CN112551586A - Preparation and application of bimetal ion doped porous hollow nanorod material - Google Patents
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Abstract
The invention relates to a preparation method and application of a bimetallic ion doped porous hollow nanorod material. The preparation method comprises the following steps: mixing a sulfur source, a molybdenum source, a nickel source and a cobalt source with octylamine according to a certain proportion, and then carrying out ultrasonic dissolution; adding a certain amount of ethanol into the solution, and stirring for a period of time until the mixture is fully mixed; then transferring the uniform solution into a 50 mL high-pressure reaction kettle lining for hydrothermal reaction, centrifugally washing until the solution is colorless, and obtaining a precursor material after cold drying; and carbonizing the obtained precursor material under the protection of argon to obtain the porous hollow nanorod electrode material doped with bimetallic ions. The preparation process is simple and has controllability; the prepared porous hollow nanorod electrode material doped with the bimetallic ions has the advantages of stable structure, excellent electrochemical performance, good cycle performance, high specific capacitance and the like, and is very suitable for being applied to the field of sodium ion batteries as an electrode material.
Description
Technical Field
The invention belongs to the technical field of new energy electronic materials, and relates to preparation and application of a bimetallic ion doped porous hollow nanorod material.
Background
Sodium ion battery (SIBs) have attracted considerable interest in the field of energy storage due to their high energy density, stable cycling performance and environmental friendliness. Molybdenum disulfide (MoS) due to a unique two-dimensional (2D) layer structure with considerable inter-layer spacing (— 0.62 nm) and weak van der Waals interactions2) Is considered to be a promising energy storage material. These structural features can provide diffusion paths for reversible insertion/extraction of sodium ions during charge/discharge, thereby having a high theoretical specific capacity. Nevertheless, Na is caused by limited interlayer spacing and poor intrinsic conductivity+Diffusion impaired, bare MoS2The anode typically provides rapid capacity fade and poor rates. Su et al, assisted by the interlayer nano-confinement effect, prepared fully dispersed in CoS2Nanopabular scaffolds (MoS)2/ CoS2) MoS of (1)2The nano sheet is used as an anode nano material of SIB, and the composite material has the following advantages: (i) dual active MoS2Nanosheets and CoS2Synergistic effect of scaffolds from Co (OH)2Host derived and having relatively good electronic conductivity and thermal stability; (ii) MoS due to interlayer confinement2The nano-sheets are uniformly dispersed in the CoS2In the nanobeam. (Yu Su, Chunxiao Wu, Hui Li, Feijiang Chen, Ying Guo, Lan Yang, Sailong Xu, MoS)2 nanoplatelets scaffolded within CoS2 nanobundles as anode nanomaterials for sodium-ion batteries，Journal of Alloys and Compounds)。
Chinese patent document CN201810994407.9 discloses a preparation method of a porous carbon material, comprising the following steps: 1) dissolving a molybdenum source and a nickel/cobalt source in water to obtain a mixed solution; 2) adding a vulcanizing agent and a reducing agent into the mixed solution, and dispersing to form a suspension; 3) transferring the suspension to a hydrothermal reaction kettle, heating for reaction, and cooling; 4) and after cooling, taking out the black solid obtained in the hydrothermal reaction kettle, and after centrifugal separation, washing and vacuum drying, obtaining the nickel/cobalt modified molybdenum disulfide nanoflower materials with different shapes and sizes. The nano flower synthesized by the method has uneven appearance, small flower ball and no obvious improvement on the specific surface area and the porosity.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the preparation and the application of the bimetallic ion doped porous hollow nanorod material with high specific capacitance and good cycle performance.
The technical scheme of the invention is as follows:
according to the invention, the preparation method of the porous hollow nanorod electrode material doped with the bimetallic ions comprises the following steps:
(1) mixing a sulfur source, a molybdenum source, a nickel source and a cobalt source with octylamine according to a certain proportion, and then carrying out ultrasonic dissolution;
(2) adding a certain amount of ethanol into the mixed solution in the step (1);
(3) transferring the mixed solution obtained in the step (2) into a 50 mL high-pressure reaction kettle lining, reacting at 220 ℃ for a period of time, cooling to room temperature after the reaction is finished, centrifugally washing to be colorless, and cooling to dry to obtain a precursor material;
(4) processing the precursor material obtained in the step (3) at a high temperature for a period of time under the protection of argon;
according to the present invention, preferably, the molybdenum source in step (1) is molybdenum alkenyl acetylacetonate, and the sulfur source is elemental sulfur; all of which are commercially available.
According to the present invention, it is preferred that Ni: Co: S =1:2:4 in step (1).
According to the present invention, it is preferred that the metal salt in step (1) is nickel nitrate, cobalt nitrate, which is commercially available.
According to the present invention, it is preferred that the volume of ethanol in step (2) is 20 mL.
According to the present invention, it is preferred that the reaction time in step (3) is 8 hours.
According to the present invention, it is preferred that the carbonization temperature in step (3) is 800 ℃ and the holding time is 1.5 hours.
