CN110165161A - A kind of titanium carbide-carbon/manganese dioxide composite material and preparation method and application - Google Patents
A kind of titanium carbide-carbon/manganese dioxide composite material and preparation method and application Download PDFInfo
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- CN110165161A CN110165161A CN201910339260.4A CN201910339260A CN110165161A CN 110165161 A CN110165161 A CN 110165161A CN 201910339260 A CN201910339260 A CN 201910339260A CN 110165161 A CN110165161 A CN 110165161A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of applications of titanium carbide-carbon/manganese dioxide composite material and preparation method and the positive electrode as Zinc ion battery, pass through chemical vapour deposition technique, it under the conditions of 750~850 DEG C of temperature, reacts 1~2 hour, generates titanium carbide-carbon nano rod of Ti6Al4V load.Pass through hydro-thermal method again, using 0.02~0.1mol/L potassium permanganate and deionized water as reaction source, it is reacted 1~6 hour at a temperature of 120~160 DEG C, titanium carbide-carbon/manganese dioxide composite material is obtained after taking out drying, manganese dioxide nano-plates are uniformly supported on titanium carbide-carbon beam surface and form core-shell structure.Titanium carbide-carbon/manganese dioxide composite material in the present invention has high specific capacitance, high rate capability and high circulation service life, has broad application prospects in fields such as mobile communication, electric car and aerospaces.
Description
Technical field
The present invention relates to the positive electrode fields of Zinc ion battery, and in particular to a kind of titanium carbide-carbon/manganese dioxide is compound
The application of material and preparation method thereof and the positive electrode as Zinc ion battery.
Background technique
Currently, lithium ion battery occupies maximum commercial market, electric car has been widely used in it and mobile phone is mobile logical
The fields such as news.But lithium metal resource is limited, expensive.Meanwhile the harsh conditions that battery must make in water-less environment make
Its production cost increases.In addition, the organic electrolyte that lithium ion battery uses is usually toxic and inflammable, there are security risks.Water
It is ionic conductivity 2 orders of magnitude higher than organic electrolyte of electrolyte, thus water system battery is usual and has higher power close
Degree, and easily produce with it is at low cost.The aquo-lithium ion battery studied at present, the current potential that proton can be stabilized in the electrolytic solution
Window is relatively narrow, has many side reactions, such as the total insertion reaction of proton and ion in charge and discharge process, and electrode material is in water
In it is soluble, these factors limit the development of aquo-lithium ion battery.Zinc exceeds electricity with what low equilibrium potential and hydrogen were reacted
Position is the minimum element of all elements Plays current potential that can efficiently restore from aqueous solution.It can stablize in aqueous solution
Metallic element in, the energy of zinc is also highest.Meanwhile metallic zinc has resourceful, hypotoxicity and easy to handle etc. excellent
Point.Therefore cheap, highly-safe, non-environmental-pollution and high-power secondary zinc ion water system battery are ideal green electricity
Pond body system.
The ionic radius of zinc ion is 0.074nm, with lithium ion close to (0.076nm).But the atomic mass of zinc is big, zinc from
There are strong electrostatic interaction slow, the coulombic efficiencies that causes it to transport dynamics between son and the crystal structure of positive electrode
Low, high rate performance is poor.It therefore, can be as the type of Zinc ion battery positive electrode and few.Currently, Zinc ion battery is positive
Material category mainly includes Mn oxide, vanadium-based materials and prussian blue three categories.Three classes material respectively has the advantage and disadvantage of oneself,
In contrast, Mn-based material has higher energy density, and vanadium-based materials have higher power density.Mn oxide is current
The Zinc ion battery positive electrode of most study.Wherein δ type manganese dioxide has the layer structure of 1 × ∞, can effectively hold
The quick of zinc ion that receive is embedded in and deviates from, and has high capacity.But the low electric conductivity of Mn oxide leads to the high rate performance of its difference
And cycle performance.Manganese dioxide and carbon material are carried out compound being that the one kind for improving its electric conductivity and structural stability there are efficacious prescriptions
Formula.This mainly has benefited from the good characteristics such as carbon material its lightweight, high conductivity, high-specific surface area.Meanwhile manganese dioxide nano-plates
The contact area of electrode material and electrolyte is increased, the transmission of electronics and charge is conducive to, is capable of providing high capacitance.This
Outside, titanium carbide-carbon nano rod provides stable structural support for manganese dioxide, so that manganese dioxide is in charge discharge mistake
Stable structure is kept in journey, is not easy to collapse, to obtain good multiplying power and cycle performance.Above-mentioned scheme combines carbon material
It is the available strategy for constructing high-performance Zinc ion battery with the two-fold advantage of manganese dioxide.
