CN109273281A - A kind of NiSe2/Ti3C2TxThe preparation method of high-performance ultra-capacitor nanocomposite - Google Patents
A kind of NiSe2/Ti3C2TxThe preparation method of high-performance ultra-capacitor nanocomposite Download PDFInfo
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- 239000003990 capacitor Substances 0.000 title claims abstract description 20
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229910009819 Ti3C2 Inorganic materials 0.000 claims abstract description 39
- QHASIAZYSXZCGO-UHFFFAOYSA-N selanylidenenickel Chemical compound [Se]=[Ni] QHASIAZYSXZCGO-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 10
- 239000002738 chelating agent Substances 0.000 claims abstract description 5
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000002131 composite material Substances 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 239000013049 sediment Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- 229960001484 edetic acid Drugs 0.000 claims 3
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical class NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims 1
- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 claims 1
- 150000001336 alkenes Chemical class 0.000 claims 1
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 17
- 239000007772 electrode material Substances 0.000 abstract description 8
- 238000004146 energy storage Methods 0.000 abstract description 7
- 239000002105 nanoparticle Substances 0.000 abstract description 3
- 239000011232 storage material Substances 0.000 abstract description 2
- 238000012546 transfer Methods 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract 2
- 229910009818 Ti3AlC2 Inorganic materials 0.000 abstract 1
- 238000005260 corrosion Methods 0.000 abstract 1
- 230000007797 corrosion Effects 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- -1 Transition metal selenides Chemical class 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 239000011149 active material Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- XUCNUKMRBVNAPB-UHFFFAOYSA-N fluoroethene Chemical compound FC=C XUCNUKMRBVNAPB-UHFFFAOYSA-N 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 2
- 239000011669 selenium Substances 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- HTXDPTMKBJXEOW-UHFFFAOYSA-N iridium(IV) oxide Inorganic materials O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007777 multifunctional material Substances 0.000 description 1
- 239000002060 nanoflake Substances 0.000 description 1
- 239000002055 nanoplate Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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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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- Materials Engineering (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Composite Materials (AREA)
- Manufacturing & Machinery (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
A kind of NiSe2/Ti3C2TxThe preparation method of high-performance ultra-capacitor nanocomposite, belongs to energy storage material technical field.The present invention is with NiSe2With Ti3C2TxIt combines and prepares the good electrode material for super capacitor of chemical property.More particularly to one kind using LiF and HCl as corrosive liquid, by Ti3AlC2Al layer corrosion, obtain Ti3C2Tx, then by Se powder and NiCl2It mixes by certain mol proportion, is reacted under the action of chelating agent, generate NiSe2Nano particle, while Ti3C2TxThin slice is deposited on NiSe2On particle, finally by washing, drying, electrode material for super capacitor is obtained.The present invention NiSe high using theoretical specific capacitance2Material, and have the shortcomings that electric conductivity is bad for it, using hydro-thermal method, by the good Ti of electric conductivity3C2TxNanometer sheet and NiSe2Particles dispersed obtains NiSe2/Ti3C2TxNanocomposite makes material possess better electric charge transfer and more available active site, and improves NiSe2/Ti3C2TxThe durability of nanocomposite, to improve the performance of supercapacitor.
Description
Technical field
The present invention relates to a kind of NiSe2/Ti3C2TxThe preparation method of high-performance super capacitor nanocomposite, belongs to
A kind of energy storage material technical field, and in particular to preparation method of electrode material for super capacitor.The technical characterstic of this method exists
In the NiSe that theoretical specific capacitance is high2The Ti of material and good conductivity3C2TxMaterial carries out compound, excellent super of processability
Capacitor electrode material.
