CN110085829A - A kind of MXene@C@Co9S8Compound and preparation method thereof - Google Patents
A kind of MXene@C@Co9S8Compound and preparation method thereof Download PDFInfo
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- CN110085829A CN110085829A CN201910338741.3A CN201910338741A CN110085829A CN 110085829 A CN110085829 A CN 110085829A CN 201910338741 A CN201910338741 A CN 201910338741A CN 110085829 A CN110085829 A CN 110085829A
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
- H01M4/366—Composites as layered products
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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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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- 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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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 belongs to technical field of material, specially a kind of MXene@C@Co9S8Compound and preparation method thereof.Co9S8Has high specific capacity, but huge volume expansion limits its application in its poor electric conductivity and chemical reaction.The present invention uses solution coprecipitation, and carbon-coated Co is loaded on Mxene9S8Nano particle, while passing through the double-deck confinement effect and the common promotion Co of nanosizing effect9S8As the chemical property of electrode material, the composite material MXene@C@Co of preparation9S8As lithium ion battery negative material, in 100mAg‑1Under current density, 1680mAhg is still protected after circulation 100 times‑1Specific capacity；As anode material of lithium-ion battery, in 100mAg‑1Under current density, 585 mAhg are still maintained after circulation 100 times‑1Specific capacity；As aluminum cell negative electrode material, in 1000mAg‑1Under current density, 107 mAhg are still maintained after circulation 1000 times‑1Specific capacity.
Description
Technical field
The invention belongs to technical field of material, and in particular to MXene@C@Co9S8Compound and preparation method thereof.
Background technique
The new problems such as a large amount of consumption, the discharge of greenhouse gases and the multiplication of demand for energy with fossil fuel arrive
, finding clean reproducible energy and storing utilization in addition is current facing mankind " energy crisis " problem to be solved.Mesh
How preceding main clean energy resource converts electric energy picture storage fossil for them and fires from wind energy, water energy and solar energy etc.
Material equally stores stand-by.This problem of the battery system very good solution that grows up at the beginning of 21 century at the end of the 20th century.
By migration of the ion in Different electrodes material, realize that electric energy is converted into the chemical energy in material, so as to complete electric energy
Storage and secondary use 1.Undergo more than two decades research progress and Market Selection after, with lithium transition-metal oxide be anode and
Graphite is that the lithium ion battery of cathode gradually occupies the market of Portable secondary battery (can repeated charge pond), mobile phone,
The fields such as laptop, electric car have played huge effect.However as the further development of science and technology, to the following energy storage
The requirement of system (the especially energy density, power density and cycle life of energy storage device) further increases, and is limited to mesh
The relatively low specific capacity of positive and negative anodes and part scarce resource is non-renewable in preceding lithium ion battery, and exploitation higher energy is close
The secondary cell of new generation extremely urgent 2 of degree.The exploitation of metal sulfide electrode material can effectively avoid above-mentioned disadvantage.In addition
The development and application of the new type of energy storage device such as sodium, aluminum cell is also the inexorable trend 1,3 of electrochemistry development.It is of the invention initiative
The MXene@C@Co for being prepared for loading in situ9S8Compound has obtained finely dispersed MXene@C@using PVP is amphipathic
Co9S8Compound is used for lithium ion battery, sodium-ion battery and aluminium ion battery electrode material, shows preferable electrification
Learn performance.Wherein, the MXene@C@Co of 20% MXene load capacity9S8Compound as lithium ion battery negative material,
100mAg-1Under current density, 1680mAhg is still maintained after circulation 100 times-1Specific capacity；As sodium-ion battery cathode
Material, in 100mAg-1Under current density, 585 mAhg are still maintained after circulation 100 times-1Specific capacity；It is negative as aluminum cell
Pole material, in 1000mAg-1Under current density, 107 mAhg are still maintained after circulation 1000 times-1Specific capacity.
Bibliography:
1、Yuxiang Hu, Delai Ye, Bin Luo, Han Hu, Xiaobo Zhu, Songcan Wang, Linlin
Li,Shengjie Peng,and Lianzhou Wang.A Binder-Free and Free-Standing Cobalt
Sulfide @Carbon Nanotube Cathode Material for Aluminum-Ion Batteries.Adv.
Mater. 2018, 30, 1703824.
2、Shuai Wang, Zhijing Yu, Jiguo Tu, Junxiang Wang, Donghua Tian, Yingjun
Liu,and Shuqiang Jiao;A Novel Aluminum-Ion Battery: Al/AlCl3-[EMIm]Cl/Ni3S2@
Graphene;Adv. Energy Mater. 2016, 1600137.
