CN110190263A - A kind of graphene oxide doped FeS composite nano materials and its preparation method and application - Google Patents
A kind of graphene oxide doped FeS composite nano materials and its preparation method and application Download PDFInfo
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- CN110190263A CN110190263A CN201910514575.8A CN201910514575A CN110190263A CN 110190263 A CN110190263 A CN 110190263A CN 201910514575 A CN201910514575 A CN 201910514575A CN 110190263 A CN110190263 A CN 110190263A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
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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
- H01M4/36—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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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 present invention discloses a kind of graphene oxide doped FeS composite nano materials and its preparation method and application, 1) preparation method is the following steps are included: take analytically pure ammonium ferric oxalate, urea mixed grinding to obtain mixture A；2) mixture A is heat-treated in low temperature tube furnace and obtains product B；3) taking graphene oxide and CTAB that deionized water system ultrasonic treatment is added keeps graphene oxide fully dispersed；4) product B is mixed to suction filtration, freeze-drying after being centrifuged with solution C and obtains product D；5) mixture E is obtained after taking product D and sulphur source mixed grinding, is heat-treated to obtain graphene oxide doped FeS composite nano materials under argon nitrogen atmosphere in low temperature tube furnace；The present invention uses two-step synthesis method, and the addition of Surfactant CTAB increases the dispersion degree of graphene sheet layer, so that graphene is uniform in conjunction with carbon-coating, stability of material is good, and structure is not easy to collapse and be crushed, and the electrochemistry for improving FeS negative electrode material stores up sodium performance.
Description
Technical field
The invention belongs to composite materials to synthesize field, and in particular to a kind of graphene oxide doped FeS composite nano materials
And its preparation method and application.
Background technique
Due to sodium element widely distributed and rich reserves, in recent years research and development of room temperature sodium ion charge-discharge battery in the earth
It has been considered as substituting lithium ion battery in the fields such as extensive energy storage, especially smart grid, effectively to solve lithium ion
Battery mineral lay in the low and high cost problem of lithium source effective way.In numerous anode material of lithium-ion battery systems, carbon, gold
Belong to oxide or the alloy-types material such as sulfide and Sn, Sb is a few class material systems that scholars most pay close attention to.Wherein, FeS makees
For the electrode of sodium-ion battery, the material with nano-scale structures can reduce the conveying length of electronics, shorten the expansion of ion
Path is dissipated, and mitigates the mechanical stress due to caused by the big volume fluctuation generated in duplicate film forming/degenerative process, in detail
See file [1].It is resourceful due to theoretical capacity with higher, low toxicity, the advantages that electric conductivity is preferable is potential sodium from
The negative electrode material of sub- battery.However FeS electric conductivity it is not high, with the interface compatibility of organic electrolyte is poor, the microcosmic ruler of electrode material
Very little deficiency big, that effective charge and discharge active site utilization rate is low greatly hinders the ability of its electrochemistry storage sodium, is detailed in file
[2].Simultaneously as FeS resistivity is larger, voltage decline is very fast when electric discharge, can especially generate in high-rate battery discharge tight
The polarization phenomena of weight, greatly shorten the working life of battery, are detailed in file [3].Therefore, FeS is promoted as negative electrode material in sodium
Circulation volume and sustainability in ion battery are the directions needed to be studied at present.
[1]Y.X.Wang,S.L.Chou,D.Wexler,H.K.Liu,S.X.Dou,Chem.Eur.J.2014,20,
9607.
[2]Y.Y.Zhu,P.Nie,L.F.Shen,S.Y.Dong,Q.Sheng,H.S.Li,H.F.Luo,X.G.Zhang,
Nanoscale 2015,7,3309；b)Y.Zheng,T.F.Zhou,C.F.Zhang,J.F.Mao,H.K.Liu,Z.P.Guo,
Angew.Chem.Int.Ed.2016,55,3408.
