CN114956214A - Nickel disulfide cross nanoflower material and preparation method and application thereof - Google Patents

Nickel disulfide cross nanoflower material and preparation method and application thereof Download PDF

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Publication number
CN114956214A
CN114956214A CN202210590700.5A CN202210590700A CN114956214A CN 114956214 A CN114956214 A CN 114956214A CN 202210590700 A CN202210590700 A CN 202210590700A CN 114956214 A CN114956214 A CN 114956214A
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China
Prior art keywords
nanoflower
nickel
nickel disulfide
nanoflower material
crossed
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CN202210590700.5A
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Chinese (zh)
Inventor
闵永刚
成伟翔
刘屹东
邱文俊
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Huimai Material Technology Guangdong Co ltd
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Huimai Material Technology Guangdong Co ltd
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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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • 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
    • H01M4/581—Chalcogenides or intercalation compounds thereof
    • H01M4/5815—Sulfides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/11—Sulfides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention belongs to the field of lithium ion battery electrode materials, and discloses a nickel disulfide crossed nanoflower material, and a preparation method and application thereof. The material is prepared by a simple one-step hydrothermal method. The nickel disulfide cross nanoflower material has a very large specific surface area. When the lithium ion battery negative electrode is applied to a lithium ion battery negative electrode, more lithium ions can be loaded, and the battery capacity is improved. In addition, the unique flower-shaped structure can improve the mobility of electrons and ions in the charging and discharging process, thereby improving the cycle performance and rate capability of the battery; in addition, the material can prevent the occurrence of byproducts, and the flower-like structure thereof can improve the mechanical properties of the battery by accommodating volume contraction and expansion during cycling.

