CN114628669B - Carbon carrier nitrogen doped Fe 2 O 3 @ NC, preparation and application thereof - Google Patents

Carbon carrier nitrogen doped Fe 2 O 3 @ NC, preparation and application thereof Download PDF

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CN114628669B
CN114628669B CN202011455760.3A CN202011455760A CN114628669B CN 114628669 B CN114628669 B CN 114628669B CN 202011455760 A CN202011455760 A CN 202011455760A CN 114628669 B CN114628669 B CN 114628669B
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nitrogen
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CN114628669A (en
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李先锋
王灿沛
郑琼
张华民
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Dalian Institute of Chemical Physics of CAS
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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
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
    • 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
    • H—ELECTRICITY
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    • 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
    • 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
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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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
    • 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
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    • Y02E60/10—Energy storage using batteries

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Abstract

The invention discloses a carbon carrier nitrogen doped Fe 2 O 3 An NC particle, a preparation method and application thereof, belonging to the technical field of alkali metal batteries. Firstly, taking a surfactant as a template and a carbon source, ethanol and water as solvents, taking dopamine hydrochloride (DA) as a nitrogen source and a carbon source of a precursor, sequentially adding an iron source and an organic ligand, and performing self-polymerization to form Fe 2 O 3 Precursor of NC complex; then heating the synthesized precursor to 600-800 ℃ in Ar atmosphere, calcining for a period of time, cooling to room temperature, and then placing in air for a period of time to obtain Fe 2 O 3 @ NC. The carbon carrier nitrogen doped Fe prepared by the invention 2 O 3 The @ NC particles are capable of inhibiting Fe 2 O 3 The growth of the nano particles shortens the transmission path of ions, improves the reaction rate, shows higher electrochemical activity, and has better multiplying power performance and high multiplying power cycle stability.

