CN105293475A - Graphene and nickel diselenide composite and preparation method thereof - Google Patents
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Abstract
The invention discloses a graphene and nickel diselenide composite and a preparation method thereof. The preparation method comprises the steps that a reducing agent is mixed with a graphene oxide solution, even stirring is conducted to form a brown solution, the brown solution is added into a stainless steel reaction kettle with a polytetrafluoroethylene liner, and selenium containing matter and nickel containing inorganic salt are filled into the reaction kettle; the reaction kettle is closed to conduct the reaction; after the reaction is conducted, natural cooling is conducted, suction filtration is conducted on a mixture in the reaction kettle, repeated washing and suction filtration are conducted through distilled water and absolute ethyl alcohol, and the product is collected for storing after drying is conducted. According to the prepared graphene and nickel diselenide composite, nickel diselenide nanoparticles are wrapped with the graphene, nickel diselenide is closely combined with graphene sheets, and the composite has larger specific surface area. According to the graphene and nickel diselenide composite and the preparation method thereof, a simple solvothermal method is adopted, reduction of graphene oxide and preparation of the graphene oxide and the nickel diselenide composite are conducted synchronously, the technology is simple, the reaction temperature is low, the cost is low, the preparation method is green and controllable, and the graphene and nickel diselenide composite is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of matrix material and preparation method thereof, particularly relate to a kind of Graphene and two nickelous selenide matrix materials and preparation method thereof; Belong to inorganic nano composite material field.
Background technology
Nickelous selenide, as a kind of semiconductor material, due to electricity and the magnetic performance of its uniqueness, shows wide application prospect in fields such as optical recording material, solar cell, sensor, laserable material and optical fiber.At present, the research for selenide is fewer, and semi-conductor two nickelous selenide nano material has the advantages such as narrower energy gap, high electronic conductivity, higher specific storage, unique electricity and magnetic performance.As a kind of good electric conductor and Pauli paramagnetic material, two nickelous selenides belong to weak paramagnetic material and its susceptibility varies with temperature less, in nano material, have very important Research Significance.
Liu etc. utilize NiCl
2be raw material with selenium powder, hydrazine hydrate is reductive agent, uses the method for solvent thermal to prepare to have two nickelous selenide nanoparticle (LiuXH of sea urchin pattern at a lower temperature, ZhangN, YiR, etal.MaterialsScienceandEngineeringB, 2007,140,38-43).Single nickel salt and the NaSeO such as Zhuang
3for raw material, single nickel salt and NaSeO
3the ratio of amount of substance be 1:3, hydro-thermal reaction 20 hours, prepares two nickelous selenide nano particles.
Graphene is a kind of New Two Dimensional material be found in recent years, and its stable chemical structure, good electroconductibility, excellent mechanics and thermal property, cause the extensive concern of scholar.Graphene has very high specific surface area, can improve the degree of scatter of semiconductor material, effectively increases the reaction active site of composite system.The matrix material of nanometer two nickelous selenide and Graphene was not also reported.
Summary of the invention
The invention provides a kind of method preparing Graphene/bis-nickelous selenide matrix material that technique is simple, temperature of reaction is low, with low cost, green is controlled, achieve the coated combination of two nickelous selenides and Graphene.
For achieving the above object, the invention provides the preparation method of a kind of Graphene and two nickelous selenide matrix materials, the method uses conventional equipment and raw material one step original position to obtain Graphene and two nickelous selenide matrix materials, what achieve prepared by the reduction of graphene oxide and itself and two nickelous selenide matrix materials synchronously carries out, temperature of reaction is low, with low cost, in reaction process, nonhazardous gas produces.
The present invention prepares the method for Graphene and two nickelous selenide matrix materials, comprises the following steps:
(1) reductive agent mixes with graphene oxide solution, stirs and adds in polytetrafluoro inner liner stainless steel reactor after forming brown solution;
(2) load in reactor containing selenium material and nickeliferous inorganic salt;
(3) capping still reacts;
(4) naturally cooling after reaction, by mixture suction filtration in reactor, and with distilled water and dehydrated alcohol repetitive scrubbing, suction filtration;
(5) dry rear product of collecting is preserved.
Wherein, in step (1), graphene oxide solution is in one or more solvents in graphene oxide is water-soluble, pyridine, tetrahydrofuran (THF), ethanol, methyl alcohol, DMF, NMP.
