CN114373934A - Lithium-oxygen battery two-dimensional composite nano metal catalyst and preparation method thereof - Google Patents
Lithium-oxygen battery two-dimensional composite nano metal catalyst and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a two-dimensional composite nano metal catalyst for a lithium-oxygen battery, a preparation method thereof and multilayer Ti3C2-MXene powder is added to a chloroplatinic acid solution; placing in a closed reaction box containing ultraviolet lamp irradiation, stirring, and irradiating by an ultraviolet lamp; turning off the ultraviolet lamp, preserving heat or heating, and continuously stirring for 1-5 h; evaporating the solvent and vacuum drying to obtain Ti3C2-MXene and precious metal Pt composite material Pt-Ti3C2. Dangerous operations such as high-temperature calcination, reducing atmosphere quenching and the like are not required, and the method is simple in steps, safe and efficient; the ultra-low-amount noble metal simple substances are uniformly dispersed on the surface and among layers of the obtained composite electrode material, so that the catalytic activity can be ensured, the cost can be fundamentally reduced, and the composite electrode material has ultra-strong electronic conductivity.
Description
Technical Field
The invention relates to a two-dimensional composite nano metal catalyst for a lithium-oxygen battery and a preparation method thereof, which are used as a positive electrode material of the lithium-oxygen battery and belong to the technical field of material chemistry.
Background
The development and popularization of the lithium ion battery greatly alleviate the problem of rapid environmental deteriorationHowever, the limited energy density is a deadly shortboard for long-endurance electric vehicle applications and popularity. Li-O2As a new secondary battery technology, the battery has the highest energy density in the existing battery field, almost matches with petroleum, so that the battery has great potential in the field of electric vehicles pursuing long-term endurance and high power density, and related research work is one of global research hotspots. However, Li-O2Practical applications of batteries are largely limited to their high overpotentials and poor cycling performance. For this reason, the discharge product Li is predominant2O2Has the characteristics of difficult solubility and insulation, and particularly needs to consume more energy barrier to decompose the energy barrier in the charging process, thereby causing high charging overpotential and further influencing the cycle life and stability of the battery.
Based on the above considerations, it is highly desirable to find a material with excellent conductivity to improve the inert interface property between the discharge product and the positive electrode, and to boost Li2O2Thereby reducing Li-O2The battery is charged and discharged with overpotential, and the cycle performance is improved. Ti3C2The MXene material is a graphene-like two-dimensional material, and the super-strong electronic conductivity of the MXene material is beneficial to improving Li2O2And the interface property between the anode and the cathode accelerates the charging and discharging process, thereby realizing lower overpotential. And Ti3C2The characteristic of the multi-tunnel structure is favorable for the transmission of oxygen and lithium ions, and more enough space is provided for Li2O2To be stored. Thus, Ti3C2Preparation of Li-O from MXene2Potential of battery diffusion electrode, however single Ti3C2the-MXene material lacks enough catalytic active sites, so that the progress of charge and discharge can be really promoted only by loading a high-efficiency catalyst to the surface of the material to form a composite electrode material, and the Li-O content is reduced2The battery is overpotential, and the cycle life is prolonged. In general, noble metal catalysts are mostly used as high-efficiency electrocatalysts because of their large number of unfilled d-electron orbitals making their surfaces prone to adsorb reactants and favoring the formation of intermediate "active compounds"And are now widely used in energy storage devices. However, it is undeniable that the noble metal catalyst often has the problems of easy sintering, catalyst poisoning and the like, and the preparation and synthesis often requires harsh conditions of high temperature, reducing gas quenching and the like, and in addition, Ti3C2The disadvantages that the MXene material is not high-temperature resistant and is easy to oxidize and the like also restrict the use of the method. Thus, a calcination-free Ti is sought3C2The preparation method of the-MXene-based nano metal catalyst is particularly important. To the present position, with respect to calcination-free Ti3C2The preparation method of the-MXene supported nano metal catalyst is rarely reported.
