CN110649262A - Preparation method and application of nano cubic bimetal selenide material - Google Patents
Preparation method and application of nano cubic bimetal selenide material Download PDFInfo
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- CN110649262A CN110649262A CN201910929538.3A CN201910929538A CN110649262A CN 110649262 A CN110649262 A CN 110649262A CN 201910929538 A CN201910929538 A CN 201910929538A CN 110649262 A CN110649262 A CN 110649262A
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- 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 sodium ion batteries, and particularly discloses a preparation method of a nano cubic bimetal selenide material, which comprises the following steps: 1) weighing two different metal precursors, respectively dissolving the two different metal precursors in deionized water, uniformly mixing, stirring to obtain a suspension, and centrifuging, washing with water and washing with alcohol to obtain a nanocube double metal hydroxide; 2) and weighing the selenium source and the nano cubic double metal hydroxide, and selenizing to obtain the selenium-enriched nano cubic double metal hydroxide. In order to improve the specific capacity and cycle life of the battery when the transition metal is used as the cathode material of the sodium-ion battery, a certain amount of transition metal precursor is weighed to prepare a cubic bimetal hydroxide precursor by a solution method, and then selenylation treatment is carried out by a hydrothermal method or a calcination method to obtain the nano cubic bimetal selenide material.
Description
Technical Field
The invention relates to the technical field of sodium ion batteries, in particular to a preparation method and application of a nanocube bimetal selenide material.
Background
With the development of society and the progress of science and technology, energy shortage and environmental pollution become important problems in the development of the current society. The lithium ion battery, as a novel and efficient electric energy storage device, has the advantages of high capacity, long cycle life and the like, and is paid attention and paid attention by more and more researchers. As is well known, lithium ion batteries have undergone several generations of innovation and have penetrated into the daily lives of people. However, as a strategic national resource, metallic lithium has either an expensive price or a limited storage capacity, which does not limit the application prospect of lithium ion batteries. In comparison, the sodium ion battery has the advantages of wide distribution of sodium element in the earth crust, abundant content, environmental friendliness, low oxidation-reduction potential and the like, and thus becomes a novel energy device with great potential in recent years. However, the research on sodium ion batteries is still in the initial stage, and how to improve the performance of sodium ion batteries (such as long cycle life, high energy/power density, excellent rate capability, and stable low-temperature and high-temperature performance) has become a major problem to be solved.
However, most of the currently studied negative electrode materials for sodium ion batteries are materials with a de-intercalation mechanism (carbon-based, titanium-based, etc.), wherein most of carbon materials have the problems of low first coulombic efficiency and poor cycle performance to different degrees, and the high specific capacity of the electrode material has an important significance for the safety of the battery in the charging and discharging processes.
Therefore, in order to solve the problems of small specific capacity and poor cycle performance of the conventional negative electrode material of the sodium-ion battery, the design of a preparation method and application of a nano cubic bimetallic selenide material becomes a problem which needs to be solved at present.
Disclosure of Invention
The invention aims to provide a preparation method of a nano cubic bimetallic selenide material and application of the nano cubic bimetallic selenide material in a sodium ion battery, which are used for solving the problems of small specific capacity and poor cycle performance of the battery of the negative electrode material of the current sodium ion battery in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for preparing a nano cubic bimetal selenide material is characterized by comprising the following steps:
1) weighing two different metal precursors with the molar ratio of 0.5-1:1, respectively dissolving in deionized water, mixing uniformly after fully dissolving, magnetically stirring for 1-24 hours to obtain a suspension, and centrifuging, washing with water and washing with alcohol to obtain a nano cubic double metal hydroxide;
2) weighing a selenium source and the nano cubic double metal hydroxide obtained in the step 1), and selenizing by a hydrothermal method or a calcination method to obtain the nano cubic double metal selenide material;
in the step 1), the metal precursor is hydrochloride, nitrate, sulfate or potassium hydrochloride of transition metal (including late transition metal) containing copper, zinc, nickel, cobalt or tin.
