CN113077993A - FeOOH/GO composite electrode material and preparation method and application thereof - Google Patents
FeOOH/GO composite electrode material and preparation method and application thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 64
- 229910002588 FeOOH Inorganic materials 0.000 title claims abstract description 55
- 239000007772 electrode material Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
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- 239000004202 carbamide Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 13
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 13
- 150000003839 salts Chemical class 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- 239000013543 active substance Substances 0.000 claims description 8
- 239000003990 capacitor Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000006185 dispersion Substances 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
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- 238000000926 separation method Methods 0.000 claims description 6
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- 230000009471 action Effects 0.000 claims description 5
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 4
- 229910001447 ferric ion Inorganic materials 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 3
- 238000013329 compounding Methods 0.000 claims description 2
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- 241000764238 Isis Species 0.000 claims 1
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- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- 230000005518 electrochemistry Effects 0.000 abstract description 2
- 229940044631 ferric chloride hexahydrate Drugs 0.000 abstract 2
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 abstract 2
- 238000001914 filtration Methods 0.000 abstract 1
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- 239000000243 solution Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
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- 238000002474 experimental method Methods 0.000 description 4
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention relates to a preparation method and application of an FeOOH and Graphene Oxide (GO) composite electrode material: belongs to the technical field of electrochemistry. The preparation method of the composite electrode material is that ferric chloride hexahydrate (FeCl) is used by an ultrasonic water bath chemical method3·6H2O), urea and GO are taken as raw materials, a uniform solution is prepared, and then the solution is put into an ultrasonic instrument to be subjected to ultrasonic water bath synthesis at a certain temperature. And finally, filtering, washing and drying to obtain the FeOOH/GO composite material. The preparation method has the advantages of unique preparation process, mild condition, simple operation and easy realization, and the obtained composite material has good performance.
Description
Technical Field
The invention relates to a super capacitor negative electrode material and a preparation method and application thereof, belonging to the technical field of electrochemistry.
Background
Due to the rapid development of society, the human society has an increasing demand for energy. Therefore, the demand for various energy storage devices is increasing, and the super capacitor is receiving attention as a high-performance energy storage device. In order to further improve the performance of the super capacitor, i.e. to improve the energy density of the whole device as much as possible while maintaining the advantages of high power density, etc., the use of the transition metal compound having the electric double layer capacitance and faraday pseudocapacitance behavior as the super capacitor electrode material has become one of the main research hotspots in the field at present. However, the research on the high specific capacitance transition metal oxide positive electrode material has been carried out more deeply, while the research on the negative electrode material for the supercapacitor is relatively less, and the negative electrode material widely used at present is still a carbon material, but the specific capacitance of the carbon material is smaller and is difficult to match with the high specific capacitance positive electrode material, so that the improvement of the specific energy of the whole device is limited.
Therefore, in order to meet the requirement of capacity matching between the positive electrode and the negative electrode, it is necessary to develop a negative electrode material having high specific capacitance and good performance. The transition metal iron element has the advantages of rich resources, low price, environmental friendliness, high theoretical specific capacitance and the like, so that the transition metal iron element has a huge development prospect when being used as the cathode active component of the super capacitor. However, iron-based materials have problems such as poor conductivity and cycle stability and low practical capacity, and thus, many researchers have made extensive efforts around these problems. FeOOH has various different crystal structures and is easy to prepare, so that the FeOOH has wide application in the fields of catalysis, environment (mainly used for adsorbing heavy metal ions) and the like at present, but has less research on electrochemical energy storage. In terms of the self-performance of FeOOH, the FeOOH has low electronic conductivity and is difficult to be directly used as a cathode material of a supercapacitor, and the FeOOH is also required to be compounded with a carbon material in the past application in the field of partial electrocatalysis. However, in these fields, the conventional hydrothermal method is mainly adopted to prepare the FeOOH/GO composite material, the method has the problems of difficult control of conditions, high equipment requirement, high energy consumption and the like, and the prepared composite material adopts uneven distribution of active components, so that the utilization rate of active substances is inevitably low and the purpose of preparing a high specific capacitance material is difficult to achieve if the material is directly used as a cathode material of a super capacitor. When the conventional hydrolysis method is adopted to prepare FeOOH/GO, FeOOH generated by hydrolysis is easy to aggregate and poor in dispersibility, so that the material performance is poor. Therefore, a preparation method of an FeOOH/GO composite material with mild conditions and simple and convenient operation is needed to be found at present, so that the conductivity of the material is improved, and meanwhile, a corresponding buffer space is provided for ion transmission and FeOOH volume change in the electrode reaction process, and the overall electrical property of the material is improved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides an FeOOH/GO composite electrode material and a novel preparation method thereof.