Disclosure of Invention
The invention provides a lithium-oxygen battery two-dimensional composite nano metal catalyst and a preparation method thereof, which aims to avoid the harsh conditions of preparation of noble metal catalysts such as high-temperature calcination, reducing atmosphere quenching and the like, and is a calcination-free two-dimensional material-based metal catalyst. The method comprises the step of growing Pt, Pd, Ir, Rh, Ru, Au, Ag and Mo nano metal simple substances obtained by ultraviolet light decomposition of chloroplatinic acid, chloropalladic acid, chloroiridic acid, chlororhodic acid, chlororuthenic acid, chloroauric acid, chloroarsinic acid and chloromolybdic acid in situ on Ti by an ultraviolet light-assisted decomposition method3C2MXene (including other MXenes, graphene, silicane, MoS)2Isobidimensional material) surface and interlayer of the material, the catalyst being Li-O2The battery anode has a great application prospect. The method overcomes the hidden danger risks brought by the steps of high-temperature calcination, reducing atmosphere quenching and the like, can realize ultra-low-quantity uniform loading, reduces the material cost, and has great significance for the application of the nano metal catalyst and the popularization of MXene materials.
The invention is realized by the following technical scheme:
the preparation method of the lithium-oxygen battery two-dimensional composite nano metal catalyst adopts an ultraviolet light assisted decomposition method to grow metal nano particles on the surface and the layers of a two-dimensional material in situ, thus obtaining the lithium-oxygen battery two-dimensional composite nano metal catalyst.
Specifically, the method comprises the following steps:
(1) preparing a metal precursor solution:
weighing a certain amount of metal precursor, dissolving the metal precursor in a mixed solvent containing ethanol and deionized water, stirring until the metal precursor is completely dissolved, and storing the metal precursor in a dark place;
(2) preparing a two-dimensional composite nano metal catalyst:
adding a certain amount of two-dimensional material into the metal precursor solution, and stirring until the two-dimensional material is dissolved; then placing the mixture in a closed box body containing an ultraviolet lamp, carrying out ultraviolet light-assisted decomposition reaction, and continuously stirring and maintaining the mixture; and then turning off the ultraviolet lamp, evaporating the solvent to dryness, and finally drying in vacuum to obtain the two-dimensional composite nano metal catalyst.
The two-dimensional material is Ti3C2-MXene、graphene、silicene、MoS2Or one or two or more of other two-dimensional materials.
The generated nano metal particles are one or the composition of two or more of Pt, Pd, Ir, Rh, Ru, Au, Ag, Mo and the like.
In the mixed solvent, the volume ratio of ethanol to deionized water is 9: 1.
The wavelength of the ultraviolet lamp is 254-365 nm.
The stirring speed in the step (2) is 200-500 rpm, the temperature is 25-60 ℃, and the holding time is 30-60 min.
And (3) evaporating the solvent in the step (2) at the temperature of 60-90 ℃ for 1-5 h.
In the step (2), the vacuum drying temperature is 40-60 ℃, and the time is 8-24 h.
The invention has the following beneficial effects:
(1) the two-dimensional composite nano metal catalyst prepared by the invention does not need dangerous operations such as high-temperature calcination, reducing atmosphere quenching and the like, and has simple steps, safety and high efficiency;
(2) the two-dimensional composite nano metal catalyst prepared by the invention has the advantages that the metal nano particles are uniformly dispersed, the ultra-low-amount load can be realized, the catalytic activity can be ensured, and the cost can be fundamentally reduced;
(3) the super-strong electronic conductivity of the two-dimensional composite nano metal catalyst prepared by the invention is beneficial to improving the interface property between the anode and the discharge product and accelerating Li2O2Thereby reducing Li-O2Charging and discharging overpotential of the battery;
drawings
FIG. 1 shows Pt @ Ti synthesized in example 1 of the present invention3C2XRD pattern of the catalyst.
FIG. 2 shows Pt @ Ti synthesized in example 1 of the present invention3C2SEM image of catalyst.
