CN113912027B - MoSe 2 Negative electrode material of/C/rGO composite lithium ion battery, and preparation method and application thereof - Google Patents

MoSe 2 Negative electrode material of/C/rGO composite lithium ion battery, and preparation method and application thereof Download PDF

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CN113912027B
CN113912027B CN202111089993.0A CN202111089993A CN113912027B CN 113912027 B CN113912027 B CN 113912027B CN 202111089993 A CN202111089993 A CN 202111089993A CN 113912027 B CN113912027 B CN 113912027B
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郑成
林芳妃
陈永
韦雅庆
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Hainan University
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Abstract

The invention provides a MoSe 2 Negative electrode material of/C/rGO composite lithium ion battery, preparation method and application thereof, and MoSe 2 the/C/rGO compound takes molybdenum acetylacetonate, o-phenanthroline and graphene oxide as raw materials, and the molybdenum metal organic complex/graphene oxide compound precursor dispersion liquid is generated by reaction, and MoSe is prepared from the precursor dispersion liquid 2 a/C/rGO complex. Compared with similar products, the product obtained by the method has the advantages of simple method, good repeatability and MoSe 2 High dispersity and high rate capability.

Description

MoSe 2 Negative electrode material of/C/rGO composite lithium ion battery, and preparation method and application thereof
Technical Field
The invention relates to MoSe 2 The field of negative electrode materials of base lithium ion batteries, in particular to a MoSe 2 Negative electrode material of/C/rGO composite lithium ion battery, and preparation method and application thereof.
Background
MoSe 2 As a typical two-dimensional material, a special Se-Mo-Se sandwich layer structure is provided, the layers are connected by covalent bonds, and the layers are attracted by Van der Waals force, so that the material has a structure similar to graphite. MoSe, compared to graphite 2 The larger interlayer spacing (about 0.65 nm) is very suitable for intercalation and deintercalation of ions, and is considered as a very promising lithium storage material. However, moSe 2 Poor conductivity, thereby affecting the high rate performance, and volume change during the process of intercalation/deintercalation, so as to lead MoSe to 2 And fall off the current collector, resulting in rapid decay of capacity. The like products generally improve MoSe by constructing porous structures, ultrathin nano layered structures, carbon composite structures and the like 2 The synthesis process of the method is relatively complex, and the high rate performance is not outstanding enough.
Disclosure of Invention
In view of this, the present invention proposes a MoSe 2 The negative electrode material of the/C/rGO composite lithium ion battery and the preparation method and the application thereof overcome the defects of the prior art.
The technical scheme of the invention is realized as follows:
MoSe 2 The preparation method of the negative electrode material of the/C/rGO composite lithium ion battery comprises the following steps:
(1) Dissolving molybdenum acetylacetonate in absolute ethyl alcohol to prepare a solution A, wherein the mol volume ratio mol/L of the molybdenum acetylacetonate to the absolute ethyl alcohol is 0.5:10;
dissolving o-phenanthroline in absolute ethyl alcohol to prepare solution B, wherein the mol volume ratio mol/L of the o-phenanthroline to the absolute ethyl alcohol is 0.5:10;
the mol ratio of the molybdenum acetylacetonate to the o-phenanthroline is 1:1;
adding N, N-dimethylformamide dispersion liquid of graphene oxide into the preparation of the solution A or the solution B; the concentration of graphene oxide in the N, N-dimethylformamide dispersion liquid of the graphene oxide is 1mg/mL, and 2g of graphene oxide is used per mol of molybdenum acetylacetonate.
(2) Dropwise adding the solution B into the solution A or dropwise adding the solution A into the solution B under the condition of intense stirring; and after the dripping is completed, a molybdenum metal organic complex/graphene oxide complex precursor dispersion liquid is generated.
(3) Taking molybdenum metal organic complex/graphene oxide complex precursor dispersion liquid obtained in the step (2), dropwise adding a solution C prepared from selenium powder and hydrazine hydrate under the condition of intense stirring, transferring the product into a polytetrafluoroethylene reaction kettle after the dropwise adding is finished, sealing, performing solvothermal reaction at 160-200 ℃ for 12-24 hours, centrifuging, cleaning and drying the obtained precipitate to obtain a primary product;
(4) Transferring the initial product obtained in the step (3) to a reaction vessel containing H 2 Calcining and reacting for 2h in a tube furnace with Ar mixed atmosphere at 600-700 ℃ to obtain the final product MoSe 2 /C/rGO。
Further, moSe 2 When the/C/rGO compound is applied to a lithium ion battery anode material, mo is added into the compositeSe 2 the/C/rGO compound, acetylene black and sodium alginate are mixed and ground according to the mass ratio of 7:2:1, dispersed in water, and then uniformly coated on copper foil to serve as a working electrode.