Summary of the invention
It is an object of the invention to be directed to the electrode material poorly conductive of current Zinc ion battery, high rate performance difference etc. is asked
Topic, provides a kind of titanium carbide-carbon/manganese dioxide composite material and preparation method and the positive electrode as Zinc ion battery
Application, which inhibits manganese dioxide structure to collapse, accelerates the advantages such as reaction rate with high conductivity.
A kind of preparation method of titanium carbide-carbon/manganese dioxide composite material, includes the following steps:
(1) it by after titanium alloy-based bottom material dilute hydrochloric acid ultrasound, then is cleaned with deionized water and ethyl alcohol and removes surface several times
Greasy dirt, obtain pretreated titanium alloy substrate；
(2) the pretreated titanium alloy substrate that step (1) obtains is placed in tube furnace, under argon gas and hydrogen atmosphere
700~850 DEG C are warming up to, then carbonaceous liquid is introduced into cavity with the mode being bubbled, it is small that 1~2 is kept the temperature at 850 DEG C
When, growth is obtained after taking-up titanium carbide-carbon material titanium alloy substrate；
(3) growth for obtaining step (2) has titanium carbide-carbon material titanium alloy substrate to be immersed in potassium permanganate solution
In, it is then placed in reaction kettle, is heated to 120~160 DEG C, heating time is 2~6 hours, after reaction kettle is cooling, is taken out anti-
Product is answered, titanium carbide-carbon/manganese dioxide composite material is obtained after drying.
In step (1), the titanium alloy is Ti6Al4V.
The condition of the dilute hydrochloric acid ultrasound are as follows: temperature is 25 DEG C~30 DEG C, and dilute hydrochloric acid concentration is 1~3mol/L, ultrasound
Time is 10~20 minutes.
In step (2), the volume ratio of the argon gas and hydrogen is 5:1-15:1.
In step (2), the carbonaceous liquid is one or more of acetonitrile, acetone, ethyl alcohol.
In step (3), the concentration of the potassium permanganate solution is 0.02~0.1mol/L.According to actual needs, may be used
To control its changes of contents by adjusting reaction density and material.
Titanium carbide-the carbon/manganese dioxide composite electrode material (i.e. titanium carbide-carbon/manganese dioxide composite material), packet
It includes titanium alloy substrate, titanium carbide-carbon material for being grown in the titanium alloy substrate and be uniformly grown in the titanium carbide-
The manganese dioxide nano-plates of carbon material surface, the titanium carbide-carbon material be it is rod-shaped, including titanium carbide in the shape of a rod and cover
The carbon-coating on the titanium carbide surface is covered, is uniformly grown in titanium carbide-carbon beam surface, the carbonization titanium di is 10~
100nm, carbon layers having thicknesses are 5~20nm, and the manganese dioxide nano-plates are uniformly supported on titanium carbide-carbon nano rod table
Face.
The titanium carbide-carbon nano rod/manganese dioxide composite electrode material is used as the anode of Zinc ion battery
Material.Zinc ion battery titanium carbide-carbon nano rod/manganese dioxide composite electrode material in the present invention has height ratio capacity and height
Cycle life, high rate capability have in fields such as small-sized movable electronic equipment, electric car, solar power generation and aerospaces
Have broad application prospects.
Compared with prior art, the present invention has the advantage that
It is compound to prepare titanium carbide-carbon/manganese dioxide by hydro-thermal method method using titanium carbide-carbon as carbon material by the present invention
Material.The preparation method is simple and convenient, easily controllable.
