CN109903999A - A kind of Ti3C2/NiCo2O4Combination electrode material and preparation method thereof - Google Patents
A kind of Ti3C2/NiCo2O4Combination electrode material and preparation method thereof Download PDFInfo
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Abstract
The present invention is a kind of Ti3C2/NiCo2O4Combination electrode material and preparation method thereof.Ti in the combination electrode3C2And NiCo2O4Mass ratio be 1:0.5~1:3.Preparation method includes the following steps: that (1) will pass through pretreated Ti3C2Powder is scattered in ethylene glycol solution；Then cobalt salt, nickel salt and surfactant stirring is added, adds urea, continues to be sufficiently stirred, obtain suspension；(2) suspension for obtaining step (1) carries out 2~16h of hydro-thermal reaction at 160~200 DEG C；(3) it takes product obtained in step (2) to calcine 1~4 hour at 300~400 DEG C, Ti is made3C2/NiCo2O4Composite powder material.In the composite material that the present invention synthesizes, NiCo2O4Nano particle is evenly distributed on the Ti of stratiform3C2The surface of particle and interlayer form stable Ti3C2/NiCo2O4Nano composite structure, and there is biggish specific capacitance and preferable stable charge/discharge.
Description
Technical field
The invention belongs to combination electrode material and its preparation technical field, in particular to a kind of Ti3C2/NiCo2O4Electrode material
Material and preparation method thereof.
Background technique
Supercapacitor is a kind of electrochemical energy storage equipment, it combines the traditional storage of battery high energy amount and tradition
The advantages of capacitor high power transmission, has higher power and more long circulation life.And electrode material is to determine super capacitor
The performance of device and the key of cost.
It can be from Ti using HF caustic solution3AlC2Material prepares a kind of novel two-dimensional layered structure compound
Ti3C2T (T=O, F, OH) (M.Naguib, M.Kurtoglu, V.Presser, J.Lu, J.J.Niu, M.Heon, L.Hultman,
Y.Gogotsi,M.W.Barsoum.Two-dimensional nanocrystals produced by exfoliation of
Ti3AlC2.Adv.Mater.23(2011)4248–4253).This compound has the structure and performance similar to graphene,
Including excellent hydrophilic nmature, excellent electric conductivity, electrochemical property test can be carried out in the solution of different pH values
Deng, thus receive vast researcher it is very big concern (B.Anasori, Y.Xie, M.Beidaghi, J.Lu,
B.C.Hosler,L.Hultman,P.R.Kent,Y.Gogosti,M.W.Barsoum.Two-dimensional,ordered,
double transition metals carbides(MXenes).ACS Nano 9(2015)9507).Compared with carbon material,
Ti3C2The electric conductivity of T is poor, specific surface area is small, the lamella of its organ shape is easy to build up superposition, these disadvantages illustrate Ti3C2Electricity
Chemical property has to be hoisted, significantly limits Ti3C2Application as electrode material.
Because having faster oxidation-reduction dynamic, high theoretical specific capacity, cheap price and environmental-friendly etc. many
Advantage, the favor of the oxide of nickel and cobalt in transition metal by researcher, it is considered to be the electrode material haveing excellent performance.
