CN112397697A - Preparation method of flower-shaped nickel oxide/carbon composite material - Google Patents
Preparation method of flower-shaped nickel oxide/carbon composite material Download PDFInfo
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- CN112397697A CN112397697A CN202011276231.7A CN202011276231A CN112397697A CN 112397697 A CN112397697 A CN 112397697A CN 202011276231 A CN202011276231 A CN 202011276231A CN 112397697 A CN112397697 A CN 112397697A
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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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- 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
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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
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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 relates to the technical field of energy materials, and discloses a preparation method of a flower-shaped nickel oxide/carbon composite material, which is characterized by comprising the following steps of: A. preparing a proper amount of nickel acetate tetrahydrate, nickel chloride hexahydrate, nickel nitrate hexahydrate, waste rubber, concentrated hydrochloric acid and ammonia water for later use; b: cleaning and processing waste rubber into blocks, calcining the processed waste rubber blocks in a muffle furnace, soaking and filtering the obtained product by using 3mol/L HCl solution, and drying the obtained precipitate in an oven to obtain a product C. The preparation process is simple and environment-friendly, the material preparation cost is low, large-scale commercial production can be realized, meanwhile, the flower-shaped nickel oxide prepared by the method has wide application prospects in micron devices, and meanwhile, the composite material prepared by the method has good lithium storage performance, can be used as a lithium battery cathode material, and has huge potential commercial value.
Description
Technical Field
The invention relates to the technical field of energy materials, in particular to a preparation method of a flower-shaped nickel oxide/carbon composite material.
Background
NiO is a special metal oxide and is widely applied to the fields of catalysts, gas sensors, magnetic materials, lithium ion batteries and the like, and recent research finds that the performance of NiO is closely related to the morphology of NiO, so NiO particles with various morphologies are prepared for improving the performance of NiO.
Research reports show that compared with other transition metal oxides, NiO has the advantages of low potential, low cost, low toxicity and the like, and can be used as a lithium ion battery cathode material, and recent research shows that the single NiO has poor conductivity, and the volume of the single NiO is easy to expand in the charging and discharging process, so that the battery capacity is rapidly attenuated, therefore, people mix carbon with different morphologies into the NiO to improve the electrochemical performance of the NiO. Accordingly, one skilled in the art has provided a method for preparing a flower-shaped nickel oxide/carbon composite material to solve the problems set forth in the background art described above.
Disclosure of Invention
The invention aims to provide a preparation method of a flower-shaped nickel oxide/carbon composite material, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a flower-shaped nickel oxide/carbon composite material comprises the following steps:
A. preparing a proper amount of nickel acetate tetrahydrate, nickel chloride hexahydrate, nickel nitrate hexahydrate, waste rubber, concentrated hydrochloric acid and ammonia water for later use;
b: cleaning and processing waste rubber into blocks, placing the processed waste rubber blocks in a muffle furnace for calcining, soaking and filtering the obtained product by using 3mol/L HCl solution, and placing the obtained precipitate in an oven for drying to obtain a product C;
c: dispersing 1g of C and 6g of nickel salt together into 50mL of distilled water, carrying out ultrasonic treatment for 30min, adding a plurality of drops of ammonia water to adjust the pH value of the solution to 10, placing the obtained solution into a reaction kettle, carrying out hydrothermal treatment at 150 ℃ for 8-12 h, carrying out suction filtration and drying, and calcining the obtained precipitate in a muffle furnace to obtain the flower-shaped nickel oxide/carbon composite material.
As a still further scheme of the invention: and B, calcining the muffle furnace at the temperature of 300-500 ℃ for 1-6 h.
As a still further scheme of the invention: the drying temperature of the oven is 80 ℃, and the drying time is 6 h.
As a still further scheme of the invention: and C, calcining the muffle furnace at the temperature of 300-500 ℃ for 1-6 h.
As a still further scheme of the invention: the mass of C and the mass of the nickel salt in the step C are respectively 1g and 6 g.
As a still further scheme of the invention: the nickel salt is any one of nickel acetate tetrahydrate, nickel chloride hexahydrate and nickel nitrate hexahydrate.
Compared with the prior art, the invention has the beneficial effects that: the preparation process is simple and environment-friendly, the material preparation cost is low, large-scale commercial production can be realized, meanwhile, the flower-shaped nickel oxide prepared by the method has wide application prospects in micron devices, and meanwhile, the composite material prepared by the method has good lithium storage performance, can be used as a lithium battery cathode material, and has huge potential commercial value.