Zinc ion battery titanium carbide-carbon/manganese dioxide composite electrode material prepared by the present invention, titanium carbide-carbon material tool
There is higher conductivity, meanwhile, manganese dioxide nano-plates provide bigger more effectively active reaction area, mention for electrochemical reaction
For good ion and electrons spread channel, the diffusion length of ion is shortened, accelerates electrochemical reaction process, improves its circulation
Stability and high rate performance, to realize with high-energy density, excellent cycle newly can and reliable and secure new zinc from
Sub- battery electrode material.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of titanium carbide-carbon nano rod obtained in embodiment 1；
Fig. 2 is the scanning electron microscope (SEM) photograph of titanium carbide-carbon/manganese dioxide composite material obtained in embodiment 1；
Fig. 3 is titanium carbide-carbon nano rod obtained in embodiment 1 and the transmission of titanium carbide-carbon/manganese dioxide composite material
Electron microscope, wherein (a) is titanium carbide-carbon nano rod transmission electron microscope picture in Fig. 3, and (b) is titanium carbide-carbon/manganese dioxide in Fig. 3
Transmission electron microscope picture.
Specific embodiment
Below with reference to embodiment, the present invention will be described in detail, but the present invention is not limited to this.
Embodiment 1
After Ti6Al4V substrate (titanium alloy, trade mark TC4) material dilute hydrochloric acid ultrasound, the condition of dilute hydrochloric acid ultrasound are as follows:
Temperature is 28 DEG C, and dilute hydrochloric acid concentration is 2mol/L, and ultrasonic time is 15 minutes, then is cleaned with deionized water and ethyl alcohol and removed several times
The greasy dirt on surface obtains pretreated Ti6Al4V base material.
Pretreated Ti6Al4V base material is placed in tube furnace, under argon gas and hydrogen atmosphere (volume ratio 5:
1) 750 DEG C are warming up to.Then acetone is introduced into cavity with the mode being bubbled, keeps the temperature 1 hour at 750 DEG C, growth is made
Titanium carbide-carbon nanometer bar material in Ti6Al4V substrate.Electronic Speculum is scanned to obtained titanium carbide-carbon nanometer bar material
(SEM) it is analyzed with transmission electron microscope (TEM), as shown in figures 1 and 3, it is seen that: titanium carbide average diameter is 50nm, and carbon layers having thicknesses are about
For 8nm, carbon-coating is covered on the outer surface of titanium carbide.
Next it weighs 3.16g potassium permanganate and is dissolved in 1000ml deionized water, stirring is made into 0.02mol/L to being completely dissolved
Potassium permanganate solution.Then it takes 50ml potassium permanganate solution to be put into polytetrafluoroethylene (PTFE) high pressure hydro-thermal tank, and is put into above-mentioned
Titanium carbide-carbon material, autoclave is sealed, the hydro-thermal reaction 2 hours under conditions of 120 DEG C.25 are cooled to room temperature after reaction
DEG C, drying is washed with deionized, titanium carbide-carbon/manganese dioxide composite material is made.To obtained titanium carbide-carbon/titanium dioxide
Manganese composite material is scanned Electronic Speculum (SEM) and transmission electron microscope (TEM) analysis, as shown in Figures 2 and 3, it is seen that: manganese dioxide is received
Rice piece is uniformly grown in titanium carbide-carbon beam surface, forms core-shell structure.
Embodiment 2
After Ti6Al4V substrate (titanium alloy, trade mark TC4) material dilute hydrochloric acid ultrasound, the condition of dilute hydrochloric acid ultrasound are as follows:
Temperature is 25 DEG C, and dilute hydrochloric acid concentration is 3mol/L, and ultrasonic time is 10 minutes, then is cleaned with deionized water and ethyl alcohol and removed several times
The greasy dirt on surface obtains pretreated Ti6Al4V base material.
Pretreated Ti6Al4V base material is placed in tube furnace, (volume ratio is under argon gas and hydrogen atmosphere
10:1) it is warming up to 800 DEG C.Then acetone is introduced into cavity with the mode being bubbled, keeps the temperature 1.5 hours at 800 DEG C, life is made
Grow titanium carbide-carbon nanometer bar material in Ti6Al4V substrate.