Preferably, graphene oxide solution is the water-soluble solution of graphene oxide.
In step (1), graphene oxide solution concentration is 0.1 ~ 20mg/ml.
Preferably, graphene oxide solution concentration is 1mg/ml.
In step (1), reductive agent comprises: one or more in hydrazine, hydrazine hydrate, dimethylhydrazine, vitamins C, hydrogen iodide, sodium borohydride, formaldehyde, acetaldehyde, Resorcinol, Ursol D, quadrol, butanediamine.Preferably, reductive agent is hydrazine hydrate.
Further, in step (2), selenium material is elemental selenium, Sodium Selenite, potassium selenite or tin anhydride; Nickeliferous inorganic salt are nickelous oxalate, nickelous chloride, single nickel salt, nickelous nitrate or nickelous perchlorate.
Preferably, selenium material is Sodium Selenite, and nickeliferous inorganic salt are single nickel salt.
In step (2), the mol ratio containing selenium material and nickeliferous inorganic salt is 2 ~ 3:1.
Preferably, the mol ratio containing selenium material and nickeliferous inorganic salt is 3:1.
In step (2), the volume ratio of reductive agent and graphene oxide solution is 5 ~ 10:10 ~ 50 (mL).
Preferably, the volume ratio of reductive agent and graphene oxide solution is 5:10 (mL).
In step (3), temperature of reaction is 100 ~ 250 DEG C, and the reaction times is 0.5 ~ 72 hour.
Preferably, in step (3), temperature of reaction is 120 ~ 150 DEG C, and the reaction times is 5 ~ 10 hours.
In step (5), drying temperature is 40 ~ 100 DEG C, and time of drying is 0.5 ~ 24 hour.
Preferably, in step (5), drying temperature is 50 ~ 70 DEG C, and time of drying is 2 ~ 6 hours.
The reduction reaction of graphene oxide and itself and two nickelous selenide compounds are prepared and are synchronously carried out, and namely a step original position obtains described matrix material.
On the other hand, present invention also offers a kind of Graphene of obtaining according to above-mentioned chemical preparation process and two nickelous selenide matrix materials.
In the Graphene that obtains produced according to the present invention and two nickelous selenide matrix materials, the pattern of two nickelous selenides is nanometer spherical particulate state, and median size is 5 ~ 20nm.
Remarkable advantage of the present invention is:
1. the present invention adopts simple hydrothermal method one step to reduce and obtains Graphene and two nickelous selenide matrix materials, and its preparation technology is simple, and equipment requirements is low, and raw material sources enriches, and low production cost, production process is controlled, is applicable to suitability for industrialized production.
2. Graphene/bis-nickelous selenide the matrix material prepared of the present invention, the pattern of two nickelous selenides is nanometer spherical particulate state, and median size is 5 ~ 20nm; And graphene film is coated with two nickelous selenide nano particles, and two nickelous selenides and graphene film are combined closely, and has high specific surface area.
3. preparation method of the present invention can be extended to the Nano-composite materials of other selenide and Graphene.
Be described further below with reference to the technique effect of accompanying drawing to design of the present invention, concrete structure and generation, to understand object of the present invention, characteristic sum effect fully.
Accompanying drawing explanation
Fig. 1 is the SEM figure of Graphene/bis-nickelous selenide matrix material prepared by embodiments of the invention 1;
Fig. 2 is the TEM figure of Graphene/bis-nickelous selenide matrix material prepared by embodiments of the invention 1;
Fig. 3 is the XPS figure of Graphene/bis-nickelous selenide matrix material prepared by embodiments of the invention 1;
Fig. 4 is the XRD figure of Graphene/bis-nickelous selenide matrix material prepared by embodiments of the invention 1.
Embodiment
The present invention is will be further understood that from following examples.
Embodiment 1
The graphene oxide water solution being 0.1mg/ml by 5mL hydrazine hydrate and 10mL concentration mixes, stir and join in polytetrafluoro inner liner stainless steel reactor after forming brown solution, 1mmol Sodium Selenite and 0.5mmol single nickel salt are loaded in aforesaid reaction vessel, closes and tighten reactor, make it seal; Put into baking oven, temperature is set in 100 DEG C, after reaction 0.5h, take out reactor, make its naturally cooling, by mixture suction filtration in reactor, and with distilled water and dehydrated alcohol repetitive scrubbing, suction filtration, last in vacuum drying oven dry 0.5h at 40 DEG C, collect sample retention in moisture eliminator.
