CN109904000A - A kind of preparation method and applications of the Ni-based complex electrode material of nanometer of threadiness - Google Patents
A kind of preparation method and applications of the Ni-based complex electrode material of nanometer of threadiness Download PDFInfo
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Abstract
The present invention discloses the preparation method and applications of the Ni-based complex electrode material of a kind of nanometer of threadiness, preparation method comprises the following specific steps that: after divalent inorganic nickel salt, nitrilotriacetic acid, deionized water and isopropanol are mixed, it is transferred to and is reacted in reaction kettle to get the linear Ni-based complex electrode material of the nanometer with 1-dimention nano cable architecture is arrived after being sufficiently stirred.Nitrilotriacetic acid is coordinated to form the Ni-based complex of one-dimensional nano line shape with the nickel ion for being adsorbed on its surface under hydrothermal conditions, this method obtains that the linear Ni-based complex electrode material uniform properties of nanometer, pattern are single can be increased effective contact area, shorten electron-transport distance, applied to electrode material for super capacitor, higher specific capacitance and high rate performance are shown.
Description
Technical field
The invention belongs to electrode material for super capacitor technical fields, and in particular to the Ni-based complex electricity of a kind of nanometer of threadiness
The preparation method and applications of pole material.
Background technique
With non-renewable oil-fired lasting consumption, the following problem of environmental pollution causes people unprecedented
Concern, therefore develop a kind of new and effective environmental-friendly electrochemical energy storing device and carry out storage energy and advocating sustainable development
The today's society of exhibition is particularly important.In energy storage device, supercapacitor (electrochemical capacitor) has had nearly 40
The history of year application and development, since it has the characteristics that power density is big, have extended cycle life, the charging time is short, energy efficiency is high
It is widely used in the fields such as consumer electronics industry, novel distribution power grid, pure (mixed) electric car.
Core component in supercapacitor is electrode material, according to the difference of electrode material energy storage principle, can be divided into two
Major class: double layer electrodes material, fake capacitance electrode material., mainly using carbon-based material as representative, the latter is then with transition for the former
Derivative based on metallic compound or conducting polymer, such as transition metal oxide (ruthenic oxide, manganese dioxide), mistake
Cross metal sulfide (cobalt sulfide, nickel sulfide etc.), using MOFs as complex of representative etc..The full name of MOFs is Metal-
Organic Frameworks (metal organic frame) there is various structures, bigger serface, porosity and hole to hold controllable etc.
Feature in ion exchange, gas storage and the fields such as separates, is catalyzed, senses and have potential application.In recent years, scientific research personnel
The complexs application field such as MOFs is expanded in supercapacitor, if Yang et al. is for the first time by a kind of the Ni-based of layer structure
MOFs is as electrode material for super capacitor (Metal-organic frameworks:a new promising class of
materials for a high performance supercapacitor electrode,Journal of
Materials Chemistry A, 2014,2,16640), Liu et al. people has found that layered cobalt base MOFs also can be used as supercapacitor
Electrode material (Cobalt-Based Layered Metal-Organic Framework as an Ultrahigh
Capacity Supercapacitor Electrode Material,ACS Applied Materials&Interfaces,
2016,8,4585-4591), Gao et al. synthesizes the Ni-based MOFs of cuboid pattern for supercapacitor (Facile
synthesis of cuboid Ni-MOF for high performance supercapacitors,Journal
OfMaterials Science, 2018,53,6807-6818), Li et al. people reports a kind of two-dimensional slice shape complex for surpassing
Grade capacitor (2D Nanoflakes of metal-polyphenolic coordination assembly for
highperformance supercapacitor,Inorganic Chemistry Communications,2018,90,51-
56), we organize also reports two-dimentional porous Ni-base MOFs (Aporous 2D Ni-MOF material with a high recently
supercapacitive performance,Journal of Solid State Chemistry,2018,265,244-
247) and cadmium base MOFs is as electrode material for super capacitor (Structural Elucidation and
Supercapacitive Performance in a 1D Cadmium(II)Polymer Based on Pyrazole
Carboxylic Acid,Journal of Inorganic and Organometallic Polymers and
Materials,doi.org/10.1007/s10904-019-01119-x).Ni-based match currently, yet there are no about nanometer is linear
Object is closed in the relevant report of super capacitor.