Specifically, the metal in the metal precursor is one of transition metals (including post-transition metals) such as copper, zinc, nickel, cobalt or tin, and the precursor is one of hydrochloride, nitrate, sulfate and potassium salt corresponding to each metal.
As a further scheme of the invention: the hydrochloride, nitrate, sulfate or sylvite of transition metal (including late transition metal) containing copper, zinc, nickel, cobalt or tin is potassium stannate, zinc sulfate, copper nitrate, nickel nitrate or cobalt chloride.
As a still further scheme of the invention: in the step 2), the selenium source is selenium powder or selenium dioxide.
As a still further scheme of the invention: in the step 1), the dispersion concentration of the metal precursor in deionized water is 0.15-0.3 g/mL-1。
As a still further scheme of the invention: in the step 1), the temperature of the magnetic stirring is 10-50 ℃.
As a still further scheme of the invention: in the step 2), the molar ratio of the nano cubic double metal hydroxide to the selenium source is 0.001-100: 1.
As a still further scheme of the invention: in the step 2), the conditions of the hydrothermal selenization are as follows: dispersing the nanocube bimetal hydroxide and the selenium source in deionized water, then placing the mixture in a polytetrafluoroethylene reaction kettle, adding sodium hydroxide and sodium borohydride for selenylation reaction at the reaction temperature of 150 ℃ and 300 ℃ for 1-12 hours.
As a still further scheme of the invention: in the step 2), the selenizing conditions of the calcining method are as follows: placing the nano cubic double metal hydroxide and the selenium source in different boats (containers) respectively, and calcining the nano cubic double metal hydroxide and the selenium source together in the atmosphere of hydrogen/argon, wherein the temperature rise speed of the calcination is 1-10 ℃/min, the temperature of the calcination is 300-800 ℃, and the heat preservation time of the calcination is 1-5 hours.
The invention also provides the nano cubic bimetallic selenide material prepared by the preparation method.
The application of the nano cubic bimetal selenide material in a sodium ion battery.
The preparation method of the nano cubic bimetallic selenide material is applied to the preparation of sodium ion battery products.
Compared with the prior art, the invention has the beneficial effects that:
1. the method has the advantages of short process flow and simple equipment, the prepared nano cubic double metal hydroxide material forms the double metal selenide micro-crystal boundary, a buffer area can be provided, the problem of volume expansion in the charging and discharging process can be effectively solved, and the structural stability of the material can be remarkably improved by combining a cubic block structure, so that the cycle performance and the service life of the battery are improved.
2. The nano cubic double metal selenide is introduced as an active substance, so that the nano cubic double metal selenide has strong structural advantages, the structural stability in the charging and discharging processes of the battery can be effectively improved, the cycle stability of the battery is improved, the nano structure can effectively shorten the distance of sodium ions embedded into the material, and the specific capacity of the battery is effectively improved.
3. The preparation method has the advantages of cheap and easily-obtained raw materials, environmental friendliness, simple and controllable process parameters, convenience in technical popularization, capability of solving the problems of small specific capacity and poor cycle performance of the battery of the negative electrode material of the conventional sodium ion battery, and wide market prospect.
Drawings
Fig. 1 is a scanning electron microscope image of nano cubic tin zinc selenide prepared in example 1 of the present invention.
Fig. 2 is a graph showing the charge and discharge curves of two previous cycles of the nano cubic tin zinc selenide prepared in example 1 of the present invention as a negative electrode material of a sodium ion battery.
Fig. 3 is a discharge specific capacity cycle diagram of nano cubic tin zinc selenide prepared in example 1 of the present invention as a sodium ion battery anode material.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. These are all protection enclosures of the present invention.
The technical solution of the present invention will be described in further detail with reference to specific embodiments.