Description

Nickel disulfide cross nanoflower material and preparation method and application thereof
Technical Field
The invention belongs to the technical field of novel energy materials, and particularly relates to a preparation method of a nickel disulfide crossed nanoflower material and application of the nickel disulfide crossed nanoflower material in a lithium ion battery.
Background
Lithium ion batteries, one of the best green/clean energy sources, have been in widespread practical use in many fields such as mobile phones, notebook computers, airplane models, electric tools, and the like over the last 30 years. However, the relatively low energy density of batteries (almost <280Wh/kg) has limited their use in the field of electric vehicles, which are currently under vigorous development worldwide. The lack of suitable anode materials limits the applications of lithium ion batteries. Among many non-carbon negative electrode materials, metal sulfides have a high capacity, and are considered as the most promising ideal negative electrode material for lithium ion batteries and have been widely noticed and studied. However, the conductive property is poor, and the electrode is easily crushed due to large volume expansion in the circulation process. At present, the research focuses on a reasonably designed nano-structure material, and the volume change of the metal sulfide material can be effectively relieved to a certain extent.
Disclosure of Invention
In order to solve the defects existing in the prior art, the primary object of the present invention is to provide a nickel disulfide crossed nano-flower material, wherein the unique crossed flower-like structure of the material has a larger specific surface area, so that the material has a very high capacity, and the unique flower-like structure can effectively alleviate the volume change existing in the lithium intercalation/deintercalation process, and can effectively enhance the cycle performance and rate performance of the material in a lithium ion battery.
The invention also aims to provide a preparation method of the nickel disulfide crossed nanoflower material, which is simple, low in cost, high in yield and suitable for small-batch production.
The invention further aims to provide application of the nickel disulfide crossed nanoflower material.
The purpose of the invention is realized by the following modes:
the nickel disulfide cross nanoflower material is characterized in that the nickel disulfide cross nanoflower material is in a cross nanoflower-shaped structure, and raw materials required for synthesis are as follows: the molar mass ratio of the nickel chloride hexahydrate to the vulcanizing agent is 1: 4.
preferably, the sulfurizing agent is L-cysteine.
A method for preparing a nickel disulfide crossed nanoflower material comprises the following steps:
s1: 1mmol of nickel chloride hexahydrate (NiCl) was weighed 2 ·6H 2 O) is poured into 30ml of deionized water and stirred until the nickel chloride hexahydrate is completely dissolved;
s2: weighing 1mmol of urea, adding the urea into the deionized water in which the nickel chloride hexahydrate is dissolved in the S1, and stirring until the urea is completely dissolved;
s3: weighing 4mmol of L-cysteine, adding the L-cysteine into the solution obtained after the operation of S2, and stirring until the L-cysteine is completely dissolved;
s4: adding 50ml of deionized water into the solution treated in the step S3, and then ultrasonically cleaning for 1h in an ultrasonic cleaning machine;
s5: adding the solution treated in the step S4 into a high-temperature high-pressure reaction kettle with a 100ml polytetrafluoroethylene lining, and reacting for 24 hours at 200 ℃;
s6: centrifuging the solution generated after the step S5 in a centrifuge for a period of time, and washing 6 times with deionized water (30mL) and ethanol (30 mL);
s7: and (3) drying the precipitate obtained after the step S6 in a vacuum oven at 60 ℃ for 24 hours to obtain the product of the nickel disulfide cross nanoflower.
Preferably, the molar mass ratio of the weighed nickel chloride hexahydrate to the vulcanizing agent L-cysteine is 1: 4; the step S1 is carried out for 2-3 min by magnetic stirring; the step S2 is carried out for 2-3 min by magnetic stirring; the step S3 is that the magnetic stirring time is 5-10 min; the hydrothermal reaction temperature is 200 ℃, and the reaction time is 24 hours; and the rotating speed and the time of the S6 centrifugal treatment are 4000-4500 r/min and 5-10 min respectively.
Preferably, the nickel disulfide cross nanoflower material has large capacity of loading lithium ions, low cost and convenient manufacture, and can be applied to next-generation energy density lithium ion batteries in a large scale. An application of a nickel disulfide cross nanoflower material in the field of lithium ion battery cathode materials.
Compared with the prior art, the invention has the following beneficial effects:
1. when the nickel disulfide cross nanoflower is used for a lithium ion battery cathode, the nickel disulfide cross nanoflower has extremely high capacity, cycle performance and rate performance; and the unique flower-like structure can prevent the occurrence of byproducts, and the flower-like structure can also improve the mechanical property of the lithium ion battery by adapting to volume contraction and expansion in the circulating process.
2. The invention has simple manufacturing method, low cost and high yield and is suitable for batch production.
Drawings
Figure 1 is an SEM image of nickel disulfide crossed nanoflower material.
Figure 2 is a comparison of the cycling performance of an example of nickel disulfide interdigitated nanoflower material with a comparative example.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited thereto. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art. The practice, methods and apparatus of the present invention are those conventional in the art, except as otherwise indicated.
Example 1
Step 1, adding NiCl 2 ·6H 2 O、CH 4 N 2 O、HSCH 2 CH(NH 2 )CO 2 H is represented by 1: after mixing according to the stoichiometric ratio of 1:4, stirring for 5min by magnetic force to completely melt the mixture in 20ml of deionized water;
step 2, adding 50ml of deionized water into the solution obtained in the step 1, and ultrasonically cleaning for 1 h;
step 3, pouring the solution obtained in the step 2 into a high-temperature high-pressure reaction kettle with a 100ml polytetrafluoroethylene lining, and reacting for 24 hours at 200 ℃;
step 4, when the solution reacted in the step 3 is cooled to room temperature, centrifuging for 5min at the speed of 4000 r/min;
step 5, washing the solution after centrifugation for 3 times by using 30ml of deionized water, and then washing for three times by using 30ml of ethanol solution;
step 6, putting the precipitate washed in the step 5 into a vacuum drying oven at 60 ℃ for drying for 24 hours to obtain a nickel disulfide crossed nano flower material;
and 7, mixing the nickel disulfide crossed nanoflower material obtained in the 6 processes, SP and PVDF according to the ratio of 75: 15: 10, adding NMP, mixing, coating the obtained electrode slurry on a copper foil with the thickness of 100 microns, carrying out vacuum drying at 60 ℃ for a whole night, taking out, and cutting into a negative pole piece with the diameter of 1 mm;
step 8, mounting the negative pole piece prepared in the step 7 into a button battery in a vacuum glove box, and carrying out an electrochemical performance test on an electrochemical workstation after the negative pole piece is placed aside for 12 hours;
and 9, other steps are carried out without changing the cross nano flower of the nickel disulfide, wherein SP is as follows: x: y, X + Y25; and (3) carrying out repeated experiments according to the steps in sequence, wherein X is 5, 10 and 20, and repeating 3 groups of experiments, which are marked as examples 2-4.
The figure is an SEM image of a nickel disulfide crossed nanoflower material, and the nickel disulfide crossed nanoflower material is obviously seen to be in a cross nanoflower-shaped structure, has a very large specific surface area, and can accommodate a large amount of lithium ions so as to optimize the electrochemical performance of the battery.
Comparative example 1
Step 1, adding NiCl 2 ·6H 2 O、CH 4 N 2 O、HSCH 2 CH(NH 2 )CO 2 H is represented by 1: after mixing according to the stoichiometric ratio of 1:2, stirring for 5min by magnetic force to completely melt the mixture in 20ml of deionized water;
step 2, adding 50ml of deionized water into the solution obtained in the step 1, and ultrasonically cleaning for 1 h;
step 3, pouring the solution obtained in the step 2 into a high-temperature high-pressure reaction kettle with a 100ml polytetrafluoroethylene lining, and reacting for 24 hours at 200 ℃;
step 4, when the solution reacted in the step 3 is cooled to room temperature, centrifuging for 5min at the speed of 4000 r/min;
step 5, washing the solution after centrifugation for 3 times by using 30ml of deionized water, and then washing for three times by using 30ml of ethanol solution;
step 6, putting the precipitate washed in the step 5 into a vacuum drying oven at 60 ℃ for drying for 24 hours to obtain a nickel disulfide crossed nano flower material;
and 7, mixing the nickel disulfide crossed nanoflower material obtained in the 6 processes, SP and PVDF according to the ratio of 75: 15: 10 and adding NMP for mixing, coating the obtained electrode slurry on a copper foil with the thickness of 100 microns, and carrying out vacuum drying at 60 ℃ for a whole night; taking out and cutting into negative pole pieces with the diameter of 1 mm;
and 8, mounting the negative pole piece prepared in the step 7 into a button battery in a vacuum glove box, and carrying out an electrochemical performance test on an electrochemical workstation after the negative pole piece is placed aside for 12 hours.
Second, the circulation performance of the nickel disulfide cross nano-flower material is compared with that of the comparative example, and NiCl can be obviously seen from the figure 2 ·6H 2 O、CH 4 N 2 O、HSCH 2 CH(NH 2 )CO 2 H is represented by 1: 1:4 sample is compared to NiCl 2 ·6H 2 O、CH 4 N 2 O、HSCH 2 CH(NH 2 )CO 2 H is represented by 1: the 1:2 sample had high cycling stability, demonstrating the feasibility of example 1.
The above examples are illustrative of the preferred embodiments of the present invention, but the present invention is not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and they are included in the scope of the present invention.