Description

Carbon carrier nitrogen doped Fe 2 O 3 @ NC, preparation and application thereof
Technical Field
The invention belongs to the technical field of alkali metal batteries, and in particular relates to a carbon carrier nitrogen-doped Fe synthesized by a natural oxidation method 2 O 3 NC, and preparation and use thereof.
Background
Recently sodium ion batteries have attracted extensive attention from various schools as potential alternatives to lithium ion batteries in large-scale energy storage systems, mainly due to the abundant resources and low cost characteristics of sodium. Sodium (Na) and lithium (Li) in the periodic Table of elements belong to the same main group and exhibit a similar physicochemical property to lithiumThis is of nature, which is advantageous for the development of sodium ion battery technology. However, since the radius of sodium ions (about 0.102 nm) is larger than the radius of lithium ions (about 0.076 nm), the electrode material of most lithium ion batteries is difficult to carry sodium ions. Thus, the development of sodium ion batteries has left to explore suitable host materials to accommodate larger Na + . Over the past few years, a large number of positive and negative electrode materials have been investigated for sodium ion batteries and have made great progress, such as Prussian blue-based materials, sodium layered oxides and phosphate materials. However, because of the small interlayer distance (0.34 nm) between the graphite layers, which is detrimental to intercalation of sodium ions in commercial graphite anodes, development of high performance anode materials is currently a major challenge in sodium ion battery research.
Transition metal oxides have received great attention due to their high theoretical capacity, abundant resources and environmental friendliness. Wherein Fe is 2 O 3 Because of its high theoretical capacity (1007 mA h g) -1 ) Is abundant in resources, low in cost and environmentally friendly and is considered as a relatively promising candidate negative electrode material in sodium ion batteries. However, fe 2 O 3 Is severely hampered by the low inherent conductivity and large volume change during sodium ion intercalation/extraction. In addition, because of the larger radius of sodium ions, fe 2 O 3 The volume change of the material serving as the negative electrode of the sodium ion battery is larger than that of the lithium ion battery. The vast volume changes can lead to pulverization of the active material particles, loss of electrical contact between the active material and the electrode frame, and continued growth of very thick Solid Electrolyte Interface (SEI) films, all of which can lead to rapid decay of capacity during cycling.
In order to solve the above problems, although the prior art has adopted a method including manufacturing Fe having different nanostructures 2 O 3 Or Fe (Fe) 2 O 3 The nanoparticles are dispersed into different carbon matrices, such as carbon nanotubes, carbon nanofibers and graphene. However, most reported Fe for sodium ion batteries 2 O 3 Is based on Fe 2 O 3 Constructed by combining Fe 2 O 3 Nanoparticle anchoring dispersion in nitrogenThe related research on the use of the doped three-dimensional carbon skeleton for developing high-performance anode materials has not been reported yet.
Disclosure of Invention
In view of the above, the object of the present invention is to provide a carbon-supported nitrogen-doped Fe 2 O 3 Preparation method and application of @ NC.
The invention is realized by the following modes:
fe is synthesized by in situ carbonization of the polymer followed by natural oxidation in air 2 O 3 Nanoparticle anchoring of Fe dispersed in nitrogen-doped three-dimensional carbon skeleton 2 O 3 Complex (Fe) 2 O 3 @NC)。
Firstly, taking a surfactant as a template and a carbon source, ethanol and water as solvents, taking dopamine hydrochloride (DA) as a nitrogen source and a carbon source of a precursor, sequentially adding an iron source and an organic ligand, and performing self-polymerization to form Fe 2 O 3 Precursor of NC complex; then heating the synthesized precursor to 600-800 ℃ in Ar atmosphere, calcining for a period of time, cooling to room temperature, and then placing in air for a period of time to obtain Fe 2 O 3 @NC。
Further, the surfactant is an addition polymer of polypropylene glycol and ethylene oxide (F127), polyvinylpyrrolidone (PVP) or hexadecylsulfonic acid.
Further, the concentration of the surfactant is 5 to 15 (mg/ml).
Further, the concentration of dopamine hydrochloride is 0-15 (mg/ml).
Further, the iron source is Fe (NO 3 ) 3 ·9H 2 O、Fe(NO 3 ) 3 、FeCl 3 、Fe 2 (SO 4 ) 3 、FeSO 4 ，Fe(NO 3 ) 2 、FeCl 2 One or more than two of them.
Further, the organic ligand is one or more than two of 1,3, 5-benzene tricarboxylic acid, terephthalic acid and dimethyl imidazole.
Further, the organic ligand is 1,3, 5-benzene tricarboxylic acid, and Fe (NO) 3 ) 3 ·9H 2 O is preferably in a molar ratio of2：1～1:2。
Further, the heating rate is 0.1-3 ℃ for min -1 。
Further, the calcination temperature is 600 to 800 ℃.
Further, the calcination time is 2 to 6 hours.
