CN108091838B - Method for preparing core-shell structure nano α -Fe2O3@ C composite material in one step - Google Patents

Method for preparing core-shell structure nano α -Fe2O3@ C composite material in one step Download PDF

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CN108091838B
CN108091838B CN201711192592.1A CN201711192592A CN108091838B CN 108091838 B CN108091838 B CN 108091838B CN 201711192592 A CN201711192592 A CN 201711192592A CN 108091838 B CN108091838 B CN 108091838B
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core
shell structure
absorbent cotton
composite material
salt solution
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CN108091838A (en
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彭年才
连崑
陈振秋
胡飞
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Xian Jiaotong University
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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
    • 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
    • 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
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • 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
    • 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
    • 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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
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Abstract

One-step preparation of core-shell structure nano α -Fe2O3The method of the @ C composite material comprises the steps of preparing an iron salt solution, filling medical absorbent cotton into a quartz crucible, pouring the iron salt solution into the quartz crucible, extruding the absorbent cotton by a glass rod to enable all the absorbent cotton to be fully soaked, placing the quartz crucible into a tube furnace, introducing nitrogen, heating to 280-plus-material temperature of 600 ℃, preserving heat for 1-3 hours, naturally cooling, removing residual cotton wool to obtain the core-shell structure nano α -Fe2O3The invention can quickly prepare the core-shell structure nano α -Fe with complete structure and good dispersion2O3The @ C composite material has the advantages of short period of the whole preparation process, simplicity and convenience in operation and easiness in realization of large-scale batch production.