Example 1
A method for preparing a nano cubic bimetal selenide material comprises the following steps:
weighing 1.5g of potassium stannate, dissolving in 5mL of deionized water, weighing 1.4g of zinc sulfate, dissolving in 45mL of deionized water, mixing after fully dissolving, placing on a magnetic stirrer, stirring for 4 hours at 25 ℃ to obtain white suspension, centrifuging, washing with water, and washing with alcohol to obtain white cubic ZnSn (OH)6；
1g of ZnSn (OH) thus obtained was weighed out6And 2g of selenium powder in two boats at 5% H2Calcining in a tube furnace under the atmosphere of 95% Ar at the heating rate of 2 ℃/min at the temperature of 400 ℃ for 3 hours, and naturally cooling to room temperature to obtain the nano cubic selenideThe nano cubic zinc tin selenide material is characterized by a scanning electron microscope, and a specific scanning electron microscope image is shown in figure 1, so that the prepared nano cubic zinc tin selenide material is uniform in particle and cubic in particle.
Further, in this embodiment, the nanocube zinc tin selenide material is used as a sodium ion battery anode material for electrochemical tests. Specifically, the sodium ion battery is prepared by using the nano cubic tin zinc selenide material as the negative electrode material by adopting the prior art method, and electrochemical performance test is performed on the sodium ion battery, and fig. 2 and fig. 3 are electrochemical test results of the sodium ion battery, wherein fig. 2 is a charging and discharging curve diagram of two previous circles of the nano cubic tin zinc selenide prepared by the embodiment as the negative electrode material of the sodium ion battery, and fig. 3 is a discharge specific capacity cycle diagram of the nano cubic tin zinc selenide prepared by the embodiment as the negative electrode material of the sodium ion battery.
As can be seen from FIG. 2, when the prepared nano cubic zinc tin selenide material is used as a cathode material of a sodium ion battery, the first two circles can reach 560 mAh.g-1Left and right specific discharge capacities; as can be seen from fig. 3, the prepared nanocube zinc tin selenide material has excellent cycle performance when being used as a sodium ion battery cathode material, and can maintain stable specific discharge capacity even when being cycled to 50 cycles without rapid decay.
In the embodiment, the nano cubic bimetallic selenide material prepared by the preparation method has strong structural advantages, and can be used as a negative electrode material of a sodium ion battery.
In the embodiment, the preparation method of the nano cubic bimetallic selenide material is applied to the preparation of sodium ion battery products.
Example 2
A method for preparing a nano cubic bimetal selenide material comprises the following steps:
weighing 1.5g of copper nitrate and dissolving in 10mL of deionized water, weighing 1.4g of zinc sulfate and dissolving in 30mL of deionized water, mixing after fully dissolving, placing under magnetic stirringStirring for 5 hours at room temperature to obtain a suspension, and centrifuging, washing with water and washing with alcohol to obtain cubic ZnCu (OH)4；
1g of the ZnCu (OH) thus obtained was weighed4And 3g of selenium powder in two boats at 5% H2Calcining in a tubular furnace under the atmosphere of 95% Ar at the heating rate of 5 ℃/min, keeping the temperature at 500 ℃ for 2 hours, and then naturally cooling to room temperature to obtain the nano cubic block zinc copper selenide material which can be used as a cathode material of a sodium ion battery to prepare the sodium ion battery.
Example 3
A method for preparing a nano cubic bimetal selenide material comprises the following steps:
weighing nickel nitrate and zinc sulfate with a molar ratio of 0.5:1, respectively dissolving the nickel nitrate and the zinc sulfate in deionized water, wherein the dispersion concentration of the nickel nitrate and the zinc sulfate in the deionized water is 0.15 g/mL-1After fully dissolving, uniformly mixing, placing on a magnetic stirrer, stirring for 1 hour at 10 ℃ to obtain a suspension, and centrifuging, washing with water and washing with alcohol to obtain a nano cubic double metal hydroxide;
weighing and dispersing nanocube bimetal hydroxide and selenium dioxide in deionized water (the molar ratio of the nanocube bimetal hydroxide to the selenium dioxide is 0.001:1), then placing the nanocube bimetal hydroxide and the selenium dioxide in a polytetrafluoroethylene reaction kettle, adding sodium hydroxide and sodium borohydride for selenylation reaction at the reaction temperature of 150 ℃ for 1 hour, and naturally cooling the reaction product to room temperature to obtain the nanocube bimetal hydroxide material which can be used as a sodium ion battery cathode material for preparing a sodium ion battery.
