CN113140728B - Potassium iron sulfide thin film electrode and preparation method and application thereof - Google Patents
Potassium iron sulfide thin film electrode and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to the technical field of electrode materials, in particular to a potassium iron sulfide thin film electrode and a preparation method and application thereof. The invention provides a preparation method of a potassium iron sulfide thin film electrode, which comprises the following steps: mixing alkali liquor, metal sulfide solution and sublimed sulfur to obtain electrolyte; placing an iron matrix in the electrolyte, and carrying out hydrothermal reaction to obtain the potassium iron sulfide thin film electrode; the solute of the alkali liquor comprises potassium hydroxide. According to the invention, an iron matrix is placed in electrolyte for hydrothermal reaction, iron simple substance is combined with potassium ions and sulfur ions to generate potassium iron sulfide, the potassium iron sulfide and sublimed sulfur can induce the growth of nanowires, and the power density and energy density of the nanowires can be further improved by the growth of the nanowires; the alkaline system in the electrolyte can maintain the stability of the metal matrix.
Description
Technical Field
The invention relates to the technical field of electrode materials, in particular to a potassium iron sulfide thin film electrode and a preparation method and application thereof.
Background
In the present context, there is a pressing need for efficient, renewable and clean energy sources (e.g., solar, wind and tidal energy) to meet the ever increasing demand. Researchers are working on developing environmentally friendly and high power/energy density energy storage devices. Lead-acid batteries and lithium-ion batteries which are widely used so far still have the troublesome problems, such as low power density and short cycle life, and more seriously, the lithium-ion batteries adopt flammable and combustible organic liquid electrolytes and have the defect of insufficient electrochemical and thermal stability, so that the improvement of the energy density of the batteries is limited. Solid-state batteries have the advantages of high energy density, high safety, long cycle life, and the like, and are expected to overcome the disadvantages of conventional batteries, and thus may be one of the most desirable energy storage devices. The essential constituent active materials occupy the most important position in the solid-state battery, and therefore, it is of great practical significance to develop an electrode material with high energy density and high safety to improve the performance of the solid-state battery.
The iron-based material has the advantages of high theoretical capacity, no toxicity, high safety, low cost, easy obtainment of raw materials and the like, and is proved to be a potential electrode material. Although current electrode materials have higher power densities, improvements and enhancements in energy density are needed. Therefore, it is imperative to develop a dual high electrode material with both high energy and power density.
Disclosure of Invention
The invention aims to provide a potassium iron sulfide thin film electrode and a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a potassium iron sulfide thin film electrode, which comprises the following steps:
mixing alkali liquor, metal sulfide solution and sublimed sulfur to obtain electrolyte;
placing an iron matrix in the electrolyte, and carrying out hydrothermal reaction to obtain the potassium iron sulfide thin film electrode;
the solute of the alkali liquor comprises potassium hydroxide.
Preferably, the alkali liquor further comprises sodium hydroxide;
the metal sulfide in the metal sulfide solution comprises potassium sulfide and/or sodium sulfide.
Preferably, the concentration of the alkali liquor is 1-450 g/L.
Preferably, the concentration of the metal sulfide solution is 50-250 g/L.
Preferably, the dosage ratio of the alkali liquor to the metal sulfide solution to the sublimed sulfur is (10-20) mL: (2-10) mL: (0.5-4) g.
Preferably, the temperature of the hydrothermal reaction is 120-250 ℃ and the time is 6-56 hours.
Preferably, before the iron matrix is placed in the electrolyte, the iron matrix is pretreated;
the pretreatment comprises the step of sequentially soaking the iron matrix in hydrochloric acid and ethanol solution.
The invention also provides the potassium iron sulfide thin film electrode prepared by the preparation method in the technical scheme, wherein the thickness of the potassium iron sulfide thin film is 1-20 mu m;
the potassium iron sulfide in the potassium iron sulfide thin film is of a nanowire structure.
