CN113948703B - MoSe used as lithium ion battery cathode 2 /NC submicron sphere composite material - Google Patents

MoSe used as lithium ion battery cathode 2 /NC submicron sphere composite material Download PDF

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CN113948703B
CN113948703B CN202111201238.7A CN202111201238A CN113948703B CN 113948703 B CN113948703 B CN 113948703B CN 202111201238 A CN202111201238 A CN 202111201238A CN 113948703 B CN113948703 B CN 113948703B
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mose
composite material
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CN113948703A (en
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郑成
林芳妃
陈永
韦雅庆
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Hainan University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
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    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

The invention relates toAnd the technical field of lithium ion battery cathodes, in particular to MoSe used as a lithium ion battery cathode 2 The preparation method of the/NC submicron sphere composite material comprises the following steps: s1, dissolving 0.3-0.7 mmol of molybdenum acetylacetonate in 10mL of absolute ethyl alcohol, and fully stirring to prepare a solution A; s2, dissolving 0.4-0.6 mmol of o-phenanthroline in 10mL of absolute ethanol to prepare a solution B; the MoSe is synthesized by taking molybdenum acetylacetonate and o-phenanthroline as raw materials through a solvothermal method and a subsequent calcining method 2 the/NC submicron sphere composite material. Compared with the similar products, the product obtained by the method has the advantages of simple method, high repeatability and MoSe 2 High dispersity, less layers and high cyclic stability.