NiCo2O4It is a kind of with spinel structure, the bimetallic oxide containing two kinds of elements of nickel and cobalt.As supercapacitor
Electrode material, NiCo2O4There are higher electro-chemical activity (Z.Wu, Y.Zhu, X.Ji, NiCo2O4 -based materials
for electrochemical supercapacitors,J.Mater.Chem.A 2(2014)14759-14772)。
Studies have shown that being modified load in different ways, it can obtain what chemical property was been significantly enhanced
Ti3C2Based composites.For example, Rakhi R B et al. passes through direct chemically synthesized method in Ti3C2TxSurface is prepared for MnO2
Nanocrystal obtains MnO2/Ti3C2TxComposite material, specific capacity when current density is 1A/g in three-electrode system are
205F/g has approached Ti3C2TxTheoretical specific capacity, and recycle 6000 times after still have 93% capacity retention, show fabulous
Cyclical stability (Rakhi R B, Ahmed B, Anjum D, et al.Direct Chemical Synthesis of
MnO2Nanowhiskers on Transition-Metal Carbide Surfaces for Supercapacitor
Applications.ACS Appl.Mater.Inter.8(2016)18806-18814).Wang Y et al. is by Ti3C2Tx
Surface grows nickel aluminium layered double hydroxide (LDH) in due course and is prepared for three-dimensional porous LDH/Ti3C2TxComposite material, electricity
Current density be 1A/g when, after cycle charge-discharge 250 times, specific capacity still can achieve 155F/g (Wang Y,
Dou H,Wang J,et al.Three-Dimensional Porous MXene/Layered Double Hydroxide
Composite for High Performance Supercapacitors.J.Power Sources 327(2016)221-
228).It is reported above to show that composite modified is a kind of raising Ti3C2The effective way of electrode performance.And at present there has been no about
Ti3C2/NiCo2O4The report of combination electrode and its synthetic method.Therefore, this patent is successfully made for the first time using simple hydro-thermal method
Standby Ti out3C2/NiCo2O4Composite material, i.e., pretreated Ti3C2It is added in the mixed solution of nickel salt, cobalt salt and urea,
Then hydro-thermal reaction and low temperature calcination are carried out, coated with uniform NiCo is obtained2O4Ti3C2Composite material improves Ti3C2
Chemical property, extend Ti3C2Application as electrode material.
Summary of the invention
The technical problems to be solved by the invention include two aspect: one is to invented a kind of Ti3C2/NiCo2O4Compound electric
Pole material；Second is that providing Ti for the first time3C2/NiCo2O4The preparation method of combination electrode.With pure Ti3C2Electrode is compared, the compound electric
The specific capacitance of pole material improves 135%.Also, the preparation process of this combination electrode is simple and convenient to operate.The present invention is first
By pretreated Ti3C2It is dispersed in the mixed solution of nickel salt and cobalt salt, and add surfactant to make NiCo2O4Presoma is equal
It is even to be distributed in Ti3C2Surface；Then urea is added in mixed suspension as reducing agent and precipitating reagent；Thereafter, by preparation
Suspension is transferred in water heating kettle, obtains Ti by hydro-thermal reaction3C2/NiCo2O4The presoma of composite material；Finally, lower
At a temperature of calcined to obtain Ti3C2/NiCo2O4Combination electrode.
The present invention solves technical solution used by the technical problem:
A kind of Ti3C2/NiCo2O4Combination electrode material, wherein Ti3C2And NiCo2O4Mass ratio be 1:0.5~1:3.
The Ti3C2/NiCo2O4The preparation method of combination electrode material, includes the following steps:
(1) by Ti3C2It is added in dimethyl sulfoxide, after successively carrying out ultrasonic disperse, cleaning, filtering and vacuum drying, obtains
Pass through pretreated Ti3C2Powder；Wherein, 0.5~3gTi is added in every 200 milliliters of dimethyl sulfoxides3C2；
(2) pretreatment Ti will be passed through obtained in step (1)3C2Powder is added in ethylene glycol, obtains mixing after stirring molten
Liquid；Then cobalt salt, nickel salt and surfactant are added in mixed solution, are sufficiently stirred to obtain the first suspension；It adds
Precipitating reagent urea obtains the second suspension after stirring；
Wherein, molar ratio is Ni ion: Co ion=1:2；In first suspension Ni ion concentration be 0.0125~
0.075mol/L；Molar ratio is urea: (Ni ion+Co ion)=1~6:1；Molar ratio surfactant unimolecule: (Ni from
Son+Co ion)=3~9:1；Molar ratio Ti3C2: Ni ion=1:0.348~2.091；
(3) the second suspension that step (2) obtains is transferred in stainless steel water heating kettle, water is carried out at 160~200 DEG C
2~16h of thermal response, hydrothermal product is centrifuged, and obtained product is successively cleaned with dehydrated alcohol and deionized water, so
After dry；
(4) it takes product obtained in step (3) to calcine 1~4 hour at air atmosphere, 300~400 DEG C, Ti is made3C2/
NiCo2O4Composite powder material.