Background technique
The continuous growth of sustainable clean energy resource and renewable energy demand, is greatly facilitated energy storage and transformation technology
Development.In various energy storage devices, supercapacitor (SCs) has energy density high, has extended cycle life and charge and discharge
The advantages that electric rate is fast, can provide energy more higher than ordinary capacitor and power more higher than secondary cell and longer circulation
Service life becomes portable energy storage apparatus field one of device most with prospects.Currently, being used as the material of supercapacitor
Material mainly has Pt, RuO2、IrO2Deng not being able to satisfy practical application request however, the at high cost of these materials, storage capacity are low.Cause
This, seeking active high, cheap and high energy storage rate material is the top priority for preparing high-performance super capacitor.
Transition metal selenides, such as CoSe2、PtSe2、FeSe2、NiSe2Deng, electro-chemical activity with higher, good
Electric conductivity and thermal stability, wherein selenium nickel compound has been applied to chargeable due to unique electronic structure and multiple oxidation state
Lithium ion battery, super capacitor, elctro-catalyst and photovoltaic cell.Studies have shown that two nickelous selenide (NiSe2) there is good electricity
Chemical activity and high capacity can be used as the multifunctional material of supercapacitor.However, pure NiSe2Cyclical stability it is poor, lead
Electric rate is low, and electro-chemical activity site is insufficient.And by carrying out compound raising performance with conductive material, it is having of solving these problems
One of efficacious prescriptions method.
Mxenes is a kind of New Two Dimensional transition metal carbonitrides material of discovered in recent years, and this material has similar
The conductivity of metal, and because hydroxyl and other oxygen-containing groups are contained in surface, surface hydrophilicity is good.In lithium ion battery and super electricity
The potential purposes of many of container, research find Mxenes and other active materials is compound, and changeable active material is led
Electrically, to improve the chemical property of composite material.In presently found more than 20 kinds of Mxenes materials, Ti3C2TxResearch
At most and electric conductivity is best.Therefore, Ti is used3C2TxNano flake and NiSe2Nano-particles reinforcement prepares NiSe2/Ti3C2TxIt is multiple
Condensation material is used as electrode material, can overcome NiSe2The disadvantage of material conductivity difference, plays the synergistic effect of two kinds of materials, is expected to
The electrode material for super capacitor haveing excellent performance is prepared, and yet there are no relevant report in document at present.
Summary of the invention
Present invention aim to address NiSe2There are poorly conductives, energy as electrode material for super capacitor for nano particle
Metric density and the limited problem of endurance quality.
To realize the present invention purpose and the technical solution adopted is that preparing a kind of NiSe2/Ti3C2TxHigh-performance ultra-capacitor
Nanocomposite, which comprises the following steps:
1)Ti3C2TxThe preparation of nanometer sheet:
1.1) 2g LiF is added in 20ml HCl and is stirred to clarify.
1.2) by the Ti of 2g3AlC2Powder is added in the solution of step 1.1), and solution heats 40 DEG C, and constant temperature keeps 48h,
Solution after reaction is repeatedly washed with deionized water, is centrifuged, until supernatant liquor pH is about 6.
1.3) solid for being centrifuged step 1.2), 60 DEG C of vacuum drying 12h, obtains Ti3C2Tx powder.
1.4) step 1.3) Ti obtained is weighed3C2Tx powder 100mg, is added in the water of 10ml, and solution is carried out ultrasound
Processing, can be obtained 10mgmL-1Ti3C2TxThin slice solution.
2)NiSe2/Ti3C2TxThe preparation of nanocomposite:
2.1) 1-4mmol Se powder is dissolved in 5ml KOH solution, forms maroon solution.
2.2)0.5-2mmol NiCl2It is dissolved in 19mL deionized water, adds 1.6mmol chelating agent such as ethylenediamine tetraacetic
Acetic acid (EDTA) forms blue solution.
2.3) solution of 1mL step 1.4), ultrasonic disperse 30-60min are added into the solution of step 2.2).
2.4) solution of step 2.3) is added in the solution of step 2.1), is transferred to poly- the four of 50mL after mixing
In vinyl fluoride autoclave, 180 DEG C of reaction 12-24h.