Description

MoSe used as lithium ion battery cathode 2 NC submicron sphere composite material
Technical Field
The invention relates to the technical field of lithium ion battery cathodes, in particular to MoSe serving as a lithium ion battery cathode 2 the/NC submicron sphere composite material.
Background
MoSe 2 As a typical two-dimensional material, the material has a special Se-Mo-Se sandwich layered structure, the layers are connected by covalent bonds inside, and the layers are mutually attracted by Van der Waals force, and the material has a structure similar to graphite. MoSe compared with graphite 2 The interlayer spacing is larger (about 0.65 nm), is very suitable for the intercalation and deintercalation of ions, and is considered as a promising lithium storage material. However, moSe 2 The conductivity of the material is poor, thereby affecting the performance of large multiplying power, and in addition, the volume change can occur in the process of lithium intercalation/deintercalation, so that MoSe can be obtained 2 Fall off the current collector, resulting in a rapid decay of capacity. The similar products usually improve MoSe by constructing a porous structure, an ultrathin nano-layered structure, a carbon composite structure and the like 2 The electrochemical performance of (2) is relatively complex, and the repeatability is not high.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides MoSe serving as a negative electrode of a lithium ion battery 2 the/NC submicron sphere composite material.
In order to achieve the purpose, the invention adopts the following technical scheme:
MoSe used as lithium ion battery cathode 2 The preparation method of the/NC submicron sphere composite material comprises the following steps:
s1, dissolving 0.3-0.7 mmol of molybdenum acetylacetonate in 10mL of absolute ethyl alcohol, and fully stirring to prepare a solution A;
s2, dissolving 0.4-0.6 mmol of o-phenanthroline in 10mL of absolute ethanol to prepare a solution B;
s3, dropwise adding the solution B into the solution A under the condition of vigorous stirring, and generating a molybdenum metal organic complex precursor dispersion liquid after dropwise adding is completed;
s4, then dropwise adding a solution C prepared from 1.5-2.5 mmol of selenium powder and 10mL of hydrazine hydrate under the condition of vigorous stirring, transferring the product into a polytetrafluoroethylene reaction kettle after dropwise adding is finished, carrying out solvothermal reaction for 18-32H at 155-165 ℃ after sealing, drying the obtained precipitate after repeatedly washing for 3-5 times by centrifugation and ethanol cleaning, and then transferring the precipitate to a container containing H 2 Calcining for 1.5-2.5 h in a tubular furnace with a mixed Ar atmosphere at the temperature of 630-660 ℃;
s5, after solvothermal and calcination reactions, in-situ selenizing Mo in the precursor dispersion liquid into MoSe 2 And the organic component is converted into nitrogen-doped carbon in situ to finally generate MoSe 2 /NC submicron sphere composite material.
Preferably, in the step S3, the dropping speed is 10 to 60 drops/min; in the step S4, the dripping speed is 20-60 drops/min.
Preferably, in the S3, the temperature is 20-40 ℃ in the dropping process; in the S4, the temperature is 20-50 ℃ in the dropping process.
Preferably, the composite material is a solid sphere with the diameter of 80-120 nanometers, and flaky substances are arranged on the surface of the solid sphere.
The invention has the beneficial effects that: the MoSe is synthesized by taking molybdenum acetylacetonate and o-phenanthroline as raw materials through a solvothermal method and a subsequent calcining method 2 a/NC composite material. Compared with the similar products, the product obtained by the method has the advantages of simple method, high repeatability and MoSe 2 High dispersity, few layers,the circulation stability is good.
Drawings
FIG. 1 shows MoSe according to the present invention 2 The X-ray powder diffraction pattern of the/NC submicron sphere composite material;
FIG. 2 shows MoSe according to the present invention 2 A transmission electron microscope photo of the/NC submicron sphere composite material;
FIG. 3 shows MoSe according to the present invention 2 A high-resolution transmission electron microscope photo of the NC submicron sphere composite material;
FIG. 4 is an elemental distribution diagram of a MoSe2/NC submicron sphere composite material according to the present invention;
FIG. 5 shows the present invention in terms of MoSe 2 A cycle performance diagram of the/NC submicron sphere composite material under the current density of 5A/g.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
In example 1, a MoSe cathode for a lithium ion battery 2 The preparation method of the/NC submicron sphere composite material comprises the following steps:
s1, dissolving 0.3mmol of molybdenum acetylacetonate in 10mL of absolute ethyl alcohol, and fully stirring to prepare a solution A;
s2, dissolving 0.4mmol of o-phenanthroline in 10mL of absolute ethyl alcohol to prepare a solution B;
s3, dropwise adding the solution B into the solution A under the condition of vigorous stirring, and generating a molybdenum metal organic complex precursor dispersion liquid after dropwise adding is completed;
s4, then dropwise adding a solution C prepared from 1.5mmol of selenium powder and 10mL of hydrazine hydrate under the condition of vigorous stirring, transferring the product to a polytetrafluoroethylene reaction kettle after dropwise adding, carrying out solvothermal reaction for 18H at 155 ℃ after sealing, repeatedly washing the obtained precipitate for 3 times by centrifugation and ethanol cleaning, drying, and then transferring the precipitate to a reaction kettle containing H 2 Calcining at 630 ℃ in a tubular furnace with/Ar mixed atmosphere1.5h；
S5, after solvothermal and calcination reactions, in-situ selenizing Mo in the precursor dispersion liquid into MoSe 2 And the organic component is converted into nitrogen-doped carbon, moSe, in situ 2 /NC submicron sphere composite material.
Further, in the step S3, the dropping speed is 10 drops/min; in the step S4, the dropping speed is 20 drops/min.
Further, in the S3, the temperature is 20 ℃ in the dropping process; in the S4, the temperature is 20 ℃ in the dropping process.
Further, in said S4, H 2 Volume ratio to Ar was 5.
Furthermore, the composite material is a solid sphere with the diameter of 80-120 nanometers, and flaky substances are arranged on the surface of the solid sphere.
Further, the obtained MoSe 2 the/NC submicron sphere composite material, acetylene black and sodium alginate are mixed and ground according to the mass ratio of 7.
In example 2, example 1, a MoSe for use as a negative electrode in a lithium ion battery 2 The preparation method of the/NC submicron sphere composite material comprises the following steps:
s1, dissolving 0.7mmol of molybdenum acetylacetonate in 10mL of absolute ethanol, and fully stirring to prepare a solution A;
s2, dissolving 0.6mmol of o-phenanthroline in 10mL of absolute ethyl alcohol to prepare a solution B;
s3, dropwise adding the solution B into the solution A under the condition of vigorous stirring, and generating a molybdenum metal organic complex precursor dispersion liquid after dropwise adding is completed;
