CN103035918A - SnO2-C compound, preparation method thereof and application of SnO2-C compound as negative electrode material of lithium ion battery casing - Google Patents

SnO2-C compound, preparation method thereof and application of SnO2-C compound as negative electrode material of lithium ion battery casing Download PDF

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Publication number
CN103035918A
CN103035918A CN2013100096777A CN201310009677A CN103035918A CN 103035918 A CN103035918 A CN 103035918A CN 2013100096777 A CN2013100096777 A CN 2013100096777A CN 201310009677 A CN201310009677 A CN 201310009677A CN 103035918 A CN103035918 A CN 103035918A
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compound
sno
sno2
preparation
lithium ion
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郭洪
王薇
毛瑞
杨项军
王世雄
陈景
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Yunnan University YNU
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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
    • 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

A SnO2-C compound, a preparation method thereof and an application of the SnO2-C compound as a negative electrode material of a lithium ion battery casing belong to a metallurgic powder material and a preparation method and an application thereof. The compound provided by the invention is a 2-4-micrometer spherule, and the spherule is a nanometer aggregate consisting of 20-30-nanometer granules. The SnO2-C compound is prepared in the manner that alcoholysis is carried out on Sn salt by using glycerol and ethanol as solvents, the form of the compound changes with time at a certain temperature, and the compound is baked at a high temperature. The highest reversible capacity of the SnO2-C compound applied as the negative electrode material of the lithium ion battery casing is 630 mAh/g, the reversible capability is still greater than or equal to 590 mAh/g after recycled utilization for 100 times, and the specific capacity is kept at 84%. The SnO2-C compound and the preparation method and the application thereof have the advantages of simple technology, low cost and wide industrial production prospects.

