CN107591253A - A kind of ultracapacitor graphene/zinc sulfide nano-material and preparation method thereof - Google Patents
A kind of ultracapacitor graphene/zinc sulfide nano-material and preparation method thereof Download PDFInfo
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- CN107591253A CN107591253A CN201710806468.3A CN201710806468A CN107591253A CN 107591253 A CN107591253 A CN 107591253A CN 201710806468 A CN201710806468 A CN 201710806468A CN 107591253 A CN107591253 A CN 107591253A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 53
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 35
- 239000005083 Zinc sulfide Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229910052984 zinc sulfide Inorganic materials 0.000 title claims abstract description 13
- 239000002131 composite material Substances 0.000 claims abstract description 28
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000000137 annealing Methods 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 11
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002105 nanoparticle Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- -1 graphite alkene Chemical class 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000007772 electrode material Substances 0.000 abstract description 8
- 239000003990 capacitor Substances 0.000 abstract description 6
- 238000013019 agitation Methods 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 description 10
- 239000010410 layer Substances 0.000 description 6
- 238000004146 energy storage Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 150000001336 alkenes Chemical class 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 206010068052 Mosaicism Diseases 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 210000003765 sex chromosome Anatomy 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention discloses a kind of ultracapacitor graphene/zinc sulfide nano-material and preparation method thereof, the graphene is two-dimensional layered structure, and zinc sulphide is graininess, and size is 30 100nm, the 3nm of graphene thickness about 1, zine sulfide nano particles are uniformly attached on graphene.The invention also discloses the preparation method of above-mentioned composite nano materials, comprise the following steps：1）Graphene powder is mixed with zinc sulfide powder according to certain mass percent, mechanical agitation is well mixed；2）Above-mentioned mixing material is placed in H2Annealed in S atmosphere, atmosphere pressure is normal pressure, 900 1100 DEG C of annealing temperature, annealing time 35 hours；3）After annealing terminates, room temperature is naturally cooled in the H2S atmosphere of normal pressure, obtains graphene/sulfide composite nano materials.Graphene/zinc sulphide composite nano materials electrochemical performance of the present invention, is a kind of preferable electrode material for super capacitor.
Description
Technical field
The present invention relates to the composite nano materials field of grapheme material field, especially graphene and sulfide.
Background technology
In recent years, along with NETWORK STRUCTURE PRESERVING POWER SYSTEM the grid-connected scale of increasingly sophisticated and regenerative resource rapid expansion, electricity
The safety and stability sex chromosome mosaicism of network operation becomes increasingly conspicuous.As one of the problem effective workaround, the application of electric energy storing system
Demand is continuously increased.In existing all kinds of energy storage are not standby, super capacitor utensil high power density and energy efficiency, overlength
Cycle life and relative moderate production cost, thus as high-performance energy storage device ideal chose.Ultracapacitor
Electric double layer capacitance, device and pseudocapacitor are divided into according to its energy storage mechnism.Wherein, double layer capacitor passes through in electrode and electrolyte
Interface forms electric double layer to store electric energy, and pseudocapacitor is then by the way that reversible chemistry occurs in electrode surface or body phase
Inhale the Faradaic processes such as de- or redox and carry out storage energy, although the energy storage mechnism of two class ultracapacitors is different, its electricity
The structure and property of pole material are all undoubtedly the key factors for determining its final performance.
For double layer capacitor, in order to quickly form substantial amounts of double electrical layerses, its electrode material must have larger
Specific surface area, higher electrical conductivity and suitable pore-size distribution.And the porous carbon materials such as most currently used activated carbon
Although with larger specific surface area, its poor electric conductivity hinders the further raising of capacitor performance
Graphene is a kind of two-dimensional layer carbon material of the monoatomic thickness found first in 2004.It is special due to its structure
Property, graphene have a higher electrical conductivity than traditional super capacitance electrode material, bigger specific surface area and more rich
Rich interlayer structure.Based on these good characteristics, graphene is considered as to be best suitable for the alternate electrode material for ultracapacitor
Material one of and be widely studied in recent years.The composite nano materials of graphene and sulfide also have more report.But stone
The composite nano materials of black alkene and sulfide are generally prepared in the solution, and preparation process is complicated, and stability is bad.