The invention relates to an FeOOH/GO composite electrode material which is formed by compounding FeOOH and GO dispersion liquid under the combined action of ultrasonic waves and a water bath to enable FeOOH to uniformly grow on GO.
The invention relates to a method for preparing an FeOOH/GO composite electrode material, which comprises the following steps:
step one
Adding urea into the ferric ion aqueous solution, and uniformly stirring to obtain a mixed solution 1;
step two
Dispersing the GO dispersion liquid uniformly under the action of ultrasound, adding the mixed solution 1 formed in the step one into the GO dispersion liquid, and stirring and ultrasonically mixing uniformly; obtaining a mixture;
step three
Carrying out ultrasonic water bath treatment on the mixture obtained in the step two;
step four
After the reaction is finished, cooling and carrying out solid-liquid separation; and washing and drying the obtained solid to obtain the FeOOH/GO composite material.
The invention relates to a method for preparing FeOOH/GO composite electrode material, comprising the step of firstly, adding FeCl3·6H2Dissolving O in water to obtain a ferric ion aqueous solution; in the mixed solution 1, FeCl3·6H2The concentration of the O salt is 0.01-0.5 mol/L, preferably 0.05-0.2 mol/L. In the mixed solution 1, the concentration of urea is 1 to 5 times, preferably 1 to 3 times that of iron salt.
The invention relates to a method for preparing FeOOH/GO composite electrode material, and in the second step, FeCl is adopted3·6H2The mass ratio of the O salt to the GO is 150-1: 1, preferably 150-25: 1, and more preferably 50-25: 1.
In the third step, the ultrasonic frequency in the ultrasonic water bath treatment is 40 KHz-100 KHz, preferably 90-100KHz, and further preferably 100 KHz.
The invention relates to a method for preparing an FeOOH/GO composite electrode material, which comprises the third step of controlling the water bath temperature to be 60-100 ℃, preferably 80-90 ℃. If the water bath temperature is too high, a large amount of heat transfer medium (water) can be volatilized, if other heat transfer medium (such as high-boiling-point oil) is adopted and ultrasonic synthesis is carried out at high temperature, safety risk exists, and the reaction speed is greatly increased along with the rise of the temperature, so that the product quality can be rapidly reduced, and if ultrasonic water bath synthesis is carried out in a sealed environment, the design of a reactor system becomes complicated, and the reaction temperature cannot be effectively controlled.
The invention relates to a method for preparing an FeOOH/GO composite electrode material, which comprises the third step of carrying out ultrasonic water bath for 1-5 hours, preferably 2-3 hours.
The invention relates to a method for preparing FeOOH/GO composite electrode material, comprising the fourth step of realizing solid-liquid separation by suction filtration or centrifugal treatment; and after solid-liquid separation, washing with ethanol and/or pure water until the eluate is neutral, drying at 50-120 ℃, preferably 70-100 ℃ for more than 5 hours.
The invention relates to an application of an FeOOH/GO composite electrode material, wherein the composite electrode material is used as a cathode of a super capacitor, and the mass specific capacitance of an active substance is 300-600F/g under an alkaline condition.
