CN110311119A - A kind of preparation method of lithium ion battery negative material SnS/ND-CN - Google Patents

A kind of preparation method of lithium ion battery negative material SnS/ND-CN Download PDF

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CN110311119A
CN110311119A CN201910621206.9A CN201910621206A CN110311119A CN 110311119 A CN110311119 A CN 110311119A CN 201910621206 A CN201910621206 A CN 201910621206A CN 110311119 A CN110311119 A CN 110311119A
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lithium ion
ion battery
battery negative
negative material
sns
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殷立雄
宋佳琪
李书航
黄剑锋
杨军
蔺英
韩浪
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Shaanxi University of Science and Technology
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Priority to PCT/CN2020/089806 priority patent/WO2021004150A1/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/362Composites
    • H01M4/366Composites as layered products
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/58Selection 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
    • H01M4/581Chalcogenides or intercalation compounds thereof
    • H01M4/5815Sulfides
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624Electric conductive fillers
    • H01M4/625Carbon or graphite
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The invention discloses the preparation methods of lithium ion battery negative material SnS/ND-CN a kind of, step 1: melamine being placed in be placed in calcining furnace in high-temperature resistant container and is calcined, g-C is obtained3N4Presoma;By g-C3N4Presoma and magnesium powder are mixed and are kept the temperature in an inert gas atmosphere, obtain dry ND-CN after coccoid washs;Step 2: ND-CN being added in ethylene glycol after stirring and dissolving and add CN again2H4S dissolves to obtain solution B;Step 3: taking SnCl2·2H2O and solution B and by SnCl2·2H2O, which is added in solution B, stirs and dissolves and to obtain solution C;Step 4: solution C being placed in water heating kettle hydro-thermal reaction, obtains muddy liquid precursor;Step 5: taking out dry lithium ion battery negative material SnS/ND-CN after muddy liquid precursor centrifuge washing.Its cell negative electrode material prepared, which is applied to negative electrode of lithium ion battery, has excellent cyclical stability.

Description

A kind of preparation method of lithium ion battery negative material SnS/ND-CN
Technical field
The invention belongs to lithium ion battery negative material preparation method technical fields, are related to a kind of negative electrode of lithium ion battery material Expect the preparation method of SnS/ND-CN.
Background technique
According to " planning of automobile industry Long-and Medium-term Development " of country's publication, by 2025, lithium-ion-power cell energy was close Degree need to reach 350Wh kg-1More than.Currently on the market using graphite as the energy density of the power lithium-ion battery of negative electrode material Generally in 240Wh kg-1Hereinafter, and the capacity of graphite electrode very close theoretical capacity, room for promotion are limited.Therefore, it opens It is extremely important to send out novel high-capacity negative electrode material.SnS sill is due to having many advantages, such as that high capacity, hypotoxicity, easily preparation cause The extensive concerns of scientists.
The research of SnS electrode material is less, has lower intercalation potential and higher theoretical capacity (782mAh/g). SnS is a kind of important group IV-VI compound semiconductor materials, by controlling the concentration of tin element, can show n-type half The property of conductor, and the property of p-type semiconductor can be shown.Unit cell is crossed over two layers, and the C uranium pile along crystal is folded, belongs to orthorhombic System, structure cell coefficient a=433pm, b=1118pm, c=398pm, crystal have distortion NaCl type structure, and Sn is former in each layer Son and S atom are by stronger Covalent bonding together, and atom between layers is combined by weaker Van der Waals force. SnS becomes potential lithium ion battery negative material due to its unique structure and higher theoretical capacity.