FIG. 3 shows Pt @ Ti synthesized in example 1 of the present invention3C2TEM images of the catalyst.
FIG. 4 shows Pt @ Ti synthesized in example 1 of the present invention3C2First cycle voltage profile of the catalyst in a lithium-oxygen cell.
Detailed Description
The technical solutions of the present invention will be described more clearly and completely with reference to the following embodiments of the present invention. The described embodiments are to be considered as illustrative only, and not restrictive, and all changes coming within the spirit and terms of the invention are intended to be embraced therein.
Example 1
3 2Preparation of 0.5% Pt @ TiCCatalyst and process for preparing same
First step, chloroplatinic acid (H)2PtCl6·6H2O) preparation of solution:
measuring 45mL of absolute ethyl alcohol and 5mL of deionized water, and uniformly mixing to generate a solution A;
6.67mg of H are weighed2PtCl6·6H2And adding O powder into the solution A, stirring until the O powder is completely dissolved, and storing in the dark to obtain a solution B.
Second, 0.5% Pt @ Ti3C2Preparing a composite material:
weighing 500mg of multilayer Ti3C2Adding the powder into the solution B;
placing in a closed box containing ultraviolet lamp irradiation, stirring at 25 deg.C with rotation speed of 300rpm, and irradiating with ultraviolet lamp for 60min to obtain mixed solution;
turning off the ultraviolet lamp, adjusting the temperature to 90 ℃, adjusting the rotating speed to 300rpm, and continuously stirring for more than 3 hours until the solvent is evaporated to dryness;
the product is dried in vacuum for 24h at the temperature of 60 ℃, and 0.5 percent Pt @ Ti is obtained3C2A composite material.
XRD test results, as shown in FIG. 1, indicate 0.5% Pt @ Ti prepared in example 13C2The composite electrode material contains Ti3C2And a characteristic diffraction peak of the Pt simple substance; from the SEM image shown in fig. 2, it can be seen that the surface of the composite electrode material is uniformly covered with the Pt metal simple substance, and Ti is well maintained3C2An accordion structure of material; from the TEM results shown in fig. 3, it is known that the simple substance of noble metal Pt is a nanoparticle and can be uniformly distributed in Ti3C2The surface of the material. The method is suitable for loading Ti on ultra-low Pt elementary substance3C2A material.
Third, manufacturing an electrode and assembling Li-O2The cell was subjected to electrochemical testing:
with 0.5% Pt @ Ti thus prepared3C2The composite material is a positive active material, the Super P is a conductive agent, the polyvinylidene fluoride (PVDF) is a binder, and the content of Pt @ Ti is 0.5 percent3C2Putting the Super P and PVDF in a mass ratio of 8:1:1 into an agate mortar, uniformly mixing, gradually dripping N-methylpyrrolidone (NMP) to grind to form uniform slurry, respectively dripping the slurry on Hydrophilic Carbon Paper (HCP) in equal amount with the loading of 1mg, and then putting the Hydrophilic Carbon Paper (HCP) into a constant-temperature drying oven to be dried in vacuum for more than 12 hours, namely 0.5 percent of Pt @ Ti3C2-HCP electrode preparation is complete;
using metal lithium as a cathode, 1M LiTFSI-TEGDME as electrolyte, glass fiber (GF/D) as a diaphragm, and Swagelok as Li-O2A battery testing mold, wherein batteries are assembled in a glove box under the condition that argon and moisture are lower than 0.01 ppm;
continuously introducing high-purity oxygen (99.999%) for 30min, standing the battery for 6h, and performing constant-current charge-discharge test.
The voltage curve is shown in FIG. 4, where it can be seen that 0.5% Pt @ Ti3C2Composite materials in Li-O2Performance in batteryLow charging overpotential (0.12V). It is demonstrated that the electrode material helps to accelerate ORR and OER kinetics and progression, thereby reducing overpotential.