[3]a)X.H.Xia,C.R.Zhu,J.S.Luo,Z.Y.Zeng,C.Guan,C.F.Ng,H.Zhang,H.J.Fan,
Small 2014,10,766；b)Y.K.Startsev,A.A.Pronkin,I.A.Sokolov,I.V.Murin,Glass
Phys.Chem.2011,37,263；c)Y.C.Du,X.S.Zhu,X.S.Zhu,L.Y.Hu,Z.H.Dai,J.C.Bao,
J.Mater.Chem.A 2015,3,6787.
Summary of the invention
The object of the present invention is to provide a kind of graphene oxide doped FeS composite nano materials and preparation method thereof and answer
With this method is readily synthesized, preparation cost is low, and the graphene oxide doped FeS composite nano materials of preparation have high sodium
Ion storage performance.
In order to achieve the above objectives, the technical solution adopted by the present invention is that:
A kind of graphene oxide doped FeS composite nano materials preparation method, comprising the following steps:
1) 1:(1~7 in mass ratio) analytically pure ammonium ferric oxalate, urea are taken, mixture A is obtained after mixed grinding；
2) mixture A is heat-treated in low temperature tube furnace, 500 are warming up to the heating rate of 2~20 DEG C/min~
1200 DEG C of heat preservation 1h~5h take out after cooling, obtain product B；
3) 3:1 in mass ratio takes graphene oxide and CTAB, and the solution C that deionized water is prepared into 1-3mg/ml is added, and surpasses
Sonication keeps graphene oxide fully dispersed；
4) product B is mixed with solution C, magnetic agitation is uniform, filters, is freeze-dried after centrifugation, obtains product D；
5) 1:(5~10 in mass ratio) take product D and sulphur source mixed grinding after obtain mixture E；
6) mixture E is heat-treated under argon nitrogen atmosphere in low temperature tube furnace, with the heating rate of 5~10 DEG C/min
300~600 DEG C of heat preservation 30min~1h are warming up to, are taken out after cooling to get graphene oxide doped FeS composite nano materials are arrived.
Further, the sulphur source is sublimed sulfur, thioacetamide, thiocarbamide or trithiocyanuric acid.
Further, sonication treatment time is 3h in the step 3).
Further, it is described 4) in the magnetic agitation time be for 24 hours.
A kind of graphene oxide doped FeS composite nano materials, the application as anode material of lithium-ion battery.
The utility model has the advantages that
The present invention prepares FeS composite oxygen graphene nano material using two-step synthesis method, and preparation method simple and stable can
Repeated strong, low in raw material price can significantly reduce the preparation cost for having the material reported in the literature.Surfactant CTAB
Addition increase the dispersion degree of graphene sheet layer so that graphene in conjunction with carbon-coating uniformly, when in battery charge and discharge process,
The volume change of vulcanization iron material as cell negative electrode material is absorbed by carbon-coating and graphene mostly, is played buffer function, is made
Material shows better stability, and material structure is not easy to collapse and broken, battery after cycling the phase can also show it is biggish
Charge/discharge capacity.
Method of the invention combine the high capacity of vulcanization iron material, be readily synthesized, preparation cost is low and graphene oxide is led
The advantages that electric energy power is strong, the electrochemistry for improving FeS negative electrode material store up sodium performance.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph that embodiment 1 prepares product；
Fig. 2 is the product of the preparation of embodiment 2 as anode material of lithium-ion battery cycle performance figure；
Specific embodiment
Present invention is further described in detail combined with specific embodiments below, but not as a limitation of the invention.