An application of a porous hollow nanorod electrode material doped with bimetallic ions in an electrode material of a sodium-ion battery.
The technical advantages of the invention are as follows:
(1) the preparation method is simple in preparation process and controllable, and the structural morphology and the number of active sites can be regulated and controlled by controlling the ratio of Ni to Co to S.
(2) The bimetallic ion doped porous hollow nanorod electrode material prepared by the invention has the advantages of stable structure, excellent electrochemical performance, good cycle performance, high specific capacitance and the like, and is very suitable for being applied to the field of sodium ion batteries as an electrode material.
Drawings
FIG. 1 is a transmission electron microscope image of the bimetallic ion-doped porous hollow nanorod electrode material prepared in example 1 of the present invention.
FIG. 2 is a graph showing the cycle of efficiency of the bi-metal ion doped porous hollow nanorod electrode material prepared in example 1 of the present invention.
Detailed Description
The present invention will be further described with reference to the following embodiments and drawings, but is not limited thereto.
Meanwhile, the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1:
159 parts of molybdenum alkenyl acetylacetonate, 40 parts of elemental sulfur, 9 parts of nickel nitrate, 18 parts of cobalt nitrate and 600 parts of octylamine are subjected to ultrasonic mixing; then adding 2000 parts of ethanol, stirring for a period of time, fully mixing, transferring the mixed solution into the lining of a high-pressure reaction kettle, heating for 8 hours at 220 ℃, centrifugally washing to be colorless, and freeze-drying to obtain a precursor material; the obtained precursor material is carbonized for 1.5 h at 800 ℃ under the protection of argon gas, and the porous hollow nanorod electrode material doped with bimetallic ions is obtained.
A blue electric test system is adopted for testing, under the current density of 1A/g, the initial discharge specific capacity is 478mAh/g, the discharge specific capacity after 250 cycles is 358.1mAh/g, the coulombic efficiency is 98.96%, and the cycling stability is good.
This implementationExample A transmission electron microscope image of the prepared porous hollow nanorod electrode material doped with bimetallic ions is shown in FIG. 1, and the polymer C/MoS can be obtained from FIG. 12The porous hollow nano-rods are formed by alternately stacking.
The efficiency cycle performance of the porous hollow nanorod electrode material doped with the bimetallic ions prepared in the embodiment is shown in fig. 2, and as can be seen from fig. 2, under the current density of 1A/g, the initial specific discharge capacity is 478mAh/g, the specific discharge capacity after 250 cycles is 358.1mAh/g, the coulombic efficiency is 98.96%, and the cycle stability is good.
Example 2:
159 parts of molybdenum alkenyl acetylacetonate, 40 parts of elemental sulfur, 18 parts of nickel nitrate, 18 parts of cobalt nitrate and 600 parts of octylamine are subjected to ultrasonic mixing; then adding 2000 parts of ethanol, stirring for a period of time, fully mixing, transferring the mixed solution into the lining of a high-pressure reaction kettle, heating for 8 hours at 220 ℃, centrifugally washing to be colorless, and freeze-drying to obtain a precursor material; the obtained precursor material is carbonized for 1.5 h at 800 ℃ under the protection of argon gas, and the porous hollow nanorod electrode material doped with bimetallic ions is obtained.
Example 3:
159 parts of molybdenum alkenyl acetylacetonate, 40 parts of elemental sulfur, 0 part of nickel nitrate, 18 parts of cobalt nitrate and 600 parts of octylamine are subjected to ultrasonic mixing; then adding 2000 parts of ethanol, stirring for a period of time, fully mixing, transferring the mixed solution into the lining of a high-pressure reaction kettle, heating for 8 hours at 220 ℃, centrifugally washing to be colorless, and freeze-drying to obtain a precursor material; the obtained precursor material is carbonized for 1.5 h at 800 ℃ under the protection of argon gas, and the porous hollow nanorod electrode material doped with bimetallic ions is obtained.
Example 4:
159 parts of molybdenum alkenyl acetylacetonate, 40 parts of elemental sulfur, 9 parts of nickel nitrate, 0 part of cobalt nitrate and 600 parts of octylamine are subjected to ultrasonic mixing; then adding 2000 parts of ethanol, stirring for a period of time, fully mixing, transferring the mixed solution into the lining of a high-pressure reaction kettle, heating for 8 hours at 220 ℃, centrifugally washing to be colorless, and freeze-drying to obtain a precursor material; the obtained precursor material is carbonized for 1.5 h at 800 ℃ under the protection of argon gas, and the porous hollow nanorod electrode material doped with bimetallic ions is obtained.
Example 5:
159 parts of molybdenum alkenyl acetylacetonate, 40 parts of elemental sulfur, 0 part of nickel nitrate, 0 part of cobalt nitrate and 600 parts of octylamine are subjected to ultrasonic mixing; then adding 2000 parts of ethanol, stirring for a period of time, fully mixing, transferring the mixed solution into the lining of a high-pressure reaction kettle, heating for 8 hours at 220 ℃, centrifugally washing to be colorless, and freeze-drying to obtain a precursor material; the obtained precursor material is carbonized for 1.5 h at 800 ℃ under the protection of argon gas, and the porous hollow nanorod electrode material doped with bimetallic ions is obtained.
