surface characteristic good for Graphene and excellence is combined with the distinctive high surface locus trait of phosphide, make composite have both the advantage character of the two, the relatively single nano material of composite electric property has been had and significantly improves.
(3) cost of the present invention is low, and raw material is easy to get, and preparation technology is simple, reproducible, has a good application prospect.
Accompanying drawing explanation
Fig. 1 is the XRD figure of graphene-supported nickel phosphide cobalt composite material prepared by embodiment 1.
Fig. 2 is the SEM figure of graphene-supported nickel phosphide cobalt composite material prepared by embodiment 1.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in detail.
Embodiment 1
A preparation method for graphene-supported nickel phosphide cobalt composite material, comprises the following steps:
1) in beaker, add the deionized water that volume is 20mL, add 0.325g tetra-hydration nickel acetate, 0.286g Cobalt monosulfate heptahydrate, stir until dissolve completely, form clear transparent solutions;
2) by standby by Hummers legal system and be dissolved in the conical flask that 15mL deionized water is housed by the graphene oxide that freeze drying obtains, ultrasonic until form homogeneous graphene oxide solution, graphene oxide concentration is 0.35g/L;
3) by step 2) gained solution joins step 1) beaker in continue to stir, then homogeneous liquid rotating is moved on in polytetrafluoroethyllining lining;
4) to step 3) liquid in add 0.260g red phosphorus, being stirred to solution surface has suspension to occur, polytetrafluoroethyllining lining is sealed in stainless steel mould, in confined conditions by room temperature heating and add thermal response 10h at 200 DEG C;
5) after having reacted, with stove cool to room temperature, then use fast quantification Filter paper filtering, obtain crude product;
6) wash crude product with deionized water and absolute ethyl alcohol respectively successively, insert in vacuum drying chamber by the product after washing, vacuum drying 4h at 55 DEG C, obtains graphene-supported nickel phosphide cobalt composite material.
As depicted in figs. 1 and 2, wherein nickel phosphide cobalt nanometer particle diameter is about 20nm for the XRD collection of illustrative plates of the composite that the present embodiment 1 is prepared and SEM picture.
Embodiment 2
By step 1 in embodiment 1) in 0.325g tetra-hydration nickel acetate change 0.438g Nickel dichloride hexahydrate into, other conditions are constant.In the graphene-supported nickel phosphide cobalt composite material of gained, nickel phosphide cobalt average grain reduces, and coated situation is substantially identical.
Embodiment 3
By step 1 in embodiment 1) 0.286g Cobalt monosulfate heptahydrate change 0.347g cobalt chloride hexahydrate into, other conditions are constant, in the graphene-supported nickel phosphide cobalt composite material of gained, particle granules becomes large, and covering amount is less simultaneously, can observe more exposed smooth Graphene.
Embodiment 4
By step 4 in embodiment 1) in add red phosphorus quality and change 0.530g into, other conditions are constant, after reaction terminates, find that obvious hole appears in the graphenic surface in gained graphene-supported nickel phosphide cobalt composite material, its reason is because red phosphorus is too much excessive, destroys Graphene self structure.
Embodiment 5
By step 4 in embodiment 1) in reaction temperature become 180 DEG C, other conditions are constant, and occur the Graphene that exhibiting high surface is smooth in gained graphene-supported nickel phosphide cobalt composite material, nano particle is little, illustrate that reaction temperature is that 180 DEG C of temperature are too low, nano particle generates and is obstructed.
Be described in detail description to specific embodiments of the invention above, and be described the product phenomenon of different embodiments, but it is just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and substituting also all among category of the present invention.Therefore, equalization conversion done without departing from the spirit and scope of the invention and amendment, all should contain within the scope of the invention.