It weighs 7.9g potassium permanganate and is dissolved in 1000ml deionized water, stirring is made into 0.05mol/L permanganic acid to being completely dissolved
Aqueous solutions of potassium.Then it takes 50ml potassium permanganate solution to be put into polytetrafluoroethylene (PTFE) high pressure hydro-thermal tank, and is put into above-mentioned preparation
Titanium carbide-carbon substrate, autoclave is sealed, the hydro-thermal reaction 4 hours under conditions of 140 DEG C.25 DEG C are cooled to room temperature after reaction,
Drying is washed with deionized, titanium carbide-carbon/manganese dioxide composite material is made.
Embodiment 3
After Ti6Al4V substrate (titanium alloy, trade mark TC4) material dilute hydrochloric acid ultrasound, the condition of dilute hydrochloric acid ultrasound are as follows:
Temperature is 30 DEG C, and dilute hydrochloric acid concentration is 1mol/L, and ultrasonic time is 20 minutes, then is cleaned with deionized water and ethyl alcohol and removed several times
The greasy dirt on surface obtains pretreated Ti6Al4V base material.
Pretreated Ti6Al4V base material is placed in tube furnace, (volume ratio is under argon gas and hydrogen atmosphere
15:1) it is warming up to 850 DEG C.Then acetone is introduced into cavity with the mode being bubbled, keeps the temperature 2 hours at 850 DEG C, life is made
Grow titanium carbide-carbon nanometer bar material in Ti6Al4V substrate.
It weighs 15.8g potassium permanganate and is dissolved in 1000ml deionized water, stirring is made into 0.1mol/L permanganic acid to being completely dissolved
Aqueous solutions of potassium.Then it takes 50ml potassium permanganate solution to be put into polytetrafluoroethylene (PTFE) high pressure hydro-thermal tank, and is put into above-mentioned preparation
Titanium carbide-carbon substrate, autoclave is sealed, the hydro-thermal reaction 6 hours under conditions of 160 DEG C.25 DEG C are cooled to room temperature after reaction,
Drying is washed with deionized, titanium carbide-carbon/manganese dioxide composite material is made.
Performance test
Using titanium carbide made of above-described embodiment 1~3-carbon/manganese dioxide composite material as the anode of Zinc ion battery,
Metal zinc metal sheet tests Zinc ion battery performance as cathode respectively in two electrode systems.Electrolyte be 2mol/L zinc sulfate and
0.2mol/L manganese sulfate solution, charging/discharging voltage are 1.0~1.8V, circulation measurement titanium carbide-carbon/bis- in 25 ± 1 DEG C of environment
Reversible charge and discharge specific capacitance, charge-discharge performance and the high-rate characteristics of manganese oxide composite material.
The performance test results are as follows:
Titanium carbide-carbon/manganese dioxide composite electrode material of embodiment 1, embodiment 2 and embodiment 3 is in 0.5A/g electric current
Specific capacitance of discharging under density is respectively 180F/g, 245F/g and 276F/g, and electric discharge specific capacitance conservation rate reaches after 1000 circulations
94% or more.As it can be seen that Zinc ion battery titanium carbide obtained above-carbon/manganese dioxide composite material charge/discharge capacity is high, circulation
Stability is good.
Titanium carbide-carbon/manganese dioxide composite electrode material of embodiment 1, embodiment 2 and embodiment 3 is close in 5A/g electric current
The lower electric discharge specific capacitance of degree is respectively 165F/g, 221F/g and 248F/g.As it can be seen that Zinc ion battery titanium carbide-carbon obtained above/
The high rate capability of manganese dioxide composite electrode material is good.
This is because titanium carbide-carbon material introduces the electric conductivity for improving entire composite material, the manganese dioxide of crosslinking
Nanometer sheet is conducive to increase the contact area of electrode and electrolyte, and provides more effective active reaction area, while being electricity
Chemical reaction provides good ion and electrons spread channel, shortens the diffusion length of ion, improves Zinc ion battery performance.
Therefore, Zinc ion battery titanium carbide-carbon/manganese dioxide composite electrode material of the present invention has height ratio capacity and Gao Xun
Ring service life, high rate capability have in fields such as small-sized movable electronic equipment, electric car, solar power generation and aerospaces
Wide application prospect.