Drawings
FIG. 1 is an XRD pattern of a material prepared in a method for preparing a flower-like nickel oxide/carbon composite material;
FIG. 2 is an SEM image of a prepared material in a preparation method of a flower-shaped nickel oxide/carbon composite material;
FIG. 3 is a discharge specific capacity cycle diagram of a method for preparing a flower-like nickel oxide/carbon composite material.
Detailed Description
Referring to fig. 1 to 3, in embodiment 1 of the present invention, a method for preparing a flower-shaped nickel oxide/carbon composite material includes the following steps: cleaning and processing waste rubber into blocks, then placing the processed waste rubber blocks in a muffle furnace to calcine for 5 hours at the temperature of 350 ℃, soaking and filtering the obtained product with 3mol/L HCl solution, drying the obtained precipitate in an oven at 80 ℃ for 6 hours to obtain a product C, then dispersing and dissolving 1g of C and 6g of nickel nitrate hexahydrate in 50mL of distilled water, carrying out ultrasonic treatment for 30 minutes, adding a plurality of drops of ammonia water to adjust the pH value of the solution to be 10, placing the obtained solution in a reaction kettle, carrying out hydrothermal treatment for 9 hours at 150 ℃, carrying out suction filtration and drying, and calcining the obtained precipitate in the muffle furnace at 350 ℃ for 5 hours to obtain the flower-shaped nickel oxide/carbon composite material.
The attached figure 1 of the specification is an XRD (X-ray diffraction) pattern of the prepared material, wherein the diffraction peak of the material can be well matched with the diffraction peak of nickel oxide in a standard card, and the diffraction peak of amorphous carbon appears, which indicates that the main components of the prepared material are nickel oxide and amorphous carbon.
The attached figure 2 in the specification is an SEM picture of the prepared material magnified by 2.5 ten thousand times, and the observed picture shows that the prepared material is flaky and gathered into a flower shape, and the test result of the attached figure 1 shows that the prepared material is a flower-shaped NiO/C composite material.
The attached drawing of the specification is a discharge specific capacity circulation diagram of a half battery assembled by preparing the material as one pole and the elementary substance lithium sheet as one pole and circulating for 20 circles under 100mA g < -1 >, and the discharge specific capacity of the material is attenuated to 518mAh g < -1 > from 1014mAh g < -1 > after 20 circles under 100mA g < -1 >, but the value is far greater than the theoretical capacity (372mAh g < -1 >), so that the prepared material has good lithium storage performance and is expected to replace a graphite material to become a new generation of cathode materials of a lithium battery.
Example 2
A preparation method of a flower-shaped nickel oxide/carbon composite material comprises the following steps: cleaning and processing waste rubber into blocks, then placing the processed waste rubber blocks in a muffle furnace to calcine for 3 hours at the temperature of 400 ℃, then soaking and filtering the obtained product with 3mol/L HCl solution, then drying the obtained precipitate in an oven at 80 ℃ for 6 hours to obtain a product C, then dispersing and dissolving 1g of C and 6g of nickel chloride hexahydrate in 50mL of distilled water, carrying out ultrasonic treatment for 30 minutes, then adding a plurality of drops of ammonia water to adjust the pH value of the solution to be 10, then placing the obtained solution in a reaction kettle, carrying out hydrothermal treatment for 10 hours at the temperature of 150 ℃, carrying out suction filtration and drying, calcining the obtained precipitate in the muffle furnace at the temperature of 350 ℃ for 4 hours to obtain a flower-shaped nickel oxide/carbon composite material, assembling a half cell by taking the composite material as a pole and a simple substance lithium sheet as a pole, carrying out charge and discharge tests, the result shows that after 20 circles of treatment under 100mA g-1, the specific discharge capacity of the material is attenuated to 500mAh g-1 from 1002mAh g-1, and the material shows good lithium storage performance.
