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 PDFInfo
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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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- 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
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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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
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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
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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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- 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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy 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
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.
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| PCT/CN2020/089806 WO2021004150A1 (en) | 2019-07-10 | 2020-05-12 | Preparation method for negative electrode material sns/nd-cn of lithium-ion battery |
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| WO2021004150A1 (en) * | 2019-07-10 | 2021-01-14 | 陕西科技大学 | Preparation method for negative electrode material sns/nd-cn of lithium-ion battery |
| CN113745474A (en) * | 2021-08-13 | 2021-12-03 | 湖南理工学院 | PANI @ CN/SnS lithium ion battery anode material and preparation method thereof |
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| CN114094074A (en) * | 2021-11-15 | 2022-02-25 | 中博龙辉装备集团股份有限公司 | Carbon cloth supported tin disulfide @ carbon flexible composite electrode material and preparation method and application thereof |
| CN114420916B (en) * | 2022-01-24 | 2023-08-25 | 福州大学 | Positive electrode material of lithium-sulfur battery, and preparation method and application thereof |
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Cited By (2)
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| WO2021004150A1 (en) * | 2019-07-10 | 2021-01-14 | 陕西科技大学 | Preparation method for negative electrode material sns/nd-cn of lithium-ion battery |
| CN113745474A (en) * | 2021-08-13 | 2021-12-03 | 湖南理工学院 | PANI @ CN/SnS lithium ion battery anode material and preparation method thereof |
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Application publication date: 20191008 |