Fig. 1 and Fig. 2 is SEM and the TEM figure of sample prepared by the present embodiment.As can be seen from the figure two nickelous selenides preparing gained are spheroidal particle, and it is comparatively evenly distributed on graphene film, and median size is 5 ~ 20nm.
Embodiment 2
The graphene oxide water solution being 20mg/ml with 50mL concentration by 1mL hydrazine, 1mL dimethylhydrazine, 1mL vitamins C, 2mL hydrogen iodide mixes, stir and join in polytetrafluoro inner liner stainless steel reactor after forming dark brown solution, 1mmol potassium selenite and 0.2mmol nickelous nitrate, 0.3mmol nickelous perchlorate are loaded in aforesaid reaction vessel, close and tighten reactor, make it seal; Put into baking oven, temperature is set in 250 DEG C, after reaction 72h, take out reactor, make its naturally cooling, by mixture suction filtration in reactor, and with distilled water and dehydrated alcohol repetitive scrubbing, suction filtration, last in vacuum drying oven dry 24h at 100 DEG C, collect sample retention in moisture eliminator.
Embodiment 3
The graphene oxide water solution being 1mg/ml with 10mL concentration by 2mL sodium borohydride, 2mL formaldehyde, 2mL acetaldehyde, 2mL Resorcinol, 2mL Ursol D mixes, stir and join in polytetrafluoro inner liner stainless steel reactor after forming dark brown solution, 1.5mmol elemental selenium and 0.5mmol nickelous oxalate are loaded in aforesaid reaction vessel, close and tighten reactor, make it seal; Put into baking oven, temperature is set in 150 DEG C, after reaction 24h, take out reactor, make its naturally cooling, by mixture suction filtration in reactor, and with distilled water and dehydrated alcohol repetitive scrubbing, suction filtration, last in vacuum drying oven dry 12h at 60 DEG C, collect sample retention in moisture eliminator.
Embodiment 4
The graphene oxide water solution being 5mg/ml by 10mL quadrol and 50mL concentration mixes, stir and join in polytetrafluoro inner liner stainless steel reactor after forming dark brown solution, 1mmol tin anhydride and 0.5mmol nickelous chloride are loaded in aforesaid reaction vessel, close and tighten reactor, make it seal; Put into baking oven, temperature is set in 200 DEG C, after reaction 2h, take out reactor, make its naturally cooling, by mixture suction filtration in reactor, and with distilled water and dehydrated alcohol repetitive scrubbing, suction filtration, last in vacuum drying oven dry 3h at 70 DEG C, collect sample retention in moisture eliminator.
Embodiment 5
The graphene oxide water solution being 12mg/ml by 5mL butanediamine and 10mL concentration mixes, stir and join in polytetrafluoro inner liner stainless steel reactor after forming dark brown solution, 1mmol Sodium Selenite and 0.5mmol single nickel salt are loaded in aforesaid reaction vessel, close and tighten reactor, make it seal; Put into baking oven, temperature is set in 120 DEG C, after reaction 1h, take out reactor, make its naturally cooling, by mixture suction filtration in reactor, and with distilled water and dehydrated alcohol repetitive scrubbing, suction filtration, last in vacuum drying oven dry 1h at 60 DEG C, collect sample retention in moisture eliminator.
Embodiment 6
The graphene oxide water solution being 20mg/ml by 10mL hydrazine hydrate and 10mL concentration mixes, stir and join in polytetrafluoro inner liner stainless steel reactor after forming dark brown solution, 1mmol selenium powder and 0.5mmol single nickel salt are loaded in aforesaid reaction vessel, closes and tighten reactor, make it seal; Put into baking oven, temperature is set in 100 DEG C, after reaction 72h, take out reactor, make its naturally cooling, by mixture suction filtration in reactor, and with distilled water and dehydrated alcohol repetitive scrubbing, suction filtration, last in vacuum drying oven dry 24h at 40 DEG C, collect sample retention in moisture eliminator.
