CN112928258A - Preparation method of pre-lithiated MXenes material and application of pre-lithiated MXenes material in battery electrode material - Google Patents
Preparation method of pre-lithiated MXenes material and application of pre-lithiated MXenes material in battery electrode material Download PDFInfo
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Abstract
The invention discloses a preparation method of a pre-lithiated MXene material, which comprises the steps of etching MAX-phase ceramic powder by using a mixed solution of sodium fluoride and hydrochloric acid to obtain a two-dimensional carbide MXene; the pre-lithiated MXenes is prepared by adopting a simple self-discharge principle, and the preparation method is simple, safe and low in cost; and Li+Can enlarge the layer of MXenesAnd the space is increased, more surface active sites are exposed, ion transmission channels are increased, and the problem of stacking and agglomeration of MXenes sheets in the circulating process is solved. The pre-lithiated MXenes are used as an electrode material of the lithium ion battery, so that the loss of lithium ions in the first charging process can be made up, the coulombic efficiency of first charging and discharging is improved, and the storage capacity of the MXenes on the lithium ions is improved to a greater extent. The pre-lithiated MXenes is used as an electrode material of a magnesium ion battery, realizes magnesium-lithium co-intercalation, improves multiplying power and cycle performance, and is an excellent electrode material.
Description
Technical Field
The invention relates to the field of novel energy storage, in particular to a preparation method of a pre-lithiated MXenes material and application of the pre-lithiated MXenes material in a battery electrode material.
Background
MXene is a novel two-dimensional layered transition metal carbide or carbonitride nano material with a graphene-like structure. The element A in the MAX phase of the precursor is etched by using an HF solution or a mixed solution of a fluorine salt and an acid. Wherein M is a transition metal element, A represents IIIA/IVA element, and X is carbon or nitrogen element. Currently, MXene synthesized in laboratory has Ti mainly3C2、Ti2C、Mo2C、(Ti0.5Nb0.5)2C、Ti3CN、Sc2C、Ta4C3、Nb2C、V2C and Nb4C3. Due to the diversity of MXene species and the characteristics of excellent conductivity, hydrophilicity and chemical stability, studies by many scholars have been initiated in recent years, so that MXene has been applied to a plurality of fields, especially the fields of energy storage and conversion, such as: super capacitor, lithium ion battery, sodium ion battery, sensor, etc.
Patent CN108682812A discloses an MXene coated silicon composite electrode material and a preparation method thereof; patent CN110540236A discloses an MXene material and a preparation method and application thereof. Although the MXene material has good conductivity and excellent chemical stability, the coulombic efficiency (about 60%) of the MXene material in the first charge and discharge in the lithium ion battery is low, so that the obtained capacity is low, and the application prospect of the MXene in the lithium ion battery is limited to a great extent; in addition, although the MXene material has higher theoretical capacity (1050 mAg/h) in the field of magnesium ion batteries, laboratory test results show that the obtained magnesium storage specific capacity is lower (96mAh/g, 50mA/g), the cycle life is shorter (<50 times), because the potential interlayer energy storage space is not fully utilized, and if the interlayer distance of the MXene material can be further expanded, the first coulombic efficiency and the lithium storage capacity of the MXene material as a lithium ion battery electrode material and the storage capacity of the MXene material as a magnesium ion battery electrode material are expected to be greatly improved.
Disclosure of Invention
The invention aims to solve the technical problem that MXene is stacked and agglomerated in the circulating process of the conventional lithium ion battery, so that the first coulombic efficiency and the first storage capacity of an electrode material are influenced.
The invention solves the technical problems through the following technical means:
a method for preparing a pre-lithiated MXene material, comprising the steps of:
(1) immersing MAX-phase ceramic powder into a mixed solution of sodium fluoride and hydrochloric acid according to a solid-to-liquid ratio of 1:20, stirring for 24-72h at 60-90 ℃, cooling to room temperature, then pouring into a centrifuge tube, repeatedly centrifuging for several times by using deionized water until the solution in the centrifuge tube is neutral, separating out an upper-layer solution, putting a sample left at the bottom of the centrifuge tube into a vacuum drying oven for drying, and obtaining solid powder which is a two-dimensional carbide MXene after drying;
(2) preparation of prelithiated MXene: placing a glass sheet, a lithium foil, a two-dimensional carbide MXene, a steel sheet and a glass sheet in sequence from top to bottom; after being placed, the electrolyte LiPF is dripped from the side6Applying certain pressure to the uppermost glass bottle sheet to ensure that the lithium sheet is fully contacted with the electrode plate; after 5-30min of pre-lithiation treatment, removing electrolyte LiPF remained on the surface of MXene which is a two-dimensional carbide by using acetonitrile6And then vacuum drying is carried out to prepare the pre-lithiated MXene.
