CN113380999A - Preparation method of silver-iron oxide porous nanocube negative electrode material for molten salt battery - Google Patents
Preparation method of silver-iron oxide porous nanocube negative electrode material for molten salt battery Download PDFInfo
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Abstract
The invention relates to a preparation method of a silver-iron oxide porous nanocube anode material for a molten salt battery, which comprises the steps of providing Prussian blue; dispersing prussian blue into water or ethanol to form a dispersion liquid; adding a silver nitrate solution into the dispersion liquid, stirring to form silver and Prussian blue nanocubes, and allowing silver ions to permeate into Prussian blue to enter vacant sites of the Prussian blue nanocubes; and putting the silver and Prussian blue nanocubes into a tube furnace to calcine to obtain the silver-iron oxide porous nanocubes. According to the preparation method of the silver-iron oxide porous nanocube cathode material for the molten salt battery, the process of silver ion permeation to Prussian blue is carried out in the solution, the uniform dispersion of deposited metal elements can be realized, the preparation method is simple and convenient to operate, low in cost and high in synthesis efficiency, silver ions can enter vacancies of Prussian blue nanocubes through silver nitrate and Prussian blue impregnation, and the metal framework is utilized to restrain the silver ions, so that the effect of stable structure is achieved.
Description
Technical Field
The invention relates to an energy material, in particular to a preparation method of a silver-iron oxide porous nanocube anode material for a molten salt battery.
Background
With the development of socio-economy, the energy demand is increasing, and the development of renewable energy technology has higher requirements on advanced energy storage systems. Taking a lithium ion battery as an example, it has been widely used in daily life as one of high-efficiency energy storage devices. But the energy density, rate capability and cycle stability aspects also require continuous optimization by researchers. Prussian Blue (PB) is a cyanide of a transition metal, has an iron-based metal-organic framework structure, is characterized by an open framework, a large gap position and stability, has great potential in electrode materials, and has been widely used for research of the electrode materials. Silver element can reduce charge transfer resistance, and silver deposited on the electrode material can increase the oxidation-reduction reaction rate of the electrode material, so that the electrochemical reaction activity of the electrode material is obviously improved, and the compounding of the electrode material and the silver element is one of the methods for improving the property of the electrode material.
At present, some methods for realizing the metal-Prussian blue composite are reported in the literature.
For example, Chunjin Shi et al first etched prussian blue analogs with acetic acid, which acid etching was capable of dissociating the backbone moietyThus, prussian blue exposes unsaturated metal centers which form chemical bonds with the metal in solution for complexing purposes (Advanced science2021,7: 8). Specifically, 20mg of prussian blue analogue cubes were dispersed into a mixed solution of acetic acid (5mL) and ethylene glycol (40mL) by sonication, and then 0.4mmoL TiF was added4. After thorough mixing, the suspension was transferred to a 60mL autoclave and heated at 180 ℃ for 8h to finally obtain Prussian blue analogue and TiO2The composite structure of (1). However, the prussian blue etching by acid needs to be carried out in a high-pressure reaction kettle, and the acid concentration, the reaction time and the reaction temperature need to be accurately regulated and controlled.
Such as Yasuaki Einaga (Inorg. chem.2012,51,6, 3648-4Fe(CN)6Solution and metal salt (Co (NO)3)2，Ni(NO3)2，KNO3) The solution mixing reaction realizes the metal ion (K)+) Vacancy, Co, into Prussian blue nanocube structures2+And Ni2+Fe replacing vertex position of Prussian blue nanocube2+The reaction is to introduce metal ions during the formation of prussian blue nanocubes, but this method is not applicable to all ions.
