CN102910615A - Preparation method of graphene oxide/iron disulfide composite nano particles - Google Patents
Preparation method of graphene oxide/iron disulfide composite nano particles Download PDFInfo
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- CN102910615A CN102910615A CN2012103033900A CN201210303390A CN102910615A CN 102910615 A CN102910615 A CN 102910615A CN 2012103033900 A CN2012103033900 A CN 2012103033900A CN 201210303390 A CN201210303390 A CN 201210303390A CN 102910615 A CN102910615 A CN 102910615A
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Abstract
The invention relates to nano FeS2 materials, and particularly relates to a preparation method of graphene oxide/iron disulfide composite nano particles. According to the preparation method of the graphene oxide/iron disulfide composite nano particles, ferrous chloride tetrahydrate (FeCl2.4H2O) and sulfur powder are used as raw materials, are dissolved in water together with surfactant polyvinyl alcohol (PVA) and polyvinylpyrrolidone (PVP), and then mixed with graphene oxide under a certain pH (potential of hydrogen) condition; the obtained mixed solution is arranged in a reaction kettle and sealed, is held for 12 hours to 24 hours in a constant-temperature box at 180 DEG C to 200 DEG C by using a hydrothermal method, is cooled to normal temperature, stood and separated, centrifugally washed and dried, finally the graphene oxide/iron disulfide composite nano particles can be obtained.
Description
Technical field
The present invention relates to nanometer Fe S
2Material particularly, is a kind of graphene oxide/pyrite (GO/FeS
2) the composite nanometer particle preparation method.
Background technology
The FeS of isometric system
2Has suitable energy gap, higher photoabsorption coefficient, the element reserves are abundant, Environmental compatibility is good, preparation cost is lower, more have good photovoltaic conversion performance, the researchist has launched intensive research around many-sides such as its crystalline structure, photoelectric properties, photoelectrochemical behaviour, film technique and electrooptical device application in recent decades, so that FeS
2Obtained significant progress in the application aspect the depolarized anode material of photoelectrochemical cell, lithium ion battery and hydrogen manufacturing device.
Because nanometer Fe S
2Material more has its special characteristics, development in recent years low-dimensional FeS
2The preparations of nanomaterials method.Mainly contain: electrochemical deposition method, hydrothermal method, solvent-thermal method and mechanical ball milling method etc., the having relatively high expectations of electrochemical deposition method in this several method must have S
2-Existence, and the mechanical ball milling method is difficult to solve FeS
2Oxidized problem, so hydrothermal method and solvent-thermal method are comparatively ideal, but its requirement is still very high, for example, Qian etc. adopt the solvent thermal synthetic technology, make particulate state FeS take toluene as solvent
2Powder crystal; Obtained to have the FeS of irregular pattern take quadrol as solvent
2Nanometer rod, but aforesaid method need to be tested under anhydrous state having relatively high expectations of testing.
The present invention adopts one step hydro thermal method synthetic, introduces tensio-active agent, has simplified processing step, has effectively solved to a certain extent size and the homogeneity question of pyrite particle.
Summary of the invention
The object of the present invention is to provide a kind of graphene oxide/pyrite (GO/FeS
2) the composite nanometer particle preparation method, utilize the premium properties raising of Graphene and expand pyrite in performance and the application of the aspects such as photoelectricity, the size that the method can solve the pyrite nano particle reaches easily oxidized problem, and the pyrite nano particle for preparing all has highly same tropism in size and growth orientation.
Above-mentioned purpose is achieved by the following technical solution:
With Iron dichloride tetrahydrate (FeCl
24H
2O), the sulphur powder is raw material, be dissolved in the water with surface active agent polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP), under certain PH condition, mix with graphene oxide, the mixing solutions that obtains places reactor, after the sealing, adopt hydrothermal method 180-200 ° of C insulation 12-24 h in thermostat container, be cooled to room temperature, standing separation can get graphene oxide/pyrite composite nanometer particle after the centrifuge washing drying.
Particularly, comprise the steps:
(1) with Iron dichloride tetrahydrate (FeCl
24H
2O) be dissolved in the deionized water, be stirred to dissolving, obtain the solution that concentration is 0.04-0.08 mol/L;
(2) be that 3% PVA solution and PVP add in the mentioned solution with massfraction, stirring and dissolving, the volume ratio of PVA solution and deionized water are 1:4-3:4, and PVP is 1:2-2:1 with the ratio of Iron dichloride tetrahydrate amount of substance;
(3) stirring is lower dropwise adds sodium hydroxide solution in mentioned solution, sodium hydroxide is 4:1-2:1 with the ratio of Iron dichloride tetrahydrate amount of substance;
(4) in mentioned solution, add the sulphur powder, stirring and dissolving, the sulphur powder is 4:1-7:1 with the ratio of Iron dichloride tetrahydrate amount of substance;
(5) add graphene oxide in mentioned solution, ultra-sonic dispersion is to even, and the mass ratio of graphene oxide and Iron dichloride tetrahydrate material is 6:1-4:1;
(6) mentioned solution is changed in the stainless steel cauldron, carry out the hydro-thermal reaction of 12-24 h under 180-200 ° of C environment, cooling is left standstill, and can get graphene oxide/pyrite composite nanometer particle after centrifugal.