The invention relates to an FeOOH/GO composite electrode material, wherein the electrochemical test conditions of the composite electrode are as follows:
weighing a proper amount of the prepared FeOOH/GO composite material as an active material, acetylene black (a conductive agent) and PVDF (a binder, wherein a solvent is methyl pyrrolidone), mixing and grinding uniformly according to a ratio of 7:2:1, and then uniformly coating the mixture on carbonOn fiber paper (acetone, alcohol, H respectively)2O ultrasonic washing and drying), and vacuum drying at 100 ℃ for 10 hours. Finally, carrying out electrochemical test, using 1mol/L potassium hydroxide aqueous solution as electrolyte, using the FeOOH/GO composite electrode designed and prepared by the invention as a working electrode, and the area is 4 multiplied by 4cm2The platinum electrode is a counter electrode assembled three-electrode system, and cyclic voltammetry and constant current charge and discharge tests are carried out, wherein the test potential range is 0 to-1.2V (relative to Hg/HgO).
Principles and advantages
The principle is as follows:
the invention provides a method for synthesizing FeOOH/GO composite material by an ultrasonic water bath chemical method, which promotes Fe by free radicals and the like generated by molecular dissociation in a liquid phase through cavitation of ultrasonic waves and accompanying mechanical effect, thermal effect, chemical effect and the like3+The synthesized FeOOH mainly grows on the surface of the fully dispersed GO, so that the two components of the composite material are tightly combined and the reaction is accelerated. And the water bath heating further promotes the decomposition and crystallization growth processes of various substances in the solution, so that the uniform FeOOH/GO composite material is efficiently and quickly synthesized under the combined action of the two.
The advantages are that:
(1) the preparation method can well avoid the agglomeration problem of the material in the preparation process, can realize the uniform combination of FeOOH and GO, is beneficial to providing more reactive sites, and enables the electroactive component in the composite material to fully play the role of the electroactive component.
(2) According to the invention, the ultrasonic water bath synergistic effect with appropriate parameters is utilized to realize the adhesion growth of FeOOH on the surface of GO, so that the volume expansion of FeOOH is inhibited in the charging and discharging processes, and GO can be partially reduced in the reaction process, thereby improving the conductivity of the composite material, facilitating the electron transmission in an electrode, and enabling the FeOOH/GO composite material to show good electrochemical performance.
(3) The composite electrode material is synthesized in one step by an ultrasonic water bath method, the process flow is simple, the operation is easy, the requirements on equipment and environment are low, and the time is saved.
Drawings
FIG. 1 is a cyclic voltammogram of a FeOOH/GO composite electrode material prepared in example one.
FIG. 2 is an XRD pattern of FeOOH/GO composite electrode material prepared in example one.
The cycling of the FeOOH/GO composite electrode material prepared in example one can be seen in FIG. 1.
As can be seen from fig. 2: the FeOOH characteristic diffraction peak displayed by the diffraction peak of the FeOOH/GO composite electrode material is matched with the characteristic peak of a standard beta-FeOOH PDF card, which indicates that the prepared composite material contains beta-FeOOH.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specified, the reagents and materials used in the present invention are commercially available products or products obtained by a known method.
The specific embodiment of the invention is as follows:
the first embodiment is as follows:
weighing appropriate amount of FeCl3·6H2Dissolving O salt in water, adding urea, stirring and dissolving until a transparent yellow solution is formed, adding the transparent yellow solution into a certain amount of GO dispersion liquid under stirring, and performing ultrasonic dispersion uniformly. The mixture was prepared at 0.1mol/LFeCl3·6H2O, 0.1mol/L urea, and FeCl3·6H2The mass ratio of O salt to GO is 27: 1. And carrying out ultrasonic water bath treatment on the prepared mixed solution, wherein the ultrasonic frequency is 100kHz, the water bath temperature is 80 ℃, and the ultrasonic water bath time is 2 hours. After the reaction is finished, washing the reaction product by using ethanol and pure water until the reaction product is neutral, and carrying out vacuum drying for 5 hours at 70 ℃ to obtain the FeOOH/GO composite material.
And (3) using the obtained composite material to manufacture an electrode as a working electrode, a platinum electrode as a counter electrode, an Hg/HgO electrode as a reference electrode to assemble a three-electrode system, and using 1mol/L potassium hydroxide aqueous solution as electrolyte to perform electrochemical test, wherein the test potential window is 0-minus 1.2V. The cyclic voltammogram of this electrode at a scan rate of 10mV/s is shown in FIG. 1. The mass specific capacitance of the electrode active substance prepared from the composite material is 594F/g when the current density is 5A/g through constant current charge and discharge tests.