Silver salts (AgNO) for Sudip Mukherjee et al3) And potassium ferricyanide K3Fe(CN)6Reacting to replace potassium ion with silver ion to synthesize Ag3Fe(CN)6(ACS Biomate. Sci. Eng.2020,6,1, 690-704). Specifically, 5mL of K3Fe(CN)65mL of AgNO was added3Stirring for 1-2 min, adding PVP into the reaction mixture, and continuously stirring the mixture for 6h to obtain Ag3Fe(CN)6The morphology of the nano material, but not the structure similar to Prussian blue nanocubes, is very important for the nano material, and the change of the morphology often causes the change of the properties and the functions. Meanwhile, the report indicates that silver ions are dissociated under the condition of weak acid (PH is 6) to synthesize Ag3Fe(CN)6Is an unstable structure.
Disclosure of Invention
In order to solve the problems of harsh conditions of metal-Prussian blue compounding or unstable synthetic structure and the like in the prior art, the invention provides a preparation method of a silver-iron oxide porous nanocube negative electrode material for a molten salt battery.
The preparation method of the silver-iron oxide porous nanocube anode material for the molten salt battery comprises the following steps: s1, providing Prussian blue (Fe)4[Fe(CN)6]3) (ii) a S2, dispersing Prussian blue into water or ethanol to form a dispersion liquid; s3, adding the silver nitrate solution into the dispersion, and stirring to form silver and prussian blue nanocubes (i.e., silver-prussian blue nanocubes), wherein silver ions permeate into prussian blue to enter vacancies of the prussian blue nanocubes; and S4, putting the silver and Prussian blue nanocubes into a tube furnace, and calcining to obtain the silver-iron oxide porous nanocubes.
In the invention, the metal ion introduction step S2 is carried out after the Prussian blue synthesis step S1, so that silver ions directly enter the vacancy of the Prussian blue nanocube structure, iron ions at the vertex of the Prussian blue nanocube are avoided being replaced in the Prussian blue forming process, and the problem that silver elements and Prussian blue are difficult to compound is solved. The cubic structure of the Prussian blue is not changed after being filled with silver ions, the cubic structure is still maintained, and the silver ions are embedded into the vacant positions in the Prussian blue nano structure and are not combined in the cubic structure through chemical bonds, so that dissociation cannot occur due to a weakly acidic environment. In the calcining process, prussian blue forms an iron oxide porous nanocube, silver ions are changed into simple substance silver and are retained in the porous iron oxide, and a heterogeneous structure of the silver-iron oxide porous nanocube is formed.
Preferably, in step S1, polyvinylpyrrolidone (PVP) and potassium ferrocyanide (K) are mixed4Fe(CN)6) Adding into dilute hydrochloric acid solution, stirring and dissolving at room temperature to obtain Prussian blue solution, heating the Prussian blue solution in a drying oven, washing with anhydrous ethanol, centrifuging, and drying to obtain Prussian blue powder.
Preferably, in step S2, the solubility of Prussian blue in the dispersion is 1-10g/L, corresponding to a molar concentration of iron element in the dispersion of 0.0163-0.1630 mol/L. In a preferred embodiment, the solubility of Prussian blue in the dispersion is 5g/L, corresponding to a molar concentration of iron element in the dispersion of 0.0815 mol/L.
Preferably, the silver/iron molar ratio in the silver and prussian blue nanocubes is between 2% and 20%.
Preferably, in step S3, the molar solubility of the silver nitrate solution is equal to the molar concentration of the iron element in the dispersion. In a preferred embodiment, the molar solubility of the silver nitrate solution is 0.0815 mol/L.
Preferably, 0.2 to 2ml of silver nitrate solution is added to the dispersion and stirred. In a preferred embodiment, when the amount of the silver nitrate solution is 0.2 to 2ml, the molar ratio of silver/iron in the obtained silver-prussian blue nanocubes is 2 to 20%, and when the amount of the silver nitrate solution exceeds 2ml, the molar ratio of silver/iron in the silver-prussian blue nanocubes does not increase when reaching the upper limit.
Preferably, in step S3, the stirring time is 1-2 h.
Preferably, in step S3, the silver nitrate solution is added into the dispersion liquid and stirred at normal temperature, after the reaction is finished, the precipitate is collected by centrifugation, and finally washed and dried by deionized water and absolute ethyl alcohol to obtain silver and prussian blue nanocubes.