Description

One-step preparation of core-shell structure nano α -Fe2O3Method for @ C composite material
Technical Field
The invention relates to the technical field of preparation of nano iron-carbon composite materials, in particular to a method for preparing nano α -Fe with a core-shell structure by one step2O3@ C composite material.
Background
The search for a new generation of high specific energy cathode material is always a hot spot of the research of the electrode material of the lithium ion battery, and the transition metal oxide such as MnO2、α-Fe2O3、Fe3O4The lithium ion battery cathode material has attracted wide attention because of providing reversible capacity of over 700mAh/g, and is a new generation of lithium ion battery electrode material with great potential, wherein α -Fe2O3As a lithium ion battery cathode material, the material has wide attention due to the advantages of theoretical specific capacity as high as 1007mAh/g, low price, environmental friendliness and the like, but the practical application of the material is limited by the defects of poor conductivity, low energy efficiency, easy capacity attenuation and the like2O3Complexing with carbon materialsSynthesis of α -Fe2O3The @ C composite material is used for enhancing the conductivity and structural stability of the material, reducing the polarization phenomenon, inhibiting the agglomeration of active material particles in the charge and discharge process and achieving the purpose of improving the electrochemical performance of the material.
By comparing the existing nano α -Fe2O3A literature search of the preparation technology of the @ C composite material shows that the formula \37477is published in the university of Wuhan proceedings 2016, volume 62, pages 4, 338 and 344 by the et al, and the two-morphology nanometer α -Fe is obtained2O3Preparation of @ C and adsorption Property thereof' the article mentions that α -Fe with two morphologies of litchi shape and diamond shape is prepared by utilizing stepwise hydrothermal and hydrogen peroxide oxidation assisted pH value regulation2O3@ C core-shell structured nanomaterial, however α -Fe prepared by the method2O3The @ C particle size is more than several microns, the preparation period is long, and the experimental operation is complex.
In addition, plum culture et al published in "New materials of chemical industry" 2015, volume 43, phase 9, pages 48 to 50 "solution combustion method for preparing nano Fe2O3The 'C super capacitor electrode material' refers to that under the air atmosphere, ferric nitrate, citric acid and ammonium nitrate are used as raw materials, and a solution combustion method is adopted to synthesize nano Fe in one step2O3The preparation method of the/C composite material basically realizes the advantages of simple preparation process, high yield and low cost, but the prepared Fe2O3The particle shape of the/C material is irregular, and the agglomeration is serious.
Therefore, how to prepare the core-shell structure nano α -Fe with complete structure, good dispersion, particle size below micron, short reaction period and simple operation2O3The @ C composite material becomes a key technical difficulty to be broken through at present.
Disclosure of Invention
In order to overcome the disadvantages of the prior art, the invention aims to provide a one-step preparation method of the core-shell structure nanometer α -Fe2O3The method of the @ C composite material can quickly prepare the core-shell structure nano α -Fe with complete structure and good dispersion2O3@ C composite material, andthe whole reaction period is short, the operation is simple and convenient, and the large-scale batch production is easy to realize.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
one-step preparation of core-shell structure nano α -Fe2O3A method of @ C composite, comprising the steps of:
1) weighing FeCl3·6H2Adding water into a beaker, stirring until the water is completely dissolved, and preparing into 0.05-0.2 g/mL of iron salt solution;
2) filling medical absorbent cotton in a quartz crucible, pouring the ferric salt solution prepared in the step 1) into the quartz crucible, and extruding the absorbent cotton by using a glass rod to fully soak all the absorbent cotton;
3) putting the quartz crucible into a tube furnace, introducing nitrogen, heating to 280 plus materials at the speed of 5 ℃/min, preserving the heat for 1-3h, naturally cooling, removing residual cotton wool to obtain the core-shell structure nanometer α -Fe2O3@ C composite material.
The core-shell structure is nanometer α -Fe2O3The @ C composite material has a complete core-shell structure, the average particle size of the composite material is 80-200 nanometers, and the thickness of a coated carbon layer is 3-5 nanometers.
The method has the beneficial effects that the absorbent cotton is adopted to adsorb FeCl3·6H2O, and micropores on the absorbent cotton provide small chambers for subsequent reactions. FeCl adsorbed in micropores of absorbent cotton under high-temperature and oxygen-free environment3·6H2Reacting with O water solution to generate Fe (OH) when iron ions and hydroxide ions in the solution3Then, α -Fe is generated due to further water loss caused by high temperature2O3Grains filled in the micropores of the absorbent cotton and finally forming dispersed α -Fe completely coated by the carbon layer along with the decomposition of the absorbent cotton at high temperature2O3@ C particles.
Compared with the prior art, the method can quickly prepare the nanometer α -Fe with the core-shell structure by only using absorbent cotton to adsorb iron salt solution and keeping the temperature of 280-600 ℃ for 1-3h under the anaerobic condition2O3The micropores on the absorbent cotton provide small chambers for the reaction so that the final product has a complete structure, and the carbon coating layer is α -Fe2O3The complete coating of the grains allows good dispersion of the final product without agglomeration between the particles. The whole preparation process has short period, only needs 3 hours at most, is simple and convenient to operate, can be heated and insulated by a tubular furnace and other equipment, and is easy to realize large-scale batch production.
Drawings
FIG. 1(a) shows the core-shell structure of nanometer α -Fe prepared according to the first embodiment of the present invention2O3TEM image (50nm) of @ C composite material, FIG. 1(b) is nano α -Fe with core-shell structure prepared in the first embodiment of the invention2O3TEM image of @ C composite (10 nm).
FIG. 2 shows the core-shell structure of nanometer α -Fe prepared according to the first embodiment of the present invention2O3@ C composite XRD pattern.
Detailed Description
The present invention will be described in detail below with reference to examples and the accompanying drawings.
EXAMPLE one step preparation of core-shell structured Nano α -Fe2O3A method of @ C composite, comprising the steps of:
1) weighing 3g FeCl3·6H2Adding 30mL of water into a beaker, stirring until the water is completely dissolved, and preparing into 0.1g/mL of iron salt solution;
2) weighing 5g of medical absorbent cotton, filling the medical absorbent cotton into a quartz crucible, pouring the ferric salt solution prepared in the step 1) into the quartz crucible, and extruding the absorbent cotton by using a glass rod to fully soak all the absorbent cotton;
3) putting the quartz crucible into a tube furnace, introducing nitrogen, heating to 350 deg.C at a speed of 5 deg.C/min, keeping the temperature for 2 hr, naturally cooling to room temperature, closing nitrogen, removing residual cotton wool to obtain powder product, i.e. core-shell structure nanometer α -Fe2O3@ C composite material.
Referring to FIG. 1, FIG. 1(a) shows the core-shell structure of nanometer α -Fe prepared in the first example2O3@ C composite TEM image (50 nm);FIG. 1(b) is the core-shell structure nano α -Fe prepared in the first example2O3TEM image (10nm) of @ C composite As can be seen from FIG. 1(a), the prepared core-shell structured nano α -Fe2O3The @ C composite material is different from 80nm to 200nm, and as can be seen from figure 1(b), the prepared core-shell structure nano α -Fe2O3The @ C composite material has a C coating layer with a thickness of 3-5nm, and the coating layer is α -Fe2O3A perfect coating is formed.
Referring to FIG. 2, FIG. 2 shows the core-shell structure nano α -Fe prepared in the first example2O3The XRD pattern of the @ C composite material is shown in the corresponding condition of diffraction peaks in the pattern and standard PDF card 33-0664, and the prepared material is α -Fe2O3。
EXAMPLE two, one-step preparation of core-shell structured Nano α -Fe2O3A method of @ C composite, comprising the steps of:
1) 1.5g FeCl was weighed3·6H2Adding 30mL of water into a beaker, stirring until the water is completely dissolved, and preparing into 0.05g/mL of iron salt solution;
2) weighing 5g of medical absorbent cotton, filling the medical absorbent cotton into a quartz crucible, pouring the ferric salt solution prepared in the step 1 into the quartz crucible, and extruding the absorbent cotton by using a glass rod to fully soak all the absorbent cotton;
3) putting the quartz crucible into a tube furnace, introducing nitrogen, heating to 280 ℃ at the speed of 5 ℃/min, preserving heat for 1h, naturally cooling the furnace to room temperature, closing the nitrogen, removing residual cotton wool to obtain a powdery product, namely the core-shell structure nano α -Fe2O3@ C composite material.
EXAMPLE III one-step preparation of core-shell structured Nano α -Fe2O3A method of @ C composite, comprising the steps of:
1) 6g FeCl was weighed3·6H2Adding 30mL of water into a beaker, stirring until the water is completely dissolved, and preparing into 0.2g/mL of iron salt solution;
2) weighing 5g of medical absorbent cotton, filling the medical absorbent cotton into a quartz crucible, pouring the ferric salt solution prepared in the step 1) into the quartz crucible, and extruding the absorbent cotton by using a glass rod to fully soak all the absorbent cotton;
3) putting the quartz crucible into a tube furnace, introducing nitrogen, heating to 600 deg.C at a speed of 5 deg.C/min, keeping the temperature for 3 hr, naturally cooling to room temperature, closing nitrogen, removing residual cotton wool to obtain powder product, i.e. core-shell structure nanometer α -Fe2O3@ C composite material.

