CN104465077A - Electrode material and manufacturing method thereof - Google Patents
Electrode material and manufacturing method thereof Download PDFInfo
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- CN104465077A CN104465077A CN201410768447.3A CN201410768447A CN104465077A CN 104465077 A CN104465077 A CN 104465077A CN 201410768447 A CN201410768447 A CN 201410768447A CN 104465077 A CN104465077 A CN 104465077A
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Abstract
The invention discloses an electrode material and a manufacturing method of the electrode material. The electrode material comprises a base layer, a tungsten trioxide thin film on the outer layer and a middle-layer material located between the base layer and the outer layer. The middle-layer material is composed of, by weight, 20-30 parts of graphite, 4-5 parts of Al2O3, 2-2.5 parts of Pb3O4, 1-1.2 parts of TiO2, 2-3 parts of PVA, 0.8-1.2 parts of CeO2, 0.6-1 part of Bi2O3 and 0.05-0.5 part of La2O3. The invention further provides the manufacturing method of the electrode material. The manufacturing method includes the steps that firstly, heating is conducted for five minutes in hydrogen at the temperature of 1200-1300 DEG C, a surface oxide layer of the base layer is removed, the surface of the base layer is coated with the middle-layer material, heating is conducted for 1-3 hours at the temperature of 700-800 DEG C, and a sample is fast cooled to the room temperature; secondly, Na2WO4.2H2O is dissolved in an oxalic acid solution, and the sample in the first step is immersed into the solution and heated to react for 12 hours at the temperature of 180-200 DEG C; thirdly, the sample obtained through the reaction in the second step is cleaned with water and dried, and the electrode material is obtained.
Description
Technical field
The present invention relates to a kind of electrode material field, particularly a kind of electrode material and preparation method thereof.
Background technology
The problem that the ubiquity in production and selling of electrode material in the market maximum discharge and recharge number of times is few, charging rate is slow and current density is little.
Material with carbon element is a kind of general energy storage material, and graphite is a kind of allotrope of elemental carbon, and the periphery of each carbon atom links other three carbon atoms of work with covalent bonds, forms covalent molecule.Graphite is wherein the softest a kind of mineral, also can be used for manufacturing pencil-lead and lubricant.
Composite material is a potential ideal material, because Graphene has outstanding electric property, and uncommon mechanical strength, high chemical stability, and graphite cost is low, can gather in a large number, and that based on Graphene, prepares ultracapacitor also has a lot.
Three-dimensional grapheme material, has three-dimensional hollow porous network structure, and have high heat conduction, high temperature resistant, corrosion-resistant, high ductibility, pliability are good, single-layer and transparent degree is good.Three-dimensional grapheme material, have the feature of the Graphene being different from two dimension, and the grapheme material of its surface area ratio two dimension is high in stuctures and properties.From the graphite dry cell till now to the research of three-dimensional grapheme, material with carbon element is the energy and material that people pay close attention to always.
Summary of the invention
For above-mentioned demand, invention especially provides a kind of electrode material and preparation method thereof.
Object of the present invention can be achieved through the following technical solutions:
A kind of electrode material, comprises basalis, outer WO 3 film and the intermediate layer material between basalis and skin;
Described intermediate layer material is made up of the component comprising following weight portion:
Graphite 20-30 part,
Al2O3 4-5 part,
Pb3O4 2-2.5 part,
TiO2 1-1.2 part,
PVA 2-3 part,
CeO2 0.8-1.2 part,
Bi2O3 0.6-1 part,
La2O3 0.05-0.5 part.
Described Al2O3 is Al2O3 whisker.
The diameter of described Al2O3 whisker is 3-4nm.
Described basalis is nickel screen or copper mesh.
A preparation method for electrode material, comprises the steps:
(1) under hydrogen, 1200-1300 DEG C condition, heat 5 minutes removal substrate surface oxide skin(coating)s, substrate surface is smeared intermediate layer material, heats 1-3 hour under 700-800 DEG C of condition, heat and sample is cooled to room temperature rapidly;
(2) Na2WO4 ﹒ 2H2O is dissolved in oxalic acid solution, the sample of step 1 is immersed in above-mentioned solution, at 180-200 DEG C, add thermal response 12 hours;
(3), after the sample clean water be obtained by reacting by second step, drying, electrode material is obtained.