Claims (10)
1. a kind of titanium carbide-carbon/manganese dioxide composite material preparation method, which comprises the steps of:
(1) by after titanium alloy-based bottom material dilute hydrochloric acid ultrasound, then the oil for removing surface several times is cleaned with deionized water and ethyl alcohol
Dirt obtains pretreated titanium alloy substrate；
(2) the pretreated titanium alloy substrate that step (1) obtains is placed in tube furnace, is heated up under argon gas and hydrogen atmosphere
To 700~850 DEG C, then carbonaceous liquid is introduced into cavity with the mode being bubbled, 1~2 hour is kept the temperature at 850 DEG C, takes
Growth is obtained after out titanium carbide-carbon material titanium alloy substrate；
(3) growth for obtaining step (2) has titanium carbide-carbon material titanium alloy substrate to be immersed in potassium permanganate solution,
Then it is placed in reaction kettle, is heated to 120~160 DEG C, heating time is 2~6 hours, after reaction kettle is cooling, takes out reaction
Product obtains titanium carbide-carbon/manganese dioxide composite material after drying.
2. titanium carbide according to claim 1-carbon/manganese dioxide composite material preparation method, which is characterized in that step
(1) in, the titanium alloy is Ti6Al4V.
3. titanium carbide according to claim 1-carbon/manganese dioxide composite material preparation method, which is characterized in that step
(1) in, the condition of the dilute hydrochloric acid ultrasound are as follows: temperature is 25 DEG C~30 DEG C, and dilute hydrochloric acid concentration is 1~3mol/L, when ultrasonic
Between be 10~20 minutes.
4. titanium carbide according to claim 1-carbon/manganese dioxide composite material preparation method, which is characterized in that step
(2) in, the volume ratio of the argon gas and hydrogen is 5:1-15:1.
5. titanium carbide according to claim 1-carbon/manganese dioxide composite material preparation method, which is characterized in that step
(2) in, the carbonaceous liquid is one or more of acetonitrile, acetone, ethyl alcohol.
6. titanium carbide according to claim 1-carbon/manganese dioxide composite material preparation method, which is characterized in that step
(3) in, the concentration of the potassium permanganate solution is 0.02~0.1mol/L.
7. titanium carbide-carbon/manganese dioxide composite material of described in any item preparation method preparations according to claim 1~6.
8. titanium carbide-carbon/manganese dioxide composite material of preparation method preparation according to claim 7, which is characterized in that
Including titanium alloy substrate, the titanium carbide-carbon material being grown in the titanium alloy substrate and uniformly it is grown in the carbonization
Titanium-carbon material surface manganese dioxide nano-plates.
9. titanium carbide-carbon/manganese dioxide composite material of preparation method preparation according to claim 8, the carbonization
Titanium-carbon material be it is rod-shaped, including titanium carbide in the shape of a rod and be covered on the carbon-coating on the titanium carbide surface.
10. according to titanium carbide-carbon/manganese dioxide composite material of the preparation of preparation method described in claim 7,8 or 9 as zinc
The application of the positive electrode of ion battery.
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Cited By (3)
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| CN110993908A (en) * | 2019-11-27 | 2020-04-10 | 浙江大学 | Vertical graphene/manganese dioxide composite material and preparation method and application thereof |
| CN113548695A (en) * | 2021-07-13 | 2021-10-26 | 浙江大学 | High-crystallinity birnessite type manganese dioxide nano flower ball and preparation method and application thereof |
| CN113636554A (en) * | 2021-08-12 | 2021-11-12 | 电子科技大学长三角研究院(湖州) | Titanium carbide-carbon core-shell array loaded vertical graphene/manganese dioxide composite material and preparation method and application thereof |
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Cited By (4)
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| CN113548695A (en) * | 2021-07-13 | 2021-10-26 | 浙江大学 | High-crystallinity birnessite type manganese dioxide nano flower ball and preparation method and application thereof |
| CN113636554A (en) * | 2021-08-12 | 2021-11-12 | 电子科技大学长三角研究院(湖州) | Titanium carbide-carbon core-shell array loaded vertical graphene/manganese dioxide composite material and preparation method and application thereof |
| CN113636554B (en) * | 2021-08-12 | 2022-12-20 | 电子科技大学长三角研究院(湖州) | Titanium carbide-carbon core-shell array loaded vertical graphene/manganese dioxide composite material and preparation method and application thereof |
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