Embodiment 7
The graphene oxide water solution being 1mg/ml by 10mL hydrazine hydrate and 10mL concentration mixes, stir and join in polytetrafluoro inner liner stainless steel reactor after forming dark brown solution, 1mmol Sodium Selenite and 0.5mmol single nickel salt are loaded in aforesaid reaction vessel, close and tighten reactor, make it seal; Put into baking oven, temperature is set in 250 DEG C, after reaction 0.5h, take out reactor, make its naturally cooling, by mixture suction filtration in reactor, and with distilled water and dehydrated alcohol repetitive scrubbing, suction filtration, last in vacuum drying oven dry 0.5h at 100 DEG C, collect sample retention in moisture eliminator.
Embodiment 8
The graphene oxide water solution being 0.1mg/ml by 5mL hydrazine hydrate and 10mL concentration mixes, stir and join in polytetrafluoro inner liner stainless steel reactor after forming dark brown solution, 1mmol Sodium Selenite and 0.5mmol single nickel salt are loaded in aforesaid reaction vessel, close and tighten reactor, make it seal; Put into baking oven, temperature is set in 250 DEG C, after reaction 72h, take out reactor, make its naturally cooling, by mixture suction filtration in reactor, and with distilled water and dehydrated alcohol repetitive scrubbing, suction filtration, last in vacuum drying oven dry 24h at 100 DEG C, collect sample retention in moisture eliminator.
More than describe preferred embodiment of the present invention in detail.Should be appreciated that the ordinary skill of this area just design according to the present invention can make many modifications and variations without the need to creative work.Therefore, all technician in the art, all should by the determined protection domain of claims under this invention's idea on the basis of existing technology by the available technical scheme of logical analysis, reasoning, or a limited experiment.
Claims (10)
1. the preparation method of Graphene and two nickelous selenide matrix materials, it is characterized in that, the method comprises the following steps:
(1) reductive agent mixes with graphene oxide solution, stirs and adds in polytetrafluoro inner liner stainless steel reactor after forming brown solution;
(2) load in reactor containing selenium material and nickeliferous inorganic salt;
(3) capping still reacts;
(4) naturally cooling after reaction, by mixture suction filtration in reactor, and with distilled water and dehydrated alcohol repetitive scrubbing, suction filtration;
(5) dry rear product of collecting is preserved.
2. the preparation method of Graphene according to claim 1 and two nickelous selenide matrix materials, it is characterized in that, step (1) described graphene oxide solution is in one or more solvents in graphene oxide is water-soluble, pyridine, tetrahydrofuran (THF), ethanol, methyl alcohol, DMF, NMP.
3. the preparation method of Graphene according to claim 1 and 2 and two nickelous selenide matrix materials, is characterized in that, the described graphene oxide solution concentration of step (1) is 0.1 ~ 20mg/mL.
4. the preparation method of Graphene according to claim 1 and two nickelous selenide matrix materials, it is characterized in that, step (1) described reductive agent is: one or more in hydrazine, hydrazine hydrate, dimethylhydrazine, vitamins C, hydrogen iodide, sodium borohydride, formaldehyde, acetaldehyde, Resorcinol, Ursol D, quadrol, butanediamine.
5. the preparation method of Graphene according to claim 1 and two nickelous selenide matrix materials, is characterized in that, containing selenium material described in step (2) is elemental selenium, Sodium Selenite, potassium selenite or tin anhydride; Described nickeliferous inorganic salt are nickelous oxalate, nickelous chloride, single nickel salt, nickelous nitrate or nickelous perchlorate.
6. the preparation method of Graphene and two nickelous selenide matrix materials according to claim 1 or 5, is characterized in that, is 2 ~ 3:1 containing the mol ratio of selenium material and nickeliferous inorganic salt described in step (2).
7. the preparation method of Graphene according to claim 1 and two nickelous selenide matrix materials, is characterized in that, described in step (2), the volume ratio of reductive agent and graphene oxide solution is 5 ~ 10:10 ~ 50.
8. the preparation method of Graphene according to claim 1 and two nickelous selenide matrix materials, is characterized in that, described in step (3), temperature of reaction is 100 ~ 250 DEG C, and the reaction times is 0.5 ~ 72 hour.
9. the preparation method of Graphene according to claim 1 and two nickelous selenide matrix materials, is characterized in that, described in step (5), drying temperature is 40 ~ 100 DEG C, and time of drying is 0.5 ~ 24 hour.