Claims (5)

1. One-step preparation of core-shell structure nano α -Fe2O3A method of a @ C composite, characterised by the steps of:
1) weighing FeCl3·6H2Adding water into a beaker, stirring until the water is completely dissolved, and preparing into 0.05-0.2 g/mL of iron salt solution;
2) filling medical absorbent cotton in a quartz crucible, pouring the ferric salt solution prepared in the step 1) into the quartz crucible, and extruding the absorbent cotton by using a glass rod to fully soak all the absorbent cotton;
3) putting the quartz crucible into a tube furnace, introducing nitrogen, heating to 280 plus materials at the speed of 5 ℃/min, preserving the heat for 1-3h, naturally cooling, removing residual cotton wool to obtain the core-shell structure nanometer α -Fe2O3@ C composite material.
2. The one-step preparation of the core-shell structure nano α -Fe according to claim 12O3The method of the @ C composite material is characterized in that the core-shell structure nanometer α -Fe2O3The @ C composite material has a complete core-shell structure, the average particle size of the composite material is 80-200 nanometers, and the thickness of a coated carbon layer is 3-5 nanometers.
3. The one-step preparation of the core-shell structure nano α -Fe according to claim 12O3A method of a @ C composite, characterised by the steps of:
1) weighing 3g FeCl3·6H2Adding 30mL of water into a beaker to prepare 0.1g/mL of iron salt solution;
2) weighing 5g of medical absorbent cotton;
3) heating to 350 deg.C at a speed of 5 deg.C/min, and maintaining for 2 hr.
4. The one-step preparation of the core-shell structure nano α -Fe according to claim 12O3A method of a @ C composite, characterised by the steps of:
1) 1.5g FeCl was weighed3·6H2Adding 30mL of water into a beaker to prepare 0.05g/mL of iron salt solution;
2) weighing 5g of medical absorbent cotton;
3) heating to 280 ℃ at the speed of 5 ℃/min, and preserving heat for 1 h.
5. The one-step preparation of the core-shell structure nano α -Fe according to claim 12O3A method of a @ C composite, characterised by the steps of:
1) 6g FeCl was weighed3·6H2Adding 30mL of water into a beaker to prepare 0.2g/mL of iron salt solution;
2) weighing 5g of medical absorbent cotton;
3) heating to 600 deg.C at a speed of 5 deg.C/min, and maintaining for 3 hr.
CN201711192592.1A 2017-11-24 2017-11-24 Method for preparing core-shell structure nano α -Fe2O3@ C composite material in one step Active CN108091838B (en)

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CN109507242B (en) * 2018-10-26 2021-07-20 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of porous structure C @ ferric oxide composite nano material, product and application thereof
CN110649237B (en) * 2019-09-27 2021-05-14 厦门理工学院 Iron oxide @ carbon nanocomposite and preparation method and application thereof

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CN106848277A (en) * 2017-01-22 2017-06-13 曲阜师范大学 A kind of magnesium iron oxygen/carbon composite and preparation method thereof
CN107275640A (en) * 2017-07-03 2017-10-20 中国科学院过程工程研究所 One step prepares the double-doped cotton base porous carbon of sulphur nitrogen
CN107331832A (en) * 2017-05-10 2017-11-07 苏州冠洁纳米抗菌涂料科技有限公司 A kind of preparation method of composite

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Publication number Priority date Publication date Assignee Title
WO2007095454A2 (en) * 2006-02-10 2007-08-23 Board Of Supervisors Of Louisiana State University And Agricultural And Mechanical College Carbon-encased metal nanoparticles and sponges, methods of synthesis, and methods of use
CN102208614A (en) * 2011-04-26 2011-10-05 中国矿业大学 Method for preparing lithium ion battery cathode material coated iron sesquioxide
CN104157832A (en) * 2014-09-04 2014-11-19 湖北工程学院 Preparation method for electrode material of ferroferric oxide/carbon composite lithium ion battery
CN106848277A (en) * 2017-01-22 2017-06-13 曲阜师范大学 A kind of magnesium iron oxygen/carbon composite and preparation method thereof
CN107331832A (en) * 2017-05-10 2017-11-07 苏州冠洁纳米抗菌涂料科技有限公司 A kind of preparation method of composite
CN107275640A (en) * 2017-07-03 2017-10-20 中国科学院过程工程研究所 One step prepares the double-doped cotton base porous carbon of sulphur nitrogen

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