Example 2
3 2Preparation of 0.5% Ir @ TiCCatalyst and process for preparing same
First step, chloroiridic acid (H)2IrCl6·6H2O) preparing a solution;
measuring 45mL of absolute ethyl alcohol and 5mL of deionized water, and uniformly mixing to generate a solution A;
6.41mg of H are weighed2IrCl6·6H2And adding O powder into the solution A, stirring until the O powder is completely dissolved, and storing in the dark to obtain a solution B.
Second, 0.5% Ir @ Ti3C2Preparation of composite materials
Weighing 500mg of multilayer Ti3C2Adding the powder into the solution B;
placing in a closed box containing ultraviolet lamp irradiation, stirring at 25 deg.C with rotation speed of 300rpm, and irradiating with ultraviolet lamp for 60min to obtain mixed solution;
turning off the ultraviolet lamp, adjusting the temperature to 90 ℃, adjusting the rotating speed to 300rpm, and continuously stirring for more than 3 hours until the solvent is evaporated to dryness;
the product is dried in vacuum for 24 hours at the temperature of 60 ℃, and 0.5 percent Ir @ Ti is obtained3C2A composite material.
Third, manufacturing an electrode and assembling Li-O2The cell was subjected to electrochemical testing:
as 0.5% Ir @ Ti prepared3C2The composite material is a positive active material, the Super P is a conductive agent, the PVDF is a binder, and the proportion is 0.5% Ir @ Ti3C2Putting the Super P and PVDF in a mass ratio of 8:1:1 into an agate mortar for uniform mixing, gradually dripping NMP to grind into uniform slurry, respectively dripping HCP with the same amount and the loading amount of 1mg, and then putting the slurry into a constant-temperature drying oven for vacuum drying for more than 12 hours, namely 0.5% Ir @ Ti3C2-HCP electrode preparation is complete;
using metal lithium as cathode, 1M LiTFSI-TEGDME as electrolyte, glass fiber (GF/D)As a separator, Swagelok is Li-O2A battery testing mold, wherein batteries are assembled in a glove box under the condition that argon and moisture are lower than 0.01 ppm;
continuously introducing high-purity oxygen (99.999%) for 30min, standing the battery for 6h, and performing constant-current charge-discharge test.
Example 3
3 2Preparation of 0.5% Au @ TiCCatalyst first step, chloroauric acid (HAuCl)4·4H2O) preparing a solution;
measuring 45mL of absolute ethyl alcohol and 5mL of deionized water, and uniformly mixing to generate a solution A;
5.23mg of HAuCl was weighed out4·4H2And adding O powder into the solution A, stirring until the O powder is completely dissolved, and storing in the dark to obtain a solution B.
Second, 0.5% Au @ Ti3C2Preparation of composite materials
Weighing 500mg of multilayer Ti3C2Adding the powder into the solution B;
placing in a closed box containing ultraviolet lamp irradiation, stirring at 25 deg.C with rotation speed of 300rpm, and irradiating with ultraviolet lamp for 60min to obtain mixed solution;
turning off the ultraviolet lamp, adjusting the temperature to 90 ℃, adjusting the rotating speed to 300rpm, and continuously stirring for more than 3 hours until the solvent is evaporated to dryness;
the product is dried in vacuum for 24h at the temperature of 60 ℃, and 0.5 percent Au @ Ti is obtained3C2A composite material.
Third, manufacturing an electrode and assembling Li-O2The cell was subjected to electrochemical testing:
as 0.5% Au @ Ti thus prepared3C2The composite material is a positive active material, the Super P is a conductive agent, the PVDF is a binder, and the content of the composite material is 0.5% of Au @ Ti3C2Putting the Super P and PVDF in a mass ratio of 8:1:1 into an agate mortar for uniform mixing, gradually dripping NMP to grind into uniform slurry, respectively dripping the uniform slurry onto HCP with the loading of 1mg in equal amount, and then putting the slurry into a constant-temperature drying oven for vacuum drying for more than 12 hours, namely 0.5% Au @ Ti3C2-HCP electrode preparation is complete;
using metal lithium as a cathode, 1M LiTFSI-TEGDME as electrolyte, glass fiber (GF/D) as a diaphragm, and Swagelok as Li-O2A battery testing mold, wherein batteries are assembled in a glove box under the condition that argon and moisture are lower than 0.01 ppm;
continuously introducing high-purity oxygen (99.999%) for 30min, standing the battery for 6h, and performing constant-current charge-discharge test.