Example 4
A method for preparing a nano cubic bimetal selenide material comprises the following steps:
weighing cobalt chloride and zinc sulfate with a molar ratio of 1:1, respectively dissolving the cobalt chloride and the zinc sulfate in deionized water, wherein the dispersion concentration of the cobalt chloride and the zinc sulfate in the deionized water is 0.3 g/mL-1After fully dissolving, uniformly mixing, placing on a magnetic stirrer, stirring at 50 ℃ for 24 hours to obtain a suspension, and centrifuging, washing with water and washing with alcohol to obtain the productA nanocube double metal hydroxide;
weighing and dispersing nanocube bimetal hydroxide and selenium dioxide in deionized water (the molar ratio of the nanocube bimetal hydroxide to the selenium dioxide is 100:1), then placing the nanocube bimetal hydroxide and the selenium dioxide in a polytetrafluoroethylene reaction kettle, adding sodium hydroxide and sodium borohydride for selenylation reaction at the reaction temperature of 300 ℃ for 12 hours, and naturally cooling the reaction product to room temperature to obtain the nanocube bimetal hydroxide material which can be used as a sodium ion battery cathode material for preparing a sodium ion battery.
The nano cubic double metal hydroxide material prepared by the method integrates two advantages, the formed double metal selenide microcrystal boundary can provide a buffer area and effectively inhibit the problem of volume expansion in the charging and discharging processes, and the structural stability of the material can be obviously improved by combining a cubic block structure, so that the cycle performance and the service life of a battery are improved; in addition, the nano cubic double-metal selenide prepared by the invention has strong structural advantages, effectively improves the specific capacity and the cycle life of a battery when transition metal is used as a cathode material of the sodium-ion battery, and can effectively improve the structural stability in the charging and discharging processes of the battery, thereby improving the cycle stability of the battery.
The invention aims at the problems of small reversible capacity, poor cycle performance and the like of the current sodium-ion battery cathode material, introduces the nano cubic double-metal selenide as an active substance, has strong structural advantages, and can effectively improve the structural stability in the battery charging and discharging process, thereby improving the cycle stability of the battery; the nano structure can effectively shorten the distance of sodium ions embedded into the material, thereby effectively improving the specific capacity of the battery, the double-metal selenide integrates two advantages, the formed microcrystal boundary can provide a buffer area and effectively inhibit the volume expansion problem in the charging and discharging process, the structure stability of the material can be obviously improved by combining the cubic block structure, thereby improving the cycle performance and the service life of the battery, and the battery has wide market prospect.
While the preferred embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the scope of the invention.
Claims (10)
1. A method for preparing a nano cubic bimetal selenide material is characterized by comprising the following steps:
1) weighing two different metal precursors with the molar ratio of 0.5-1:1, respectively dissolving in deionized water, mixing uniformly after fully dissolving, magnetically stirring for 1-24 hours to obtain a suspension, and centrifuging, washing with water and washing with alcohol to obtain a nano cubic double metal hydroxide;
2) weighing a selenium source and the nano cubic double metal hydroxide obtained in the step 1), and selenizing by a hydrothermal method or a calcination method to obtain the nano cubic double metal selenide material;
wherein the metal precursor is hydrochloride, nitrate, sulfate or potassium containing copper, zinc, nickel, cobalt or tin.