Claims (5)

1. The nickel disulfide cross nanoflower material is characterized in that the nickel disulfide cross nanoflower material is in a cross nanoflower-shaped structure, and raw materials required for synthesis are as follows: the molar mass ratio of the nickel chloride hexahydrate to the vulcanizing agent is 1: 4.
2. the nickel disulfide cross nanoflower material of claim 1, wherein the vulcanizing agent is L-cysteine.
3. A method of making the nickel disulfide interdigitated nanoflower material of claim 2, comprising the steps of:
s1, weighing 1: 1: adding nickel chloride hexahydrate, urea and L-cysteine powder in a proportion of 2 into deionized water, magnetically stirring uniformly, adding deionized water, and performing ultrasonic cleaning treatment;
s2: adding the solution obtained in the step S1 into a high-temperature high-pressure reaction kettle with a polytetrafluoroethylene lining, and reacting for 24 hours at 200 ℃;
s3: the mixed solution obtained after the treatment of S2 was centrifuged and filtered.
4. The method for preparing the nickel disulfide crossed nanoflower material according to claim 3, wherein the rotation speed of the centrifugal treatment in the step S3 is 4000r/min, and the time is 5-10 min.
5. The application of the nickel disulfide crossed nanoflower material according to any one of claims 1-2, wherein the nickel disulfide crossed nanoflower material can be applied to the field of lithium ion battery negative electrode materials.
CN202210590700.5A 2022-05-27 2022-05-27 Nickel disulfide cross nanoflower material and preparation method and application thereof Pending CN114956214A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104261490A (en) * 2014-09-22 2015-01-07 江苏师范大学 New method for two-step process preparation of nickel sulfide
KR20160119912A (en) * 2015-04-06 2016-10-17 울산과학기술원 Preparing method of graphene oxide dopeded with cobalt disulfide
CN106207127A (en) * 2016-08-30 2016-12-07 安徽师范大学 The preparation method of a kind of nickel sulfide/graphene nanocomposite material, lithium ion battery negative, lithium ion battery
CN110165171A (en) * 2019-05-16 2019-08-23 广东工业大学 A kind of primary reconstruction nano flower-like cobalt disulfide/rGO composite material and preparation method and application
CN113562764A (en) * 2021-06-30 2021-10-29 华东师范大学 Flower-like VS based on two-dimensional material2@Ti3C2Nano composite material and preparation method and application thereof
CN114497541A (en) * 2022-01-27 2022-05-13 广东工业大学 Preparation and application of hollow nickel disulfide ball

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104261490A (en) * 2014-09-22 2015-01-07 江苏师范大学 New method for two-step process preparation of nickel sulfide
KR20160119912A (en) * 2015-04-06 2016-10-17 울산과학기술원 Preparing method of graphene oxide dopeded with cobalt disulfide
CN106207127A (en) * 2016-08-30 2016-12-07 安徽师范大学 The preparation method of a kind of nickel sulfide/graphene nanocomposite material, lithium ion battery negative, lithium ion battery
CN110165171A (en) * 2019-05-16 2019-08-23 广东工业大学 A kind of primary reconstruction nano flower-like cobalt disulfide/rGO composite material and preparation method and application
CN113562764A (en) * 2021-06-30 2021-10-29 华东师范大学 Flower-like VS based on two-dimensional material2@Ti3C2Nano composite material and preparation method and application thereof
CN114497541A (en) * 2022-01-27 2022-05-13 广东工业大学 Preparation and application of hollow nickel disulfide ball

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Title
杜意恩: "特定晶面暴露的锐钛矿型TiO2的制备及其性能研究", 中国原子能出版社, pages: 33 *

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