The invention also provides the application of the potassium iron sulfide thin-film electrode in the solid-state battery.
The invention provides a preparation method of a potassium iron sulfide thin film electrode, which comprises the following steps: mixing alkali liquor, metal sulfide solution and sublimed sulfur to obtain electrolyte; placing an iron matrix in the electrolyte, and carrying out hydrothermal reaction to obtain the potassium iron sulfide thin film electrode; the solute of the alkali liquor comprises potassium hydroxide. According to the invention, an iron matrix is placed in electrolyte for hydrothermal reaction, iron simple substance is combined with potassium ions and sulfur ions to generate potassium iron sulfide, the potassium iron sulfide and sublimed sulfur can induce the growth of nanowires, and the power density and energy density of the nanowires can be further improved by the growth of the nanowires; the alkaline system in the electrolyte can maintain the stability of the metal matrix.
Compared with the prior art, the invention also has the following advantages:
1. the raw materials are simple, the operation is easy, and the production cost is low;
2. the prepared product has high energy storage activity and is suitable for industrial mass production.
Drawings
FIG. 1 is an SEM photograph of a thin film electrode of potassium iron sulfide prepared in example 1;
FIG. 2 is a spectrum of energy of a thin film electrode of potassium iron sulfide prepared in example 1;
FIG. 3 is a charging and discharging curve of the thin film electrode of potassium iron sulfide prepared in the example in 350g/LKOH electrolyte solution under different current densities;
FIG. 4 is a charge-discharge curve of the thin-film electrode of potassium iron sulfide prepared in example 2 in a KOH electrolyte solution of 200 g/L;
FIG. 5 is a charge-discharge curve of the thin film electrode of potassium iron sulfide prepared in example 3 in a KOH electrolyte solution of 280 g/L;
FIG. 6 is a graph showing the charge and discharge curves of the thin film electrode of potassium iron sulfide prepared in example 4 in a KOH electrolyte solution of 400 g/L.
Detailed Description
The invention provides a preparation method of a potassium iron sulfide thin film electrode, which comprises the following steps:
mixing alkali liquor, metal sulfide solution and sublimed sulfur to obtain electrolyte;
placing an iron matrix in the electrolyte, and carrying out hydrothermal reaction to obtain the potassium iron sulfide thin film electrode;
the solute of the alkali liquor comprises potassium hydroxide.
In the present invention, all the starting materials for the preparation are commercially available products known to those skilled in the art unless otherwise specified.
The invention mixes alkali liquor, metal sulfide solution and sublimed sulfur to obtain electrolyte. In the present invention, the mixing is preferably carried out under stirring, and the stirring is not particularly limited in the present invention and may be carried out by a process known to those skilled in the art. In the present invention, the mixing is preferably performed by mixing an alkali solution and a metal sulfide solution to obtain a mixed solution, and then adding the sublimed sulfur to the mixed solution.
In the present invention, the solute of the lye comprises potassium hydroxide, or a mixture of potassium hydroxide and sodium hydroxide; when the solute of the lye comprises a mixture of potassium hydroxide and sodium hydroxide, the volume ratio of potassium hydroxide to sodium hydroxide is preferably 1: 1. In the invention, the concentration of the alkali liquor is preferably 1-450 g/L, more preferably 200-400 g/L, and most preferably 280-350 g/L.
In the present invention, the metal sulfide in the metal sulfide solution preferably includes potassium sulfide and/or sodium sulfide; when the metal sulfide is potassium sulfide and sodium sulfide, the volume ratio of potassium sulfide to sodium sulfide is preferably 1: 1. The concentration of the metal sulfide solution is preferably 50-250 g/L, more preferably 120-200 g/L, and most preferably 150 g/L.
In the invention, the dosage ratio of the alkali liquor, the metal sulfide solution and the sublimed sulfur is preferably (10-20) mL: (2-10) mL: (0.5-4) g, more preferably (12-16) mL: (4-8) mL: (0.5-3.5) g, most preferably (14-15) mL: (5-6) mL: (1-2) g.