Embodiment 1:
1) analytically pure ammonium ferric oxalate 2g, urea 2g are taken, obtains mixture after mixed grinding in glass mortar, this is mixed
It closes object and is denoted as A；
2) mixture A is heat-treated in low temperature tube furnace, is taken out after cooling, obtains product B, heat treatment heating rate is
2 DEG C/min, heat treatment temperature is 500 DEG C, time 5h；
3) 3:1 in mass ratio mixes graphene oxide with cetyl trimethylammonium bromide CTAB, and deionized water is added
It is prepared into the solution of 1mg/ml, 3h is ultrasonically treated, is denoted as C；
4) product B is mixed with solution C, magnetic stirrer for 24 hours, filters after centrifugation, is freeze-dried, obtain product D；
5) product 1g sample D and 5g sublimed sulfur are obtained into mixture in glass mortar after mixed grinding, mixture note
For E；
6) mixture E being heat-treated under argon nitrogen atmosphere in low temperature tube furnace again, heat treatment heating rate is 5 DEG C/min,
Heat treatment temperature is 300 DEG C, soaking time 1h, takes out after cooling, obtains product F, i.e. vulcanization iron nano-particle.
As can be seen that FeS nano particle dense growth, outside has coated one layer of oxidation stone from the scanning figure of Fig. 1 sample
Black alkene, this structure can improve the stability and electric conductivity of material.
Embodiment 2:
1) analytically pure ammonium ferric oxalate 2g, urea 6g are taken, obtains mixture after mixed grinding in glass mortar, this is mixed
It closes object and is denoted as A；
2) mixture A is heat-treated in low temperature tube furnace, is taken out after cooling, obtains product B, heat treatment heating rate is
10 DEG C/min, heat treatment temperature is 800 DEG C, time 3h；
3) 3:1 in mass ratio mixes graphene oxide with cetyl trimethylammonium bromide CTAB, and deionized water is added
It is prepared into the solution of 2mg/ml, 3h is ultrasonically treated, is denoted as C；
4) product B is mixed with solution C, magnetic stirrer for 24 hours, filters after centrifugation, is freeze-dried, obtain product D；
5) product 1g sample D and 10g thioacetamide are obtained into mixture in glass mortar after mixed grinding, the mixing
Object is denoted as E；
6) mixture E being heat-treated under argon nitrogen atmosphere in low temperature tube furnace again, heat treatment heating rate is 8 DEG C/min,
Heat treatment temperature is 500 DEG C, soaking time 40min, takes out after cooling, obtains product F, i.e. vulcanization iron nano-particle.
Resulting product is prepared into button-shaped sodium-ion battery, specific encapsulation step is as follows: by product direct slicing
It is assembled into sodium ion half-cell later, constant current charge-discharge test, test voltage are carried out to battery using new prestige electrochemical workstation
For 0.01V-3.0V, resulting materials are assembled into button cell and test its anode material of lithium-ion battery performance, as shown in Figure 2
It is the cycle performance figure of the battery, battery presents the capacity of 400mAh/g, 100 circle of circulation under the current density of 100mA/g
Still it can keep stable later.
Embodiment 3:
1) analytically pure ammonium ferric oxalate 2g, urea 14g are taken, obtains mixture after mixed grinding in glass mortar, it should
Mixture is denoted as A；
2) mixture A is heat-treated in low temperature tube furnace, is taken out after cooling, obtains product B, heat treatment heating rate is
20 DEG C/min, heat treatment temperature is 1200 DEG C, time 1h；
3) 3:1 in mass ratio mixes graphene oxide with cetyl trimethylammonium bromide CTAB, and deionized water is added
It is prepared into the solution of 3mg/ml, 3h is ultrasonically treated, is denoted as C；
4) product B is mixed with solution C, magnetic stirrer for 24 hours, filters after centrifugation, is freeze-dried, obtain product D；
5) product 1g sample D and 10g thiocarbamide are obtained into mixture in glass mortar after mixed grinding, which is denoted as
E；
6) mixture E being heat-treated under argon nitrogen atmosphere in low temperature tube furnace again, heat treatment heating rate is 10 DEG C/min,
Heat treatment temperature is 600 DEG C, soaking time 30min, takes out after cooling, obtains product F, i.e. vulcanization iron nano-particle.