3、Ziliang Chen, Renbing Wu, Miao Liu, Hao Wang, Hongbin Xu, Yanhui Guo,
Yun Song,Fang Fang, Xuebin Yu, and Dalin Sun;General Synthesis of Dual
Carbon-Confined Metal Sulfides Quantum Dots Toward High-Performance Anodes
for Sodium-Ion Batteries;Adv. Funct. Mater. 2017, 27, 1702046。
Summary of the invention
It is an object of the present invention to provide a kind of synthesis technologies simply, the MXene@C@Co of electrochemical performance9S8Compound and
Preparation method, to meet producing scientific research demand.
MXene@C@Co provided by the invention9S8The principle of compound preparation method, reaction is:
The specific steps of preparation are as follows:
(1) preparation of ZIF-67: cabaltous nitrate hexahydrate is dissolved in methanol, forms solution A;2-methylimidazole is dissolved in methanol
In, form solution B;Solution B is poured into solution A, 1-24h is stirred at room temperature；Product is denoted as ZIF-67；
(2) preparation of PVP-ZIF-67: will ZIF-67 dispersion in PVP, wherein ZIF-67 and PVP mass ratio are 20-40；It produces
Object is denoted as PVP-ZIF-67；
(3) preparation of PVP-MXene: will MXene dispersion in PVP, wherein MXene and PVP mass ratio are 20-40；Product note
For PVP-MXene；
(4) preparation of MXene-ZIF-67: PVP-ZIF-67 and PVP-MXene are stirred and evenly mixed, wherein the glue stick time is 1-
24h；Product is denoted as) MXene-ZIF-67；
(5) MXene@C@Co9S8The preparation of compound: MXene-ZIF-67 is placed in tube furnace, under nitrogen atmosphere protection,
500 ~ 800 DEG C are warming up to the rate of 4 ~ 6 DEG C/min, 1 ~ 5 h of reaction time is to get MXene load C o9S8, it is denoted as
MXene@C@Co9S8。
In the present invention, by adjusting the ratio of MXene, MXene@C@Co is controlled9S8Synthesis: the quality percentage of ZIF-67
Number is 40 ~ 90 %, and the mass percent of MXene is 60-10 %.
In the present invention, Co9S8Since electric conductivity is bad and huge volume expansion leads to electrochemistry in electrochemical reaction
Circulation and high rate performance are very poor, and by means of the present invention, by MXene and Co9S8It is compound, it is shown as electrode material
The service life of the circulation of overlength.Therefore, the material that the present invention is studied has superior chemical property.
MXene and Co9S8Electrochemical property test of the composite material as electrode material:
The assembling of button cell can substantially be divided into following steps: slurrying, smear dry piece, punching, pole piece weighing, assembly electricity
Pond.
By active material, conductive agent (Super-p), binder (CMC) according to 8:1:1 ratio mixing paste, and when slurry it is first
CMC is dissolved in distilled water, mass ratio is 1%(matching while using), then active material and conductive agent are weighed into loading in proportion
In weighing bottle, CMC solution is added in proportion for dry stir after 10min, persistently stirs 8h-10h.When smear, first copper foil is used
Alcohol swab is wiped clean, and drying is uniformly coated on slurry using scraper.After drying (80 DEG C keep for 24 hours), sheet-punching machine is used
It is washed into the disk of diameter 15mm, and is weighed.The material containing amount of each pole piece is about 1mg/cm2.Pole piece is transferred to gloves
(H in case2O and O2Content in 0.1ppm or less), by anode cover, pole piece, thin membrane, thick skirt, lithium piece, stainless steel pad
The sequence assembling of piece, spring washer, negative electrode casing, and appropriate electrolyte is added, assembling lithium/sode cell battery case uses 3025
Type.Assembling aluminum cell battery case is self-control die battery shell.It is finally transferred out of glove box, the solid content of each slurrying compares one
It causes.
Charge-discharge test
Charge-discharge test of the present invention is carried out by Landian battery testing system.Steps are as follows:
Lithium/sode cell test: standing, returns to initial work step to execute at constant-current discharge to 0.01V, standing, constant-current charge to 3V
Loop command.Wherein, the setting of constant current value is set according to the quality of pole piece active material.
Aluminum cell test: standing, constant-current discharge to 0.01V, standing, constant-current charge to 1.62V, return to initial work step with
Execute loop command.Wherein, the setting of constant current value is set according to the quality of pole piece active material.
The present invention has the following aspects remarkable advantage:
(1) simple process, synthesis are convenient；
(2) technique is not high to equipment requirement, it is easy to accomplish.
