CN111916694B - Preparation method of graphene iron-based composite material - Google Patents
Preparation method of graphene iron-based composite material Download PDFInfo
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- CN111916694B CN111916694B CN202010644625.7A CN202010644625A CN111916694B CN 111916694 B CN111916694 B CN 111916694B CN 202010644625 A CN202010644625 A CN 202010644625A CN 111916694 B CN111916694 B CN 111916694B
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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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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
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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
- 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
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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 preparation method of a graphene iron-based composite material, which comprises the following steps: (1) cutting stainless steel into metal plates, and pretreating with corundum gauze; (2) cutting a ceramic wafer into required samples, and roughening the surface of the ceramic wafer by using abrasive paper; (3) placing stainless steel in an induction heating machine, placing a ceramic wafer on a steel sheet, scattering graphite powder on one surface of the polished ceramic wafer, and placing another ceramic wafer on the polished ceramic wafer; (4) heating the sample; (5) heating, putting the mixture and potassium ferrate into a polyurethane ball ink tank for wet ball milling; (6) putting the mixed powder subjected to ball milling into a vacuum drying oven for drying; (7) and performing dry ball milling on the dried mixed powder again to obtain the required sample. According to the invention, an induction thermal decomposition mode is added, and graphite is converted into single-layer or thin-layer graphene oxide in advance; the wet ball milling is firstly carried out, and then the dry ball milling is carried out, so as to achieve the purpose of connection.
Description
Technical Field
The invention relates to a preparation method of a graphene iron-based composite material, and belongs to the technical field of iron-based composite materials.
Background
At present, graphene reinforced iron-based composite material is more and more valued by people, firstly: the graphene has good conductivity, namely a good electron transmission channel, and the stability of the iron-based/graphene nanocomposite material in the use process is ensured because the graphene has good heat conductivity; secondly, the method comprises the following steps: the graphene is single-layer graphite with only one carbon atom, the thickness is 0.335 nm, and the ultrathin graphene sheet can be used as a barrier to prevent the aggregation of nano particles and increase the cycle performance of the battery; thirdly, the method comprises the following steps: the graphene is an active material for storing lithium ions, so that the reversible specific capacity of the lithium ion battery is improved; fourthly: the iron-based nanoparticles are fixed on the surface of the curled graphene, so that the transmission distance of lithium ions on the iron-based nanoparticles is shortened, and the lithium ion battery has high rate performance. For the above reasons, graphene reinforced iron-based composites have been increasingly used in the field of batteries. However, the technology has an obvious defect that how to ensure the uniform attachment of iron ions on the surface of graphene and increase the dispersibility of the composite material.
The prior art and literature search show that: chinese patent CN106566942A discloses a preparation method of a graphene reinforced aluminum-based composite material, which comprises the steps of preparing graphene oxide, carrying out surface modification on aluminum powder to prepare flaky aluminum powder, and preparing graphene/aluminum hydroxide/aluminum multilayer coating structure powder; mixing graphene and aluminum powder, adding the mixture into an alcohol solution, and then carrying out ultrasonic treatment for 0.1-1 h at the temperature of 30-50 ℃ to prepare graphene/aluminum hydroxide/aluminum multilayer coating structure powder; and putting the prepared graphene/aluminum hydroxide/aluminum multilayer coating structure powder into a hot-pressing sintering mold, loading a pressure of 100-200MPa, and carrying out argon or nitrogen protection, and carrying out hot-pressing sintering to obtain the high-performance graphene reinforced aluminum-based composite material.
Chinese patent 105355873a discloses an iron-based metal organic framework compound, an iron-based metal organic framework compound/graphene composite material formed by the same and graphene, and application thereof as a negative active material in a lithium ion battery. The iron-based metal organic framework compound and the iron-based metal organic framework compound/graphene composite material are used as negative active materials for lithium ion batteries.
The technologies are respectively the preparation of the graphene reinforced aluminum-based composite material and the graphene reinforced iron-based composite material, the problem of dispersibility of graphene and a matrix powder material is considered, but the dispersion effect cannot be controlled, the agglomeration phenomenon of the graphene cannot be controlled, and meanwhile, the graphene is directly used as a reinforcement in the above patents, so that the cost is high.
Disclosure of Invention
The invention aims to obtain a graphene reinforced iron-based composite material with good connectivity, and provides a foundation for synthesis and preparation of the graphene reinforced iron-based composite material in batteries and other related fields.
The invention improves the connectivity of iron in the graphene oxide by means of induction thermal decomposition of graphite and ball milling, and provides a proper treatment method for relevant research and preparation processes based on the iron-based graphene composite material. The invention firstly ensures that the graphite can achieve good thermal decomposition effect in the induction heating process, so that the graphite can achieve high enough temperature after being conducted by the thin ceramic chip in the heating process; secondly, the connection between the graphene oxide and the iron-based material in the wet ball milling process is ensured, and the isotropy of the composite material is promoted; thirdly, the re-agglomeration phenomenon of the graphene in the drying process is reduced as much as possible, and a vacuum drying method is adopted as much as possible; fourthly, the re-agglomerated graphene oxide can be connected during dry ball milling.