The preparation method of described intermediate layer material comprises the steps: graphite 20-30 weight portion, Al2O34-5 weight portion, Pb3O42-2.5 weight portion, PVA2-3 weight portion, TiO21-1.2 weight portion, CeO20.8-1.2 weight portion and Bi2O30.6-1 weight portion, wet ball-milling method is adopted to mix 8 hours, at 750-800 DEG C of temperature, insulation 2-3 hour, pulverize fine grinding 1-2 hour, add La2O30.05-0.5 weight portion, mix, obtain intermediate layer material.
compared with prior art, its beneficial effect is in the present invention:
(1) the electrode material quality that obtains of the present invention is higher, and Mingzhi's structure formed is highly stable, and its electrode capacitance value is far above general capacitor.
(2) contact area between the electrode material that invention is obtained and electrolyte is large, thus more effectively can carry out transferring charge.
(3) electrode material that invention is obtained has excellent conductivity, pliability, ductility and mechanical strength, and electronics can be made can more effectively to transmit during rushing discharge and recharge fast.
(4) electrode material that obtains of the present invention, its preparation method is simple, is easy to suitability for industrialized production.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment 1
(1) intermediate layer material is prepared: Al2O3 whisker 4kg, Pb3O42kg, PVA3kg, TiO21kg, CeO20.8kg and Bi2O30.8kg of by graphite 20kg, diameter being 3nm, wet ball-milling method is adopted to mix 8 hours, at 750 DEG C of temperature, be incubated 2 hours, pulverize fine grinding 2 hours, add La2O30.05kg, mix, obtain intermediate layer material;
(2) under hydrogen, 1200 DEG C of conditions, heat 5 minutes removal basalis nickel screen oxide layer, by basalis nickel screen surface smear intermediate layer material, heat 1 hour under 700 DEG C of conditions, heat and sample is cooled to room temperature rapidly;
(3) Na2WO4 ﹒ 2H2O is dissolved in oxalic acid solution, the sample of step 1 is immersed in above-mentioned solution, at 180 DEG C, add thermal response 12 hours;
(4), after the sample clean water be obtained by reacting by second step, drying, electrode material is obtained.
The performance test results of obtained electrode material is as shown in table 1.
Embodiment 2
(1) intermediate layer material is prepared: Al2O3 whisker 5kg, Pb3O42kg, PVA2kg, TiO21.2kg, CeO21.2kg and Bi2O31kg of by graphite 30kg, diameter being 3nm, wet ball-milling method is adopted to mix 8 hours, at 800 DEG C of temperature, be incubated 2 hours, pulverize fine grinding 1 hour, add La2O30.05kg, mix, obtain intermediate layer material;
(2) under hydrogen, 1300 DEG C of conditions, heat 5 minutes removal basalis nickel screen oxide layer, by basalis nickel screen surface smear intermediate layer material, heat 3 hours under 800 DEG C of conditions, heat and sample is cooled to room temperature rapidly;
(3) Na2WO4 ﹒ 2H2O is dissolved in oxalic acid solution, the sample of step 1 is immersed in above-mentioned solution, at 200 DEG C, add thermal response 12 hours;
(4), after the sample clean water be obtained by reacting by second step, drying, electrode material is obtained.
The performance test results of obtained electrode material is as shown in table 1.
Embodiment 3
(1) intermediate layer material is prepared: Al2O3 whisker 4kg, Pb3O42.5kg, PVA3 kg, TiO21kg, CeO21kg and Bi2O30.6kg of by graphite 30kg, diameter being 4nm, wet ball-milling method is adopted to mix 8 hours, at 750 DEG C of temperature, be incubated 3 hours, pulverize fine grinding 2 hours, add La2O30.5kg, mix, obtain intermediate layer material;
(2) under hydrogen, 1250 DEG C of conditions, heat 5 minutes removal basalis copper mesh oxide layer, by basalis copper mesh surface smear intermediate layer material, heat 2 hours under 750 DEG C of conditions, heat and sample is cooled to room temperature rapidly;
(3) Na2WO4 ﹒ 2H2O is dissolved in oxalic acid solution, the sample of step 1 is immersed in above-mentioned solution, at 180 DEG C, add thermal response 12 hours;
(4), after the sample clean water be obtained by reacting by second step, drying, electrode material is obtained.