Compared with the prior art, the invention has the beneficial effects that:
(1) The method takes molybdenum acetylacetonate, o-phenanthroline and graphene oxide as raw materials to prepare and generate molybdenum metal organic complex/graphene oxide complex precursors, thereby synthesizing MoSe 2 a/C/rGO composite. Compared with similar products, the product obtained by the method has the advantages of simple method, good repeatability and MoSe 2 High dispersity and high rate capability.
(2) The invention has high repeatability and simple process, and MoO after solvothermal and calcination reactions 2 Mo element in (acac) (phen) is selenized into MoSe 2 While the organic component is converted to semi-graphitized carbon (C), both of which are in situ converted, can form MoSe 2 With C, such a structure can effectively suppress MoSe 2 The volume change in the charge and discharge process prevents the material from falling off the rGO surface, thereby improving the circulation stability. In addition, the presence of rGO is beneficial to improve the conductivity of the material, thereby improving high current performance.
Drawings
FIG. 1 MoSe of example 1 2 X-ray powder diffraction pattern of/C/rGO.
FIG. 2 MoSe of example 1 2 Scanning electron microscope photograph of/C/rGO.
FIG. 3 MoSe of example 1 2 Transmission electron microscope photograph of/C/rGO.
FIG. 4 shows the rate performance of the sample obtained in example 1 at different current densities.
Fig. 5 shows the rate performance of the samples obtained in example 2 at different current densities.
FIG. 6 shows the rate performance of the samples obtained in example 3 at different current densities.
FIG. 7 is a scanning electron micrograph of the product of comparative example 1.
Detailed Description
In order to better understand the technical content of the present invention, the following provides specific examples to further illustrate the present invention.
The experimental methods used in the embodiment of the invention are conventional methods unless otherwise specified.
Materials, reagents, and the like used in the examples of the present invention are commercially available unless otherwise specified.
The present invention is not intended to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Example 1
MoSe 2 Preparation of the/C/rGO complex:
(1) Molybdenum acetylacetonate 0.5mmol is taken and dissolved in 10mL absolute ethanol, and 10mL of N, N-dimethylformamide dispersion of Graphene Oxide (GO) with the concentration of 1mg/mL is added, and the solution A is prepared after full stirring. Dissolving 0.5mmol of o-phenanthroline in 10mL of absolute ethyl alcohol to prepare solution B.
(2) Dropwise adding the solution B into the solution A under the condition of intense stirring, and generating molybdenum metal organic complex/graphene oxide complex precursor (MoO) after the dropwise adding is completed 2 (acac) (phen)/GO) dispersion.
(3) Then dropwise adding a solution C prepared from 2mmol of selenium powder and 10mL of hydrazine hydrate under the condition of vigorously stirring the dispersion liquid, transferring the product into a polytetrafluoroethylene reaction kettle after the dropwise adding, sealing, performing solvothermal reaction for 24 hours at 160 ℃, repeatedly washing the obtained precipitate for 3 times through centrifugation and ethanol cleaning, and drying to obtain a primary product;
(4) The initial product is then transferred to a reaction vessel containing H 2 Calcining in a tube furnace with Ar mixed atmosphere (volume ratio of 5:95) at 650 ℃ for 2h.
MoO after solvothermal and calcination reactions 2 Mo element in (acac) (phen) is selenized in situ to MoSe 2 While the organic component is in situ converted to semi-graphitized carbon (C) and GO is reduced to reduced graphene oxide (rGO) to give the final product MoSe 2 a/C/rGO complex.
FIG. 1 is a schematic view ofThe X-ray powder diffraction spectrum of the obtained product is characterized in that the peak at about 26 degrees is attributed to the (002) crystal face of the reduced graphene oxide (rGO) skeleton, the peak packet at 23-29 degrees is mainly attributed to semi-graphitized carbon, and the rest of diffraction peaks are attributed to MoSe 2 . Indicating that the synthesized product is MoSe 2 A complex of semi-graphitized carbon (C) and rGO.
Fig. 2 is a scanning electron micrograph of the resulting product, which is seen to be flaky, mainly due to the presence of rGO forming a skeleton, with other components uniformly grown on the rGO skeleton surface.
FIG. 3 is a transmission electron micrograph of the resulting product, in which lamellar MoSe is observed 2 (002) crystal face of (a) and MoSe 2 The number of layers is less, most 2-3 layers, and a small number is 5-6 layers. Furthermore, no significant lattice fringes corresponding to the semi-graphitized carbon (C) were observed in the hatched portion. The whole large-scale lamellar structure is rGO, while MoSe 2 And semi-graphitized carbon is uniformly dispersed on the rGO framework.