Claims (4)
1. a preparation method for graphene-supported nickel phosphide cobalt composite material, is characterized in that, comprise the following steps:
1) in beaker, add the deionized water that volume is 10 ~ 20mL, in every ml deionized water, add the nickel salt of 0.006g ~ 0.015g, 0.006g ~ 0.015g cobalt salt, stir until dissolve completely, form clear transparent solutions;
2) by standby by Hummers legal system and be dissolved in the conical flask that 15 ~ 25mL deionized water is housed by the graphene oxide that freeze drying obtains, ultrasonic until form homogeneous graphene oxide solution, graphene oxide concentration is 0.2 ~ 0.8g/L;
3) by step 2) gained solution joins step 1) beaker in continue to stir, then homogeneous liquid rotating is moved on in polytetrafluoroethyllining lining;
4) to step 3) liquid in add red phosphorus, 0.005 ~ 0.010g is added in every milliliter of clear solution, being stirred to solution surface has suspension to occur, polytetrafluoroethyllining lining is sealed in stainless steel mould, heats by room temperature in confined conditions and add thermal response 8 ~ 16h at 180 ~ 220 DEG C;
5) after having reacted, with stove cool to room temperature, then use fast quantification Filter paper filtering, obtain crude product;
6) wash crude product with deionized water and absolute ethyl alcohol respectively successively, insert in vacuum drying chamber by the product after washing, vacuum drying 4h at 50 ~ 60 DEG C, obtains graphene-supported nickel phosphide cobalt composite material.
2. the preparation method of a kind of graphene-supported nickel phosphide cobalt composite material according to claim 1, is characterized in that: described nickel salt is Nickel dichloride hexahydrate, four hydration nickel acetates.
3. the preparation method of a kind of graphene-supported nickel phosphide cobalt composite material according to claim 1, is characterized in that: described cobalt salt is four hydration cobalt acetates, cobalt sulfate and cobalt chloride hexahydrate.
4. the preparation method of a kind of graphene-supported nickel phosphide cobalt composite material according to claim 1, it is characterized in that: described polytetrafluoroethyllining lining is 50mL, compactedness is 60 ~ 80%.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107256950A (en) * | 2017-06-07 | 2017-10-17 | 安徽师范大学 | Magnetic metal phosphide/the preparation method of graphene nanocomposite material, negative electrode of lithium ion battery, lithium ion battery |
| CN108671947A (en) * | 2018-04-11 | 2018-10-19 | 西安石油大学 | Ni for biological oil hydrodeoxygenation reaction2P/ redox graphene catalyst and preparation method thereof |
| CN108786868A (en) * | 2018-05-18 | 2018-11-13 | 燕山大学 | A kind of preparation method of nickel phosphorus/fluorine doped reduction-oxidation graphite liberation of hydrogen composite material |
| CN108864636A (en) * | 2018-08-08 | 2018-11-23 | 燕山大学 | A kind of nickel phosphide/fluorinated graphene-ptfe composite and its preparation method and application |
| CN110124702A (en) * | 2019-04-22 | 2019-08-16 | 浙江大学 | A kind of preparation method of double-metal phosphide composite reduction graphene nano electrocatalysis material |
| CN110323073A (en) * | 2019-06-28 | 2019-10-11 | 中国地质大学（北京） | A kind of oxygen doping phosphatization cobalt nickel-redox graphene composite material and its application |
| CN112687477A (en) * | 2020-12-10 | 2021-04-20 | 郑州轻工业大学 | Preparation method and application of double-transition metal phosphide graphene composite material CoNiP-rGO |
| CN112931531A (en) * | 2021-02-08 | 2021-06-11 | 泉州师范学院 | Carbon-doped nickel phosphide composite antibacterial material and preparation method and application thereof |
| CN114959735A (en) * | 2022-04-28 | 2022-08-30 | 东华大学 | Preparation method and application of graphene/nickel cobalt phosphide film |