10. what the preparation method described in claim 1 ~ 9 prepared is Graphene and two nickelous selenide matrix materials, and the pattern of two nickelous selenides is nanometer spherical particulate state, and median size is 5 ~ 20nm.
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| CN105609745A (en) * | 2016-03-27 | 2016-05-25 | 华南理工大学 | Nickel selenide/graphene sodium ion battery composite negative material as well as preparation method and application thereof |
| CN106024395A (en) * | 2016-07-01 | 2016-10-12 | 淮阴工学院 | Preparation method and application of foamed nickel-based Ni3Se2 nano material |
| CN106206042A (en) * | 2016-08-10 | 2016-12-07 | 三峡大学 | A kind of DSSC NiSe preparation method to electrode |
| CN106587028A (en) * | 2017-02-09 | 2017-04-26 | 山东佳星环保科技有限公司 | Method of preparing graphene by oxidation and reduction process |
| CN108376612A (en) * | 2018-01-24 | 2018-08-07 | 复旦大学 | Preparation method of the used by dye sensitization solar battery graphene/nickelous selenide to electrode |
| CN109273281A (en) * | 2018-08-27 | 2019-01-25 | 重庆大学 | A kind of NiSe2/Ti3C2TxThe preparation method of high-performance ultra-capacitor nanocomposite |
| CN110327946A (en) * | 2019-08-09 | 2019-10-15 | 黑龙江科技大学 | A kind of molybdenum disulfide/nickelous selenide composite material and preparation method and application |
| CN110660981A (en) * | 2019-09-28 | 2020-01-07 | 华南理工大学 | Graphene-coated bimetallic selenide material and preparation method and application thereof |
| CN110683521A (en) * | 2019-10-16 | 2020-01-14 | 蚌埠学院 | Preparation and sodium-electricity application of nickel diselenide-graphene composite material |
| CN111203243A (en) * | 2020-01-19 | 2020-05-29 | 西北师范大学 | Preparation and application of nickel selenide/graphene composite material |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105609745A (en) * | 2016-03-27 | 2016-05-25 | 华南理工大学 | Nickel selenide/graphene sodium ion battery composite negative material as well as preparation method and application thereof |
| CN105609745B (en) * | 2016-03-27 | 2018-09-14 | 华南理工大学 | A kind of nickelous selenide NiSe2/ graphenes sodium-ion battery composite negative pole material and the preparation method and application thereof |
| CN106024395A (en) * | 2016-07-01 | 2016-10-12 | 淮阴工学院 | Preparation method and application of foamed nickel-based Ni3Se2 nano material |
| CN106206042A (en) * | 2016-08-10 | 2016-12-07 | 三峡大学 | A kind of DSSC NiSe preparation method to electrode |
| CN106587028A (en) * | 2017-02-09 | 2017-04-26 | 山东佳星环保科技有限公司 | Method of preparing graphene by oxidation and reduction process |
| CN108376612A (en) * | 2018-01-24 | 2018-08-07 | 复旦大学 | Preparation method of the used by dye sensitization solar battery graphene/nickelous selenide to electrode |
| CN109273281A (en) * | 2018-08-27 | 2019-01-25 | 重庆大学 | A kind of NiSe2/Ti3C2TxThe preparation method of high-performance ultra-capacitor nanocomposite |
| CN110327946A (en) * | 2019-08-09 | 2019-10-15 | 黑龙江科技大学 | A kind of molybdenum disulfide/nickelous selenide composite material and preparation method and application |
| CN110327946B (en) * | 2019-08-09 | 2022-02-08 | 哈尔滨师范大学 | Molybdenum disulfide/nickel selenide composite material and preparation method and application thereof |
| CN110660981A (en) * | 2019-09-28 | 2020-01-07 | 华南理工大学 | Graphene-coated bimetallic selenide material and preparation method and application thereof |
| CN110660981B (en) * | 2019-09-28 | 2022-06-21 | 华南理工大学 | Graphene-coated bimetallic selenide material and preparation method and application thereof |
| CN110683521A (en) * | 2019-10-16 | 2020-01-14 | 蚌埠学院 | Preparation and sodium-electricity application of nickel diselenide-graphene composite material |
| CN111203243A (en) * | 2020-01-19 | 2020-05-29 | 西北师范大学 | Preparation and application of nickel selenide/graphene composite material |
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