In the invention, the alkali liquor has the function of maintaining the stability of the metal matrix, the metal sulfide solution has the function of inducing the growth and the shape control of the nanowires, and the sublimed sulfur has the function of inducing the growth and the shape control of the nanowires.
After the electrolyte is obtained, the iron matrix is placed in the electrolyte for hydrothermal reaction to obtain the potassium iron sulfide thin film electrode. Before the iron matrix is placed in the electrolyte, the invention also preferably comprises a pretreatment of the iron matrix. The pretreatment preferably comprises sequentially soaking the iron substrate in hydrochloric acid and ethanol solutions. In the present invention, the iron matrix is preferably a foamed iron matrix or a flat plate iron. In the present invention, the concentration of the hydrochloric acid is preferably 5 mol/L; the volume fraction of the ethanol solution is preferably 95%. In the invention, the time for soaking the iron matrix in the hydrochloric acid and ethanol solution is preferably 5min respectively; the soaking is preferably carried out under ultrasonic conditions. After the soaking is completed, the present invention also preferably includes washing and drying. In the invention, the cleaning is preferably performed by using deionized water; the drying is preferably vacuum drying, and the temperature of the vacuum drying is preferably 60-80 ℃. The vacuum drying time is not particularly limited in the present invention, and may be performed using a time known to those skilled in the art.
In the invention, the pretreatment can remove oxides on the surface and oil stains on the surface layer, and the crystal lattice defect which is beneficial to the growth of the crystal structure is obtained.
In the present invention, the process of placing the iron matrix in the electrolytic solution is preferably to place the area of 1cm2The foamed iron or iron plate of (2) was placed in 20mL of the electrolyte.
In the present invention, the process of placing the iron matrix in the electrolyte is preferably performed in an oxygen-free environment.
In the invention, the temperature of the hydrothermal reaction is preferably 120-250 ℃, more preferably 150-200 ℃, and most preferably 160-180 ℃; the time of the hydrothermal reaction is preferably 6-56 hours, more preferably 12-48 hours, and most preferably 30-38 hours. In the present invention, the hydrothermal reaction is preferably carried out in a hydrothermal reaction vessel.
In the invention, in the hydrothermal reaction process, the elemental iron, potassium ions and sulfur ions ionized from substances generate potassium iron sulfide.
After the hydrothermal reaction is finished, the method also preferably comprises the steps of taking out the iron matrix obtained after the hydrothermal reaction, and then sequentially cleaning and drying; preferably, deionized water and absolute ethyl alcohol are sequentially adopted for cleaning; the drying is not particularly limited in the present invention and may be carried out by a process known to those skilled in the art.
The invention also provides the potassium iron sulfide thin film electrode prepared by the preparation method in the technical scheme, wherein the thickness of the potassium iron sulfide thin film is 1-20 mu m;
the potassium iron sulfide in the potassium iron sulfide thin film is of a nanowire structure.
In the invention, the thickness of the potassium iron sulfide thin film is preferably 5-16 μm; the length of the nanowire in the nanowire structure is preferably 8-20 mu m, and the diameter of the nanowire structure is preferably 0.1-0.2 mu m.
The invention also provides the application of the potassium iron sulfide thin-film electrode in the solid-state battery. The method of the present invention is not particularly limited, and may be carried out by a method known to those skilled in the art.