The cobalt salt is cobalt nitrate, cobalt chloride, cobaltous sulfate or cobalt acetate or their hydrate.
The nickel salt is nickel nitrate, nickel chloride, nickel sulfate or nickel acetate or their hydrate.
The surfactant is polyvinylpyrrolidone.
The beneficial effects of the present invention are:
(1) present invention is prepared for Ti by hydro-thermal method and low temperature calcination method by using appropriate technique3C2/NiCo2O4
Nanocomposite.As depicted in figs. 1 and 2, by controlling synthesis technology, the product that the present invention obtains is by Ti3C2And NiCo2O4
, there is not TiO in two phase compositions2, the impurity phases such as CoO and NiO.As shown in figure 3, NiCo2O4Nano particle is evenly distributed on stratiform
Ti3C2The surface of particle and interlayer form stable Ti3C2/NiCo2O4Nano composite structure.
(2) composite material prepared by the present invention has excellent chemical property.As shown in figure 4, mass ratio is 1:1's
Ti3C2/NiCo2O4Specific capacitance of the combination electrode material under different charging and discharging currents density be above pure Ti3C2Electrode.Especially
Be current density be 0.2A/g when the combination electrode specific capacitance reached 87.5F/g, relative to Ti3C2Electrode, specific capacitance
135% is improved, and charging and discharging curve is in symmetrical isosceles triangle.This illustrates Ti3C2/NiCo2O4Composite electrode has
Biggish specific capacitance and more excellent stable charge/discharge are a kind of outstanding potential capacitor electrode materials of tool.
(3) the method for the present invention instrument equipment is simple, easy to operate, low in cost, the stable structure and performance of product
It is excellent, be conducive to produce on a large scale.
Detailed description of the invention:
The present invention will be further described with reference to the accompanying drawings and examples.
Fig. 1 is the Ti of the embodiment of the present invention 13C2、NiCo2O4The Ti for being 1:1 with mass ratio3C2/NiCo2O4The X-ray of sample
Diffraction (XRD) comparison diagram.
Fig. 2 is the LR laser raman map of the different samples prepared in the present invention, and wherein Fig. 2 (a) mass ratio is 1:1's
Ti3C2/NiCo2O4The LR laser raman map of combination electrode, Fig. 2 (b) and Fig. 2 (c) are NiCo respectively2O4And Ti3C2The laser of material
Raman map.
Fig. 3 is the scanning electron microscope (SEM) photograph of the microstructure of the different samples prepared in the present invention, wherein Fig. 3 (a), Fig. 3 (b),
Fig. 3 (c) and Fig. 3 (d) is NiCo respectively2O4, mass ratio 1:0.5, the Ti that mass ratio is 1:1 and mass ratio is 1:33C2/
NiCo2O4The SEM of composite material schemes.
Fig. 4 is the charging and discharging curve figure of the different samples prepared in the present invention, and it is 1:1 that wherein Fig. 4 (a), which is mass ratio,
Ti3C2/NiCo2O4The charging and discharging curve of combination electrode, Fig. 4 (b) are Ti3C2The charging and discharging curve of electrode.