Another object of the present invention is to provide nitrogen-doped Fe of the carbon support prepared by the above method 2 O 3 Use of @ NC in an alkali metal ion battery.
Further, the carbon support nitrogen doped Fe 2 O 3 NC as an alkali metal ion battery anode active material.
Further, the alkali metal ion battery is a sodium ion battery, a lithium ion battery, and a potassium ion battery.
Compared with the prior art, the invention has the following beneficial effects:
1. most of Fe existing at present 2 O 3 The size of the composite material is relatively large, while the Fe of the invention 2 O 3 Nanoparticles anchored and dispersed on a carbon substrate of several hundred nanometers, capable of suppressing Fe 2 O 3 The growth of the nano particles shortens the transmission path of ions, improves the reaction rate and shows higher electrochemical activity.
2. The hard carbon material with the widest application in the sodium ion battery has low specific capacity, low multiplying power and poor cycle performance, and the carbon carrier nitrogen doped Fe 2 O 3 The multiplying power performance and the cycle stability of the @ NC composite material are obviously improved.
3. The method of the invention obtains the Fe/C compound by stirring and calcining at normal temperature, and then obtains Fe by natural oxidation in air 2 O 3 The @ NC compound has simple process and easy operation, and can realize large-scale production.
Drawings
In order to more clearly illustrate the embodiments of the present invention, the drawings to which the embodiments relate will be briefly described.
Fig. 1: example 1 and example 4 synthetic Fe 2 O 3 X of @ NCRD diagram.
Fig. 2: EXAMPLE 1 Fe synthesized 2 O 3 Scanning electron microscope image of @ NC.
Fig. 3: example 1 and example 4 synthetic Fe 2 O 3 Magnification performance plot @ NC.
Fig. 4: EXAMPLE 1 Fe synthesized 2 O 3 NC at 5 A.g -1 Cycling diagram at current density.
Detailed Description
The following detailed description of the invention is provided in connection with examples, but the implementation of the invention is not limited thereto, and it is obvious that the examples described below are only some examples of the invention, and that it is within the scope of protection of the invention to those skilled in the art to obtain other similar examples without inventive faculty.
Example 1
1) Synthesis of polymer particles:
1.0g of an addition polymer of polypropylene glycol and ethylene oxide (F127) and 1.0g of DA (dopamine hydrochloride) were dissolved in 100mL of 50% strength by volume ethanol water and stirred at room temperature to obtain a clear solution. 5.8083g of Fe (NO) 3 ) 3 ·9H 2 O and 3.0212g of 1,3, 5-benzene tricarboxylic acid are added to the above mixture in sequence, and after continuously stirring and reacting for 30 minutes, the mixture is centrifuged to obtain a separated product, and then washed 3 times with ethanol water with a volume concentration of 50% and dried, thus obtaining a polymer.
2.Fe 2 O 3 Synthesis of NC composite material (Fe 2 O 3 @NC)：
The synthesized polymer was subjected to Ar atmosphere at 1℃for min -1 Heating to 600 ℃ and calcining for 3 hours, cooling to room temperature, taking out, placing in air for 30 minutes, and obtaining Fe 2 O 3 @NC。
Through detection, the mass content of N in the polymer carrier NC is 1.06%, and the particle size of the carrier NC is 100-300nm;
active ingredient Fe 2 O 3 Is distributed on the inner and outer surfaces of the porous carrier NC, and is a particle with the particle diameter of 10-30 nm.
3.Fe 2 O 3 Performance test of @ NC composite:
fe prepared by the method 2 O 3 NC is an electrode active material, super P is a conductive agent, and polyvinylidene fluoride (PVDF) is a binder-formulated slurry, the composition ratio of which is 8:1:1. Copper foil is used as a current collector, the thickness of the copper foil is 80 microns, an electrode is coated by scraping, and the copper foil is dried at 60 ℃. At this time, the electrode loading was about 1mg cm -2 . Sodium sheet with diameter of 1.6mm is used as counter electrode, glass fiber membrane is used as diaphragm, 1M NaPF is used 6 DGME is used as electrolyte to assemble sodium |Fe 2 O 3 @ NC half cell. At 0.1A g -1 (Fe 2 O 3 @NC)，0.2A g -1 ，0.5A g -1 ，1A g -1 ，2A g -1 ，5A g -1 ，10A g -1 20A g -1 The charge and discharge test of the multiplying power performance is carried out under the condition of 5A g -1 The cyclic test of large current is performed at the current density of (3).
Examples 2 to 15:
fe with nitrogen doping of the same carbon Carrier as example 1 2 O 3 The preparation process of the @ NC composite material and the assembly thereof into a battery process and a performance test process are different from each other in that the concentration of F127, the concentration of dopamine hydrochloride, the kind of metal salt, the temperature rise rate, the calcination temperature, and the calcination time, the related data are shown in table 1, and the performance test data of the prepared sodium ion battery are shown in table 3.
Comparative examples 1 to 5:
fe with nitrogen doping of the same carbon Carrier as example 1 2 O 3 The preparation process of NC composite material and the assembly thereof into a battery process and a performance test process, except for the kind of organic ligand, the temperature rising rate and the order of materials, the related data are shown in table 2, and the performance test data of the prepared sodium ion battery are shown in table 3.
Table 1 preparation process parameters of examples 1-18
Table 2 process parameters of comparative examples 1-5
TABLE 3 results of Performance test of examples 1-15 and comparative examples 1-5
When Fe is synthesized from different amounts of dopamine hydrochloride (DA) 2 O 3 When @ NC was subjected to electrochemical testing, fe was synthesized in example 1 2 O 3 NC shows the best electrochemical activity. The prepared composite material is 20 A.g -1 Has a current density of 122.3 mAh.g -1 Specific capacity of 5 A.g -1 After 5000 cycles of current density, 63.1 mAh.g -1 Has better multiplying power performance and high-current long-cycle stability.
The characteristic that both ends of F127 are respectively provided with a hydrophilic group and a hydrophobic group, and the middle is long-chain is utilized, the hydrophilic group shows electronegativity, and is combined with ferric iron, so that ferric iron ions form micelle-like particles under the stirring condition; the micelle-like structure of the hydrophobic groups at the long chain and the other end can prevent the combination with other micelles, so that the agglomeration is avoided, and the dispersity is higher. The dopamine hydrochloride is mainly used as a nitrogen source, and can be self-polymerized to form polydopamine and have certain viscosity, so that certain nitrogen element can be doped; at the same time, we have found that when varying the amount of dopamine hydrochloride, fe 2 O 3 The ratio of (c) is very small and therefore does not take part in the polymerization process of the entire reaction, mainly as nitrogen source.
Fe(NO 3 ) 3 ·9H 2 O is used as an iron source, and is firstly subjected to electrostatic interaction with F127 to form micelle-like particles, and then is subjected to coordination polymerization with 1,3, 5-benzene tricarboxylic acid. On the one hand, 1,3, 5-benzene tricarboxylic acid can promote micelle through the action of Van der Waals force and the hydrophobic end of the surfactantIs assembled by the assembly of (a); on the other hand, the particles can enter the inside of the micelle to carry out coordination and recombination with metal ions, so that the size of the particles is effectively controlled.
From the experimental results, it can be seen that the change of the amount of dopamine hydrochloride can affect Fe 2 O 3 To influence Fe 2 O 3 The concentration of the preferred dopamine hydrochloride in the invention is 0-15 (mg/ml) in the whole compound; the preferable surfactant in the invention is F127, polyvinylpyrrolidone or hexadecyl sodium sulfonate, and the preferable concentration is 5-15 (mg/ml); the iron source in the invention is Fe (NO) 3 ) 3 ·9H 2 O、Fe(NO 3 ) 3 、FeCl 3 、Fe 2 (SO 4 ) 3 、FeSO 4 ，Fe(NO 3 ) 2 、FeCl 2 One or more than two of them.
The preferred ligand in the present invention is 1,3, 5-benzene tricarboxylic acid. And one or more selected from terephthalic acid and dimethyl imidazole. From the experimental results, it can be seen that Fe in the final composite 2 O 3 The proportion of (2) is mainly dependent on the molar amount of ferric ions.
When 1,3, 5-benzene tricarboxylic acid is changed into terephthalic acid, the organic framework formed by the terephthalic acid and iron ions is enlarged due to the symmetrical structure of the terephthalic acid, and the formed Fe is further formed 2 O 3 The particles become larger and thus the performance will be somewhat worse.
Because the formed colloidal particles are obtained by weak bond force combination, the structure of the colloidal particles can be damaged when the temperature rising rate is too high, the agglomeration of the elemental iron is caused, and Fe is further caused 2 O 3 The particles of (a) become larger and the properties become worse, and the heating rate is preferably 0.1-3 ℃ for min -1 。
Due to the influence of the carbonization temperature of the surfactant, the organic ligand and the dopamine hydrochloride in the colloidal particles, the carbonization temperature needs to be more than 600 ℃, when the calcination temperature is too high (such as 1200 ℃), the graphitization degree of the calcined carbon and the number of oxygen-containing groups on the surface of the calcined carbon can be influenced, and Fe and C compounds can be generated, so that the natural oxidation can be influencedAnd Fe of (2) 2 O 3 The specific gravity of the composite, and thus the overall properties of the material, will also be affected, with a calcination temperature of 600 to 800 c being preferred in the present invention.
When the calcination time is too long (such as 12 h), the agglomeration of the elemental iron particles can be caused, thereby affecting the natural oxidation effect and Fe 2 O 3 The specific gravity of the composite is reduced, so that the overall performance is deteriorated, and the calcination time is preferably 2 to 6 hours in the present invention.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.