Method provided by the present invention, production technique is simple and easy to control, the graphene oxide of preparation gained/pyrite nano particle diameter size uniform, good dispersity has good potential application foreground in fields such as solar energy photoelectric conversion technology, specific function electrode materials and electromagnetic materials.
Description of drawings
Fig. 1 is the SEM figure of the graphene oxide/pyrite composite nanometer particle of embodiment 2;
Fig. 2 is the XRD spectra of the graphene oxide/pyrite composite nanometer particle of embodiment 2;
Fig. 3 is the SEM figure of the graphene oxide/pyrite composite nanometer particle of embodiment 3;
Fig. 4 is the SEM figure of the graphene oxide/pyrite composite nanometer particle of embodiment 4;
Fig. 5 is the SEM figure of the graphene oxide/pyrite composite nanometer particle of embodiment 5.
Embodiment
Below further describe the present invention by embodiment, as known by the technical knowledge, the present invention also can describe by other the scheme that does not break away from the technology of the present invention feature, thus all within the scope of the present invention or the change that is equal in the scope of the invention all be included in the invention.
Embodiment 1:
Under ice bath, it is in 98% the vitriol oil that 0.015 g Graphite Powder 99 is distributed to 25 mL massfractions, stirs the lower potassium permanganate (KMnO that adds
4), institute adds potassium permanganate (KMnO
4) with the mass ratio of graphite be 3:1-4:1, stir, treat that temperature rises to 30 ℃, stir the deionized water of lower 45 mL of adding, and 15 mL mass concentrations are 30% H
2O
2, after stirring, centrifugation obtains the stannic oxide/graphene nano sheet behind hydrochloric acid soln, deionized water and the acetone repetitive scrubbing with mass concentration 5%.
Embodiment 2:
(1) with 0.2 g Iron dichloride tetrahydrate (FeCl
24H
2O) be dissolved in the 20 mL deionized waters, be stirred to dissolving and obtain the solution I;
(2) in the solution I, add 10 mL PVA solution (massfraction is 3%), 0.05 g PVP, dropwise add 0.75 mol/L sodium hydroxide, 5 mL after stirring and obtain the solution II;
(3) add 0.2 g sulphur powder in the solution II, stirring and dissolving obtains the solution III;
(4) add 50 mg graphene oxides in the solution III, ultra-sonic dispersion is to evenly getting solution
(5) with solution
Carry out the hydro-thermal reaction of 12 h under 180 ° of C environment, cooling is left standstill and can be got the pyrite nano particle after centrifugal, uses scanning electron microscope that prepared sample is carried out microscopic appearance and observes, the result as shown in Figure 1, sample is size uniform, the globosity of good dispersity, and mean diameter is about 300 nm.
Embodiment 3:
(1) with 0.3 g Iron dichloride tetrahydrate (FeCl
24H
2O) be dissolved in the 20 mL deionized waters, be stirred to dissolving and obtain the solution I;
(2) in the solution I, add 10 mL PVA solution (massfraction is 3%), 0.1 g PVP, dropwise add 0.75 mol/L sodium hydroxide, 5 mL after stirring and obtain the solution II;
(3) add 0.2 g sulphur powder in the solution II, stirring and dissolving obtains the solution III;
(4) add 50 mg graphene oxides in the solution III, ultra-sonic dispersion is to evenly getting solution
(5) solution
Under 200 ° of C environment, carry out the hydro-thermal reaction of 24 h, cooling is left standstill and can be got Graphene/pyrite composite nanometer particle after centrifugal, using scanning electron microscope that prepared sample is carried out microscopic appearance observes, the result as shown in Figure 2, sample is size uniform, the octahedral structure of good dispersity, mean diameter are about 1 μ m; Sample is carried out X-ray diffraction, the result as shown in Figure 3, gained sample better crystallinity degree occurs without assorted peak, and is in full accord with the PDF card of pyrite, do not occur the diffraction peak of Graphene among the figure, may be because the characteristic peak intensity of Graphene causes a little less than too.