Specific embodiment
Embodiment 1
(1) by 1g Ti3C2Powder is added to ultrasound 2h in 200mL dimethyl sulfoxide, and centrifuge separation is then cleaned with ethyl alcohol
It is 6 times, spare after vacuum drying；
(2) step (1) pretreated Ti will be passed through by weighing 0.481g (2.870mmol)3C2Powder is added to 80mL ethylene glycol
In, 1h is sufficiently stirred to disperse；2mmol Nickelous nitrate hexahydrate (Ni (NO is weighed respectively3)2·6H2) and six nitric hydrate of 4mmol O
Cobalt (Co (NO3)2·6H2O it) is added in above-mentioned solution, continues to stir 2h；2g polyvinylpyrrolidone is weighed (i.e. according to C6H9NO
Unimolecule is calculated as a mole 18mmol), it is added in above-mentioned solution, continues to stir 1h；18mmol urea is weighed to be slowly added into
In solution, suspension is obtained；(illustrate, in the embodiment of the present invention, molar ratio Ti3C2: Ni ion=1:0.348~2.091, to protect
Demonstrate,prove Ti in final product3C2And NiCo2O4Mass ratio be 1:0.5~3；)
(3) suspension that step (2) obtains is transferred in the water heating kettle liner of polytetrafluoroethylene (PTFE) material, then by liner
It is sealed in stainless steel outer sleeve, is placed in baking oven in 180 DEG C of reaction 6h；To be centrifugated out after the reaction was completed, and respectively
There are dehydrated alcohol and deionized water to clean 6 times, then dries product at 60 DEG C；
(4) product that step (3) obtains is put into porcelain boat, calcines 2h under 350 DEG C of air atmospheres, quality can be obtained
Than the Ti for 1:1 (theoretical value)3C2/NiCo2O4Composite material.
Fig. 1 is NiCo2O4、Ti3C2The Ti for being 1:1 with mass ratio3C2/NiCo2O4The XRD spectrum of composite material.Such as institute in figure
Show, two-dimentional Ti3C2XRD diffraction maximum be located at 2 θ=9.8 °, at 18.7 °, 26.8 °, 35.3 ° and 61.2 °, correspond respectively to
(002) of the two dimensional crystal, (006), (008), (010) and (110) crystal face.In pure NiCo2O4XRD spectrum in, diffraction maximum point
Not Wei Yu 2 θ=31.3 °, at 36.7 °, 44.4 °, 59.1 °, 64.9 °, respectively correspond spinel structure NiCo2O4(111),
(220), (311), (400) and (553) crystal face.The mass ratio obtained after hydro-thermal reaction and low temperature calcination is the Ti of 1:13C2/
NiCo2O4In the XRD spectrum of composite material, existing Ti3C2Diffraction maximum have NiCo again2O4Diffraction maximum, and be not observed
Other impurities phase (such as TiO2, CoO and NiO) diffraction maximum, show to successfully synthesize NiCo2O4/Ti3C2Composite material.
Fig. 2 is respectively NiCo2O4、Ti3C2The Ti for being 1:1 with mass ratio3C2/NiCo2O4The LR laser raman figure of composite material
Spectrum.As seen from the figure, NiCo2O4Raman vibration peak be located at 477.8,523 and 671cm-1Place, corresponds respectively to Eg、F2gAnd
A1gThe vibrating mode of these three Spinels.This result, which is confirmed, has synthesized NiCo by hydro-thermal reaction and low temperature calcination2O4
Powder.Mass ratio is the Ti of 1:13C2/NiCo2O4The laser Raman spectroscopy of composite material may be considered Ti3C2And NiCo2O4Two
The superposition of the laser Raman spectroscopy of kind sample, does not observe the Raman vibration peak of other impurities phase.
Fig. 3 is NiCo prepared by the present invention2O4With the Ti of different quality ratio3C2/NiCo2O4The scanning electron microscope (SEM) photograph of composite material
Piece.The NiCo of preparation can be clearly observed from Fig. 3 (a)2O4Microscopic appearance be diameter be about receiving for 80~100nm
Rice ball.Fig. 3 (c) shows that mass ratio is the Ti of 1:13C2/NiCo2O4The microscopic appearance of composite material, wherein lamellar structure belongs to
Ti3C2, in the Ti of lamellar3C2Spherical NiCo is dispersed with interlayer above2O4Nano particle.Two kinds of orderly combinations of material exist
Together, stratiform Ti3C2NiCo can be effectively improved2O4The dispersibility of nano particle, and NiCo2O4A large amount of oxidation-can be provided also
It is in situ, therefore two kinds of Material claddings get up integrally improve electro-chemical activity.