Example 3
A preparation method of a flower-shaped nickel oxide/carbon composite material comprises the following steps: cleaning and processing waste rubber into blocks, then placing the processed waste rubber blocks in a muffle furnace to calcine for 3.5h at the temperature of 450 ℃, then soaking and filtering the obtained product by using 3mol/L HCl solution, then drying the obtained precipitate in an oven at 80 ℃ for 6h to obtain a product C, then dispersing and dissolving 1g of C and 6g of nickel acetate tetrahydrate in 50mL of distilled water, carrying out ultrasonic treatment for 30min, then adding a plurality of drops of ammonia water to adjust the pH value of the solution to 10, then placing the obtained solution in a reaction kettle, carrying out hydrothermal treatment for 10h at 140 ℃, then carrying out suction filtration and drying, calcining the obtained precipitate in the muffle furnace at 350 ℃ for 4h to obtain a flower-shaped nickel oxide/carbon composite material, assembling a half cell by using a single lithium sheet as a pole, carrying out charge and discharge tests, the result shows that after 20 circles of treatment under 100mA g < -1 >, the specific discharge capacity of the material is attenuated to 515mAh g < -1 > from 1080mAh g < -1 >, and the material shows good lithium storage performance.
Example 4
A preparation method of a flower-shaped nickel oxide/carbon composite material comprises the following steps: cleaning and processing waste rubber into blocks, then placing the processed waste rubber blocks in a muffle furnace to calcine for 4 hours at the temperature of 500 ℃, then soaking and filtering the obtained product with 3mol/L HCl solution, then drying the obtained precipitate in an oven at 80 ℃ for 6 hours to obtain a product C, then dispersing and dissolving 1g of C and 6g of nickel nitrate hexahydrate in 50mL of distilled water, carrying out ultrasonic treatment for 30 minutes, then adding a plurality of drops of ammonia water to adjust the pH value of the solution to be 10, then placing the obtained solution in a reaction kettle, carrying out hydrothermal reaction for 9 hours at the temperature of 130 ℃, carrying out suction filtration and drying, calcining the obtained precipitate in the muffle furnace at the temperature of 350 ℃ for 4 hours to obtain a flower-shaped nickel oxide/carbon composite material, assembling a half cell by taking the composite material as an electrode and a simple substance lithium sheet as an electrode, carrying out charge and discharge tests, the result shows that after 20 circles of treatment under 100mA g-1, the specific discharge capacity of the material is reduced from 1050mAh g-1 to 510mAh g-1, and good lithium storage performance is shown.
Example 5
A preparation method of a flower-shaped nickel oxide/carbon composite material comprises the following steps: cleaning and processing waste rubber into blocks, then placing the processed waste rubber blocks in a muffle furnace to calcine for 3 hours at the temperature of 540 ℃, then soaking and filtering the obtained product with 3mol/L HCl solution, then drying the obtained precipitate in an oven at 80 ℃ for 6 hours to obtain a product C, then dispersing and dissolving 1g of C and 6g of nickel acetate tetrahydrate in 50mL of distilled water, carrying out ultrasonic treatment for 30 minutes, then adding a plurality of drops of ammonia water to adjust the pH value of the solution to be 10, then placing the obtained solution in a reaction kettle, carrying out hydrothermal treatment for 10 hours at 120 ℃, then carrying out suction filtration and drying, calcining the obtained precipitate in a muffle furnace at 400 ℃ for 4 hours to obtain a flower-shaped nickel oxide/carbon composite material, assembling a half cell by taking the composite material as an electrode and a simple substance lithium sheet as an electrode, carrying out charge and discharge tests, the result shows that after 20 circles of treatment under 100mA g-1, the specific discharge capacity of the material is attenuated to 520mAh g-1 from 1040mAh g-1, and good lithium storage performance is shown.
Example 6
A preparation method of a flower-shaped nickel oxide/carbon composite material comprises the following steps: cleaning and processing waste rubber into blocks, then placing the processed waste rubber blocks in a muffle furnace to calcine for 3.5h at the temperature of 550 ℃, then soaking and filtering the obtained product with 3mol/L HCl solution, then drying the obtained precipitate in an oven at 80 ℃ for 6h to obtain a product C, then dispersing and dissolving 1g of C and 6g of nickel chloride hexahydrate in 50mL of distilled water, carrying out ultrasonic treatment for 30min, then adding a plurality of drops of ammonia water to adjust the pH value of the solution to 10, then placing the obtained solution in a reaction kettle, carrying out hydrothermal treatment for 11h at 130 ℃, then carrying out suction filtration and drying, calcining the obtained precipitate in a muffle furnace at 400 ℃ for 4h to obtain a flower-shaped nickel oxide/carbon composite material, taking the composite material as an electrode and a simple substance lithium sheet as an electrode to assemble a half cell, carrying out charge and discharge tests, the result shows that after 20 circles of treatment under 100mA g-1, the specific discharge capacity of the material is attenuated to 530mAh g-1 from 1100mAh g-1, and the material shows good lithium storage performance.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention are equivalent to or changed within the technical scope of the present invention.