s4, then dropwise adding a solution C prepared from 2.5mmol of selenium powder and 10mL of hydrazine hydrate under the condition of vigorous stirring, transferring the product to a polytetrafluoroethylene reaction kettle after dropwise adding is finished, carrying out solvothermal reaction for 32 hours at 165 ℃ after sealing, drying the obtained precipitate after 5 times of repeated washing through centrifugation and ethanol cleaning, and then transferring the precipitate to a container containing H 2 Calcining for 2.5 hours in a tubular furnace with a mixed Ar atmosphere at 660 ℃;
s5, after solvothermal and calcination reactions, in-situ selenizing Mo in the precursor dispersion liquid into MoSe 2 While the organic component is converted in situ to nitrogen-doped carbon, moSe 2 the/NC submicron sphere composite material.
Further, in the step S3, the dropping speed is 60 drops/min; in the step S4, the dropping speed is 60 drops/min.
Further, in the S3, the temperature is 40 ℃ in the dropping process; in the S4, the temperature is 50 ℃ in the dropping process.
Further, in said S4, H 2 Volume ratio to Ar was 5.
Furthermore, the composite material is a solid sphere with the diameter of 80-120 nanometers, and flaky substances are arranged on the surface of the solid sphere.
Subjecting the obtained MoSe to a thermal treatment 2 the/NC submicron sphere composite material, acetylene black and sodium alginate are mixed and ground according to the mass ratio of 7.
Example 3, example 1, a MoSe for use as a negative electrode in a lithium ion battery 2 The preparation method of the/NC submicron sphere composite material comprises the following steps:
s1, dissolving 0.5mmol of molybdenum acetylacetonate in 10mL of absolute ethyl alcohol, and fully stirring to prepare a solution A;
s2, dissolving 0.5mmol of o-phenanthroline in 10mL of absolute ethanol to prepare a solution B;
s3, dropwise adding the solution B into the solution A under the condition of vigorous stirring, and generating a molybdenum metal organic complex precursor dispersion liquid after dropwise adding is completed;
s4, then dropwise adding a solution C prepared from 2mmol of selenium powder and 10mL of hydrazine hydrate under the condition of vigorous stirring, transferring the product to a polytetrafluoroethylene reaction kettle after dropwise adding is finished, carrying out solvothermal reaction for 24 hours at 160 ℃ after sealing, washing the obtained precipitate repeatedly for 3 times by centrifugation and ethanol cleaning, drying, and then transferring the precipitate to a container containing H 2 Calcining for 2 hours in a tubular furnace with an Ar mixed atmosphere at 650 ℃;
s5, after solvothermal and calcination reactions, in-situ selenizing Mo in the precursor dispersion liquid into MoSe 2 And the organic component is converted into nitrogen-doped carbon, moSe, in situ 2 the/NC submicron sphere composite material.
Further, in the step S3, the dropping speed is 10-60 drops/min; in the step S4, the dripping speed is 20-60 drops/min.
Further, in the S3, the temperature is 30 ℃ in the dropping process; in the S4, the temperature is 30 ℃ in the dropping process.
Further, in said S4, H 2 Volume ratio to Ar was 5.
Furthermore, the composite material is a solid sphere with the diameter of 80-120 nanometers, and flaky substances are arranged on the surface of the solid sphere.
Further, the obtained MoSe 2 the/NC submicron sphere composite material, acetylene black and sodium alginate are mixed and ground according to the mass ratio of 7.
The following characterization is representative of example 3:
FIG. 1 shows the MoSe obtained 2 X-ray powder diffraction pattern of/NC submicron sphere composite material, peak position and pure MoSe 2 The standard spectrum is matched to prove MoSe 2 MoSe in/NC submicron sphere compound 2 . In addition, the peak intensity of the MoSe2/NC complex was found to be low, indicating that MoSe is present 2 MoSe in/NC submicron sphere compound 2 Lower crystallinity and smaller size particles due to the presence of carbon limiting the MoSe 2 And (4) growing crystal grains. It is worth mentioning that the MoSe corresponds to the MoSe at about 13.7 DEG 2 (002) Diffraction signals of crystal faces are obviously weakened and almost disappear, and obviously deviate to a low angle, so that the number of stacked layers of a sample is small, and the interlayer distance is increased.
Fig. 2 is a transmission electron micrograph of the obtained product, which shows that the obtained product is a solid sphere with a diameter of about 100 nm, and a small amount of flaky substances are arranged on the surface of the solid sphere.
FIG. 3 shows MoSe 2 The high-resolution transmission electron microscope photo of NC for one submicron sphere can observe a large amount of layered MoSe 2 (002) crystal face of (A), uniformly distributed throughout the submicron sphere, and MoSe 2 The number of layers (A) is smaller, and most of the layers are not more than 5, which is consistent with the result shown in FIG. 1.
FIG. 4 shows MoSe 2 The element distribution diagram of/NC shows that four elements of Mo, se, C and N in the sample are uniformly distributed in submicron spheres, and the existence of the elements of C and N indicates the generation of nitrogen-doped carbon. The homogeneous distribution of several elements indicates MoSe 2 The nano-sheets are uniformly dispersed on a framework formed by nitrogen-doped carbon.
Subjecting the obtained MoSe to a thermal treatment 2 the/NC submicron sphere compound, acetylene black and sodium alginate are mixed and ground according to the mass ratio of 7 6 EC + DMC + EMC (volume ratio: EC/DMC/EMC = 1/1/1) solution, clegard 2500 microporous membrane as separator and CR2025 type button cell as test vehicle (all assembly was carried out in a glove box with inert atmosphere protection). FIG. 5 is a graph of the cycling performance of the composite at a large current density of 5A/g (the first 10 cycles are activated at 0.5A/g), the capacity is not attenuated during the cycling, the lithium storage capacity of 476mAh/g can be still displayed after 200 cycles, and the MoSe2/NC submicron sphere composite can display higher reversible capacity and good cycling stability.
In examples 1 to 3, moO of the invention 2 The components of the (acac) (phen) metal organic complex precursor are determined, and the components do not change along with the input amount between raw materials of molybdenum acetylacetonate and o-phenanthroline, so that the fault tolerance rate is high during material input, the repeatability is high, and the process is simple. After solvothermal and calcination reactions, moO 2 The Mo element in (acac) (phen) is selenized into MoSe 2 And the organic component is converted to semi-graphitized carbon (C), both of which are in situ conversions that can form MoSe 2 Coating structure with NC can effectively inhibit MoSe 2 The volume change in the charging and discharging process improves the cycle life. In addition, the invention isObtaining MoSe in the sample 2 Small particles, few layers and uniform distribution, is beneficial to exposing active sites and improving reversible capacity. The existence of nitrogen-doped carbon is beneficial to improving the conductivity, thereby improving the large-current performance.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (2)