Claims (9)

1. Carbon carrier nitrogen doped Fe 2 O 3 The preparation method of the @ NC is characterized by comprising the following steps:
(1) Taking a surfactant as a template and a carbon source, taking alcohol and water as solvents, taking dopamine hydrochloride as a nitrogen source and a carbon source of a precursor, sequentially adding an iron source and an organic ligand, and performing self-polymerization to form Fe 2 O 3 Precursor of NC complex;
(2) Heating the precursor synthesized in the step (1) to 600-800 ℃ in inert gas atmosphere, calcining 2-6 h, cooling to room temperature, and standing in air for a period of time to obtain Fe 2 O 3 @NC；
The surfactant in the step (1) is addition polymer of polypropylene glycol and ethylene oxide, polyvinylpyrrolidone or sodium hexadecyl sulfonate; the concentration of the surfactant is 5-15 mg/ml; the concentration of the dopamine hydrochloride is 0-15 mg/ml.
2. The method according to claim 1, wherein the alcohol in the step (1) is ethanol, and the volume ratio of ethanol to water is 1 (0.5-2).
3. The method of claim 1, wherein the iron source in step (1) is Fe (NO 3 ) 3 ·9H 2 O、Fe(NO 3 ) 3 、FeCl 3 、 Fe 2 (SO 4 ) 3 、FeSO 4 ，Fe(NO 3 ) 2 、FeCl 2 One or more than two of them.
4. The method according to claim 3, wherein the organic ligand in the step (1) is one or more of 1,3, 5-benzene tricarboxylic acid, terephthalic acid and dimethyl imidazole; the molar ratio of the organic ligand to Fe in the iron source is 2:1-1:2.
5. The process according to any one of claims 1 to 4, wherein the heating rate in step (2) is 0.1 to 3℃for a minute -1 The method comprises the steps of carrying out a first treatment on the surface of the The inert gas is Ar.
6. The method according to claim 5, wherein the standing time in the air in the step (2) is 20 to 40 minutes.
7. Carbon carrier nitrogen doped Fe 2 O 3 NC particle, characterized in that it is obtainable by the preparation process according to any one of claims 1 to 6.
8. The carbon-supported nitrogen-doped Fe of claim 7 2 O 3 Use of @ NC particles in alkali metal ion batteries.
9. The use according to claim 8, characterized in that the carbon support is nitrogen doped Fe 2 O 3 The @ NC particles are used as an alkali metal ion battery anode active material; the alkali metal ion battery is sodium ion battery, lithium ion battery or potassium ion batteryA sub-battery.
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CN107369825A (en) * 2017-07-26 2017-11-21 华南理工大学 A kind of nitrogen-doped carbon coated manganese oxide composite cathode material for lithium ion cell and preparation method and application
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CN110993904A (en) * 2019-11-14 2020-04-10 江苏大学 Preparation method of nitrogen-doped antimony-carbon composite material and application of nitrogen-doped antimony-carbon composite material to sodium ion battery electrode
KR20200042293A (en) * 2018-10-15 2020-04-23 한국과학기술연구원 Cathode active material for a sodium ion battery coated by N-doped carbon formed from polydopamine precursor and preperation methods thereof
AU2020101299A4 (en) * 2020-06-08 2020-08-20 Qilu University Of Technology Vanadium tetrasulfide-nitrogen-doped carbon tube composite and preparation method and use thereof

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Publication number Priority date Publication date Assignee Title
CN104617281A (en) * 2015-02-12 2015-05-13 中南大学 Method for preparing sodium-ion battery antimony/nitrogen-doped carbon nanosheet negative electrode composite material
CN107369825A (en) * 2017-07-26 2017-11-21 华南理工大学 A kind of nitrogen-doped carbon coated manganese oxide composite cathode material for lithium ion cell and preparation method and application
CN109449379A (en) * 2018-09-12 2019-03-08 华南师范大学 A kind of SnFe that nitrogen-doped carbon is compound2O4Lithium ion battery negative material and the preparation method and application thereof
KR20200042293A (en) * 2018-10-15 2020-04-23 한국과학기술연구원 Cathode active material for a sodium ion battery coated by N-doped carbon formed from polydopamine precursor and preperation methods thereof
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