The invention provides a preparation method of a graphene iron-based composite material with high connectivity, good bonding and simple operation, which comprises the following steps:
the first step is as follows: cutting 316L stainless steel into metal plates with the thickness of 15mm multiplied by 3mm, and pretreating the surface of 316L by using 600-1500-mesh corundum gauze for 1.5-2.5 h;
the second step is that: selecting a ceramic wafer with the thickness of 3-5mm, cutting and polishing the ceramic wafer into a sample with the thickness of 15 multiplied by 15mm, and preparing 2-5 parts of the ceramic wafer sample with the same specification;
the third step: polishing one surface of the two ceramic sheets for 1-3h by using 40-200 meshes of sand paper, and roughening the surface;
the fourth step: placing 316L stainless steel in an induction heating machine, placing one ceramic sheet on a 316L steel sheet with the non-polished surface facing downwards, adding 1.2-1.5g of graphite powder on the ceramic sheet, and placing the other ceramic sheet on the graphite powder with the non-polished surface facing upwards;
the fifth step: selecting the heating current of the induction heater as 260-290A, and the heating time is 80-100 s;
and a sixth step: placing the heated graphite and 7.5-8g of potassium ferrate into a polyurethane ball milling tank, selecting zirconium balls with the diameters of 3mm, 5mm and 7mm, adding 25-30ml of deionized water, selecting the rotation speed of 330 and 400r/min, and performing wet ball milling for 20-30 h;
the seventh step: placing the mixed powder after ball milling in a vacuum drying oven, wherein the drying temperature is 80-140 ℃, and the drying time is 12-15 h;
eighth step: and placing the dried mixed powder into a polyurethane ball milling tank again, and selecting dry ball milling, wherein the ball milling time is 350-400r/min, and the ball milling time is 40-48h, so as to finally obtain the required sample.
The purpose of induction heating of graphite before ball milling is to utilize high temperature to thermally decompose graphite, and the graphite is converted from a multi-layer graphite structure to single-layer or thin-layer graphene to obtain graphene oxide; the 316L stainless steel with the downward graphite is used for heating the stainless steel by using an induction heating machine, and heat is transferred to the graphite through ceramic sheets so as to achieve the aim of thermal decomposition; the aim of wet ball milling in the invention is that iron ions are better adsorbed on a graphene oxide sheet layer; the subsequent dry ball milling is to increase the connectivity by using the dry ball milling because a small amount of graphene agglomeration occurs in the drying process.
The invention has the beneficial effects that:
(1) compared with the common graphene reinforced iron-based composite material which achieves the dispersion purpose simply through a ball milling mode, the graphene reinforced iron-based composite material has the advantages that an induction thermal decomposition mode is added, and graphite is converted into single-layer or thin-layer graphene oxide in advance.
(2) Compared with the traditional graphene reinforced iron-based composite material, the graphene oxide composite material has the advantages that graphite is used as a raw material, and the graphene oxide is formed in a certain mode, so that certain resource cost is saved;
(3) the invention firstly carries out wet ball milling and then carries out dry ball milling, aims to achieve the purpose of separating and attaching, and then achieves the purpose of optimization through the dry ball milling, has more ideal effect compared with the common single ball milling mode, and finally achieves the purpose of connection;
(4) the invention achieves the purpose of connecting the graphene iron-based composite material by a ball milling method, and is simpler compared with a common chemical method.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail with reference to the embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. The technical solutions of the present invention are described in detail below with reference to examples, but the scope of protection is not limited thereto.
Example 1
Firstly, cutting 316L stainless steel into metal plates with the thickness of 15mm multiplied by 3mm, and pretreating the surface of 316L by using 600-1500-mesh corundum gauze for 1.5 h; selecting a ceramic wafer with the thickness of 5mm, cutting and polishing the ceramic wafer into a sample with the thickness of 15 multiplied by 15mm, and preparing 3 parts of the ceramic wafer sample with the same specification; then, using 40-200 meshes of sand paper to polish one surface of the two ceramic sheets for 3h, and roughening the surface; placing 316L stainless steel in an induction heating machine, placing one ceramic sheet on a 316L steel sheet with the non-polished surface facing downwards, adding 1.5g of graphite powder on the ceramic sheet, and placing the other ceramic sheet on the graphite powder with the non-polished surface facing upwards; selecting the heating current of an induction heater as 260A and the heating time as 90 s; putting the heated graphite and 7.6g of potassium ferrate into a polyurethane ball milling tank, selecting three zirconium balls with the diameters of 3mm, 5mm and 7mm, adding 25ml of deionized water, and selecting the rotation speed of 350r/min and the wet ball milling time of 20 h; placing the mixed powder after ball milling in a vacuum drying oven, wherein the drying temperature is 120 ℃, and the drying time is 13 h; and placing the dried mixed powder into a polyurethane ball milling tank again, and selecting a dry ball milling method, wherein the ball milling time is 350r/min and 45h, and finally obtaining the required sample.