SnS electrode material is conversion reaction and alloying reaction, SnS in the electrochemical reaction that charge and discharge process mainly occurs The reversible capacity of electrode material is mainly derived from alloying reaction, wherein SnS electrode material and lithium metal occur embedding dealkylation reaction, Conversion reaction etc. is the reaction table of its electrochemical reaction process below according to the difference of the charging/discharging voltage platform of chemical reaction Up to formula:
SnS+2Li++2e-→Sn+Li2S (1)
According to the difference of electrochemical reaction charging/discharging voltage platform, between 1.0~1.5V, SnS occurs one with lithium first A irreversible displacement reaction, generates metal Sn and amorphous Li2S, as reaction (1) is shown and the formation of SEI film.And And first charge-discharge during formed SEI film can generate biggish irreversible capacity make for the first time coulombic efficiency it is lower.Part The study found that at 1.5V, first happens is that lithium ion insertion SnS layer structure reacts but without the transformation of object phase (SnS+xLi++xe-→LiXSnS), in 1.0V or so, LixSnS and lithium ion carry out conversion reaction and generate Sn simple substance and Li2S (LiXSnS+(2-x)Li++(2-x)e-→Sn+Li2S).And alloying reaction occurs for 0.8V or less Sn simple substance and lithium ion.This is anti- It should be reversible, Sn simple substance such as reacts shown in (2) at most in combination with 4.4 lithium ions.The reversible capacity master of SnS electrode material To derive from this step.In addition, the performance of the shape battery pair of SEI film has large effect, stable SEI film can make electrochemistry Performance is very stable, and unstable SEI film will lead to performance degradation quickly.
It is more serious there are two using SnS as lithium ion battery negative material however as most of negative electrode materials The problem of: first is that there are biggish volume expansions in charge and discharge process for electrode, it can make electrode dusting even from collector It falls off, leads to its poor cyclical stability and structural stability;But its poor electric conductivity, to influence the biography of electronics Rate is passed, its more slow kinetic reaction is caused to cause it with poor chemical property.
Summary of the invention
Present invention solves the technical problem that being to provide, a kind of preparation cost is low, operating method is simple and short preparation period The preparation method of lithium ion battery negative material SnS/ND-CN, being applied to negative electrode of lithium ion battery has excellent circulation steady It is qualitative.
The present invention is to be achieved through the following technical solutions:
A kind of preparation method of lithium ion battery negative material SnS/ND-CN, comprising the following steps:
Step 1: melamine being placed in be placed in calcining furnace in high-temperature resistant container and is calcined at 550~700 DEG C, g- is obtained C3N4Presoma;By the g-C of 1~3g3N4The magnesium powder of presoma and 1~3g mixing and 700~800 DEG C in an inert gas atmosphere Lower heat preservation obtains dry ND-CN after coccoid washing;
Step 2: the ND-CN of 1~1.5g being added to after stirring and dissolve in 40~60ml ethylene glycol and add 0.5~1g CN2H4S dissolves to obtain solution B;
Step 3: by elemental mole ratios Sn:S=(0.5~2.0): (0.9~3.0) takes SnCl2·2H2O and solution B simultaneously will SnCl2·2H2O, which is added in solution B, stirs and dissolves and to obtain solution C;
Step 4: solution C being placed in water heating kettle hydro-thermal reaction at 160~200 DEG C, obtains muddy liquid precursor;
Step 5: taking out dry lithium ion battery negative material SnS/ND-CN after muddy liquid precursor centrifuge washing.
Further, high-temperature resistant container is porcelain boat in step 1;Calcining furnace is Muffle furnace and calcination time is 3~5h.
Further, inert gas is argon gas in step 1 and soaking time is 2~4h.
Further, washing is using acetic acid and water washing in step 1.
Further, dry in step 1 is that 8~12h is dried in vacuo at 60~80 DEG C.
Further, stirring is 20~40min of magnetic agitation in step 2.
Further, stirring is 20~40min of magnetic agitation in step 3.
Further, the packing ratio of water heating kettle is 40~60% in step 4;The hydro-thermal reaction time be 18~for 24 hours.
Further, centrifuge washing is washed using water and dehydrated alcohol in step 5.
Further, dry in step 5 is that 8~12h is dried in vacuo at 60~80 DEG C.