Preferably, the silver and prussian blue nanocubes have a cage structure in which silver ions occupy the vacancies of the prussian blue nanocubes.
Preferably, the drying temperature is 60-80 ℃.
Preferably, the drying time is 6-12 h.
Preferably, in step S4, the calcination temperature is 300-350 ℃, and the calcination time is 6-12 h.
According to the preparation method of the silver-iron oxide porous nanocube cathode material for the molten salt battery, the process of silver ion permeation into Prussian blue is carried out in the solution, the uniform dispersion of deposited metal elements can be realized, the preparation method is simple and convenient to operate, the cost is low, the synthesis efficiency is high, and the silver-iron oxide porous nanocube cathode material can be impregnated by silver nitrate and Prussian blueSo that silver ions enter the vacant sites of the Prussian blue nanocubes, and the metal framework is utilized to restrain the silver ions, thereby achieving the effect of stable structure. Compared with the Ag in the prior report3Fe(CN)6The silver and prussian blue nanocubes according to the present invention do not dissociate and have a more robust structure. According to the preparation method of the silver and Prussian blue nanocube, the silver and Prussian blue nanocube are compounded, Prussian blue is dispersed into water or ethanol, and a silver nitrate solution is added and stirred at normal temperature to obtain the silver-Prussian blue nanocube structure. Compared with an etching method, the preparation method disclosed by the invention is simple and convenient in reaction conditions, mild in reaction conditions, short in reaction time, and capable of being safely carried out by stirring at normal temperature. The preparation method realizes the compounding of silver and Prussian blue cubes, can realize that silver ions enter the vacant sites of the Prussian blue nanocubes, utilizes the metal framework to restrain the silver ions, limits the silver ions in the cubic structure, and achieves the effect of stable structure, thereby solving the problems of infirm combination and easy falling of the silver and the Prussian blue. In the calcining process, prussian blue forms an iron oxide porous nanocube, silver ions are changed into simple substance silver and are retained in the porous iron oxide, and a heterogeneous structure of the silver-iron oxide porous nanocube is formed. When the structure is used as a cathode of a molten salt battery for a charge-discharge experiment, the uniformly distributed elemental silver plays a role in promoting the transfer of carriers, so that the battery performance is improved.
Drawings
Fig. 1 is a scanning electron micrograph of prussian blue according to example 1 of the present invention;
fig. 2 is a scanning electron micrograph of silver-prussian blue nanocubes according to example 1 of the present invention;
fig. 3 is an elemental distribution diagram of silver on silver-prussian blue nanocubes according to example 1 of the present invention;
FIG. 4 is a scanning electron micrograph on a silver-iron oxide porous nanocube according to example 1 of the present invention;
FIG. 5 is a elemental distribution diagram of silver on silver-iron oxide porous nanocubes according to example 1 of the present invention;
fig. 6 is a first 20-minute charge-discharge curve of silver-iron oxide porous nanocubes as a molten salt battery anode material according to example 1 of the present invention;
fig. 7 is a scanning electron micrograph of silver-prussian blue nanocubes according to example 2 of the present invention;
fig. 8 is an elemental distribution diagram of silver on silver-prussian blue nanocubes according to example 2 of the present invention;
FIG. 9 is a scanning electron micrograph of silver-Prussian blue nanocubes after weak acid treatment according to example 2 of the present invention;
fig. 10 is an elemental distribution diagram of silver on silver-prussian blue nanocubes after weak acid treatment according to example 2 of the present invention.
Detailed Description
The preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
Example 1
Mixing polyvinylpyrrolidone (PVP) and potassium ferrocyanide (K)4Fe(CN)6) Adding into dilute hydrochloric acid solution, stirring at room temperature to obtain Prussian blue solution, heating the Prussian blue solution in an oven, washing with anhydrous ethanol, centrifuging, oven drying to obtain Prussian blue powder, and scanning electron microscopy as shown in FIG. 1.