XRD analysis is carried out on the FeOOH/GO composite material obtained by drying, and the result is shown in figure 2.
Example two:
the operation and other conditions were the same as in example one, and the different condition parameters were as follows:
the solution is prepared into 0.05mol/L FeCl3·6H2O, and FeCl3·6H2The mass ratio of O salt to GO is 13.5: 1. The mass specific capacitance of the electrode active substance prepared from the composite material is 540F/g when the current density is 5A/g through constant current charge and discharge test.
Example three:
the operation and other conditions were the same as in example one, and the different condition parameters were as follows:
the solution is prepared into FeCl of 0.025mol/L3·6H2O, and FeCl3·6H2The mass ratio of O salt to GO is 6.75: 1. The mass specific capacitance of the electrode active substance prepared from the composite material when the current density is 5A/g is calculated to be 474F/g through a constant current charge-discharge test.
Example four:
the operation and other conditions were the same as in example one, and the different condition parameters were as follows:
the solution is prepared into 0.2mol/L FeCl3·6H2O, 0.2mol/L Urea and FeCl3·6H2The mass ratio of O salt to GO is 135: 1. The mass specific capacitance of the electrode active substance prepared from the composite material when the current density is 5A/g is calculated to be 587F/g through a constant current charge-discharge test.
Example five:
the operation and other conditions were the same as in example one, and the different condition parameters were as follows:
mixing the solutionThe FeCl is prepared into 0.05mol/L3·6H2And O, the ultrasonic water bath time is 4 h. The mass specific capacitance of the electrode active substance prepared from the composite material is 567F/g when the current density is 5A/g through constant current charge and discharge test.
Comparative example 1
The operation and other conditions were the same as in example one, and the different condition parameters were as follows:
the experiment was carried out without heating in a water bath, and only ultrasonic treatment was carried out at room temperature for 2 hours. The obtained composite material is prepared into an electrode, and the mass specific capacitance of the composite material is 275F/g when the current density is 5A/g through a constant current charge-discharge test.
Comparative example No. two
The operation and other conditions were the same as in example one, and the different condition parameters were as follows:
during the experiment, ultrasonic treatment is not carried out, and only water bath heating (treatment at 60 ℃ for 2h) is carried out. The obtained composite material is prepared into an electrode, and the mass specific capacitance of the composite material is 435F/g when the current density is 5A/g through a constant current charge and discharge test.
Comparative example No. three
The operation and other conditions were the same as in example one, and the different condition parameters were as follows:
the temperature of the water bath was adjusted to 60 ℃ during the experiment. The mass specific capacitance of the composite material is 485F/g when the current density is 5A/g through constant current charge and discharge tests.
Comparative example No. four
The operation and other conditions were the same as in example one, and the different condition parameters were as follows:
the ultrasonic frequency was adjusted to 80kHz during the experiment. The mass specific capacitance of the composite material when the current density is 5A/g is found to be 572F/g through constant current charge and discharge tests.
Claims (10)
1. An FeOOH/GO composite electrode material, which is characterized in that: the composite material is formed by compounding FeOOH and GO dispersion liquid under the combined action of ultrasonic waves and a water bath.
2. A method of making a FeOOH/GO composite electrode material according to claim 1, comprising the steps of:
step one
Adding urea into the ferric ion aqueous solution, and uniformly stirring to obtain a mixed solution 1;
step two
Dispersing the GO dispersion liquid uniformly under the action of ultrasound, adding the mixed solution 1 formed in the step one into the GO dispersion liquid, and stirring and ultrasonically mixing uniformly; obtaining a mixture;
step three
Carrying out ultrasonic water bath treatment on the mixture obtained in the step two;
step four
After the reaction is finished, cooling and carrying out solid-liquid separation; and washing and drying the obtained solid to obtain the FeOOH/GO composite material.
3. A method of making a FeOOH/GO composite electrode material according to claim 2, wherein: in step one, FeCl is added3·6H2Dissolving O in water to obtain a ferric ion aqueous solution; in the mixed solution 1, FeCl3·6H2The concentration of the O salt is 0.01-0.5 mol/L, and the concentration of the urea in the mixed solution 1 is 1-5 times of that of the ferric salt.