Description

A kind of SnO 2-C compound and preparation and as the application of lithium ion battery nucleocapsid negative material
Technical field
The invention belongs to the preparation method and application of metallurgical powder material and pure hot method.
Background technology
Long-life, high power capacity, capable of circulation, free of contamination secondary cell become the research emphasis of Industrial Green revolution, and lithium ion battery belongs to one of them.The kind selected of anode material for lithium-ion batteries is less, so its negative material becomes the main study subject that improves the energy content of battery and cycle life.The actual capacity of present business-like carbon negative pole material improves the potentiality difficult of the embedding lithium capacity of this material near its theoretical value.Insoluble another problem of carbon negative pole material is, the embedding lithium current potential of carbon negative pole material is near the lithium metal current potential, graphite-based negative material for example, and lithium diffusion velocity therein is lower, and lithium may be separated out on the surface when high magnification charges, and there is hidden danger in the fail safe of battery.
SnO 2Be a kind of N-shaped broad-band gap (Eg=3.6 eV) semi-conducting material, obtain extensive concern in applications such as gas sensor, catalyst and solar cells.In addition, because of SnO 2Have higher theoretical specific capacity (782 mAhg -1) and the characteristics that embed of lithium ion electronegative potential, can be used as lithium ion battery negative material, be expected to become and substitute commercial graphite electrode (372 mAhg -1) one of material.But because it is accompanied by the acute variation of volume in lithium ion Infix and desfix process, irreversible capacity is higher first to cause it, and the chemical property decay is very fast.And at the synthetic SnO of nano-level 2@C, SnO 2/ Graphene, SnO 2/ carbon nano-tube under the prerequisite of guaranteed capacity, can effectively be alleviated the volume drastic change in the reaction, shows preferably chemical property.
SnO 2The synthetic method of-C composite negative pole material adopts template, electrodeposition process more, magnetron sputtering method etc., and complex process, length consuming time, cost is high, and productive rate is low.Before this, the employing circumfluence method such as Ping Wu prepare template, again with the synthetic SnO of the hot method of alcohol 2-C core-shell material, when current density was 100 mA/g, circulating, reversible capacity remained on 521.9 mAhg after 50 times -1(Ping Wu, Ning Du, Hui Zhang, Chuanxin Zhai, Deren Yang, ACS Appl. Mater. Interfaces, 3 (2011): 1946 – 1952).Yun-Ho Jin etc. are with SnO 2Be fixed on the carbon nano-tube preparation MWCNT/SnO 2Compound, chemical property excellent (Yun-Ho Jin, Kyung-Mi Min, Seung-Deok Seo, Hyun-Woo Shim, Dong-Wan Kim, J. Phys. Chem. C, 115 (2011): 22062 – 22067).But domestic about lithium ion battery SnO 2The report of@C nucleocapsid negative material is less.Research and develop a kind of slightly higher than carbon negative pole embedding lithium current potential, high, the good cycling stability of electrochemical specific capacity, and production cost is low, safe and reliable, be convenient to the SnO that industrialization is produced 2The Novel cathode material for lithium ion battery that-C is compound has great importance.
Summary of the invention
Purpose of the present invention at first is to provide a kind of uniform particles tiny, the SnO that degree of crystallinity is good 2Not only technique is simple for-C compound and preparation method thereof, the method, cost is low, and has the prospect of industrialized development.Secondly, the object of the invention is to utilize this SnO 2-C compound is high as specific capacity, the lithium ion battery negative material of good cycling stability.
Purpose of the present invention realizes in the following manner:
(1) SnO 2-C compound,
This SnO 2-C compound is that crystallization is 2～4 microns bead, and bead is the nanoclusters aggressiveness that 20～30 nanometer granules form, and specific area is larger.
Described SnO 2-C compound is this SnO 2-C compound free from admixture phase.
(2) prepare described SnO 2A kind of method of-C compound
Comprise step:
(1) takes by weighing SnCl 22H2O 0.5361g is measured ethanol 46mL, and glycerine 24mL mixes the three;
(2) mixed liquor with step (1) changes in the reactor, in 110～180 ℃ of reaction 6～96h, naturally cools to room temperature;
(3) take out product, distilled water, ethanol washing several, 60 ℃ of oven dry in 450 ℃ of lower roasting 2～6h, obtain SnO with product 2-C compound;
Above SnCl 22H 2O purity〉99.9%, glycerine purity 99.9%, purity of alcohol 99%.
Described preparation method's step (2) reaction time is preferably 30h or 48h, product free from admixture phase, and the pattern of crystallization is 2～4 microns beads.
(3) SnO 2-C compound is as the application of the nucleocapsid negative material of lithium ion battery
With SnO 2-C compound adds the conductive agent acetylene black of 10 wt%, and the binding agent PVDF of 10 wt% makes slurry, evenly is applied to oven dry on the copper platinum, blocks circular cathode pole piece, forms battery with lithium metal.
SnO in the described nucleocapsid negative material 2-C compound is 1～4 micron bead for the pattern of crystallization further.
Described nucleocapsid negative material is and the composition battery of lithium metal, and its reversible capacity is up to 630mAh/g, circulates still to remain on more than the 590mAh/g after 100 times.
The beneficial effect that the present invention has is:
The present invention adopts pure hot method by the prepared SnO of pink salt 2-C compound, degree of crystallinity is high, and is 1 ~ 50 micron sphere, and the surface is comprised of 10 ~ 20 nanometer granules, and specific area is larger, utilizes this SnO 2-C compound is conducive to lithium ion at SnO as lithium ion battery negative 2Take off embedding in the-C compound, cushioned SnO 2The change in volume of-C compound in the removal lithium embedded process, thus the cyclical stability of whole lithium ion battery improved.
Simultaneously, SnO 2There is certain carbon content in the tactic pattern of-C compound, and the lithium ion battery negative material specific capacity prepared is high, stable cycle performance, and reversible capacity is up to 630mAh/g, circulates still to remain on more than the 590mAh/g after 100 times.
Technical process of the present invention simple, consuming time less, productive rate is high.
Because tin oxide as a kind of N-shaped wide bandgap semiconductor materials, is used widely in fields such as gas sensor, catalyst and solar cells, so SnO of the present invention 2-C compound and preparation method not only can be applicable to the lithium ion battery negative material of industrialization, will have development prospect in above-mentioned field equally.
Description of drawings
Fig. 1 is the synthetic SnO of the hot method of the present invention's alcohol 2The SEM figure of-C compound, 180 ℃ of reaction temperatures, the time is 6 h.
Fig. 2 is the synthetic SnO of the hot method of the present invention's alcohol 2The SEM figure of-C compound, 180 ℃ of reaction temperatures, the time is 12 h.
Fig. 3 is the synthetic SnO of the hot method of the present invention's alcohol 2The SEM figure of-C compound, 180 ℃ of reaction temperatures, the time is 24 h.
Fig. 4 is the synthetic SnO of the hot method of the present invention's alcohol 2The SEM figure of-C compound, 180 ℃ of reaction temperatures, the time is 30 h.
Fig. 5 is the synthetic SnO of the hot method of the present invention's alcohol 2The SEM figure of-C compound, 180 ℃ of reaction temperatures, the time is 48 h.
Fig. 6 is the synthetic SnO of the hot method of the present invention's alcohol 2The SEM figure of-C compound, 180 ℃ of reaction temperatures, the time is 96 h.
Fig. 7 is the synthetic SnO of the hot method of the present invention's alcohol 2The XRD figure of-C composite powder, 180 ℃ of reaction temperatures, the time is respectively 6 h, 30 h, 96 h.
Fig. 8 is the synthetic SnO of the hot method of the present invention's alcohol 2The specific capacity of-C cathode composite-cycle-index curve, 180 ℃ of reaction temperatures, the time is respectively 6 h, 12 h, 24 h, 30 h, 48 h, 96 h.
The present invention will be further described below in conjunction with embodiment, and embodiment comprises but do not limit the scope that the present invention protects.
Embodiment
Embodiment 1:
Take by weighing 0.5361g SnCl 22H 2O is measured 46 mL ethanol, and 24 mL glycerine mix, and mixed liquor is changed in the polytetrafluoroethylene reactor, places 180 ℃ of baking ovens, reacts 6 hours, naturally cools to room temperature.Take out product, distilled water, ethanol washing for several times, 60 ℃ of oven dry, with product in 450 ℃ of lower roasting 4 h.Such as Fig. 1, the XRD material phase analysis result of gained sample shows that synthetic product is SnO 2-C compound, and the pattern of crystallization is about 2 microns beads.Analyze microstructure with transmission electron microscope (TEM), micron-sized bead is the nanoclusters aggressiveness that 20 nanometers～30 nanometer granules form.
The conductive agent acetylene black that synthetic material is added 10 wt%, the binding agent PVDF of 10 wt% makes slurry, evenly be applied on the copper platinum and dry, block circular pole piece, form test cell with lithium metal, carry out the constant current charge-discharge experiment, charging and discharging currents is 200mA/g, and the charging/discharging voltage scope control is between 0.01 ~ 1.5V.The SnO of preparation 2The maximum reversible capacity of-C composite negative pole material is 460mAh/g, and the specific capacity that circulates after 100 times is 400mAh/g, and capability retention is 87.0%.
Embodiment 2:
Take by weighing 0.5361g SnCl 22H 2O is measured 46 mL ethanol, and 24 mL glycerine mix, and mixed liquor is changed in the polytetrafluoroethylene reactor, places 180 ℃ of baking ovens, reacts 12 hours, naturally cools to room temperature.Take out product, distilled water, ethanol washing for several times, 60 ℃ of oven dry, with product in 450 ℃ of lower roasting 4 h.Such as Fig. 2, the XRD material phase analysis result of gained sample shows that synthetic product is SnO 2-C compound, and the pattern of crystallization is about 2 microns beads.Analyze microstructure with transmission electron microscope (TEM), micron-sized bead is the nanoclusters aggressiveness that 20 nanometers～30 nanometer granules form.
The conductive agent acetylene black that synthetic material is added 10 wt%, the binding agent PVDF of 10 wt% makes slurry, evenly be applied to oven dry on the copper platinum, block circular pole piece, form test cell with lithium metal, carry out the constant current charge-discharge experiment, charging and discharging currents is 200mA/g, and the charging/discharging voltage scope control is between 0.01 ~ 1.5V.The SnO of preparation 2The maximum reversible capacity of-C composite negative pole material is 470mAh/g, and the specific capacity that circulates after 100 times is 390mAh/g, and capability retention is 83.0%.
Embodiment 3:
Take by weighing 0.5361g SnCl 22H 2O is measured 46 mL ethanol, and 24 mL glycerine mix, and mixed liquor is changed in the polytetrafluoroethylene reactor, places 180 ℃ of baking ovens, reacts 24 hours, naturally cools to room temperature.Take out product, distilled water, ethanol washing for several times, 60 ℃ of oven dry, with product in 450 ℃ of lower roasting 4 h.Such as Fig. 3, the XRD material phase analysis result of gained sample shows that synthetic product is SnO 2-C compound, without the existence of any impurity phase, and the pattern of crystallization is about 2 microns beads.Analyze microstructure with transmission electron microscope (TEM), micron-sized bead is the nanoclusters aggressiveness that 20 nanometers～30 nanometer granules form.
The conductive agent acetylene black that synthetic material is added 10 wt%, the binding agent PVDF of 10 wt% makes slurry, evenly be applied to oven dry on the copper platinum, block circular pole piece, form test cell with lithium metal, carry out the constant current charge-discharge experiment, charging and discharging currents is 200mA/g, and the charging/discharging voltage scope control is between 0.01 ~ 1.5V.The SnO of preparation 2The maximum reversible capacity of-C composite negative pole material is 480mAh/g, and the specific capacity that circulates after 100 times is 400mAh/g, and capability retention is 83.3%.
Embodiment 4:
Take by weighing 0.5361g SnCl 22H 2O is measured 46 mL ethanol, and 24 mL glycerine mix, and mixed liquor is changed in the polytetrafluoroethylene reactor, places 180 ℃ of baking ovens, reacts 30 hours, naturally cools to room temperature.Take out product, distilled water, ethanol washing for several times, 60 ℃ of oven dry, with product in 450 ℃ of lower roasting 4 h.Such as Fig. 4, the XRD material phase analysis result of gained sample shows that synthetic product is SnO 2-C compound, without the existence of any impurity phase, and the pattern of crystallization is about 2 microns beads.Analyze microstructure with transmission electron microscope (TEM), micron-sized bead is the nanoclusters aggressiveness that 20 nanometers～30 nanometer granules form.
The conductive agent acetylene black that synthetic material is added 10 wt%, the binding agent PVDF of 10 wt% makes slurry, evenly be applied on the copper platinum and dry, block circular pole piece, form test cell with lithium metal, carry out the constant current charge-discharge experiment, charging and discharging currents is 200mA/g, and the charging/discharging voltage scope control is between 0.01 ~ 1.5V.The SnO of preparation 2The maximum reversible capacity of-C composite negative pole material is 630mAh/g.The specific capacity that circulates after 100 times is 590mAh/g, and capability retention is 93.6%.
Embodiment 5:
Take by weighing 0.5361g SnCl 22H 2O is measured 46 mL ethanol, and 24 mL glycerine mix, and mixed liquor is changed in the polytetrafluoroethylene reactor, places 180 ℃ of baking ovens, reacts 48 hours, naturally cools to room temperature.Take out product, distilled water, ethanol washing for several times, 60 ℃ of oven dry, with product in 450 ℃ of lower roasting 4 h.Such as Fig. 5, the XRD material phase analysis result of gained sample shows that synthetic product is SnO 2-C compound, without the existence of any impurity phase, and the pattern of crystallization is about 4 microns beads.Analyze microstructure with transmission electron microscope (TEM), micron-sized bead is the nanoclusters aggressiveness that 20 nanometers～30 nanometer granules form.
The conductive agent acetylene black that synthetic material is added 10 wt%, the binding agent PVDF of 10 wt% makes slurry, evenly be applied on the copper platinum and dry, block circular pole piece, form test cell with lithium metal, carry out the constant current charge-discharge experiment, charging and discharging currents is 200mA/g, and the charging/discharging voltage scope control is between 0.01 ~ 1.5V.The maximum reversible capacity of SnO2-C composite negative pole material of preparation is 640mAh/g, and the specific capacity that circulates after 100 times is 550mAh/g, and capability retention is 85.9%.
Embodiment 6:
Take by weighing 0.5361g SnO 22H2O is measured 46 mL ethanol, and 24 mL glycerine mix, and mixed liquor is changed in the polytetrafluoroethylene reactor, places 180 ℃ of baking ovens, reacts 96 hours, naturally cools to room temperature.Take out product, distilled water, ethanol washing for several times, 60 ℃ of oven dry, with product in 450 ℃ of lower roasting 4 h.Such as Fig. 6, the XRD material phase analysis result of gained sample shows that synthetic product is SnO 2-C compound.Such as Fig. 1, the XRD material phase analysis result of gained sample shows that synthetic product is SnO 2-C compound, without the existence of any impurity phase, and the pattern of crystallization is about 4 microns beads.Analyze microstructure with transmission electron microscope (TEM), micron-sized bead is the nanoclusters aggressiveness that 20 nanometers～30 nanometer granules form.
The conductive agent acetylene black that synthetic material is added 10 wt%, the binding agent PVDF of 10 wt% makes slurry, evenly be applied on the copper platinum and dry, block circular pole piece, form test cell with lithium metal, carry out the constant current charge-discharge experiment, charging and discharging currents is 200mA/g, and the charging/discharging voltage scope control is between 0.01 ~ 1.5V.The SnO of preparation 2The maximum reversible capacity of-C composite negative pole material is 550mAh/g.The specific capacity that circulates after 100 times is 350mAh/g, and capability retention is 63.6%.
Among the above embodiment 1 ~ 6, raw material SnCl 22H 2O purity〉99.9%, glycerine purity 99.9%, purity of alcohol 99%.