Dispersing 0.1g of Prussian blue into 20ml of deionized water, adding 0.2ml of silver nitrate (0.0815mol/L) solution, stirring for 1h at normal temperature by using a magnetic stirrer, centrifugally collecting precipitates after the reaction is finished, finally washing by using deionized water and absolute ethyl alcohol, and drying for 6h at 60 ℃ to obtain silver-Prussian blue nanocubes, wherein a scanning electron microscope picture is shown as figure 2, an element distribution picture is shown as figure 3, the cubic particles are uniformly dispersed, the surfaces of the cubic particles are as smooth as Prussian blue, and no obvious particles exist. The Prussian blue nanocubes have a large number of vacancies by nature, the sizes of the vacancies can accommodate silver ions, and the element distribution diagram shows that the silver elements are uniformly distributed, so that the silver ions are considered to enter the vacancies of the Prussian blue nanocubes.
Putting the silver-Prussian blue nanocubes into a tube furnace, calcining for 12h at 300 ℃ to obtain silver-iron oxide porous nanocubes, wherein a scanning electron microscope picture is shown as figure 4, an element distribution diagram is shown as figure 5, and the silver elements are still uniformly distributed in the iron oxide porous nanocubes after calcination.
The silver-iron oxide porous nanocubes are used as the cathode material of the molten salt battery, a charge-discharge experiment is carried out to test the battery performance, and the charge-discharge curve in the first 20 minutes is shown in fig. 6.
Example 2
Mixing polyvinylpyrrolidone (PVP) and potassium ferrocyanide (K)4Fe(CN)6) Adding into dilute hydrochloric acid solution, stirring and dissolving at room temperature to obtain Prussian blue solution, heating the Prussian blue solution in a drying oven, washing with anhydrous ethanol, centrifuging, and drying to obtain Prussian blue powder.
Dispersing 0.1g of Prussian blue into 20ml of deionized water, adding 0.8ml of silver nitrate (0.0815mol/L) solution, stirring for 2 hours at normal temperature by using a magnetic stirrer, centrifugally collecting precipitates after the reaction is finished, finally washing by using deionized water and absolute ethyl alcohol, and drying for 12 hours at 80 ℃ to obtain silver-Prussian blue nanocubes, wherein a scanning electron microscope picture is shown as figure 7, an element distribution picture is shown as figure 8, the sizes of cubic particles are uniformly dispersed, and the element distribution picture shows that silver elements are uniformly distributed on the surface of the material. And dispersing the obtained silver-prussian blue nanocubes into pure water with the pH value of 6 again, standing for 6h, centrifuging to collect precipitates, washing with deionized water and absolute ethyl alcohol to obtain the silver-prussian blue nanocubes treated under the weak acid condition, wherein a scanning electron microscope image is shown in fig. 9, an element distribution diagram is shown in fig. 10, the original cubic structure of the nanocubes is maintained, dissociation does not occur, and the silver element is still uniformly distributed.
The above embodiments are merely preferred embodiments of the present invention, which are not intended to limit the scope of the present invention, and various changes may be made in the above embodiments of the present invention. All simple and equivalent changes and modifications made according to the claims and the content of the specification of the present application fall within the scope of the claims of the present patent application. The invention has not been described in detail in order to avoid obscuring the invention.
Claims (12)
1. A preparation method of a silver-iron oxide porous nanocube anode material for a molten salt battery is characterized by comprising the following steps:
s1, providing prussian blue;
s2, dispersing Prussian blue into water or ethanol to form a dispersion liquid;
s3, adding the silver nitrate solution into the dispersion, and stirring to form silver and prussian blue nanocubes, wherein silver ions permeate into prussian blue to enter vacancies of the prussian blue nanocubes.
And S4, putting the silver and Prussian blue nanocubes into a tube furnace, and calcining to obtain the silver-iron oxide porous nanocubes.
2. The preparation method according to claim 1, wherein polyvinylpyrrolidone and potassium ferrocyanide are added into a dilute hydrochloric acid solution, stirred and dissolved at room temperature to obtain a prussian blue solution, the prussian blue solution is placed into an oven to be heated, washed by absolute ethyl alcohol, centrifuged and dried to obtain prussian blue powder.