4. A method of making a FeOOH/GO composite electrode material according to claim 3, wherein: in step two, the FeCl3·6H2The mass ratio of the O salt to the GO is 150-1: 1.
5. A method of making a FeOOH/GO composite electrode material according to claim 3, wherein: in step two, the FeCl3·6H2The mass ratio of the O salt to the GO is 150-25: 1.
6. A method of making a FeOOH/GO composite electrode material according to claim 4, which isIs characterized in that: in step two, the FeCl3·6H2The mass ratio of the O salt to the GO is 50-25: 1.
7. A method of making a FeOOH/GO composite electrode material according to claim 2, wherein: in the third step, the ultrasonic frequency in the ultrasonic water bath treatment is 40 KHz-100 KHz, the water bath temperature is 60-100 ℃, and the ultrasonic water bath time is 1-5 h.
8. A method of making a FeOOH/GO composite electrode material according to claim 7, wherein: in the third step, the temperature of the water bath is 80-90 ℃; the ultrasonic water bath time is 2-3 h.
9. A method of making a FeOOH/GO composite electrode material according to claim 2, wherein: in the fourth step, solid-liquid separation is realized through suction filtration or centrifugal treatment; and after solid-liquid separation, washing with ethanol and/or pure water until the eluate is neutral, and drying at 50-120 ℃ for more than 5 hours.
10. The application of the FeOOH/GO composite electrode material in the claim 1 is characterized in that: the composite electrode material is used as a cathode of a super capacitor, and the mass specific capacitance of an active substance of the composite electrode material is 300-600F/g under an alkaline condition.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109087820A (en) * | 2018-09-05 | 2018-12-25 | 中南民族大学 | Graphene combination electrode material is prepared in situ in sonochemical method |
| CN109390573A (en) * | 2018-10-18 | 2019-02-26 | 陕西科技大学 | A kind of preparation method of super large lamella RGO load ultra-fine beta-FeOOH nano particle lithium ion battery negative material |
| CN109411747A (en) * | 2018-10-18 | 2019-03-01 | 陕西科技大学 | A kind of urea acts on the preparation method of lower ultra-fine beta-FeOOH nanometer rods self assembly hollow out microballoon |
| CN109449422A (en) * | 2018-11-12 | 2019-03-08 | 东北师范大学 | FeOOH nanometer rods/graphene oxide composite material and the preparation method and application thereof |
| CN111725003A (en) * | 2020-07-10 | 2020-09-29 | 大连理工大学 | Cubic iron-based oxyhydroxide/graphene composite material for supercapacitor and preparation method thereof |
| CN112310371A (en) * | 2020-10-19 | 2021-02-02 | 华东理工大学 | Iron oxyhydroxide/biomass charcoal composite material and preparation method thereof |
-
2021
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109087820A (en) * | 2018-09-05 | 2018-12-25 | 中南民族大学 | Graphene combination electrode material is prepared in situ in sonochemical method |
| CN109390573A (en) * | 2018-10-18 | 2019-02-26 | 陕西科技大学 | A kind of preparation method of super large lamella RGO load ultra-fine beta-FeOOH nano particle lithium ion battery negative material |
| CN109411747A (en) * | 2018-10-18 | 2019-03-01 | 陕西科技大学 | A kind of urea acts on the preparation method of lower ultra-fine beta-FeOOH nanometer rods self assembly hollow out microballoon |
| CN109449422A (en) * | 2018-11-12 | 2019-03-08 | 东北师范大学 | FeOOH nanometer rods/graphene oxide composite material and the preparation method and application thereof |
| CN111725003A (en) * | 2020-07-10 | 2020-09-29 | 大连理工大学 | Cubic iron-based oxyhydroxide/graphene composite material for supercapacitor and preparation method thereof |
| CN112310371A (en) * | 2020-10-19 | 2021-02-02 | 华东理工大学 | Iron oxyhydroxide/biomass charcoal composite material and preparation method thereof |
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Application publication date: 20210706 |