Summary of the invention
The purpose of the present invention is prepare the Ni-based complex electrode material of a kind of nanometer of threadiness；It is another object of the present invention to
Using the complex as the application of electrode material for super capacitor, the electrode of super capacitor made of the material has good
Chemical property, higher specific capacitance and stable multiplying power property.To achieve the above object, the present invention provides a kind of nanometer of threadiness
The preparation method and applications of Ni-based complex electrode material.
Technical solution of the present invention is summarized as follows:
The preparation method of the Ni-based complex electrode material of a kind of nanometer of threadiness disperses divalent inorganic nickel salt, nitrilotriacetic acid
In isopropanol and deionized water mixed solution, being obtained by hydro-thermal method single step reaction, there is the Ni-based of 1-dimention nano cable architecture to match
Close object, the preparation method specifically includes the following steps:
(1) after 1-4mmol divalent inorganic nickel salt, 0.01-0.6g nitrilotriacetic acid, deionized water and isopropanol being mixed,
After stirring 0.5-1h at room temperature, mixed solution is obtained；The volume ratio of the isopropanol and deionized water is 4:1-1:4, described different
The volume of propyl alcohol and deionized water and be 15-30mL；
(2) mixed solution that step (1) is prepared is transferred in polytetrafluoroethyllining lining reaction kettle, in 150-200
At DEG C, reaction product is obtained after hydro-thermal reaction 6-24h；
(3) the reaction product cooled to room temperature obtained to step (2), be centrifuged, wash after obtain sediment,
After drying precipitate 12h, the nanometer linear Ni-based complex electrode material will be made at 40-60 DEG C.
Preferably, the divalent inorganic nickel salt is one of nickel acetate, nickel nitrate, nickel sulfate and nickel chloride.
Preferably, the operating process of the washing are as follows: sunk respectively with what deionized water, dehydrated alcohol alternating washing were isolated
Starch 5-8 times.
The present invention also provides the nano wires that the preparation method of the linear Ni-based complex electrode material of above-mentioned nanometer is prepared
The Ni-based complex electrode material of shape.
The present invention also provides the application of the linear Ni-based complex electrode material of above-mentioned nanometer, the Ni-based complexs of this nanometer of threadiness
Electrode material is applied to electrode of super capacitor.
The preparation process of the electrode of super capacitor the following steps are included:
(1) (7-8) is pressed: (2-1): the 1 linear Ni-based complex of mass ratio mixing nanometer, conductive agent and binder, and add
Enter dehydrated alcohol, after ultrasonic disperse, slurry is made；
(2) slurry is uniformly coated in substrate, at 80-120 DEG C, after being dried in vacuo 8-16h, with the pressure of 8-15MPa
Power obtains electrode of super capacitor after carrying out compressing tablet process.
Preferably, the conductive agent is one of acetylene black, graphite and Super P.
Preferably, the binder is one of PVDF, PTFE and CMC.
Preferably, the substrate is one of nickel foam, copper foil, carbon cloth and carbon paper.
Preferably, the area of base 1-2.5cm2, the load capacity of the linear Ni-based complex of nanometer is 2- in the substrate
5mg。
In the present invention: without special instruction, Super P is the abbreviation of conductive black；PVDF is the abbreviation of Kynoar；
PTEE is the abbreviation of polytetrafluoroethylene (PTFE)；CMC is the abbreviation of sodium carboxymethylcellulose.
The invention has the benefit that
(1) present invention utilizes the carboxylic in nitrilotriacetic acid for the first time using nitrilotriacetic acid as the complexant for synthesizing Ni-based complex
Nickel ion is adsorbed in base functional group, and is coordinated and to form the Ni-based complex electrode material with 1-dimention nano cable architecture, one-dimensional linear
Design shortens the specific surface area that electron-transport distance improves complex, increases effective active site, has Ni-based complex
There are good electrochemical properties；
(2) present invention uses one step hydro thermal method, does not add any template, surfactant, and experimental implementation is simple, reacts
It is mild condition, reproducible；
(3) present invention is under hydrothermal conditions, to be orderly coordinated by nickel ion and nitrilotriacetic acid and form the one of oriented structure
Wiener rice noodles, unicity are good；
(4) the 1-dimention nano cable architecture that Ni-based complex prepared by the present invention is formed can effectively avoid making because undersized
At agglomeration traits, be conducive to the application in energy storage field；
(5) electrode of super capacitor made of material of the invention has good chemical property, higher specific capacitance
With stable multiplying power property.