Detailed description of the invention
Fig. 1 is the XRD spectra of 1 gained sample of embodiment.
Fig. 2 is lithium ion battery cyclic curve (100 mAg of current density of 2 gained sample of embodiment-1).
Fig. 3 is sodium-ion battery cyclic curve (100 mAg of current density of 1 gained sample of embodiment-1).
Fig. 4 is 3 gained sample aluminum cell cyclic curve (1000 mAg of current density of embodiment-1).
Specific embodiment
Embodiment 1,10% MXene@C@Co9S8Preparation
30mg cabaltous nitrate hexahydrate is dissolved in 1ml methanol, solution A is formed;0.8g 2-methylimidazole is dissolved in 14ml methanol
In, form solution B;Solution B is poured into solution A, is stirred at room temperature for 24 hours；By ZIF-67 dispersion in PVP, wherein ZIF-67 and PVP
Mass ratio is 20；By MXene dispersion with PVP, wherein MXene and PVP mass ratio are 20；By PVP-ZIF-67 and PVP-
MXene is stirred and evenly mixed, and wherein the splash bar time is for 24 hours；MXene-ZIF-67 is placed in tube furnace, under nitrogen atmosphere protection,
500 DEG C are warming up to the rate of 4 DEG C/min, 2 h of reaction time is to get MXene load C o9S8, it is denoted as 10%-MXene@C@
Co9S8。
2. 20% MXene@C@Co of embodiment9S8Preparation
30mg cabaltous nitrate hexahydrate is dissolved in 1ml methanol, solution A is formed;0.8g 2-methylimidazole is dissolved in 14ml methanol
In, form solution B;Solution B is poured into solution A, 12h is stirred at room temperature；By ZIF-67 dispersion in PVP, wherein ZIF-67 and PVP
Mass ratio is 30；By MXene dispersion with PVP, wherein MXene and PVP mass ratio are 30；By PVP-ZIF-67 and PVP-
MXene is stirred and evenly mixed, and wherein the splash bar time is 12 h；MXene-ZIF-67 is placed in tube furnace, under nitrogen atmosphere protection,
600 DEG C are warming up to the rate of 2 DEG C/min, 2 h of reaction time is to get MXene load C o9S8, it is denoted as 20%-MXene@C@
Co9S8。
3. 30% MXene@C@Co of embodiment9S8Preparation
30mg cabaltous nitrate hexahydrate is dissolved in 1ml methanol, solution A is formed;0.8g 2-methylimidazole is dissolved in 14ml methanol
In, form solution B;Solution B is poured into solution A, 12h is stirred at room temperature；By ZIF-67 dispersion in PVP, wherein ZIF-67 and PVP
Mass ratio is 40；By MXene dispersion with PVP, wherein MXene and PVP mass ratio are 40；By PVP-ZIF-67 and PVP-
MXene is stirred and evenly mixed, and wherein the splash bar time is 10h；MXene-ZIF-67 is placed in tube furnace, under nitrogen atmosphere protection,
800 DEG C are warming up to the rate of 6 DEG C/min, 2 h of reaction time is to get MXene load C o9S8, it is denoted as 30%-MXene@C@
Co9S8。
Claims (3)
1. a kind of MXene@C@Co9S8The preparation method of compound, which is characterized in that specific steps are as follows:
(1) preparation of ZIF-67: cabaltous nitrate hexahydrate is dissolved in methanol, forms solution A；2-methylimidazole is dissolved in methanol
In, form solution B；Solution B is poured into solution A, 1-24h is stirred at room temperature, product is denoted as ZIF-67；
(2) it the preparation of PVP-ZIF-67: disperses ZIF-67 in PVP, wherein ZIF-67 is 20-40 with PVP mass ratio；It produces
Object is denoted as PVP-ZIF-67；
(3) it the preparation of PVP-MXene: disperses MXene in PVP, wherein MXene is 20-40 with PVP mass ratio；Product note
For PVP-Mxene；
(4) preparation of MXene-ZIF-67: PVP-ZIF-67 and PVP-MXene are stirred and evenly mixed, mixing time 1-24h；It produces
Object is denoted as MXene-ZIF-67；
(5) MXene@C@Co9S8The preparation of compound: MXene-ZIF-67 is placed in tube furnace, under nitrogen atmosphere protection,
500 ~ 800 DEG C are warming up to the rate of 4 ~ 6 DEG C/min, 1 ~ 5 h of reaction time is to get MXene load C o9S8, it is denoted as
MXene@C@Co9S8。
2. MXene@C@Co according to claim 19S8The preparation method of compound, which is characterized in that pass through adjusting
The load factor of MXene and the ratio of ZIF-67 control MXene@C@Co9S8Synthesis: the mass percent of ZIF-67 be 40 ~
The mass percent of 90 %, MXene are 60-10 %.