The performance test results of obtained electrode material is as shown in table 1:
Table 1
The test result of capacitance size under the different current densities of table 2 embodiment 1
The invention is not restricted to embodiment here, those skilled in the art, according to announcement of the present invention, do not depart from improvement that scope makes and amendment all should within protection scope of the present invention.
Claims (6)
1. an electrode material, is characterized in that, comprises basalis, outer WO 3 film and the intermediate layer material between basalis and skin;
Described intermediate layer material is made up of the component comprising following weight portion:
Graphite 20-30 part,
Al2O3 4-5 part,
Pb3O4 2-2.5 part,
TiO2 1-1.2 part,
PVA 2-3 part,
CeO2 0.8-1.2 part,
Bi2O3 0.6-1 part,
La2O3 0.05-0.5 part.
2. electrode material according to claim 1, it is characterized in that, described Al2O3 is Al2O3 whisker.
3. electrode material according to claim 2, it is characterized in that, the diameter of described Al2O3 whisker is 3-4nm.
4. electrode material according to claim 1, it is characterized in that, described basalis is nickel screen or copper mesh.
5. a preparation method for electrode material, is characterized in that, comprises the steps:
(1) under hydrogen, 1200-1300 DEG C condition, heat 5 minutes removal substrate surface oxide skin(coating)s, substrate surface is smeared intermediate layer material, heats 1-3 hour under 700-800 DEG C of condition, heat and sample is cooled to room temperature rapidly;
(2) Na2WO4 ﹒ 2H2O is dissolved in oxalic acid solution, the sample of step 1 is immersed in above-mentioned solution, at 180-200 DEG C, add thermal response 12 hours;
(3), after the sample clean water be obtained by reacting by second step, drying, electrode material is obtained.
6. the preparation method of electrode material according to claim 5, it is characterized in that, the preparation method of described intermediate layer material comprises the steps: graphite 20-30 weight portion, Al2O34-5 weight portion, Pb3O42-2.5 weight portion, PVA2-3 weight portion, TiO21-1.2 weight portion, CeO20.8-1.2 weight portion and Bi2O30.6-1 weight portion, wet ball-milling method is adopted to mix 8 hours, at 750-800 DEG C of temperature, insulation 2-3 hour, pulverize fine grinding 1-2 hour, add La2O30.05-0.5 weight portion, mix, obtain intermediate layer material.
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CN102531063A (en) * | 2011-11-20 | 2012-07-04 | 湖南理工学院 | Graphene load tungsten trioxide (WO3) nanowire composite material and preparation method thereof |
JP2012216513A (en) * | 2011-03-29 | 2012-11-08 | Fujifilm Corp | Aluminum base material for collector, collector, positive electrode, negative electrode, and secondary battery |
CN103077833A (en) * | 2013-01-15 | 2013-05-01 | 江苏苏美仑智能科技有限公司 | Supercapacitor combination electrode and making method thereof |
CN103531827A (en) * | 2013-10-31 | 2014-01-22 | 大连交通大学 | Method for improving electrochemical activity of graphite felt of positive electrode of flow battery |
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JP2012216513A (en) * | 2011-03-29 | 2012-11-08 | Fujifilm Corp | Aluminum base material for collector, collector, positive electrode, negative electrode, and secondary battery |
CN102531063A (en) * | 2011-11-20 | 2012-07-04 | 湖南理工学院 | Graphene load tungsten trioxide (WO3) nanowire composite material and preparation method thereof |
CN103077833A (en) * | 2013-01-15 | 2013-05-01 | 江苏苏美仑智能科技有限公司 | Supercapacitor combination electrode and making method thereof |
CN103531827A (en) * | 2013-10-31 | 2014-01-22 | 大连交通大学 | Method for improving electrochemical activity of graphite felt of positive electrode of flow battery |
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