The MoSe obtained above is subjected to 2 Mixing and grinding the/C/rGO compound, acetylene black and sodium alginate according to the mass ratio of 7:2:1, dispersing in water, uniformly coating on copper foil to obtain working electrodes, wherein the reference electrode and the counter electrode are both metallic lithium, and the electrolyte is 1M LiPF6 Ethylene Carbonate (EC) +dimethyl carbonate (DMC) +methylethyl carbonate (EMC) solution, wherein the EC, DMC, EMC volume ratio is 1:1:1, clegard 2500 microporous membrane as separator and CR2025 button cell as test carrier (all assembly was performed in glove box with inert atmosphere protection).
Fig. 4 is a graph showing the rate performance of the sample at different current densities, and it can be seen that the obtained sample shows a lithium storage capacity of 740mAh/g at a current density of 0.1A/g, and can still show a lithium storage capacity of 416mAh/g even at an ultra-large current density of 10A/g, and the current density is reduced after a large current cycle, and the capacity can still be recovered. Visible MoSe 2 the/C/rGO complex exhibits high reversible capacity and high rate capability.
Example 2
On the basis of example 1, the other conditions were unchanged, and solution a was not added to the N, N-dimethylformamide dispersion of Graphene Oxide (GO) but instead to solution B. The method comprises the following steps:
(1) Dissolving 0.5mmol of molybdenum acetylacetonate in 10mL of absolute ethyl alcohol, and stirring to prepare solution A;
dissolving 0.5mmol of o-phenanthroline in 10mL of absolute ethyl alcohol, adding 10mL of N, N-dimethylformamide dispersion liquid of graphene oxide with the concentration of 1mg/mL, and stirring to prepare a solution B;
(2) Dropwise adding the solution B into the solution A under the condition of intense stirring, and generating molybdenum metal organic complex/graphene oxide complex precursor (MoO) after the dropwise adding is completed 2 (acac) (phen)/GO) dispersion.
(3) And then dropwise adding a solution C prepared from 2mmol of selenium powder and 10mL of hydrazine hydrate under the condition of vigorously stirring the dispersion liquid, transferring the product into a polytetrafluoroethylene reaction kettle after the dropwise adding, sealing, performing solvothermal reaction for 24 hours at 160 ℃, repeatedly washing the obtained precipitate for 3 times through centrifugation and ethanol cleaning, and drying to obtain a primary product.
(4) The initial product is then transferred to a reaction vessel containing H 2 Calcining in a tube furnace with Ar mixed atmosphere (volume ratio of 5:95) at 650 ℃ for 2h.
The results showed that the samples of this example, which were tested for electrochemical performance by the same procedure as in example 1, exhibited a lithium storage capacity of 790mAh/g at a current density of 0.1A/g and a lithium storage capacity of 350mAh/g at an ultra-high current density of 10A/g, as shown in FIG. 5. The sample obtained in this example has a slightly higher discharge capacity than the sample obtained in example 1 at a smaller electrical density and a slightly lower reversible capacity than the sample obtained in example 1 at an ultra-high current density.
Example 3
Based on example 2, the calcination reaction temperature was adjusted to 600℃for 2 hours. The method comprises the following steps:
(1) Dissolving 0.5mmol of molybdenum acetylacetonate in 10mL of absolute ethyl alcohol, and stirring to prepare solution A;
dissolving 0.5mmol of o-phenanthroline in 10mL of absolute ethyl alcohol, adding 10mL of N, N-dimethylformamide dispersion liquid of graphene oxide with the concentration of 1mg/mL, and stirring to prepare a solution B;
(2) Dropwise adding the solution A into the solution B under the condition of intense stirring, and generating molybdenum metal organic complex/graphene oxide complex precursor (MoO) after the dropwise addition is completed 2 (acac) (phen)/GO) dispersion.
(3) And then dropwise adding a solution C prepared from 2mmol of selenium powder and 10mL of hydrazine hydrate under the condition of vigorously stirring the dispersion liquid, transferring the product into a polytetrafluoroethylene reaction kettle after the dropwise adding, sealing, carrying out solvothermal reaction for 12 hours at 200 ℃, and repeatedly washing the obtained precipitate for 3 times through centrifugation and ethanol cleaning, and then drying to obtain a primary product.
(4) The initial product is then transferred to a reaction vessel containing H 2 Calcining in a tube furnace with Ar mixed atmosphere (volume ratio of 5:95) at 600 ℃ for 2h.
The results showed that the samples of this example, which were tested for electrochemical performance by the same procedure as in example 1, exhibited a lithium storage capacity of 710mAh/g at a current density of 0.1A/g and a lithium storage capacity of 388mAh/g at an ultra-high current density of 10A/g, as shown in FIG. 6. This example had slightly lower reversible capacity than the sample of example 1 at both lower electrical densities and at ultra-high current densities.
Comparative example 1
Based on the embodiment 1, molybdenum acetylacetonate is replaced by ammonium molybdate, and o-phenanthroline ligand is not used. The results showed that MoSe in the resulting samples 2 Is not well dispersed on rGO surface, a large amount of MoSe 2 Agglomerated into particles and scattered outside rGO (as shown in fig. 5), not meeting the intended target of the design.