The present invention has made based on Ti3C2/NiCo2O4The electrode of composite material is to measure its chemical property.It weighs respectively
The mass ratio prepared in certain mass above-mentioned steps is the Ti of 1:13C2/NiCo2O4Sample and Ti3C2Sample as active material,
Active material, acetylene black, PTFE three are uniformly mixed according to the proportion of mass ratio 8:1:1, be then placed in agate mortar into
Row suitably grind, be properly joined into alcohol in the process, then proceed to grinding until mixture uniformly without granular sensation after, will
Mixture is pressed into thin slice, and the nickel foam on piece that surface area size is approximately (1cm × 2cm) is pressed against before thin slice quick-drying, it
This electrode is placed on to drying in 60 DEG C of baking oven afterwards and for 24 hours, respectively obtains Ti3C2/NiCo2O4Combination electrode and Ti3C2Electrode.
The chemical property that prepared electrode is tested in three-electrode system, using CHI660e electrochemical workstation
(Chenhua, Shanghai) is tested, wherein the Ti prepared3C2/NiCo2O4Combination electrode is made as working electrode, platinized platinum
For to electrode, saturated calomel electrode (SCE) is used as reference electrode, test electrolyte is 3M potassium hydroxide aqueous solution, test voltage
Window is -1~-0.2V.Fig. 4 is the Ti that mass ratio is 1:13C2/NiCo2O4Combination electrode is when current density is 0.2~2A/g
Constant current charge-discharge curve.It can be seen from the figure that the combination electrode is shown under different current densities better than Ti3C2
The specific capacity of electrode.Especially when current density is 0.2A/g, the specific capacitance of combination electrode has reached 87.5F/g, compared to
Ti3C2Electrode, specific capacitance improves 135%, and the charging and discharging curve of combination electrode shows symmetrical isosceles triangle.These
Data illustrate Ti3C2/NiCo2O4Combination electrode has biggish specific capacitance and more excellent stable charge/discharge, is a kind of outstanding
, the potential electrode for super capacitor material of tool.
Embodiment 2,3
The hydrothermal temperature of step (3) in embodiment 1 is changed to 160 and 200 DEG C, other his operations with reality
It is identical to apply example 1, obtains product with embodiment 1.
Embodiment 4,5
The hydro-thermal reaction time of step (3) in embodiment 1 is changed to 2 and 16h, other his operations are and embodiment
1 is identical, obtains product with embodiment 1.
Embodiment 6,7
The low temperature calcination temperature of step (4) in embodiment 1 is changed to 300 and 400 DEG C, other his operations with reality
It is identical to apply example 1, obtains product with embodiment 1.
Embodiment 8,9
The low temperature calcination time of step (4) in embodiment 1 is changed to 1 and 4h, other his operations with embodiment 1
It is identical, product is obtained with embodiment 1.
Embodiment 10
The mole of the used raw material Nickelous nitrate hexahydrate of step (2) and cabaltous nitrate hexahydrate in embodiment 1 is distinguished
It is changed to 1 and 2mmol, other his operations are same as Example 1, obtain the Ti that mass ratio is 1:0.53C2/NiCo2O4It is multiple
Condensation material.Shown in the microscopic appearance of the composite material such as attached drawing 3 (b), the microscopic appearance and mass ratio of the composite material are 1:1's
Ti3C2/NiCo2O4Composite material is similar, except that NiCo2O4The negligible amounts of nano particle, and Ti3C2Lamellar knot
Structure is more complete.