The thin-film potassium iron sulfide electrode provided by the present invention, the preparation method and the application thereof are described in detail with reference to the following examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Ultrasonically soaking a foamed iron matrix in 5mol/L hydrochloric acid and 95% ethanol solution in volume fraction for 5min, cleaning with deionized water, and vacuum drying to obtain a pretreated foamed iron matrix;
mixing 15mL of KOH with the concentration of 350g/L and 5mL of sodium sulfide solution with the concentration of 120g/L to obtain a mixed solution, adding 2g of sublimed sulfur, and stirring until the sublimed sulfur is fully dissolved to obtain an electrolyte;
in an oxygen-free environment, 1cm2Placing the pretreated foam iron matrix in a reaction kettle containing 20mL of electrolyte, carrying out hydrothermal reaction for 48h at the temperature of 180 ℃, taking out the iron matrix, sequentially cleaning with deionized water and absolute ethyl alcohol, and drying to obtain a potassium iron sulfide thin film electrode (the thickness is 10 mu m, the length of the potassium iron sulfide nanowire is 15 mu m, and the diameter is 0.16 mu m);
the thin film electrode of potassium iron sulfide is subjected to SEM test, and the test results are shown in fig. 1 (where (a) is an SEM image of the electrode at low magnification and (b) is an SEM image of the electrode at high magnification), and as can be seen from fig. 1, the potassium iron sulfide in the thin film electrode of potassium iron sulfide is in a nanowire structure;
the energy spectrum test is carried out on the potassium iron sulfide thin film electrode, the test result is shown in figure 2 (a is an EDS energy spectrum of the electrode, and b is an electrode element surface scanning diagram), and as can be seen from figure 2, three elements K, Fe and S can be searched on the electrode, and all the elements are uniformly distributed;
the charging and discharging test is carried out on the potassium iron sulfide thin film electrode in KOH solution with the concentration of 350g/L under the test conditions that the charging control time is 25 minutes and 30 seconds, the discharging control voltage is less than 0V, the test result is shown in figure 3, and as can be seen from figure 3, the potassium iron sulfide thin film electrode is 50 mA-cm-2、100mA·cm-2、150mA·cm-2、200mA·cm-2And 250mA · cm-2The capacity densities of the obtained solutions were 21.07, 20.04, 19.37, 18.96 and 18.84mAh cm, respectively-2；
Example 2
Ultrasonically soaking an iron plate in 5mol/L hydrochloric acid and 95% ethanol solution by volume for 5min, cleaning with deionized water, and vacuum drying to obtain a pretreated iron plate;
mixing 12mL of KOH with the concentration of 200g/L and 8mL of potassium sulfide solution with the concentration of 200g/L to obtain a mixed solution, adding 0.5g of sublimed sulfur, and stirring until the sublimed sulfur is fully dissolved to obtain an electrolyte;
in an oxygen-free environment, 1cm2Placing the pretreated iron plate substrate in a reaction kettle containing 20mL of electrolyte, carrying out hydrothermal reaction at 250 ℃ for 32h, taking out the iron substrate, sequentially cleaning with deionized water and absolute ethyl alcohol, and drying to obtain a potassium-iron sulfide thin film electrode (the thickness is 15 microns, the length of the potassium-iron sulfide nanowire is 12 microns, and the diameter is 0.14 microns);
the charging and discharging test is carried out on the potassium iron sulfide thin film electrode in KOH solution with the concentration of 200g/L under the test conditions that the charging control time is 25 minutes and 30 seconds, the discharging control voltage is less than 0V, the test result is shown in figure 4, and as can be seen from figure 4, the potassium iron sulfide thin film electrode is 50 mA-cm-2The capacity density was 20.05mAh · cm at the current density of (1)-2。
Example 3
Ultrasonically soaking an iron plate in 5mol/L hydrochloric acid and 95% ethanol solution by volume for 5min, cleaning with deionized water, and vacuum drying to obtain a pretreated iron plate;
mixing 16mL of KOH with the concentration of 280g/L and 4mL of solution of potassium sulfide and sodium sulfide with the concentration of 150g/L (the volume ratio of the potassium sulfide to the sodium sulfide is 1:1) to obtain mixed solution, adding 3.5g of sublimed sulfur, and stirring until the sublimed sulfur is fully dissolved to obtain electrolyte;