2.5) mixture that step 2.4) obtains obtains sediment, by 60 DEG C of sediment with deionized water centrifugation, washing
Lower vacuum drying 12-24h, obtains NiSe2/Ti3C2TxNanocomposite.
Compared with prior art, the present invention its remarkable advantage is as follows:
(1) the two-dimentional Ti of the invention by good conductivity3C2TxMaterial and the NiSe that electro-chemical activity is good, theoretical specific capacitance is high2
Material progress is rationally compound, prepares Novel super capacitor electrode material；
(2) NiSe prepared by the present invention2/Ti3C2TxNanocomposite not only has good chemical property, but also
There are good structural stability, excellent cyclical stability and high-energy density.It can be widely used for various ultracapacitor energy storages
Element.
(3) preparation method of the invention is simply flexible, and raw material is cheap and easy to get, and composite material can be complete using one step hydro thermal method
At process time is short, economical, environmentally friendly.
Detailed description of the invention
Fig. 1 is NiSe prepared by embodiment 12/Ti3C2TxX-ray powder diffraction (XRD) figure of composite material.
Fig. 2 is NiSe prepared by embodiment 12/Ti3C2TxElectronic Speculum (SEM) figure ((a)) and transmission electron microscope of composite material
(TEM) figure ((b)).
Fig. 3 is NiSe prepared by embodiment 12/Ti3C2TxThe 20mV s of composite material-1Cyclic voltammetry curve.
Fig. 4 is NiSe prepared by embodiment 12/Ti3C2TxComposite material is 1Ag in current density-1Under constant current fill
Discharge curve.
Fig. 5 is NiSe prepared by embodiment 12/Ti3C2TxComposite material capacitor is with current density change curve graph.
Specific embodiment
Below with reference to examples and drawings, the invention will be further described, but should not be construed the above-mentioned theme of the present invention
Range is only limitted to following examples and drawings.Without departing from the idea case in the present invention described above, common according to this field
Technological know-how and customary means make various replacements and change, should all include within the scope of the present invention.
Embodiment 1:
1)Ti3C2TxThe preparation of nanometer sheet:
1.1) 2g LiF is added in 20ml HCl and is stirred to clarify.
1.2) by the Ti of 2g3AlC2Powder is added in the solution of step 1.1), and solution heats 40 DEG C, and constant temperature keeps 48h,
Solution deionized water after reaction is repeatedly washed, is centrifuged, until supernatant liquor pH is about 6.
1.3) solid for being centrifuged step 1.2), 60 DEG C of vacuum drying 12h, obtains Ti3C2Tx powder.
1.4) step 1.3) Ti obtained is weighed3C2Tx powder 100mg, is added in the water of 10ml, and solution is carried out ultrasound
Processing, can be obtained 10mgmL-1Ti3C2TxThin slice solution.
2)NiSe2/Ti3C2TxThe preparation of nanocomposite:
2.1) 2mmol Se powder is dissolved in 5ml KOH solution, forms maroon solution.
2.2)1mmol NiCl2It is dissolved in 19mL deionized water, adds 1.6mmol chelating agent such as L ethylenediamine tetraacetic acid (EDTA)
(EDTA) blue solution is formed.
2.3) solution of 1mL step 1.4), ultrasonic disperse 30min are added into the solution of step 2.2).
2.4) solution of step 2.3) is added in the solution of step 2.1), is transferred to poly- the four of 50mL after mixing
In vinyl fluoride autoclave, 180 DEG C of reactions are for 24 hours.
2.5) mixture that step 2.4) obtains obtains sediment, by 60 DEG C of sediment with deionized water centrifugation, washing
Lower vacuum drying 12h, obtains NiSe2/Ti3C2TxComposite material is fabricated to supercapacitor and carries out chemical property survey.