Detailed description of the invention
Fig. 1 is the X-ray diffraction spectrogram (XRD) of the linear Ni-based complex electrode material of nanometer obtained by embodiment 1；
Fig. 2 is the infrared spectrogram of the linear Ni-based complex electrode material of nanometer obtained by embodiment 1；
Fig. 3 is the SEM figure of the linear Ni-based complex electrode material of nanometer obtained by embodiment 1；
Fig. 4 is the KOH electrolyte of 6mol/L of the electrode of super capacitor under different current densities obtained by embodiment 1
In constant current discharge curve graph；
Fig. 5 is specific capacitance figure of the electrode of super capacitor under different current densities obtained by embodiment 1.
Specific embodiment
The present invention is further described in detail with attached drawing combined with specific embodiments below, to enable those skilled in the art
Refer to the instruction text can be implemented accordingly.Experimental method described in following embodiments is unless otherwise specified conventional side
Method；The material, reagent etc. commercially obtain unless otherwise specified.
The Ni-based complex electrode material of 1 a kind of nanometer of threadiness of embodiment
Preparation method are as follows: weigh the nickel acetate of 2mmol, 0.4g nitrilotriacetic acid is dissolved in 7.5ml deionized water, measurement
7.5ml isopropanol is added in above-mentioned solution and is stirred for 30min, and above-mentioned mixed solution is transferred to polytetrafluoroethyllining lining
In reaction kettle, heated for 24 hours at 180 DEG C of oven temperature, reaction product is centrifugated and uses deionization by cooled to room temperature
Water, dehydrated alcohol wash 8 times, then at 40 DEG C dry 12h to get to having the linear Ni-based complex electrode material of nanometer.
By Ni-based complex electrode material obtained above and conductive agent acetylene black and binder PTFE in mass ratio 7.5:
1.5:1 mixing, is dispersed in dehydrated alcohol and forms slurry, slurry is evenly coated in area 1cm2In foam nickel base, often
The load capacity of the Ni-based complex of piece of foam nickel is 1.5mg, 60 DEG C of dry 12h in drying box, after carrying out compressing tablet process later,
Pressure is set as 10MPa to get electrode of super capacitor is arrived.It is measured using Shanghai Chen Hua electrochemical workstation, with preparation
Electrode be working electrode, platinum electrode is to electrode, and Hg/HgO electrode is reference electrode, in three electrodes of 6M KOH aqueous solution
Electrochemical property test is carried out in system.
Fig. 1 is the XRD spectra of linear Ni-based complex (Ni-NTA) electrode material of nanometer obtained by embodiment 1, spectrogram
In diffraction maximum and reactant nickel acetate (Ni (Ac)2), the characteristic diffraction peak of nitrilotriacetic acid (NTA) it is all different, both illustrate
Complexation reaction occurs.
Fig. 2 is the infrared spectrogram of the linear Ni-based complex electrode material of nanometer obtained by embodiment 1,3480cm-1It is
The distinctive absorption frequency of Ni-NTA, 3000-2800cm-1It is c h bond vibration frequency region, in the region, Ni-NTA ratio NTA is wanted
It is weak very much, deducibility Ni2+Caused by coordination, 1728cm-1It is and the Ni-NTA as produced by the C=O stretching vibration in carboxyl
In this peak disappear, instead coordination after carboxyl frequency 1644cm-1、1581cm-1。
Fig. 3 is the SEM figure of the linear Ni-based complex electrode material of nanometer obtained by embodiment 1, and Ni-based complex has
Single 1-dimention nano cable architecture, for nano wire pattern completely without fracture, smooth surface is uniform in size.
Fig. 4 is electrode of super capacitor obtained by embodiment 1 in the KOH electrolyte of 6mol/L, potential window range
Constant current discharge curve graph at 0-0.56V, different current densities.According to specific capacitance calculation formulaWork as electricity
When current density is 1A/g, the specific capacitance of electrode reaches 126.64F/g, illustrates that the material has the potential for doing supercapacitor.
Fig. 5 is the specific capacitance figure of electrode of super capacitor obtained by embodiment 1.It can be seen that in current density point
Not Wei 1A/g, 2A/g, 3A/g, 4A/g, 5A/g, 7A/g, 10A/g when, specific capacitance be respectively 126.64F/g, 120.21F/g,
114.95F/g, 110.43F/g, 105.95F/g, 100.83F/g, 97.9F/g, when current density increases to 10A/g from 1A/g
When, the specific capacitance of electrode material for super capacitor prepared by the present invention still has initial value to obtain 77%, shows good multiplying power
Performance.