Embodiment 4:
(1) with 0.25 g Iron dichloride tetrahydrate (FeCl
24H
2O) be dissolved in the 20 mL deionized waters, be stirred to dissolving and obtain the solution I;
(2) in the solution I, add 10 mL PVA solution (massfraction is 3%), 0.2 g PVP, dropwise add 0.75 mol/L sodium hydroxide, 5 mL after stirring and obtain the solution II;
(3) add 0.2 g sulphur powder in the solution II, stirring and dissolving obtains the solution III;
(4) add 50 mg graphene oxides in the solution III, ultra-sonic dispersion is to evenly getting solution
(5) solution
Under 180 ° of C environment, carry out the hydro-thermal reaction of 12 h, cooling is left standstill and can be got Graphene/pyrite composite nanometer particle after centrifugal, using scanning electron microscope that prepared sample is carried out microscopic appearance observes, the result as shown in Figure 4, sample is size uniform, dispersiveness is octahedral structure preferably, and mean diameter is about 1 μ m.
Embodiment 5:
(1) with 0.2 g Iron dichloride tetrahydrate (FeCl
24H
2O) be dissolved in the 20 mL deionized waters, be stirred to dissolving and obtain the solution I;
(2) in the solution I, add 10 mL PVA solution (massfraction is 3%), 0.3 g PVP, dropwise add 0.75 mol/L sodium hydroxide, 5 mL after stirring and obtain the solution II;
(3) add 0.2 g sulphur powder in the solution II, stirring and dissolving obtains the solution III;
(4) add 50 mg graphene oxides in the solution III, ultra-sonic dispersion is to evenly getting solution
(5) with solution
Under 200 ° of C environment, carry out the hydro-thermal reaction of 12 h, cooling is left standstill and can be got Graphene/pyrite composite nanometer particle after centrifugal, using scanning electron microscope that prepared sample is carried out microscopic appearance observes, the result as shown in Figure 5, sample is the octahedral structure of size uniform, mean diameter is about 1 μ m, and sample surfaces has a small amount of film sample material to cover, and this may be because the amount adding of tensio-active agent PVP too much causes.
Claims (1)
1. the preparation method of graphene oxide/pyrite composite nanometer particle, described graphene oxide/pyrite composite nanometer particle, size uniform, good dispersity, pattern is sphere or octahedral structure, it is characterized in that comprising the steps:
(1) Iron dichloride tetrahydrate is dissolved in the deionized water, is stirred to dissolving, obtain the solution that concentration is 0.04-0.08 mol/L;
(2) be that 3% PVA solution and PVP add in the mentioned solution with massfraction, stirring and dissolving, the volume ratio of PVA solution and deionized water are 1:4-3:4, and PVP is 1:2-2:1 with the ratio of Iron dichloride tetrahydrate amount of substance;
(4) stirring is lower dropwise adds sodium hydroxide solution in mentioned solution, sodium hydroxide is 4:1-2:1 with the ratio of Iron dichloride tetrahydrate amount of substance;
(5) in mentioned solution, add the sulphur powder, stirring and dissolving, the sulphur powder is 4:1-7:1 with the ratio of Iron dichloride tetrahydrate amount of substance;
(6) add graphene oxide in mentioned solution, ultra-sonic dispersion is to even, and the mass ratio of graphene oxide and Iron dichloride tetrahydrate material is 6:1-4:1;
(7) mentioned solution is changed in the stainless steel cauldron, carry out the hydro-thermal reaction of 12-24 h under 180-200 ° of C environment, cooling is left standstill, and can get graphene oxide/pyrite composite nanometer particle after centrifugal.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103326002A (en) * | 2013-06-26 | 2013-09-25 | 冯林杰 | Preparation method of graphene and ferrous disulfide composite positive electrode material |
| CN103602362A (en) * | 2013-11-21 | 2014-02-26 | 镇江市高等专科学校 | Preparation method of ferrous disulfide-graphene composite nano lubricant |
| CN106784829A (en) * | 2017-01-10 | 2017-05-31 | 哈尔滨工业大学 | A kind of preparation method for loading Graphene and the anode of microbial fuel cell of ferrous disulfide compound |
| CN107090586A (en) * | 2017-04-13 | 2017-08-25 | 上海应用技术大学 | A kind of FeS2RGO composites, preparation method and applications |
| CN107308956A (en) * | 2017-06-23 | 2017-11-03 | 哈尔滨工业大学 | A kind of preparation method of the efficient many iron sulfide of out-phase class fenton catalyst |