Claims (6)
1. The preparation method of the flower-shaped nickel oxide/carbon composite material is characterized by comprising the following steps of:
A. preparing a proper amount of nickel acetate tetrahydrate, nickel chloride hexahydrate, nickel nitrate hexahydrate, waste rubber, concentrated hydrochloric acid and ammonia water for later use;
b: cleaning and processing waste rubber into blocks, placing the processed waste rubber blocks in a muffle furnace for calcining, soaking and filtering the obtained product by using 3mol/L HCl solution, and placing the obtained precipitate in an oven for drying to obtain a product C;
c: dispersing 1g of C and 6g of nickel salt together into 50mL of distilled water, carrying out ultrasonic treatment for 30min, adding a plurality of drops of ammonia water to adjust the pH value of the solution to 10, placing the obtained solution into a reaction kettle, carrying out hydrothermal treatment at 150 ℃ for 8-12 h, carrying out suction filtration and drying, and calcining the obtained precipitate in a muffle furnace to obtain the flower-shaped nickel oxide/carbon composite material.
2. The method for preparing the flower-like nickel oxide/carbon composite material according to claim 1, wherein the muffle furnace in the step B is calcined at 300-500 ℃ for 1-6 h.
3. The preparation method of the flower-shaped nickel oxide/carbon composite material according to claim 1, wherein the drying temperature of the oven is 80 ℃ and the drying time is 6 hours.
4. The method for preparing the flower-like nickel oxide/carbon composite material according to claim 1, wherein the muffle furnace in the step C is calcined at 300-500 ℃ for 1-6 h.
5. The method for preparing a flower-like nickel oxide/carbon composite material according to claim 1, wherein the mass of C and the mass of the nickel salt in the step C are 1g and 6g, respectively.
6. The method for preparing a flower-like nickel oxide/carbon composite material according to claim 1, wherein the nickel salt is any one of nickel acetate tetrahydrate, nickel chloride hexahydrate and nickel nitrate hexahydrate.
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| CN202011276231.7A CN112397697A (en) | 2020-11-16 | 2020-11-16 | Preparation method of flower-shaped nickel oxide/carbon composite material |
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| CN202011276231.7A CN112397697A (en) | 2020-11-16 | 2020-11-16 | Preparation method of flower-shaped nickel oxide/carbon composite material |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090324486A1 (en) * | 2009-09-05 | 2009-12-31 | Bahari Molla Mahaleh Yaser | Fabrication of NiO nanoparticles and chip-like nanoflakes by solvothermal technique |
| CN103943379A (en) * | 2014-03-24 | 2014-07-23 | 上海大学 | Preparation method for graphene load flower-shaped porous nickel oxide composite materials |
| KR101793937B1 (en) * | 2016-05-24 | 2017-11-07 | 순천대학교 산학협력단 | composite for electrode of electrochemical capacitor and manufacturing method thereof, electrode composition for electrochemical capacitor |
| CN110357100A (en) * | 2019-06-13 | 2019-10-22 | 江苏理工学院 | A kind of method and application preparing carbon material using waste tire |
| CN110577820A (en) * | 2019-07-26 | 2019-12-17 | 郑州航空工业管理学院 | Porous structure Ni/NiO-C composite material and preparation method and application thereof |
-
2020
- 2020-11-16 CN CN202011276231.7A patent/CN112397697A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090324486A1 (en) * | 2009-09-05 | 2009-12-31 | Bahari Molla Mahaleh Yaser | Fabrication of NiO nanoparticles and chip-like nanoflakes by solvothermal technique |
| CN103943379A (en) * | 2014-03-24 | 2014-07-23 | 上海大学 | Preparation method for graphene load flower-shaped porous nickel oxide composite materials |
| KR101793937B1 (en) * | 2016-05-24 | 2017-11-07 | 순천대학교 산학협력단 | composite for electrode of electrochemical capacitor and manufacturing method thereof, electrode composition for electrochemical capacitor |
| CN110357100A (en) * | 2019-06-13 | 2019-10-22 | 江苏理工学院 | A kind of method and application preparing carbon material using waste tire |
| CN110577820A (en) * | 2019-07-26 | 2019-12-17 | 郑州航空工业管理学院 | Porous structure Ni/NiO-C composite material and preparation method and application thereof |
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