The present invention provides a kind of new graphene/sulfide composite nano materials, and provides a kind of simple and easy complete
New preparation method.
The content of the invention
It is contemplated that a kind of simple and easy brand-new graphene/sulfide composite nano materials of invention and its preparation side
Method.
The invention provides a kind of ultracapacitor graphene/zinc sulfide nano-material and preparation method thereof, the stone
Black alkene is two-dimensional layered structure, and the zinc sulphide is graininess, size 30-100nm, graphene thickness about 1-3nm, zinc sulphide
Nano particle is uniformly attached on graphene.
Present invention also offers above-mentioned graphene/zinc sulphide composite nano materials for ultracapacitor and its preparation side
Method, comprise the following steps：
1）By graphene powder and zinc sulfide powder according to mass percent 60~70:40-30 ratio mixing, then machinery stirs
Mix 7 hours, be well mixed；
2）Above-mentioned mixing material is placed in H2Annealed in S atmosphere, atmosphere pressure is normal pressure, 900-1100 DEG C of annealing temperature, is annealed
Hour time 3-5；
3）After annealing terminates, room temperature is naturally cooled in the H2S atmosphere of normal pressure, obtains graphene/sulfide composite Nano material
Material.
The useful achievement of the present invention is：
1）Graphene prepared by the present invention/zinc sulphide composite nano materials and preparation method thereof, graphene are uniformly multiple with sulfide
Close, be firmly combined with, and be compound, no other structures form appearance of two-dimensional layer graphene and Nanoparticulate zinc sulphide,
Structure is homogeneous.
2）Graphene/zinc sulphide composite nano materials of the present invention and preparation method thereof, it is not necessary to use complicated solution
Course of reaction, substantial amounts of chemical reagent can be saved, it is a large amount of to reduce solid waste and the discharge capacity of waste liquid, be advantageous to environment guarantor
Shield.
3）Graphene/zinc sulphide composite nano materials of the present invention and preparation method thereof, equipment is simple, simple process, easily
In operation, suitable for mass industrialized production.
3）Graphene prepared by the present invention/zinc sulphide composite nano materials electrochemical performance, it is a kind of preferably super
Level capacitor electrode material.
Brief description of the drawings
Fig. 1 is the transmission electron microscope for graphene/zinc sulphide composite nano materials that embodiment 1 obtains（TEM）Figure.
Fig. 2 be the obtained graphene/zinc sulphide composite nano materials of embodiment 1 as electrode when cyclic voltammetry curve,
Test the A/g of current density 3.
Embodiment
The invention will be further described with accompanying drawing in conjunction with specific embodiments in face below.
Embodiment 1
1）By graphene powder and zinc sulfide powder according to mass percent 65:35 ratio mixing, then mechanical agitation 7 is small
When, it is well mixed；
2）Above-mentioned mixing material is placed in H2Annealed in S atmosphere, atmosphere pressure is normal pressure, 1000 DEG C of annealing temperature, annealing time 4
Hour；
3）After annealing terminates, room temperature is naturally cooled in the H2S atmosphere of normal pressure, obtains graphene/sulfide composite Nano material
Material.
Morphology analysis is carried out to obtained graphene/sulfide composite nano materials, using transmission electron microscope
（TEM）.Such as the transmission electron microscope that Fig. 1 is graphene/zinc sulphide composite nano materials that the present embodiment obtains（TEM）Figure,
It can be seen that graphene is two-dimensional layered structure in figure, nano particle is uniformly attached on flake graphite alkene, and particle size is
30-100nm, graphene thickness about 1-3nm, the nano particle are zns particle.
Using graphene made from the present embodiment/sulfide composite nano materials as the electrode of ultracapacitor, electricity is carried out
Learn performance test.Test result shows that the electrode material has pseudo capacitance characteristic；Under 1 A/g current density, than
The F/g of electric capacity 1458；When current density increases to 10 A/g, specific capacitance is 1327 F/g, conservation rate 91.0%；As Fig. 2 is
The cyclic voltammetry curve when graphene that the present embodiment obtains/zinc sulphide composite nano materials are as electrode, test current density 3
A/g, after loop test 5000 times, specific capacitance conservation rate is 97.2%, and its cyclical stability is extremely excellent.