Embodiment 4:
1) analytically pure ammonium ferric oxalate 2g, urea 10g are taken, obtains mixture after mixed grinding in glass mortar, it should
Mixture is denoted as A；
2) mixture A is heat-treated in low temperature tube furnace, is taken out after cooling, obtains product B, heat treatment heating rate is
15 DEG C/min, heat treatment temperature is 110 DEG C, time 1h；
3) 3:1 in mass ratio mixes graphene oxide with cetyl trimethylammonium bromide CTAB, and deionized water is added
It is prepared into the solution of 3mg/ml, 3h is ultrasonically treated, is denoted as C；
4) product B is mixed with solution C, magnetic stirrer for 24 hours, filters after centrifugation, is freeze-dried, obtain product D；
5) product 1g sample D and 8g trithiocyanuric acid are obtained into mixture in glass mortar after mixed grinding, the mixing
Object is denoted as E；
6) mixture E being heat-treated under argon nitrogen atmosphere in low temperature tube furnace again, heat treatment heating rate is 10 DEG C/min,
Heat treatment temperature is 600 DEG C, soaking time 30min, takes out after cooling, obtains product F, i.e. vulcanization iron nano-particle.
Finally it should be noted that: the above examples are only used to illustrate the technical scheme of the present invention rather than its limitations, to the greatest extent
Pipe is described the invention in detail referring to above-described embodiment, it should be understood by those ordinary skilled in the art that: still may be used
With modifications or equivalent substitutions are made to specific embodiments of the invention, and repaired without departing from any of spirit and scope of the invention
Change or equivalent replacement, should all cover in present claims range.
Claims (6)
1. a kind of graphene oxide doped FeS composite nano materials preparation method, it is characterised in that the following steps are included:
1) 1:(1~7 in mass ratio) analytically pure ammonium ferric oxalate, urea are taken, mixture A is obtained after mixed grinding；
2) mixture A is heat-treated in low temperature tube furnace, is warming up to 500~1200 DEG C with the heating rate of 2~20 DEG C/min
1h~5h is kept the temperature, is taken out after cooling, obtains product B；
3) 3:1 in mass ratio takes graphene oxide and CTAB, is added the solution C that deionized water is prepared into 1-3mg/ml, at ultrasound
Reason keeps graphene oxide fully dispersed；
4) product B is mixed with solution C, magnetic agitation is uniform, filters, is freeze-dried after centrifugation, obtains product D；
5) 1:(5~10 in mass ratio) take product D and sulphur source mixed grinding after obtain mixture E；
6) mixture E is heat-treated under argon nitrogen atmosphere in low temperature tube furnace, is heated up with the heating rate of 5~10 DEG C/min
To 300~600 DEG C of heat preservation 30min~1h, taken out after cooling to get graphene oxide doped FeS composite nano materials are arrived.
2. graphene oxide doped FeS composite nano materials preparation method as described in claim 1, it is characterised in that: described
Sulphur source is sublimed sulfur, thioacetamide, thiocarbamide or trithiocyanuric acid.
3. graphene oxide doped FeS composite nano materials preparation method as described in claim 1, it is characterised in that: described
Sonication treatment time is 3h in step 3).
4. graphene oxide doped FeS composite nano materials preparation method as described in claim 1, it is characterised in that: described
4) the magnetic agitation time is for 24 hours in.
5. a kind of graphene oxide doped FeS composite nano materials of any one of -4 method preparations according to claim 1.
6. a kind of graphene oxide doped FeS composite nano materials as claimed in claim 5, as sodium-ion battery cathode material
The application of material.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112310391A (en) * | 2020-10-30 | 2021-02-02 | 桑顿新能源科技有限公司 | Positive electrode material precursor, positive electrode material and preparation method thereof, lithium ion battery positive electrode, lithium ion battery and electric equipment |
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