Claims (7)

1. SnO 2-C compound is characterized in that this SnO 2-C compound is that crystallization is 2～4 microns bead, and bead is the nanoclusters aggressiveness that 20～30 nanometer granules form, and specific area is larger.
2. SnO according to claim 1 2-C compound is characterized in that this SnO 2-C compound free from admixture phase.
3. one kind prepares such as SnO as described in the claim 1 ~ 2 2A kind of method of-C compound is characterized in that:
(1) takes by weighing SnCl 22H2O 0.5361g is measured ethanol 46mL, and glycerine 24mL mixes the three;
(2) mixed liquor with step (1) changes in the reactor, in 110～180 ℃ of reaction 6～96h, naturally cools to room temperature;
(3) take out product, distilled water, ethanol washing several, 60 ℃ of oven dry in 450 ℃ of lower roasting 2～6h, obtain SnO with product 2-C compound;
Above SnCl 22H 2O purity〉99.9%, glycerine purity 99.9%, purity of alcohol 99%.
4. preparation method according to claim 3 is characterized in that step (2) reaction time is preferably 30h or 48h, product free from admixture phase, and the pattern of crystallization is 2～4 microns beads.
5. an application such as the described a kind of SnO of claim 1～4 2-C compound is characterized in that SnO as the nucleocapsid negative material of lithium ion battery 2-C compound adds the conductive agent acetylene black of 10 wt%, and the binding agent PVDF of 10 wt% makes slurry, evenly is applied to oven dry on the copper platinum, blocks circular cathode pole piece, forms battery with lithium metal.
6. nucleocapsid negative material according to claim 5 is characterized in that described SnO 2The pattern of-C complex crystallization is 1～4 micron bead.
7. according to claim 5 or 6 described nucleocapsid negative materials, it is characterized in that and the composition battery of lithium metal that its reversible capacity is up to 630mAh/g, circulating still remains on more than the 590mAh/g after 100 times.
CN2013100096777A 2013-01-11 2013-01-11 SnO2-C compound, preparation method thereof and application of SnO2-C compound as negative electrode material of lithium ion battery casing Pending CN103035918A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103681004A (en) * 2013-11-25 2014-03-26 华南农业大学 High-specific-capacitance SnO2/C porous microsphere and production method thereof
CN103915612A (en) * 2014-04-18 2014-07-09 云南大学 High-capacity MoO3-SnO2@C composite lithium ion battery core-shell negative material and preparation method
CN108470882A (en) * 2018-03-30 2018-08-31 江汉大学 Tin oxide is modified carbon cloth base lithium and sodium metal negative electrode and preparation method thereof
CN111192997A (en) * 2020-01-07 2020-05-22 北京理工大学 Diaphragm for activated carbon-loaded tin oxide lithium-sulfur battery and preparation method and application thereof
CN113437287A (en) * 2021-05-10 2021-09-24 南昌航空大学 Preparation method and application of tin oxide carbon-coated carbon and carbon composite material

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103681004A (en) * 2013-11-25 2014-03-26 华南农业大学 High-specific-capacitance SnO2/C porous microsphere and production method thereof
CN103681004B (en) * 2013-11-25 2017-02-15 华南农业大学 High-specific-capacitance SnO2/C porous microsphere and production method thereof
CN103915612A (en) * 2014-04-18 2014-07-09 云南大学 High-capacity MoO3-SnO2@C composite lithium ion battery core-shell negative material and preparation method
CN108470882A (en) * 2018-03-30 2018-08-31 江汉大学 Tin oxide is modified carbon cloth base lithium and sodium metal negative electrode and preparation method thereof
CN111192997A (en) * 2020-01-07 2020-05-22 北京理工大学 Diaphragm for activated carbon-loaded tin oxide lithium-sulfur battery and preparation method and application thereof
CN113437287A (en) * 2021-05-10 2021-09-24 南昌航空大学 Preparation method and application of tin oxide carbon-coated carbon and carbon composite material

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Application publication date: 20130410