Example 2
Firstly, cutting 316L stainless steel into metal plates with the thickness of 15mm multiplied by 3mm, and pretreating the surface of 316L by 600-sand 1500-mesh corundum gauze for 1.8 h; selecting a ceramic wafer with the thickness of 4mm, cutting and polishing the ceramic wafer into a sample with the thickness of 15 multiplied by 15mm, and preparing 5 parts of the ceramic wafer sample with the same specification; then, grinding one surface of the two ceramic sheets for 1h by using 40-200 meshes of sand paper, and roughening the surface; placing 316L stainless steel in an induction heating machine, placing one ceramic sheet on a 316L steel sheet with the non-polished surface facing downwards, adding 1.2g of graphite powder on the ceramic sheet, and placing the other ceramic sheet on the graphite powder with the non-polished surface facing upwards; selecting the heating current of an induction heater as 280A, and the heating time as 100 s; putting the heated graphite and 7.8g of potassium ferrate into a polyurethane ball milling tank, selecting three zirconium balls with the diameters of 3mm, 5mm and 7mm, adding 28ml of deionized water, and selecting the rotation speed of 390r/min and the wet ball milling time of 25 h; placing the mixed powder after ball milling in a vacuum drying oven, wherein the drying temperature is 130 ℃, and the drying time is 15 h; and placing the dried mixed powder into a polyurethane ball milling tank again, and selecting dry ball milling for 370r/min and 48h to obtain the required sample.
Example 3
Firstly, cutting 316L stainless steel into metal plates with the thickness of 15mm multiplied by 3mm, and pretreating the surface of 316L by using 600-1500-mesh corundum gauze for 2.2 h; selecting a ceramic wafer with the thickness of 3mm, cutting and polishing the ceramic wafer into a sample with the thickness of 15 multiplied by 15mm, and preparing 4 parts of the ceramic wafer sample with the same specification; then, using 40-200 meshes of sand paper to polish one surface of the two ceramic plates for 2h, and roughening the surface; placing 316L stainless steel in an induction heating machine, placing one ceramic sheet on a 316L steel sheet with the non-polished surface facing downwards, adding 1.3g of graphite powder on the ceramic sheet, and placing the other ceramic sheet on the graphite powder with the non-polished surface facing upwards; selecting a heating current of an induction heater as 285A, and heating time as 80 s; putting the heated graphite and 7.9g of potassium ferrate into a polyurethane ball milling tank, selecting three zirconium balls with the diameters of 3mm, 5mm and 7mm, adding 29ml of deionized water, and selecting the rotation speed of 340r/min and the wet ball milling time of 26 h; placing the mixed powder after ball milling in a vacuum drying oven, wherein the drying temperature is 100 ℃, and the drying time is 14 h; and placing the dried mixed powder into a polyurethane ball milling tank again, and selecting a dry ball milling method, wherein the ball milling time is 380r/min, and the ball milling time is 43h, so as to obtain the required sample.
Claims (5)
1. A preparation method of a graphene iron-based composite material is characterized by comprising the following steps:
the first step is as follows: cutting 316L stainless steel into metal plates with the thickness of 15mm multiplied by 3mm, and pretreating the surfaces of the metal plates for 1.5-2.5h by using corundum gauze;
the second step is that: selecting a ceramic wafer with the thickness of 3-5mm, cutting and polishing the ceramic wafer into a sample with the thickness of 15 x 15mm, and preparing 2-5 parts of the ceramic wafer sample with the same specification;
the third step: polishing one surface of the two ceramic sheets for 1-3h by using 40-200 meshes of sand paper, and roughening the surface;
the fourth step: putting 316L stainless steel into an induction heating machine, putting one ceramic wafer on a 316L stainless steel sheet, wherein the non-polished surface faces downwards, adding graphite powder into the ceramic wafer, and putting the other ceramic wafer on the graphite powder, wherein the non-polished surface faces upwards;
the fifth step: heating the sample by an induction heating machine; the heating current is 260-290A, and the heating time is 80-100 s;
and a sixth step: placing the heated graphite and potassium ferrate into a polyurethane ball milling tank, selecting zirconium balls with the diameters of 3mm, 5mm and 7mm, adding deionized water, selecting the rotation speed of 330 and 400r/min, and performing wet ball milling for 20-30 h;
the seventh step: putting the mixed powder subjected to ball milling into a vacuum drying oven for drying;
eighth step: and placing the dried mixed powder into a polyurethane ball milling tank again, and selecting dry ball milling, wherein the ball milling time is 350-400r/min, and the ball milling time is 40-48h, so as to finally obtain the required sample.
2. The method for preparing a graphene iron-based composite material according to claim 1, wherein: the corundum gauze is 600-1500 meshes.
3. The method for preparing a graphene iron-based composite material according to claim 1, wherein: in the fourth step, 1.2 to 1.5g of graphite powder was added to the ceramic chip.
4. The method for preparing a graphene iron-based composite material according to claim 1, wherein: the potassium ferrate added in the sixth step is 7.5-8g, and the dosage of the deionized water is 25-30 ml.
5. The method for preparing a graphene iron-based composite material according to claim 1, wherein: in the seventh step, the drying temperature is 80-140 ℃, and the drying time is 12-15 h.
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