Claims (4)

1. MoSe 2 The negative electrode material of the/C/rGO composite lithium ion battery is characterized in that molybdenum acetylacetonate, o-phenanthroline and graphene oxide are taken as raw materials to react to generate molybdenum metal organic complex/graphene oxide complex precursor dispersion liquid, and MoSe is prepared from the precursor dispersion liquid 2 a/C/rGO complex;
the preparation method of the molybdenum metal organic complex/graphene oxide complex precursor dispersion liquid comprises the following steps:
(1) Dissolving molybdenum acetylacetonate in absolute ethyl alcohol to prepare a solution A;
dissolving o-phenanthroline in absolute ethyl alcohol to prepare a solution B;
adding N, N-dimethylformamide dispersion liquid of graphene oxide into the preparation of the solution A or the solution B;
(2) Dropwise adding the solution B into the solution A or dropwise adding the solution A into the solution B under the condition of intense stirring;
after the dripping is completed, molybdenum metal organic complex/graphene oxide complex precursor dispersion liquid is generated;
(3) Taking molybdenum metal organic complex/graphene oxide complex precursor dispersion liquid obtained in the step (2), dropwise adding a solution C prepared from selenium powder and hydrazine hydrate under the condition of intense stirring, transferring the product into a polytetrafluoroethylene reaction kettle after the dropwise adding, sealing, performing solvothermal reaction at 160-200 ℃ for 12-24 hours, centrifuging, cleaning and drying the obtained precipitate to obtain a primary product, and calcining to obtain a final product MoSe 2 /C/rGO。
2. MoSe according to claim 1 2 The negative electrode material of the/C/rGO composite lithium ion battery is characterized in that in the step (1), the mol volume ratio mol/L of the molybdenum acetylacetonate and the absolute ethyl alcohol is 0.5:10; the mol volume ratio mol/L of the o-phenanthroline to the absolute ethyl alcohol is 0.5:10.
3. MoSe according to claim 1 2 The negative electrode material of the/C/rGO composite lithium ion battery is characterized in that in the step (1), the mol ratio of the molybdenum acetylacetonate to the o-phenanthroline is 1:1.
4. MoSe according to claim 1 2 The negative electrode material of the/C/rGO composite lithium ion battery is characterized in that in the step (1), the concentration of graphene oxide in N, N-dimethylformamide dispersion liquid of the graphene oxide is 1mg/mL, and 2g of graphene oxide is used per mol of molybdenum acetylacetonate.
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