1. MoSe used as lithium ion battery cathode 2 The preparation method of the/NC submicron sphere composite material is characterized by comprising the following steps:
s1, dissolving 0.3-0.7 mmol of molybdenum acetylacetonate in 10mL of absolute ethyl alcohol, and fully stirring to prepare a solution A;
s2, dissolving 0.4-0.6 mmol of o-phenanthroline in 10mL of absolute ethanol to prepare a solution B;
s3, dropwise adding the solution B into the solution A under the condition of vigorous stirring, wherein the dropwise adding speed is 10-60 drops/min, the temperature is 20-40 ℃ in the dropwise adding process, and a molybdenum metal organic complex precursor dispersion liquid is generated after the dropwise adding is completed;
s4, then dropwise adding a solution C prepared from 1.5-2.5 mmol of selenium powder and 10mL of hydrazine hydrate under the condition of vigorous stirring, wherein the dropping speed is 20-60 drops/min, the temperature is 20-50 ℃ in the dropping process, transferring the product into a polytetrafluoroethylene reaction kettle after the dropping is finished, carrying out solvothermal reaction for 18-32H at the temperature of 155-165 ℃ after sealing, repeatedly washing the obtained precipitate for 3-5 times by centrifugation and ethanol, drying, and then transferring the precipitate to a reaction kettle containing H 2 Calcining for 1.5-2.5 h in a tubular furnace with a/Ar mixed atmosphere at the temperature of 630-660 ℃;
s5, after solvothermal and calcination reactions, in-situ selenizing Mo in the precursor dispersion liquid into MoSe 2 And the organic component is converted into nitrogen-doped carbon in situ to finally generate MoSe 2 the/NC submicron sphere composite material.
2. The MoSe of claim 1 used as a negative electrode of a lithium ion battery 2 the/NC submicron sphere composite material is characterized in that the composite material is a solid sphere with the diameter of 80-120 nanometers, and flaky substances are arranged on the surface of the solid sphere.
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CN105914374A (en) * 2016-05-31 2016-08-31 浙江大学 Nitrogen-doped carbon-coated molybdenum selenide/graphene core-shell array sandwich structure composite material, preparation method and application thereof

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