Compared with prior art, the invention has the following beneficial technical effects:
The preparation method of lithium ion battery negative material SnS/ND-CN provided by the invention a kind of, the SnS/ND-CN of preparation SnS nanosizing is realized, the SnS/ND-CN of flaky nanometer structure is formed, with biggish specific surface area, increases and is electrolysed The chance of liquid contact and reactivity site are conducive to the migration of lithium ion, and alleviate the volume change in charge and discharge process, Be conducive to improve the chemical property of material while also shortening lithium ion diffusion path, to achieve the purpose that fast charge;In addition, Morphological control is carried out to SnS/ND-CN by the control of hydrothermal temperature, its volume expansion can be alleviated, stablize its structure; SnS is loaded or is coated with carbon material during preparation, to provide good electron propagation ducts, Ke Yihuan for it Solve its volume expansion;SnS and active component progress are compound, and composite reactive component is reacted with lithium ion provides higher theoretical ratio Capacity, when having neither part nor lot in reaction as buffering matrix, buffer volumes expansion prevents to reunite;Its electrochemistry is improved to reach The purpose of energy.
Detailed description of the invention
Fig. 1 is the XRD diagram of lithium ion battery negative material SnS/ND-CN prepared by embodiment 3;
The SEM figure that Fig. 2 is lithium ion battery negative material SnS/ND-CN prepared by embodiment 3;
The TEM figure that Fig. 3 is lithium ion battery negative material SnS/ND-CN prepared by embodiment 3;
Fig. 4 is the Local map of Fig. 3;
Fig. 5 is the cycle performance figure of lithium ion battery negative material SnS/ND-CN prepared by embodiment 3.
Specific embodiment
Specific embodiment is given below.
Embodiment 1
A kind of preparation method of lithium ion battery negative material SnS/ND-CN, comprising the following steps:
Step 1: melamine being placed in be placed in Muffle furnace in porcelain boat and calcines 5h at 550 DEG C, obtains g-C3N4Forerunner Body;By the g-C of 1g3N4The magnesium powder of presoma and 1g mix and keep the temperature 4h at 700 DEG C in argon atmosphere, obtain coccoid using second It is dried in vacuo 12h at 60 DEG C after acid and water washing washing three times, obtains ND-CN;
Step 2: the ND-CN of 1g being added to magnetic agitation 30min in 40ml ethylene glycol and adds 1g's after dissolving CN2H4S dissolves to obtain solution B;
Step 3: taking SnCl by elemental mole ratios Sn:S=0.5:0.92·2H2O and solution B and by SnCl2·2H2O is added Magnetic agitation 30min and solution C is dissolved to obtain into solution B;
Step 4: solution C merging water heating kettle being placed in homogeneous hydro-thermal reaction instrument the hydro-thermal reaction 18h at 200 DEG C, is obtained Muddy liquid precursor;Wherein the packing ratio of water heating kettle is 40%;
Step 5: taking out true at 60 DEG C after muddy liquid precursor is washed three times using water and dehydrated alcohol alternating centrifugal The dry 12h of sky, obtains lithium ion battery negative material SnS/ND-CN.
Embodiment 2
A kind of preparation method of lithium ion battery negative material SnS/ND-CN, comprising the following steps:
Step 1: melamine being placed in be placed in Muffle furnace in porcelain boat and calcines 3h at 700 DEG C, obtains g-C3N4Forerunner Body;By the g-C of 2g3N4The magnesium powder of presoma and 1g mix and keep the temperature 2h at 800 DEG C in argon atmosphere, obtain coccoid using second It is dried in vacuo 8h at 80 DEG C after acid and water washing washing for several times, obtains ND-CN;
Step 2: the ND-CN of 1.5g being added to magnetic agitation 30min in 50ml ethylene glycol and adds 0.5g after dissolving CN2H4S dissolves to obtain solution B;
Step 3: taking SnCl by elemental mole ratios Sn:S=1:1.62·2H2O and solution B and by SnCl2·2H2O is added to Magnetic agitation 30min and solution C is dissolved to obtain in solution B;
Step 4: solution C merging water heating kettle being placed in homogeneous hydro-thermal reaction instrument the hydro-thermal reaction 20h at 180 DEG C, is obtained Muddy liquid precursor;Wherein the packing ratio of water heating kettle is 50%;
Step 5: taking out true at 60 DEG C after muddy liquid precursor is washed three times using water and dehydrated alcohol alternating centrifugal The dry 12h of sky, obtains lithium ion battery negative material SnS/ND-CN.