3. a kind of MXene@C@Co being prepared by preparation method as claimed in claim 1 or 29S8Compound.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110589786A (en) * | 2019-10-16 | 2019-12-20 | 大连理工大学 | Based on three-dimensional porous transition metal carbide Ti3C2MXene composite nano structure and general preparation method thereof |
| CN111710862A (en) * | 2020-06-28 | 2020-09-25 | 山东大学 | 3D porous Sb/Ti for high-performance potassium ion battery3C2Preparation method of MXene composite material |
| CN111755262A (en) * | 2020-07-10 | 2020-10-09 | 大连理工大学 | CoS/Ti applied to super capacitor3C2Preparation method of (1) |
| CN111924888A (en) * | 2020-08-12 | 2020-11-13 | 洛阳理工学院 | Novel Co9S8Nano-particle composite electrode material and preparation method and application thereof |
| CN112635738A (en) * | 2020-12-22 | 2021-04-09 | 江西理工大学 | Preparation method of FeNiP/C @ MXene composite anode material for lithium ion battery |
| CN112670524A (en) * | 2020-09-04 | 2021-04-16 | 华中科技大学 | Ultrathin flexible air electrode material, lithium air battery and preparation method of ultrathin flexible air electrode material |
| CN112680746A (en) * | 2020-11-26 | 2021-04-20 | 大连理工大学 | ZIF-67@ MXene composite material, and preparation method and application thereof |
| CN114162876A (en) * | 2021-12-10 | 2022-03-11 | 盐城工学院 | Preparation method and application of Co9S8@ carbon nanotube @ graphene composite material |
| CN114937761A (en) * | 2022-04-25 | 2022-08-23 | 多助科技(武汉)有限公司 | Nobaltosulfide/manganese sulfide/nitrogen-carbon composite material and preparation method and application thereof |
-
2019
- 2019-04-25 CN CN201910338741.3A patent/CN110085829A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110589786A (en) * | 2019-10-16 | 2019-12-20 | 大连理工大学 | Based on three-dimensional porous transition metal carbide Ti3C2MXene composite nano structure and general preparation method thereof |
| CN111710862A (en) * | 2020-06-28 | 2020-09-25 | 山东大学 | 3D porous Sb/Ti for high-performance potassium ion battery3C2Preparation method of MXene composite material |
| CN111755262A (en) * | 2020-07-10 | 2020-10-09 | 大连理工大学 | CoS/Ti applied to super capacitor3C2Preparation method of (1) |
| CN111755262B (en) * | 2020-07-10 | 2021-08-06 | 大连理工大学 | CoS/Ti applied to super capacitor3C2Preparation method of (1) |
| CN111924888B (en) * | 2020-08-12 | 2021-06-15 | 洛阳理工学院 | Co9S8Nano-particle composite electrode material and preparation method and application thereof |
| CN111924888A (en) * | 2020-08-12 | 2020-11-13 | 洛阳理工学院 | Novel Co9S8Nano-particle composite electrode material and preparation method and application thereof |
| CN112670524A (en) * | 2020-09-04 | 2021-04-16 | 华中科技大学 | Ultrathin flexible air electrode material, lithium air battery and preparation method of ultrathin flexible air electrode material |
| CN112680746A (en) * | 2020-11-26 | 2021-04-20 | 大连理工大学 | ZIF-67@ MXene composite material, and preparation method and application thereof |
| CN112635738A (en) * | 2020-12-22 | 2021-04-09 | 江西理工大学 | Preparation method of FeNiP/C @ MXene composite anode material for lithium ion battery |
| CN112635738B (en) * | 2020-12-22 | 2021-09-21 | 江西理工大学 | Preparation method of FeNiP/C @ MXene composite anode material for lithium ion battery |
| CN114162876A (en) * | 2021-12-10 | 2022-03-11 | 盐城工学院 | Preparation method and application of Co9S8@ carbon nanotube @ graphene composite material |
| CN114937761A (en) * | 2022-04-25 | 2022-08-23 | 多助科技(武汉)有限公司 | Nobaltosulfide/manganese sulfide/nitrogen-carbon composite material and preparation method and application thereof |
| CN114937761B (en) * | 2022-04-25 | 2023-10-13 | 多助科技(武汉)有限公司 | Nine cobalt octasulfide/manganese sulfide/nitrogen carbon composite material and preparation method and application thereof |
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Application publication date: 20190802 |