Claims (8)
1. A preparation method of a porous hollow nanorod electrode material doped with bimetallic ions comprises the following steps:
(1) mixing a sulfur source, a molybdenum source, a nickel source and a cobalt source with octylamine according to a certain proportion, and then carrying out ultrasonic dissolution;
(2) adding a certain amount of ethanol into the mixed solution in the step (1);
(3) transferring the mixed solution obtained in the step (2) into a 50 mL high-pressure reaction kettle lining, reacting at 220 ℃ for a period of time, cooling to room temperature after the reaction is finished, centrifugally washing to be colorless, and cooling to dry to obtain a precursor material;
(4) and (4) processing the precursor material obtained in the step (3) at a high temperature for a period of time under the protection of argon.
2. The method for preparing the porous hollow nanorod electrode material doped with the bimetallic ion according to claim 1, wherein the molybdenum source in the step (1) is molybdenum alkenyl acetylacetonate, and the sulfur source is elemental sulfur.
3. The method for preparing the porous hollow nanorod electrode material doped with the bimetallic ion according to claim 1, wherein Ni: Co: S =1:2:4 in the step (1).
4. The method for preparing the bimetallic ion-doped porous hollow nanorod electrode material of claim 1, wherein the metal salt in the step (1) is nickel nitrate or cobalt nitrate.
5. The method for preparing the porous hollow nanorod electrode material doped with the bimetallic ion according to claim 1, wherein the volume of the ethanol in the step (2) is 20 mL.
6. The method for preparing a porous hollow nanorod electrode material doped with bimetallic ions according to claim 1, wherein the reaction time in the step (3) is 8 h.
7. The method for preparing the porous hollow nanorod electrode material doped with the bimetallic ion according to claim 1, wherein the carbonization temperature in the step (3) is 800 ℃ and the holding time is 1.5 h.
8. An application of a porous hollow nanorod electrode material doped with bimetallic ions in an electrode material of a sodium-ion battery.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108023080A (en) * | 2017-12-01 | 2018-05-11 | 盐城工学院 | A kind of preparation method of transient metal doped molybdenum disulfide sode cell negative material and its resulting materials and application |
| CN108118362A (en) * | 2018-01-09 | 2018-06-05 | 国家纳米科学中心 | A kind of molybdenum disulfide electro-catalysis production hydrogen electrode and its preparation method and application |
| CN108975416A (en) * | 2018-08-23 | 2018-12-11 | 大连理工大学 | A kind of preparation method of transient metal sulfide composite nano materials |
| CN109174131A (en) * | 2018-08-29 | 2019-01-11 | 厦门大学 | The molybdenum disulfide nano floral material and its synthetic method of nickel cobalt modification and application |
| CN110299520A (en) * | 2019-06-24 | 2019-10-01 | 华南师范大学 | Cube nanocrystal composition, electrode slice, lithium ion battery and preparation method thereof |
| CN111992227A (en) * | 2020-08-28 | 2020-11-27 | 山东安润氢储新能源科技有限公司 | Nickel cobalt-molybdenum disulfide hollow nano composite material, synthetic method thereof and application of nickel cobalt-molybdenum disulfide hollow nano composite material in electrocatalytic hydrogen evolution |
| US20210062350A1 (en) * | 2018-10-26 | 2021-03-04 | Soochow University | Fe-doped mos2 nano-material, preparation method therefor and use thereof |
-
2020
- 2020-12-25 CN CN202011556423.3A patent/CN112551586A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108023080A (en) * | 2017-12-01 | 2018-05-11 | 盐城工学院 | A kind of preparation method of transient metal doped molybdenum disulfide sode cell negative material and its resulting materials and application |
| CN108118362A (en) * | 2018-01-09 | 2018-06-05 | 国家纳米科学中心 | A kind of molybdenum disulfide electro-catalysis production hydrogen electrode and its preparation method and application |
| CN108975416A (en) * | 2018-08-23 | 2018-12-11 | 大连理工大学 | A kind of preparation method of transient metal sulfide composite nano materials |
| CN109174131A (en) * | 2018-08-29 | 2019-01-11 | 厦门大学 | The molybdenum disulfide nano floral material and its synthetic method of nickel cobalt modification and application |
| US20210062350A1 (en) * | 2018-10-26 | 2021-03-04 | Soochow University | Fe-doped mos2 nano-material, preparation method therefor and use thereof |
| CN110299520A (en) * | 2019-06-24 | 2019-10-01 | 华南师范大学 | Cube nanocrystal composition, electrode slice, lithium ion battery and preparation method thereof |
| CN111992227A (en) * | 2020-08-28 | 2020-11-27 | 山东安润氢储新能源科技有限公司 | Nickel cobalt-molybdenum disulfide hollow nano composite material, synthetic method thereof and application of nickel cobalt-molybdenum disulfide hollow nano composite material in electrocatalytic hydrogen evolution |
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