The Ni-based complex electrode material of 2 a kind of nanometers of threadiness of embodiment
Preparation method are as follows: weigh the nickel nitrate of 1mmol, 0.01g nitrilotriacetic acid is dissolved in 12ml deionized water, measurement
30min is stirred in the above-mentioned solution of 3ml isopropanol addition and obtains mixed solution, and above-mentioned mixed solution is transferred to polytetrafluoro
In the reaction kettle of ethylene liner, 6h is heated at 150 DEG C of oven temperature, reaction product is centrifugated by cooled to room temperature,
And washed 8 times with deionized water, dehydrated alcohol respectively, dry 12h at 40 DEG C then to get the linear Ni-based complex of nanometer is arrived
Electrode material.
The Ni-based complex electrode material of 3 a kind of nanometers of threadiness of embodiment
Preparation method are as follows: weigh the nickel sulfate of 4mmol, 0.6g nitrilotriacetic acid is dissolved in 9ml deionized water, measurement 6ml
Isopropanol is added in above-mentioned solution and is stirred for 30min, and above-mentioned mixed solution is transferred to the reaction with polytetrafluoroethyllining lining
It in kettle, is heated for 24 hours at 150 DEG C of oven temperature, reaction product is centrifugated by cooled to room temperature, uses deionization respectively
Water, dehydrated alcohol wash 8 times, dry 12h at 40 DEG C then to get the linear Ni-based complex electrode material of nanometer is arrived.
The Ni-based complex electrode material of 4 a kind of nanometers of threadiness of embodiment
Preparation method are as follows: weigh the nickel chloride of 2mmol, 0.6g nitrilotriacetic acid is dissolved in 3ml deionized water, measurement 12ml
Isopropanol is added in above-mentioned solution and is stirred for 30min, and above-mentioned mixed solution is transferred to the reaction with polytetrafluoroethyllining lining
It in kettle, is heated for 24 hours at 180 DEG C of oven temperature, reaction product is centrifugated by cooled to room temperature, uses deionization respectively
Water, dehydrated alcohol wash 8 times, dry 12h at 40 DEG C then to get the linear Ni-based complex electrode material of nanometer is arrived.
The Ni-based complex electrode material of 5 a kind of nanometers of threadiness of embodiment
Preparation method are as follows: weigh the nickel chloride of 2mmol, 0.6g nitrilotriacetic acid is dissolved in 6ml deionized water, measurement 9ml
Isopropanol is added in above-mentioned solution and is stirred for 30min, and above-mentioned mixed solution is transferred to the reaction with polytetrafluoroethyllining lining
It in kettle, is heated for 24 hours at 180 DEG C of oven temperature, reaction product is centrifugated by cooled to room temperature, uses deionization respectively
Water, dehydrated alcohol wash 8 times, dry 12h at 40 DEG C then to get the linear Ni-based complex electrode material of nanometer is arrived.
The Ni-based complex electrode material of 6 a kind of nanometers of threadiness of embodiment
Preparation method are as follows: weigh the nickel acetate of 2mmol, 0.15g nitrilotriacetic acid is dissolved in 7.5ml deionized water, measurement
7.5ml isopropanol is added in above-mentioned solution and is stirred for 30min, and above-mentioned mixed solution is transferred to polytetrafluoroethyllining lining
In reaction kettle, heated for 24 hours at 180 DEG C of oven temperature, reaction product is centrifugated and uses deionization by cooled to room temperature
Water, dehydrated alcohol wash 8 times, dry 12h at 40 DEG C then to get the linear Ni-based complex electrode material of nanometer is arrived.
The Ni-based complex electrode material of 7 a kind of nanometers of threadiness of embodiment
Preparation method are as follows: weigh the nickel acetate of 2mmol, 0.35g nitrilotriacetic acid is dissolved in 7.5ml deionized water, measurement
7.5ml isopropanol is added in above-mentioned solution and is stirred for 30min, and above-mentioned mixed solution is transferred to polytetrafluoroethyllining lining
In reaction kettle, heated for 24 hours at 180 DEG C of oven temperature, reaction product is centrifugated and uses deionization by cooled to room temperature
Water, dehydrated alcohol wash 8 times, dry 12h at 40 DEG C then to get the linear Ni-based complex electrode material of nanometer is arrived.