Example 4
When the two-dimensional material is other MXene, the preparation of the composite nanometal catalyst was performed according to example 1 according to the difference of the metal species.
Example 5
When the two-dimensional material is graphene, the preparation of the composite nanometal catalyst was performed according to example 1 according to the difference of the kind of the metal.
Example 6
When the two-dimensional material was silicane, the preparation of the composite nanometal catalyst was performed according to example 1 depending on the kind of the metal.
Example 7
The two-dimensional material is MoS2At this time, the preparation of the composite nanometal catalyst was performed according to example 1 depending on the kind of the metal.
Example 8
When the two-dimensional material is other or the two materials are compounded, the preparation of the composite nano metal catalyst is performed according to the embodiment 1 according to the difference of the metal types. The invention is not the best known technology.
Claims (10)
1. The preparation method of the lithium-oxygen battery two-dimensional composite nano metal catalyst is characterized in that a metal precursor solution is decomposed by adopting an ultraviolet light-assisted decomposition method so as to generate metal nano particles on the surface and between layers of a two-dimensional material in situ.
2. The preparation method of the lithium-oxygen battery two-dimensional composite nano metal catalyst according to claim 1, characterized by comprising the following steps:
(1) preparing a metal precursor solution:
weighing a certain amount of metal precursor, dissolving the metal precursor in a mixed solvent containing ethanol and deionized water, stirring until the metal precursor is completely dissolved, and storing the metal precursor in a dark place;
(2) preparing a two-dimensional composite nano metal catalyst:
adding a certain amount of two-dimensional material into the metal precursor solution, and uniformly stirring and mixing; then placing the mixture in a closed box body containing an ultraviolet lamp, carrying out ultraviolet light-assisted decomposition reaction, and continuously stirring and maintaining the mixture; and then turning off the ultraviolet lamp, evaporating the solvent to dryness, and finally drying in vacuum to obtain the two-dimensional composite nano metal catalyst.
3. The method for preparing the lithium-oxygen battery two-dimensional composite nano-metal catalyst according to claim 2, wherein the two-dimensional material is Ti3C2-MXenes、graphene、silicene、MoS2One or two or more of them are compounded.
4. The method for preparing the lithium-oxygen battery two-dimensional composite nano metal catalyst as claimed in claim 2, wherein the metal precursor is one or a combination of two or more of chloroplatinic acid, chloropalladic acid, chloroiridic acid, chlororhodic acid, chlororuthenic acid, chloroauric acid, chloroarsinic acid and chloromolybdic acid.
5. The method for preparing the lithium-oxygen battery two-dimensional composite nano metal catalyst as claimed in claim 2, wherein the volume ratio of ethanol to deionized water in the mixed solvent is 9: 1.
6. The preparation method of the lithium-oxygen battery two-dimensional composite nano metal catalyst according to claim 2, wherein the wavelength of an ultraviolet lamp is 254-365 nm.
7. The preparation method of the lithium-oxygen battery two-dimensional composite nano metal catalyst according to claim 2, wherein the stirring speed in the step (2) is 200-500 rpm, the temperature is 25-60 ℃, and the holding time is 30-60 min.
8. The preparation method of the lithium-oxygen battery two-dimensional composite nano metal catalyst according to claim 2, wherein the temperature of the solvent evaporated in the step (2) is 60-90 ℃, and the evaporation time is 1-5 h.
9. The preparation method of the lithium-oxygen battery two-dimensional composite nano metal catalyst according to claim 2, wherein the vacuum drying temperature in the step (2) is 40-60 ℃ and the time is 8-24 h.
10. The lithium-oxygen battery two-dimensional composite nanometal catalyst, characterized in that it is obtained by the production method according to any one of claims 1 to 9.
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