Embodiment 3
A kind of preparation method of lithium ion battery negative material SnS/ND-CN, comprising the following steps:
Step 1: melamine being placed in be placed in Muffle furnace in porcelain boat and calcines 4h at 600 DEG C, obtains g-C3N4Forerunner Body;By the g-C of 3g3N4The magnesium powder of presoma and 1g mix and keep the temperature 3h at 750 DEG C in argon atmosphere, obtain coccoid using second It is dried in vacuo 10h at 70 DEG C after acid and water washing washing three times, obtains ND-CN;
Step 2: 1.36g ND-CN being added to magnetic agitation 30min in 60ml ethylene glycol and adds 0.9g after dissolving CN2H4S dissolves to obtain solution B;
Step 3: taking SnCl by elemental mole ratios Sn:S=2:32·2H2O and solution B and by SnCl2·2H2O is added to molten Magnetic agitation 30min and solution C is dissolved to obtain in liquid B;
Step 4: solution C merging water heating kettle is placed in homogeneous hydro-thermal reaction instrument at 160 DEG C that hydro-thermal reaction for 24 hours, obtains Muddy liquid precursor;Wherein the packing ratio of water heating kettle is 60%;
Step 5: taking out true at 60 DEG C after muddy liquid precursor is washed three times using water and dehydrated alcohol alternating centrifugal The dry 12h of sky, obtains lithium ion battery negative material SnS/ND-CN.
Lithium ion battery negative material SnS/ND-CN sample is taken, as shown in Figure 1, SnS and ND-CN difference in the sample The g-C that the SnS for being 39-0354 with PDF number and PDF number are 75-16213N4Standard card diffraction peak energy correspond to well; As shown in Fig. 2, the sample is nano-sheet, thickness ultrathin, and crystallinity is preferable.As shown in Figure 3 and Figure 4, the SnS in the sample Nanometer sheet has been supported in ND-CN nanometer sheet;As shown in figure 5, the sample is 100mAg in current density-1Under, initial capacity Up to 1457.6mAhg-1, 492.3mAhg is maintained at after recycling 100 circles-1, coulombic efficiency is up to 99%, the circulation of sample It has excellent performance.
Embodiment 4
A kind of preparation method of lithium ion battery negative material SnS/ND-CN, comprising the following steps:
Step 1: melamine being placed in be placed in Muffle furnace in porcelain boat and calcines 3.5h at 650 DEG C, obtains g-C3N4Forerunner Body;By the g-C of 1g3N4The magnesium powder of presoma and 2g mix and keep the temperature 3.5h at 725 DEG C in argon atmosphere, obtain coccoid use It is dried in vacuo 11h at 65 DEG C after acetic acid and water washing washing three times, obtains ND-CN;
Step 2: 1.2gND-CN being added to magnetic agitation 20min in 50ml ethylene glycol and adds 0.8g's after dissolving CN2H4S dissolves to obtain solution B;
Step 3: taking SnCl by elemental mole ratios Sn:S=0.5:32·2H2O and solution B and by SnCl2·2H2O is added to Magnetic agitation 20min and solution C is dissolved to obtain in solution B;
Step 4: solution C merging water heating kettle being placed in homogeneous hydro-thermal reaction instrument the hydro-thermal reaction 22h at 170 DEG C, is obtained Muddy liquid precursor;Wherein the packing ratio of water heating kettle is 40%;
Step 5: taking out true at 70 DEG C after muddy liquid precursor is washed three times using water and dehydrated alcohol alternating centrifugal The dry 10h of sky, obtains lithium ion battery negative material SnS/ND-CN.