Embodiment 2
1）By graphene powder and zinc sulfide powder according to mass percent 60:40 ratio mixing, then mechanical agitation 7 is small
When, it is well mixed；
2）Above-mentioned mixing material is placed in H2Annealed in S atmosphere, atmosphere pressure is normal pressure, 900 DEG C of annealing temperature, annealing time 5
Hour；
3）After annealing terminates, room temperature is naturally cooled in the H2S atmosphere of normal pressure, obtains graphene/sulfide composite Nano material
Material.
Morphology analysis is carried out to graphene made from the present embodiment/sulfide composite nano materials, shown using transmitted electron
Micro mirror（TEM）, pattern is substantially the same manner as Example 1.Using graphene made from the present embodiment/sulfide composite nano materials as
The electrode of ultracapacitor, carry out electrical performance testing.Test result shows that the electrode material has pseudo capacitance special
Property；Under 1 A/g current density, the F/g of specific capacitance 1371；When current density increases to 10 A/g, specific capacitance 1298
F/g, conservation rate 94.7%；After loop test 5000 times, specific capacitance conservation rate is 98.5%, and its specific capacitance is high, and stable circulation
Property is extremely excellent.
Embodiment 3
1）By graphene powder and zinc sulfide powder according to mass percent 70:30 ratio mixing, then mechanical agitation 7 is small
When, it is well mixed；
2）Above-mentioned mixing material is placed in H2Annealed in S atmosphere, atmosphere pressure is normal pressure, 1100 DEG C of annealing temperature, annealing time 3
Hour；
3）After annealing terminates, room temperature is naturally cooled in the H2S atmosphere of normal pressure, obtains graphene/sulfide composite Nano material
Material.
Morphology analysis is carried out to graphene made from the present embodiment/sulfide composite nano materials, shown using transmitted electron
Micro mirror（TEM）, pattern is substantially the same manner as Example 1.Using graphene made from the present embodiment/sulfide composite nano materials as
The electrode of ultracapacitor, carry out electrical performance testing.Test result shows that the electrode material has pseudo capacitance special
Property；Under 1 A/g current density, the F/g of specific capacitance 1542；When current density increases to 10 A/g, specific capacitance 1389
F/g, conservation rate 90.1%；After loop test 5000 times, specific capacitance conservation rate is 97.2%.Its specific capacitance is high, and stable circulation
Property is extremely excellent.
Obviously, although present disclosure has been made complete and clearly described with regard to its disclosed embodiment,
It is not limited only to this, and embodiments described above is only part of the embodiment of the present invention, rather than whole embodiments.It is right
For the personnel of art, obtained institute is made improvements and substitutes to the present invention by the guidance of these statements
There is other embodiment, among the present invention.
Claims (3)
- A kind of 1. ultracapacitor graphene/zinc sulfide nano-material and preparation method thereof, it is characterised in that：The graphene For two-dimensional layered structure, the zinc sulphide is Nanoparticulate, and zine sulfide nano particles are uniformly attached on flake graphite alkene.
- 2. a kind of ultracapacitor graphene/zinc sulfide nano-material and preparation method thereof according to claim 1, its It is characterised by：Zine sulfide nano particles size is 30-100nm, the graphene thickness about 1-3nm.
- 3. a kind of ultracapacitor graphene/zinc sulfide nano-material and its preparation side according to claim 1 or 2 Method, it is characterised in that comprise the following steps：1）By graphene powder and zinc sulfide powder according to mass percent 60~70:40-30 ratio mixing, then stirs 7 Hour, it is well mixed；2）Above-mentioned mixing material is placed in H2Annealed in S atmosphere, atmosphere pressure is normal pressure, 900-1100 DEG C of annealing temperature, during annealing Between 3-5 hours；3）After annealing terminates, room temperature is naturally cooled in the H2S atmosphere of normal pressure, obtains graphene/sulfide composite Nano material Material.
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|---|---|---|---|---|
| CN108232142A (en) * | 2017-12-22 | 2018-06-29 | 中国科学院福建物质结构研究所 | A kind of zinc sulfide/graphene composite material, its preparation method and application |
| CN108766783A (en) * | 2018-06-13 | 2018-11-06 | 常熟理工学院 | A kind of preparation method of fiber/graphene/zinc sulphide flexible electrode material |
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Application publication date: 20180116 |