3. The method according to claim 1, wherein the concentration of the iron element in the dispersion is 0.0163 to 0.1630 mol/L.
4. The method of claim 1, wherein the silver/iron molar ratio in the silver and prussian blue nanocubes is between 2% and 20%.
5. The method according to claim 1, wherein the silver nitrate solution has a molar solubility equal to the molar concentration of iron in the dispersion.
6. The method according to claim 5, wherein the silver nitrate solution has a molar solubility of 0.0815mol/L, and 0.2 to 2ml of the silver nitrate solution is added to the dispersion and stirred.
7. The preparation method according to claim 1, wherein the silver nitrate solution is added into the dispersion liquid and stirred at normal temperature, after the reaction is finished, the precipitate is centrifugally collected, and finally, the precipitate is washed and dried by deionized water and absolute ethyl alcohol to obtain the silver and prussian blue nanocubes.
8. The method of claim 7, wherein the silver and Prussian blue nanocubes have a cage structure in which silver ions occupy the vacancies of the Prussian blue nanocubes.
9. The method according to claim 7, wherein the drying temperature is 60 to 80 ℃.
10. The method of claim 7, wherein the drying time is 6 to 12 hours.
11. The method as claimed in claim 1, wherein the tubular furnace calcination temperature is 300-350 ℃ and the calcination time is 6-12 h.
12. The silver-iron oxide porous nanocube of claim 1, wherein silver ions are changed to elemental silver that is uniformly retained in the porous iron oxide to form a heterostructure with the iron oxide.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114410294A (en) * | 2022-03-03 | 2022-04-29 | 新疆大学 | Efficient synthesis method of Prussian blue functionalized black phosphorus quantum dot hybrid material |
| CN116040655A (en) * | 2022-12-22 | 2023-05-02 | 宿迁学院 | Preparation method and application of sub-Prussian blue-like nano particles |
Citations (3)
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|---|---|---|---|---|
| US20090211494A1 (en) * | 2005-02-17 | 2009-08-27 | National Institute Of Advanced Industrial Science And Technology | Ultrafine particles of prussian blue-type metal complex, dispersion liquid thereof and their production methods |
| CN105836762A (en) * | 2016-03-16 | 2016-08-10 | 西北大学 | Preparation method and application of hollow Prussian-blue nanometer cube |
| CN108598412A (en) * | 2018-04-23 | 2018-09-28 | 中南大学 | Silicon alloy composite negative pole material based on metallorganic and preparation method thereof |
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2021
- 2021-06-09 CN CN202110643133.0A patent/CN113380999A/en active Pending
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| US20090211494A1 (en) * | 2005-02-17 | 2009-08-27 | National Institute Of Advanced Industrial Science And Technology | Ultrafine particles of prussian blue-type metal complex, dispersion liquid thereof and their production methods |
| CN105836762A (en) * | 2016-03-16 | 2016-08-10 | 西北大学 | Preparation method and application of hollow Prussian-blue nanometer cube |
| CN108598412A (en) * | 2018-04-23 | 2018-09-28 | 中南大学 | Silicon alloy composite negative pole material based on metallorganic and preparation method thereof |
Non-Patent Citations (2)
| Title |
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| ZHIFENG JIANG, DELI JIANG, A. M. SHOWKOT HOSSAIN，ET AL.: "In situ synthesis of silver supported nanoporous iron oxide microbox hybrids from metal-organic frameworks and their catalytic application in p-nitrophenol reduction", 《PHYSICAL CHEMISTRY CHEMICAL PHYSICS》 * |
| 党丽赟: "《氧化铁纳米材料及其应用概述》", 31 March 2019, 中国原子能出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114410294A (en) * | 2022-03-03 | 2022-04-29 | 新疆大学 | Efficient synthesis method of Prussian blue functionalized black phosphorus quantum dot hybrid material |
| CN116040655A (en) * | 2022-12-22 | 2023-05-02 | 宿迁学院 | Preparation method and application of sub-Prussian blue-like nano particles |
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