The linear Ni-based complex electrode material of the nanometer that above-described embodiment 2-7 is prepared is a wiener of oriented structure
Rice noodles, unicity is good, and dispersion degree is high.
Above-described embodiment 2-7 is prepared to different electrode of super capacitor according to the method for embodiment 1, is all had
Good chemical property, higher specific capacitance and stable multiplying power property.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details.
Claims (10)
1. the preparation method of the Ni-based complex electrode material of a kind of nanometer of threadiness, which is characterized in that by divalent inorganic nickel salt, ammonia three
Acetic acid is scattered in isopropanol and deionized water mixed solution, can be prepared by that nanometer is linear Ni-based to match using hydro-thermal method single step reaction
Close object electrode material, the preparation method specifically includes the following steps:
(1) after mixing 1-4mmol divalent inorganic nickel salt, 0.01-0.6g nitrilotriacetic acid, deionized water and isopropanol, in room temperature
After lower stirring 0.5-1h, mixed solution is obtained；The volume ratio of the isopropanol and deionized water is 4:1-1:4, the isopropanol
With the volume of deionized water and be 15-30mL；
(2) mixed solution that above-mentioned steps (1) are prepared is transferred in polytetrafluoroethyllining lining reaction kettle, in 150-200
At DEG C, reaction product is obtained after hydro-thermal reaction 6-24h；
(3) the reaction product cooled to room temperature obtained to step (2), be centrifuged, wash after obtain sediment, in 40-60
After drying precipitate 12h, the nanometer linear Ni-based complex electrode material will be made at DEG C.
2. the preparation method of the linear Ni-based complex electrode material of nanometer according to claim 1, which is characterized in that described
Divalent inorganic nickel salt is one of nickel acetate, nickel nitrate, nickel sulfate and nickel chloride.
3. the preparation method of the linear Ni-based complex electrode material of nanometer according to claim 1, which is characterized in that described
The operating process of washing are as follows: alternately wash sediment 5-8 times isolated with deionized water, dehydrated alcohol respectively.
4. the preparation method of the linear Ni-based complex electrode material of nanometer as claimed in any one of claims 1-3 is prepared
The linear Ni-based complex electrode material of nanometer.
5. the application of the linear Ni-based complex electrode material of nanometer as claimed in claim 4, which is characterized in that the nano wire
The Ni-based complex electrode material of shape is applied to electrode of super capacitor.
6. the application of the linear Ni-based complex electrode material of nanometer according to claim 5, which is characterized in that described super
The preparation process of electrode for capacitors the following steps are included:
(1) by (7-8): (2-1): 1 quality Ni-based complex more linear than nanometer described in hybrid right requirement 4, conductive agent and
Binder, and dehydrated alcohol is added, after ultrasonic disperse, slurry is made；
(2) slurry is uniformly coated in substrate, at 80-120 DEG C, be dried in vacuo 8-16h after, with the pressure of 8-15MPa into
Electrode of super capacitor is obtained after row compressing tablet process.
7. the application of the linear Ni-based complex electrode material of nanometer according to claim 6, which is characterized in that the conduction
Agent is one of acetylene black, graphite and Super P.
8. the application of the linear Ni-based complex electrode material of nanometer according to claim 6, which is characterized in that the bonding
Agent is one of PVDF, PTFE and CMC.
9. the application of the linear Ni-based complex electrode material of nanometer according to claim 6, which is characterized in that the substrate is
One of nickel foam, copper foil, carbon cloth and carbon paper.
10. the application of the linear Ni-based complex electrode material of nanometer according to claim 6, which is characterized in that the substrate
Area is 1-2.5cm2, the load capacity 2-5mg of the linear Ni-based complex of nanometer in the substrate.
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| CN111508724A (en) * | 2020-06-11 | 2020-08-07 | 电子科技大学 | MOFs composite electrode material for supercapacitor, preparation method and working electrode |
| CN113957475A (en) * | 2021-09-18 | 2022-01-21 | 杭州师范大学 | Ni-N-C nano composite material and preparation method and application thereof |
| CN114388753A (en) * | 2021-12-13 | 2022-04-22 | 安徽大学 | Preparation method of edge nitrogen-doped porous hollow carbon nanorod material, prepared material and application thereof |
| CN114394627A (en) * | 2021-12-08 | 2022-04-26 | 中国民用航空飞行学院 | Preparation method of sodium ion cobalt sulfide nanowire |
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