Embodiment 11
The mole of the used raw material Nickelous nitrate hexahydrate of step (2) and cabaltous nitrate hexahydrate in embodiment 1 is distinguished
6 and 12mmol are changed to, other his operations are same as Example 1, obtain the Ti that mass ratio is 1:33C2/NiCo2O4It is compound
Material.Shown in the microscopic appearance of the composite material such as attached drawing 3 (d), the microstructure of this composite material is equally in mass ratio
The Ti of 1:13C2/NiCo2O4Composite material it is similar, but lamellar structure is unobvious.
Embodiment 12
By the quality of surfactant polyvinylpyrrolidone used in the step (2) in embodiment 1 be changed to 6g (i.e. according to
C6H9NO unimolecule is calculated as a mole 54mmol), other his operations are same as Example 1, obtain product with embodiment 1.
Embodiment 13,14
The amount of the substance of urea used in step (2) in embodiment 1 is changed to 6 and 36mmol, other his operations are equal
It is same as Example 1, product is obtained with embodiment 1.
Embodiment 15,16,17
By in embodiment 1 the used raw material nickel nitrate of step (2) and cobalt nitrate be changed to respectively nickel chloride and cobalt chloride or
Its hydrate, nickel sulfate and cobaltous sulfate or its hydrate and nickel acetate and cobalt acetate or its hydrate.Other his operations
It is same as Example 1, product is obtained with embodiment 1.
Unaccomplished matter of the present invention is well-known technique.
Claims (6)
1. a kind of Ti3C2/NiCo2O4Combination electrode material, wherein Ti3C2And NiCo2O4Mass ratio be 1:0.5~1:3.
2. Ti as described in claim 13C2/NiCo2O4The preparation method of combination electrode material, it is characterized in that this method includes such as
Lower step:
(1) layer preprocessing Ti will be passed through3C2Powder is added in ethylene glycol, and mixed solution is obtained after stirring；Then by cobalt salt,
Nickel salt and surfactant are added in mixed solution, stir to get the first suspension；Precipitating reagent urea is added, after stirring
To the second suspension；
Wherein, molar ratio is Ni ion: Co ion=1:2；Ni ion concentration is 0.0125~0.075mol/ in first suspension
L；Molar ratio is urea: (Ni ion+Co ion)=1~6:1；Molar ratio surfactant unimolecule: (Ni ion+Co ion)
=3~9:1；Molar ratio Ti3C2: Ni ion=1:0.348~2.09；
(2) the second suspension that step (1) obtains is transferred in stainless steel water heating kettle, it is anti-that hydro-thermal is carried out at 160~200 DEG C
2~16h is answered, hydrothermal product is centrifuged, obtained product is successively cleaned with dehydrated alcohol and deionized water, is then dried
It is dry；
(3) it takes product obtained in step (2) to calcine 1~4 hour at air atmosphere, 300~400 DEG C, Ti is made3C2/
NiCo2O4Composite powder material.
3. Ti as described in claim 13C2/NiCo2O4The preparation method of combination electrode material, it is characterized in that the cobalt salt is
Cobalt nitrate, cobalt chloride, cobaltous sulfate or cobalt acetate or their hydrate.
4. Ti as described in claim 13C2/NiCo2O4The preparation method of combination electrode material, it is characterized in that the nickel salt is
Nickel nitrate, nickel chloride, nickel sulfate or nickel acetate or their hydrate.
5. Ti as described in claim 13C2/NiCo2O4The preparation method of combination electrode material, it is characterized in that the surface is living
Property agent be polyvinylpyrrolidone.
6. Ti as claimed in claim 23C2/NiCo2O4The preparation method of combination electrode material, it is characterized in that the Ti3C2
The layer preprocessing of powder includes the following steps: Ti3C2It is added in dimethyl sulfoxide, successively carries out ultrasonic disperse, cleaning, mistake
After filter, vacuum drying and mechanical lapping, obtain by pretreated Ti3C2Powder；Wherein, every 200 milliliters of dimethyl sulfoxides add
Enter 0.5~3gTi3C2。
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