The reaction is carried out at room temperature, the process method is simple, the cost is low, special process equipment is not needed, and the method is convenient and efficient; the lithium ion entering can not only enlarge MXene interlamellar spacing to the maximum extent and expose more surface active sites, but also increase ion transmission channels and solve the problem of MXene stacking and agglomeration in the circulating process.
According to the invention, a certain pressure is applied to the uppermost glass bottle sheet, so that the lithium sheet is fully contacted with the electrode plate, and the content of the pre-lithiated lithium ions is increased.
Preferably, the MAX phase ceramic powder in step (1) is selected from V2AlC powder, Ti2AlC powder Ti3AlC2One kind of powder.
Preferably, the particle size of the MAX phase ceramic powder in the step (1) is 400-600 meshes.
Preferably, the concentration of the mixed solution of sodium fluoride and hydrochloric acid in the step (1) is 6 mol/L.
Preferably, the vacuum drying temperature in the step (1) is 60-80 ℃.
Preferably, the vacuum drying time in the step (1) is 10-12 h.
The lithium/magnesium battery comprises a positive electrode, a negative electrode and electrolyte, wherein the positive electrode comprises the pre-lithiated MXene prepared by the preparation method.
Further, the preparation method comprises the following steps: mixing pre-lithiated MXene, acetylene black and a binder according to the mass ratio of 8:1:1, adding N-methylpyrrolidone as a solvent, grinding into slurry, uniformly coating, and performing vacuum drying to obtain a pre-lithiated MXene electrode plate; pre-lithiated MXene electrode plate, lithium foil or AZ31Mg plate as negative electrode, and LiPF6Or 0.4mol/L phenylmagnesium chloride and aluminum chloride in tetrahydrofuran solution as electrolyte, and assembling in a glove box to obtain the lithium/magnesium battery.
Further, the binder is 5 wt% PVDF.
Further, the thickness of the coating film is 1-2mg/cm2。
According to the invention, the prepared pre-lithiated MXene is used as an electrode material of the lithium ion battery, so that the loss of lithium ions in the first charging process can be made up, the coulomb efficiency of first charging and discharging is improved, and the storage capacity of the MXene for the lithium ions is improved to a greater extent; the pre-lithiated MXenes is used as an electrode material of a magnesium ion battery, so that magnesium and lithium co-intercalation is realized, and the multiplying power and the cycle performance are improved.
The invention has the following beneficial effects:
1. the reaction is carried out at room temperature, the process method is simple, the cost is low, special process equipment is not needed, and the method is convenient and efficient; the lithium ion entering can not only enlarge MXene interlamellar spacing to the maximum extent and expose more surface active sites, but also increase ion transmission channels and solve the problem of MXene stacking and agglomeration in the circulating process.
2. According to the invention, a certain pressure is applied to the uppermost glass bottle sheet, so that the lithium sheet is fully contacted with the electrode plate, and the content of the pre-lithiated lithium ions is increased.
3. According to the invention, the prepared pre-lithiated MXene is used as an electrode material of the lithium ion battery, so that the loss of lithium ions in the first charging process can be made up, the coulomb efficiency of first charging and discharging is improved, and the storage capacity of the MXene for the lithium ions is improved to a greater extent; the pre-lithiated MXenes is used as an electrode material of a magnesium ion battery, so that magnesium and lithium co-intercalation is realized, and the multiplying power and the cycle performance are improved.
Drawings
FIG. 1 shows MXeneV pre-lithiated for 10min according to example 1 of the present invention2C, scanning electron microscope pictures;
FIG. 2 shows MXeneTi pre-lithiated for 30min according to example 5 of the present invention3C2Cycle performance test results in lithium ion batteries.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Test materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The specific techniques or conditions not specified in the examples can be performed according to the techniques or conditions described in the literature in the field or according to the product specification.