XRD (Fig. 1), SEM and TEM (Fig. 2) test show NiSe prepared by the present invention2For octahedron, Ti3C2TxNanometer
Piece is attached to its surface, particularly, in electrochemical process, Ti3C2TxNano-plates play an important role, it not only ensure that
Quick electric conductivity makes material possess better electric charge transfer and more available active site, and improves NiSe2/
Ti3C2TxThe durability of nanocomposite, to improve the performance of supercapacitor.
Embodiment 2:
Remove step 2) NiSe2/Ti3C2TxThe preparation of nanocomposite, other conditions obtain NiSe with embodiment 12,
It is fabricated to supercapacitor and carries out chemical property survey.
Claims (4)
1. a kind of NiSe2/Ti3C2TxThe preparation method of high-performance ultra-capacitor nanocomposite, it is characterised in that: including following
Step:
1)Ti3C2TxThe preparation of nanometer sheet:
1.1) 2g LiF is added in 20ml HCl and is stirred to clarify；
1.2) by the Ti of 2g3AlC2Powder is added in the solution of step 1.1), and solution heats 40 DEG C, and constant temperature keeps 48h, reaction
Solution deionized water afterwards is repeatedly washed, is centrifuged, until supernatant liquor pH is about 6；
1.3) solid for being centrifuged step 1.2), 60 DEG C of vacuum drying 12h, obtains Ti3C2Tx powder；
1.4) step 1.3) Ti obtained is weighed3C2Tx powder 100mg, is added in the water of 10ml, and solution is carried out at ultrasound
Reason, can be obtained 10mgmL-1Ti3C2TxThin slice solution；
2)NiSe2/Ti3C2TxThe preparation of nanocomposite:
2.1) 1-4mmol Se powder is dissolved in 5ml KOH solution, forms maroon solution；
2.2)0.5-2mmol NiCl2It is dissolved in 19mL deionized water, adds 1.6mmol chelating agent such as ethylenediamine tetra-acetic acid
(EDTA) blue solution is formed；
2.3) solution of 1mL step 1.4), ultrasonic disperse 30-60min are added into the solution of step 2.2)；
2.4) solution of step 2.3) is added in the solution of step 2.1), is transferred to the polytetrafluoroethyl-ne of 50mL after mixing
In alkene autoclave, 180 DEG C of reaction 12-24h；
2.5) mixture that step 2.4) obtains obtains sediment with deionized water centrifugation, washing, will be true at 60 DEG C of sediment
The dry 12-24h of sky, obtains NiSe2/Ti3C2TxComposite material is fabricated to supercapacitor and carries out chemical property survey.
2. a kind of NiSe according to claim 12/Ti3C2TxThe preparation method of high-performance ultra-capacitor nanocomposite, it is special
Sign is, the step 2.1) and Se powder and NiCl 2.2)2Molar ratio be 2: 1.
3. a kind of NiSe according to claim 12/Ti3C2TxThe preparation method of high-performance ultra-capacitor nanocomposite, it is special
Sign is that the chelating agent of the step 2.2) is not limited only to EDTA, further includes aminotriacetic acid (NTA), diethylenetriamines five
Acetic acid (DTPA) etc..
4. a kind of NiSe according to claim 12/Ti3C2TxThe preparation method of high-performance ultra-capacitor nanocomposite, it is special
Sign is that the method for the step 2.4) is hydro-thermal method.
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| CN110038604A (en) * | 2019-05-10 | 2019-07-23 | 辽宁大学 | CuCo/Ti3C2TxComposite material and preparation method and application |
| CN113628890A (en) * | 2021-08-06 | 2021-11-09 | 西南大学 | Bimetallic selenide composite Ti3C2Preparation method of material, product thereof and super capacitor |
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| CN113628890A (en) * | 2021-08-06 | 2021-11-09 | 西南大学 | Bimetallic selenide composite Ti3C2Preparation method of material, product thereof and super capacitor |
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| CN109273281B (en) | 2023-03-31 |
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