in an oxygen-free environment, 1cm2Placing the pretreated foam iron matrix in a reaction kettle containing 20mL of electrolyte, carrying out hydrothermal reaction for 12h at the temperature of 200 ℃, taking out the iron matrix, sequentially cleaning with deionized water and absolute ethyl alcohol, and drying to obtain a potassium iron sulfide thin film electrode (the thickness is 8 mu m, the length of the potassium iron sulfide nanowire is 10 mu m, and the diameter is 0.12 mu m);
the charging and discharging test is carried out on the potassium iron sulfide thin film electrode in KOH solution with the concentration of 280g/L under the test conditions that the charging control time is 25 minutes, the discharging control voltage is less than 0V, the test result is shown in figure 5, and as can be seen from figure 5, the potassium iron sulfide thin film electrode is 50 mA-cm-2The capacity density was 19.9mAh · cm at the current density of (1)-2。
Example 4
Ultrasonically soaking an iron plate in 5mol/L hydrochloric acid and 95% ethanol solution by volume for 5min, cleaning with deionized water, and vacuum drying to obtain a pretreated iron plate;
mixing 14mL of a mixed solution of 400g/LKOH and NaOH (the volume ratio of potassium hydroxide to sodium hydroxide is 1:1) and 6mL of a sodium sulfide solution with the concentration of 50g/L to obtain a mixed solution, adding 1g of sublimed sulfur, and stirring until the sublimed sulfur is fully dissolved to obtain an electrolyte;
in an oxygen-free environment, 1cm2Placing the pretreated iron plate substrate in a reaction kettle containing 20mL of electrolyte, carrying out hydrothermal reaction for 56h at the temperature of 150 ℃, taking out the iron substrate, sequentially cleaning with deionized water and absolute ethyl alcohol, and drying to obtain a potassium-iron sulfide thin film electrode (the thickness is 6 microns, the length of the potassium-iron sulfide nanowire is 8 microns, and the diameter is 0.1 micron);
filling the potassium iron sulfide thin film electrode in KOH solution with the concentration of 400g/LThe discharge test was carried out under the conditions that the charge control time was 25 minutes and the discharge control voltage was less than 0V, and the test results are shown in FIG. 6. As can be seen from FIG. 6, the thin film electrode of potassium iron sulfide was at 50mA cm-2The capacity density was 20mAh · cm at the current density of (1)-2。
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. The preparation method of the potassium iron sulfide thin film electrode is characterized by comprising the following steps of:
mixing alkali liquor, metal sulfide solution and sublimed sulfur to obtain electrolyte;
placing an iron matrix in the electrolyte, and carrying out hydrothermal reaction to obtain the potassium iron sulfide thin film electrode;
the solute of the alkali liquor comprises potassium hydroxide;
the temperature of the hydrothermal reaction is 120-250 ℃, and the time is 6-56 hours;
the potassium iron sulfide in the potassium iron sulfide thin film is of a nanowire structure.
2. The method of claim 1, wherein the lye further comprises sodium hydroxide;
the metal sulfide in the metal sulfide solution comprises potassium sulfide and/or sodium sulfide.
3. The method according to claim 2, wherein the concentration of the alkali solution is 1-450 g/L.
4. The method according to claim 2, wherein the concentration of the metal sulfide solution is 50 to 250 g/L.
5. The method according to any one of claims 1 to 4, wherein the alkaline solution, the metal sulfide solution and the sublimed sulfur are used in a ratio of (10 to 20) mL: (2-10) mL: (0.5-4) g.
6. The method of claim 1, wherein prior to placing the ferrous matrix in the electrolyte, further comprising pre-treating the ferrous matrix;
the pretreatment comprises the step of sequentially soaking the iron matrix in hydrochloric acid and ethanol solution.
7. The thin film electrode of potassium iron sulfide prepared by the preparation method of any one of claims 1 to 6, wherein the thickness of the thin film of potassium iron sulfide is 1 to 20 μm;
the potassium iron sulfide in the potassium iron sulfide thin film is of a nanowire structure.
8. Use of the thin film electrode of potassium iron sulfide as claimed in claim 7 in a solid state battery.
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