Example 1
Prelithiation MXeneV2C, preparation, comprising the following steps:
(1) the particle size of the mixture was adjusted to 1gV of 500 mesh2Immersing AlC powder in 20mL of mixed solution of hydrochloric acid with the concentration of 6mol/L and sodium fluoride, stirring for 72h at 90 ℃, cooling to room temperature, pouring into a centrifuge tube, repeatedly centrifuging for several times by using deionized water until the solution in the centrifuge tube is neutral, separating out an upper layer solution, putting a sample left at the bottom of the centrifuge tube in a vacuum drying oven, drying for 12h at 80 ℃, and obtaining a two-dimensional crystal compound MXeneV2C；
(2) Prelithiation MXeneV2Preparation of the C sheet: glass sheet, lithium foil and two-dimensional crystal compound MXeneV2C. The steel sheet and the glass sheet are sequentially placed from top to bottom; after being placed, the electrolyte LiPF is dripped from the side6Applying a certain pressure to the uppermost glass bottle sheet to make the lithium foil and the two-dimensional crystal compound MXeneV2C, fully contacting; after prelithiation for 10min, V was removed with acetonitrile2Electrolyte LiPF (lithium ion plasma) remained on surface of C electrode plate6Then dried for 12h in vacuum at 80 ℃ to prepare the pre-lithiated MXeneV2C。
The prelithiated MXeneV prepared in this example2The result of scanning the C plate by an electron microscope is shown in figure 1, and MXeneV after pre-lithiation can be seen2The thickness of the C sheet layer is increased, the surface becomes rough, which shows that after self-discharge, partial lithium ions enter the MXene sheet layers in advance to further increase the interlayer spacing, which is beneficial to Li+And Mg2+Insertion and extraction; meanwhile, a thin SEI film is formed on the surface of the lithium ion battery, so that the loss of lithium ions in the first charging process can be compensated, the coulomb efficiency of first charging and discharging is improved, and the MXeneV is improved to a greater extent2C storage capacity for lithium ions.
Example 2
Prelithiation of MXeneTi3C2The preparation method comprises the following steps:
(1) 1gTi with the grain diameter of 500 meshes3AlC2Immersing the powder into 20mL of mixed solution of hydrochloric acid with the concentration of 6mol/L and sodium fluoride, stirring for 24h at the temperature of 60 ℃, cooling to room temperature, pouring into a centrifuge tube, repeatedly centrifuging for several times by using deionized water until the solution in the centrifuge tube is neutral, separating out an upper layer solution, putting a sample left at the bottom of the centrifuge tube into a vacuum drying oven, drying for 12h at the temperature of 80 ℃ to obtain a two-dimensional crystal compound MXeneTi3C2；
(2) Prelithiation of MXeneTi3C2Preparation of tablets: glass sheet, lithium foil and two-dimensional crystal compound MXeneTi3C2The steel sheet and the glass sheet are sequentially placed from top to bottom; after being placed, the electrolyte LiPF is dripped from the side6Applying a certain pressure to the top glass bottle sheet to make the lithium foil and the two-dimensional crystal compound MXeneTi3C2Fully contacting; after prelithiation for 10min, V was removed with acetonitrile2Electrolyte LiPF (lithium ion plasma) remained on surface of C electrode plate6Then dried for 12h in vacuum at 80 ℃ to prepare the pre-lithiated MXeneTi3C2。
Example 3
Preparation of a lithium ion battery: the pre-lithiated MXeneV prepared in example 1 was weighed in a mass ratio of 8:1:12C. Mixing acetylene black with binder, adding N-methyl pyrrolidone as solvent, grinding into slurry, and uniformly coating with 1mg/cm2Then vacuum drying at 80 deg.C for 12h to obtain pre-lithiated MXene V2C, electrode slice; lithium foil as negative electrode, LiPF6And (4) taking the electrolyte, and assembling the button lithium ion battery in the glove box.
The lithium ion battery assembled in the embodiment is tested for cycle performance under the current density of 50mA/g and the voltage range of 0.01-3.0V; the test result shows that V is subjected to prelithiation for 10min2C, the lithium iron phosphate is used as an electrode material of the ion battery, the first charge-discharge capacity of the lithium iron phosphate is 656mAh/g, and the coulombic efficiency is 75%; compared with MXeneV without pre-lithiation treatment2The first charge-discharge capacity, coulombic efficiency and lithium storage capacity of C are greatly improved, which shows that the pre-lithiation expands MXeneV2The interlayer spacing of C increases the active adsorption sites on the surfaceThe loss of lithium ions in the process of first charging is compensated, the coulomb efficiency of first charging and discharging is improved, and the Li is further improved+The storage capacity of (2).
Example 4
Preparing a magnesium ion battery: prelithiation MXeneV prepared as in example 32The C electrode plate is used as a positive electrode, the magnesium plate is used as a negative electrode, 0.4M tetrahydrofuran solution of phenylmagnesium chloride and aluminum chloride and 0.4M LiCl are used as electrolyte, and the magnesium ion battery is assembled in a glove box.