2. The method of preparing a nanocube bimetallic selenide material according to claim 1, wherein the hydrochloride, nitrate, sulfate or potassium salt containing copper, zinc, nickel, cobalt or tin is potassium stannate, zinc sulfate, copper nitrate, nickel nitrate or cobalt chloride.
3. The method for preparing a nanocube bimetallic selenide material according to claim 2, wherein, in the step 1), the dispersion concentration of the metal precursor in deionized water is 0.15-0.3 g-mL-1。
4. The method for preparing a nanocube bimetallic selenide material according to claim 2, wherein the temperature of the magnetic stirring in the step 1) is 10-50 ℃.
5. The method for preparing a nanocube bimetallic selenide material according to any one of claims 1 to 4, wherein in step 2), the selenium source is selenium powder or selenium dioxide.
6. The method for preparing a nanocube bimetallic selenide material according to claim 5, wherein the molar ratio of the nanocube bimetallic hydroxide and the selenium source in step 2) is 0.001-100: 1.
7. The method for preparing the nanocube bimetallic selenide material according to claim 6, wherein in the step 2), the conditions for the hydrothermal selenization are as follows: dispersing the nanocube bimetal hydroxide and the selenium source in deionized water, then placing the mixture in a polytetrafluoroethylene reaction kettle, adding sodium hydroxide and sodium borohydride for selenylation reaction at the reaction temperature of 150 ℃ and 300 ℃ for 1-12 hours.
8. The method for preparing a nanocube bimetallic selenide material according to claim 6, wherein in the step 2), the conditions of the calcination selenization are as follows: respectively placing the nanocube bimetal hydroxide and the selenium source in different containers, and calcining together in the atmosphere of hydrogen/argon, wherein the temperature rise speed of the calcination is 1-10 ℃/min, the temperature of the calcination is 300-800 ℃, and the heat preservation time of the calcination is 1-5 hours.
9. A nanocube bimetallic selenide material prepared by the method of any of claims 1-8.
10. Use of the nanocube bimetallic selenide material of claim 9 in a sodium ion battery.
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| CN111326347A (en) * | 2020-02-28 | 2020-06-23 | 上海应用技术大学 | Zn-Cu-Se composite material and preparation method and application thereof |
| CN112079338A (en) * | 2020-09-17 | 2020-12-15 | 齐鲁工业大学 | Three-dimensional foam-like composite material, preparation method and application thereof in sodium-ion battery |
| WO2021057334A1 (en) * | 2019-09-29 | 2021-04-01 | 苏州潜寻新能源科技有限公司 | Preparation method for and application of nano cubic bimetal selenide material |
| CN113363079A (en) * | 2020-03-04 | 2021-09-07 | 华东理工大学 | Hollow Cu7Se4-CuxCo1-xSe2Nanosphere composite material and preparation method and application thereof |
| CN113690438A (en) * | 2021-06-23 | 2021-11-23 | 北京理工大学 | Selenide-containing composite material and preparation method and application thereof |
| CN114671414A (en) * | 2022-03-25 | 2022-06-28 | 浙江大学 | Iron-copper-tin ternary selenide nano material for sodium ion battery and preparation method thereof |
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| CN111326347A (en) * | 2020-02-28 | 2020-06-23 | 上海应用技术大学 | Zn-Cu-Se composite material and preparation method and application thereof |
| CN111326347B (en) * | 2020-02-28 | 2021-12-07 | 上海应用技术大学 | Zn-Cu-Se composite material and preparation method and application thereof |
| CN113363079A (en) * | 2020-03-04 | 2021-09-07 | 华东理工大学 | Hollow Cu7Se4-CuxCo1-xSe2Nanosphere composite material and preparation method and application thereof |
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| CN115246630A (en) * | 2021-10-18 | 2022-10-28 | 齐齐哈尔大学 | Preparation method of defective hollow nickel cobalt selenide nanocubes |
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Application publication date: 20200103 |