Embodiment 5
A kind of preparation method of lithium ion battery negative material SnS/ND-CN, comprising the following steps:
Step 1: melamine being placed in be placed in Muffle furnace in porcelain boat and calcines 3h at 700 DEG C, obtains g-C3N4Forerunner Body;By the g-C of 1g3N4The magnesium powder of presoma and 3g mix and keep the temperature 2.5h at 775 DEG C in argon atmosphere, obtain coccoid use It is dried in vacuo 9h at 75 DEG C after acetic acid and water washing washing three times, obtains ND-CN;
Step 2: 1.4gND-CN being added to magnetic agitation 40min in 60ml ethylene glycol and adds 0.7g's after dissolving CN2H4S dissolves to obtain solution B;
Step 3: taking SnCl by elemental mole ratios Sn:S=2:0.92·2H2O and solution B and by SnCl2·2H2O is added to Magnetic agitation 40min and solution C is dissolved to obtain in solution B;
Step 4: solution C merging water heating kettle being placed in homogeneous hydro-thermal reaction instrument the hydro-thermal reaction 19h at 190 DEG C, is obtained Muddy liquid precursor;Wherein the packing ratio of water heating kettle is 60%;
Step 5: taking out true at 80 DEG C after muddy liquid precursor is washed three times using water and dehydrated alcohol alternating centrifugal The dry 8h of sky, obtains lithium ion battery negative material SnS/ND-CN.
Example given above is to realize the present invention preferably example, and the present invention is not limited to the above embodiments.This field Technical staff's technical solution according to the present invention technical characteristic any nonessential addition, the replacement made, belong to this The protection scope of invention.

Claims (10)

1. a kind of preparation method of lithium ion battery negative material SnS/ND-CN, which comprises the following steps:
Step 1: melamine being placed in be placed in calcining furnace in high-temperature resistant container and is calcined at 550~700 DEG C, g-C is obtained3N4 Presoma;By the g-C of 1~3g3N4The mixing of the magnesium powder of presoma and 1~3g is simultaneously protected at 700~800 DEG C in an inert gas atmosphere Temperature obtains dry ND-CN after coccoid washing;
Step 2: the ND-CN of 1~1.5g being added to after stirring and dissolve in 40~60ml ethylene glycol and add 0.5~1g's CN2H4S dissolves to obtain solution B;
Step 3: by elemental mole ratios Sn:S=(0.5~2.0): (0.9~3.0) takes SnCl2·2H2O and solution B simultaneously will SnCl2·2H2O, which is added in solution B, stirs and dissolves and to obtain solution C;
Step 4: solution C being placed in water heating kettle hydro-thermal reaction at 160~200 DEG C, obtains muddy liquid precursor;
Step 5: taking out dry lithium ion battery negative material SnS/ND-CN after muddy liquid precursor centrifuge washing.
2. the preparation method of lithium ion battery negative material SnS/ND-CN according to claim 1 a kind of, feature exist In high-temperature resistant container is porcelain boat in the step 1;Calcining furnace is Muffle furnace and calcination time is 3~5h.
3. the preparation method of lithium ion battery negative material SnS/ND-CN according to claim 1 a kind of, feature exist In inert gas is argon gas in the step 1 and soaking time is 2~4h.
4. the preparation method of lithium ion battery negative material SnS/ND-CN according to claim 1 a kind of, feature exist In washing is using acetic acid and water washing in the step 1.
5. the preparation method of lithium ion battery negative material SnS/ND-CN according to claim 1 a kind of, feature exist In dry in the step 1 is to be dried in vacuo 8~12h at 60~80 DEG C.
6. the preparation method of lithium ion battery negative material SnS/ND-CN according to claim 1 a kind of, feature exist In stirring is 20~40min of magnetic agitation in the step 2.
7. the preparation method of lithium ion battery negative material SnS/ND-CN according to claim 1 a kind of, feature exist In stirring is 20~40min of magnetic agitation in the step 3.
8. the preparation method of lithium ion battery negative material SnS/ND-CN according to claim 1 a kind of, feature exist In the packing ratio of water heating kettle is 40~60% in the step 4;The hydro-thermal reaction time be 18~for 24 hours.
9. the preparation method of lithium ion battery negative material SnS/ND-CN according to claim 1 a kind of, feature exist In centrifuge washing is washed using water and dehydrated alcohol in the step 5.
10. the preparation method of lithium ion battery negative material SnS/ND-CN according to claim 1 a kind of, feature exist In dry in the step 5 is to be dried in vacuo 8~12h at 60~80 DEG C.
CN201910621206.9A 2019-07-10 2019-07-10 A kind of preparation method of lithium ion battery negative material SnS/ND-CN Pending CN110311119A (en)

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Application publication date: 20191008