The lithium ion battery assembled in the embodiment is tested for the cycle performance after 750 times of cycle under the current density of 500mA/g, the discharge capacity after 250 times of cycle is kept at 90mAh/g, and the coulomb efficiency is stabilized at more than 96%.
Example 5
Preparation of a lithium ion battery: the pre-lithiated MXeneTi prepared in example 2 was weighed in a mass ratio of 8:1:13C2Mixing acetylene black and binder, adding N-methyl pyrrolidone as solvent, grinding into slurry, and uniformly coating with 1mg/cm2Then drying the mixture for 12 hours in vacuum at the temperature of 80 ℃ to prepare the pre-lithiated MXeneTi3C2An electrode sheet; lithium foil as negative electrode, LiPF6And the electrolyte is used as the electrolyte, and the lithium ion battery is assembled in the glove box.
The lithium electronic battery assembled in the embodiment is tested to have the cycle performance under the current density of 500mA/g, and the result is shown in figure 2, and the test shows that the discharge capacity after 750 cycles is close to 320mAh/g, the coulombic efficiency is stabilized to be more than 90 percent, and therefore, the pre-lithiation MXeneTi3C2The composite material has excellent cycle stability.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation method of a pre-lithiated MXene material is characterized by comprising the following steps of:
(1) immersing MAX-phase ceramic powder into a mixed solution of sodium fluoride and hydrochloric acid according to a solid-to-liquid ratio of 1:20, stirring for 24-72h at 60-90 ℃, cooling to room temperature, then pouring into a centrifuge tube, repeatedly centrifuging for several times by using deionized water until the solution in the centrifuge tube is neutral, separating out an upper-layer solution, putting a sample left at the bottom of the centrifuge tube into a vacuum drying oven for drying, and obtaining solid powder which is a two-dimensional carbide MXene after drying;
(2) preparation of prelithiated MXene: placing a glass sheet, a lithium foil, a two-dimensional carbide MXene, a steel sheet and a glass sheet in sequence from top to bottom; after being placed, the electrolyte LiPF is dripped from the side6Applying certain pressure to the uppermost glass bottle sheet to ensure that the lithium sheet is fully contacted with the electrode plate; after 5-30min of pre-lithiation treatment, removing electrolyte LiPF remained on the surface of MXene which is a two-dimensional carbide by using acetonitrile6And then vacuum drying is carried out to prepare the pre-lithiated MXene.
2. The method of preparing a pre-lithiated MXene material of claim 1, wherein: in the step (1), the MAX phase ceramic powder is selected from V2AlC powder, Ti2AlC powder Ti3AlC2One kind of powder.
3. The method of preparing a pre-lithiated MXene material of claim 1, wherein: the particle size of the MAX phase ceramic powder in the step (1) is 400-600 meshes.
4. The method of preparing a pre-lithiated MXene material of claim 1, wherein: the concentration of the mixed solution of sodium fluoride and hydrochloric acid in the step (1) is 6 mol/L.
5. The method of preparing a pre-lithiated MXene material of claim 1, wherein: the vacuum drying temperature in the step (1) is 60-80 ℃.
6. The method of preparing a pre-lithiated MXene material of claim 1, wherein: the vacuum drying time in the step (1) is 10-12 h.
7. A lithium/magnesium battery characterized by: the pre-lithiated MXene material comprises a positive electrode, a negative electrode and an electrolyte, wherein the positive electrode comprises the pre-lithiated MXene prepared by the preparation method of the pre-lithiated MXene material according to claim 1.
8. The lithium/magnesium battery of claim 7, prepared by a process comprising the steps of: respectively weighing V according to the mass ratio of 8:1:12Mixing the C powder, acetylene black and a binder, adding N-methyl pyrrolidone serving as a solvent, grinding into slurry, uniformly coating, and performing vacuum drying to obtain a positive electrode material; lithium foil or AZ31Mg sheet is taken as a negative electrode, and LiPF is taken6Or 0.4mol/L phenylmagnesium chloride and aluminum chloride in tetrahydrofuran solution as electrolyte, and assembling in a glove box to obtain the lithium/magnesium battery.
9. A lithium/magnesium battery as claimed in claim 8, wherein: the binder is 5 wt% PVDF.
10. A lithium/magnesium battery as claimed in claim 8, wherein: the thickness of the coating film is 1-2mg/cm2。
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