| CN108144631A (en) * | 2017-12-25 | 2018-06-12 | 中国科学技术大学 | The preparation method of transition metal sulfide catalyst, preparation method and aromatic amine compound |
| CN109192550A (en) * | 2018-09-11 | 2019-01-11 | 上海应用技术大学 | A kind of redox graphene self-supporting film of inorganic nanoparticles load, preparation method and application |
| CN109626444A (en) * | 2019-01-18 | 2019-04-16 | 哈尔滨工业大学 | A kind of spherical FeS of multi-pore channel sub-micron2Preparation method |
| CN110085435A (en) * | 2019-04-15 | 2019-08-02 | 东北大学 | Nitrogen sulfur doping iron sulfide/graphene aerogel composite material and preparation method |
| CN110745869A (en) * | 2019-11-11 | 2020-02-04 | 青岛科技大学 | FeS nano-particles synthesized based on solvothermal method, preparation method and application |
| CN111717909A (en) * | 2020-05-28 | 2020-09-29 | 济南大学 | Preparation method of sandwich type photoelectrochemical sensor for detecting procalcitonin by using fullerene-stannic oxide |
| CN113201758A (en) * | 2021-04-08 | 2021-08-03 | 哈尔滨理工大学 | FeS2Preparation method and application of @ GO nitrogen fixation catalyst |
-
2012
- 2012-08-24 CN CN2012103033900A patent/CN102910615A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| BEI WANG ETAL: "Solvothermal synthesis of CoS2-graphene nanocomposite material for high-performance supercapacitors", 《JOURNAL OF MATERIALS CHEMISTRY》 * |
| DEWEI WANG ETAL: "Shape controlled growth of pyrite FeS2 crystallites via a polymer-assisted hydrothermal route", 《CRYSTENQCOMM》 * |
Cited By (18)
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| CN103326002B (en) * | 2013-06-26 | 2015-11-04 | 国网浙江嵊州市供电公司 | The preparation method of a kind of Graphene-ferrous disulfide composite positive pole |
| CN103326002A (en) * | 2013-06-26 | 2013-09-25 | 冯林杰 | Preparation method of graphene and ferrous disulfide composite positive electrode material |
| CN103602362A (en) * | 2013-11-21 | 2014-02-26 | 镇江市高等专科学校 | Preparation method of ferrous disulfide-graphene composite nano lubricant |
| CN103602362B (en) * | 2013-11-21 | 2015-04-29 | 镇江市高等专科学校 | Preparation method of ferrous disulfide-graphene composite nano lubricant |
| CN106784829B (en) * | 2017-01-10 | 2019-04-30 | 哈尔滨工业大学 | A kind of preparation method of load graphene and the anode of microbial fuel cell of ferrous disulfide compound |
| CN106784829A (en) * | 2017-01-10 | 2017-05-31 | 哈尔滨工业大学 | A kind of preparation method for loading Graphene and the anode of microbial fuel cell of ferrous disulfide compound |
| CN107090586A (en) * | 2017-04-13 | 2017-08-25 | 上海应用技术大学 | A kind of FeS2RGO composites, preparation method and applications |
| CN107308956A (en) * | 2017-06-23 | 2017-11-03 | 哈尔滨工业大学 | A kind of preparation method of the efficient many iron sulfide of out-phase class fenton catalyst |
| CN108144631A (en) * | 2017-12-25 | 2018-06-12 | 中国科学技术大学 | The preparation method of transition metal sulfide catalyst, preparation method and aromatic amine compound |
| CN108144631B (en) * | 2017-12-25 | 2020-12-25 | 中国科学技术大学 | Transition metal sulfide catalyst, method for producing same, and method for producing aromatic amine compound |
| CN109192550A (en) * | 2018-09-11 | 2019-01-11 | 上海应用技术大学 | A kind of redox graphene self-supporting film of inorganic nanoparticles load, preparation method and application |
| CN109626444A (en) * | 2019-01-18 | 2019-04-16 | 哈尔滨工业大学 | A kind of spherical FeS of multi-pore channel sub-micron2Preparation method |
| CN109626444B (en) * | 2019-01-18 | 2021-03-23 | 哈尔滨工业大学 | Porous channel submicron spherical FeS2Preparation method of (1) |
| CN110085435A (en) * | 2019-04-15 | 2019-08-02 | 东北大学 | Nitrogen sulfur doping iron sulfide/graphene aerogel composite material and preparation method |
| CN110745869A (en) * | 2019-11-11 | 2020-02-04 | 青岛科技大学 | FeS nano-particles synthesized based on solvothermal method, preparation method and application |
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| CN111717909B (en) * | 2020-05-28 | 2022-07-01 | 济南大学 | Preparation method of sandwich type photoelectrochemical sensor for detecting procalcitonin by using fullerene-stannic oxide |
| CN113201758A (en) * | 2021-04-08 | 2021-08-03 | 哈尔滨理工大学 | FeS2Preparation method and application of @ GO nitrogen fixation catalyst |
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Application publication date: 20130206 |