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| CN102354614A (en) * | 2011-09-15 | 2012-02-15 | 南开大学 | Phosphide counter electrode for dye sensitized solar cell and preparation method for phosphide counter electrode |
| CN103094540A (en) * | 2013-01-06 | 2013-05-08 | 中物院成都科学技术发展中心 | Method for compounding graphene and metallic oxide/metallic compound and composite material thereof |
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| CN103464187A (en) * | 2013-09-17 | 2013-12-25 | 天津科技大学 | Method for synthesizing bimetallic phosphide at low temperature on basis of metallic oxide |
| CN104409699A (en) * | 2014-11-19 | 2015-03-11 | 陕西科技大学 | Preparation method of graphene coated cuprous phosphide composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102354614A (en) * | 2011-09-15 | 2012-02-15 | 南开大学 | Phosphide counter electrode for dye sensitized solar cell and preparation method for phosphide counter electrode |
| US20130260286A1 (en) * | 2012-03-30 | 2013-10-03 | Kabushiki Kaisha Toshiba | Oxygen reduction catalyst and electrochemical cell |
| CN103094540A (en) * | 2013-01-06 | 2013-05-08 | 中物院成都科学技术发展中心 | Method for compounding graphene and metallic oxide/metallic compound and composite material thereof |
| CN103464187A (en) * | 2013-09-17 | 2013-12-25 | 天津科技大学 | Method for synthesizing bimetallic phosphide at low temperature on basis of metallic oxide |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107256950A (en) * | 2017-06-07 | 2017-10-17 | 安徽师范大学 | Magnetic metal phosphide/the preparation method of graphene nanocomposite material, negative electrode of lithium ion battery, lithium ion battery |
| CN108671947B (en) * | 2018-04-11 | 2021-02-02 | 西安石油大学 | Ni for hydrodeoxygenation of bio-oil2P/reduced graphene oxide catalyst and preparation method thereof |
| CN108671947A (en) * | 2018-04-11 | 2018-10-19 | 西安石油大学 | Ni for biological oil hydrodeoxygenation reaction2P/ redox graphene catalyst and preparation method thereof |
| CN108786868A (en) * | 2018-05-18 | 2018-11-13 | 燕山大学 | A kind of preparation method of nickel phosphorus/fluorine doped reduction-oxidation graphite liberation of hydrogen composite material |
| CN108864636A (en) * | 2018-08-08 | 2018-11-23 | 燕山大学 | A kind of nickel phosphide/fluorinated graphene-ptfe composite and its preparation method and application |
| CN108864636B (en) * | 2018-08-08 | 2019-08-23 | 燕山大学 | A kind of nickel phosphide/fluorinated graphene-ptfe composite and its preparation method and application |
| CN110124702A (en) * | 2019-04-22 | 2019-08-16 | 浙江大学 | A kind of preparation method of double-metal phosphide composite reduction graphene nano electrocatalysis material |
| CN110323073A (en) * | 2019-06-28 | 2019-10-11 | 中国地质大学（北京） | A kind of oxygen doping phosphatization cobalt nickel-redox graphene composite material and its application |
| CN112687477A (en) * | 2020-12-10 | 2021-04-20 | 郑州轻工业大学 | Preparation method and application of double-transition metal phosphide graphene composite material CoNiP-rGO |
| CN112687477B (en) * | 2020-12-10 | 2022-05-20 | 郑州轻工业大学 | Preparation method and application of double-transition metal phosphide graphene composite material CoNiP-rGO |
| CN112931531A (en) * | 2021-02-08 | 2021-06-11 | 泉州师范学院 | Carbon-doped nickel phosphide composite antibacterial material and preparation method and application thereof |
| CN112931531B (en) * | 2021-02-08 | 2021-11-30 | 泉州师范学院 | Carbon-doped nickel phosphide composite antibacterial material and preparation method and application thereof |
| CN114959735A (en) * | 2022-04-28 | 2022-08-30 | 东华大学 | Preparation method and application of graphene/nickel cobalt phosphide film |
| CN114959735B (en) * | 2022-04-28 | 2023-12-12 | 东华大学 | Preparation method and application of graphene/nickel cobalt phosphide film |
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