CN107069004B - A kind of preparation method of the lithium ion battery negative material of three-dimensional porous structure - Google Patents
A kind of preparation method of the lithium ion battery negative material of three-dimensional porous structure Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of the lithium ion battery negative material of three-dimensional porous structure.First, stannic oxide/glycan compound cluster is prepared using hydro-thermal method, then these clusters are dissolved in the mixed solution of water and ethyl alcohol, and sodium carboxymethylcellulose and polyvinyl alcohol are sequentially added thereto, the graphene oxide water solution of low concentration is added thereto again after mixing, and is continuously stirred at 50~70 DEG C 12 hours.Finally, the solution stirred evenly is instilled in silica gel mould, freezed from top to bottom with liquid nitrogen, sample demoulding is placed in freeze drying box and is thoroughly lyophilized, products therefrom is calcined 2~4 hours at 350~550 DEG C.Product amorphous carbon/stannic oxide/graphene nanocomposite material of the invention shows as three-dimensional porous structure, when being used as lithium ion battery negative material, due to its excellent architectural characteristic, the gram volume of superelevation, brilliant high rate performance and cyclical stability are shown.
Description
Technical field
The present invention relates to a kind of technologies of preparing of three-dimensional porous structure material, belong to the technology neck of nanocomposite preparation
Domain.
Background technique
Lithium ion battery is high with its open-circuit voltage, energy density is big, the advantages that having extended cycle life has become mobile phone, notes
The main power source of the portable devices such as this computer.In recent years, right with the rapid development of the extensive energy storage device such as electric car
More stringent requirements are proposed for the performance of lithium ion battery.An important component of the cathode as lithium ion battery, to battery
Performance plays a key role.Current commercialized lithium ion battery mostly uses graphite as cathode greatly, but due to its structure
Limitation, theoretical lithium storage content is only 372mAh/g, it is difficult to meet the requirement of extensive energy storage device, this just promotes people to seek
Look for the high specific energy negative electrode material that can substitute graphite.
Stannic oxide is due to its higher theoretical capacity (782mAh/g), lower cost, reserves abundant and nontoxic
The advantages that be considered as one of most promising next-generation lithium ion battery negative material, before there is good development potentiality and application
Scape.Although there is stannic oxide above-mentioned advantage to lead to electrode due to its huge volume change in charge and discharge process
It the problems such as dusting, capacity declines rapidly and electrode surface forms unstable solid electrolyte membrane (SEI), seriously limits
Its practical application.In order to alleviate the volume change of stannic oxide, improve the electrical contact between active material, by stannic oxide and
Compound carbon material is a kind of effective means, this can not only inhibit the volume change of stannic oxide, can also be improved leading for electrode
Electrically.In the present invention, we can be formed using sodium carboxymethylcellulose polymer with stannic oxide/glycan and graphene oxide
The two is closely linked together, by adjusting the ratio of stannic oxide/glycan and graphene oxide, is adopted by the characteristic of hydrogen bond
Amorphous carbon/stannic oxide/graphene nanocomposite material of three-dimensional porous structure, this structure are prepared for freeze-drying
There are a large amount of hole and inner spaces, in addition amorphous carbon and the good flexibility of graphene, restrained effectively titanium dioxide
The volume change of tin, and this porous structure is conducive to the infiltration of electrolyte, shortens lithium ion diffusion length, while graphite
Alkene forms three-dimensional continuous conductive network, greatly improves the electric conductivity of electrode.In addition, amorphous carbon and graphene are wrapped in
Around stannic oxide, avoids it and be directly exposed in electrolyte, therefore stabilize SEI.When it is used as negative electrode of lithium ion battery
When, greatly improve capacity, cyclical stability and high rate performance.
Summary of the invention
Technical problem: the object of the present invention is to provide a kind of systems of the lithium ion battery negative material of three-dimensional porous structure
Preparation Method.When the material is used as negative electrode of lithium ion battery, solves the problems, such as that stannic oxide capacity attenuation is very fast, improve simultaneously
The electric conductivity of electrode.Realize the targets such as electrode material high capacity, long circulating, high magnification.
Technical solution: a kind of preparation method of the lithium ion battery negative material of three-dimensional porous structure of the invention include with
Lower step:
Step 1: glucose, potassium stannate are added sequentially to fill in the container of deionized water, it is then that above-mentioned mixing is molten
Liquid stirs 0.5~1.5 hour, and the mass ratio of glucose and potassium stannate is 2:1~3:1；Obtained colourless solution is packed into hydro-thermal
It in reaction kettle, seals, and reaction kettle is placed in 160~180 DEG C of drying box and is heated 4~8 hours, to produce after reaction
Object centrifugation, outwells supernatant, and sediment is thoroughly cleaned up, will obtain stannic oxide/glycan sepia solid and be placed in 60
It is 8~12 hours dry in~80 DEG C of vacuum oven；
Step 2: product obtained in step 1 is added in the container of the mixed solution of the water and ethyl alcohol that fill, surpass
Sonication 0.5~1.5 hour, wherein the volume ratio of water and ethyl alcohol was 2:3~3:2, states in mixed solution and successively adds then up
Sodium carboxymethylcellulose and polyvinyl alcohol stir 5~20 minutes, then that concentration is water-soluble for the graphene oxide of 1~3mg/mL
Liquid is added in above-mentioned solution, and container was placed at 50~70 DEG C and continuously stirs 8~12 hours after 0.5~1.5 hour by ultrasound,
The solution stirred evenly is instilled in silica gel mould, is from top to bottom freezed it completely with liquid nitrogen, is freezed after sample is demoulded dry
Dry 48~72 hours；
Step 3: product obtained in step 2 is carried out calcination processing in tube furnace, the wherein temperature of calcination processing
Be 350~550 DEG C, heating rate be 3~5 DEG C/min, soaking time be 2~4 hours, obtain three-dimensional porous amorphous carbon/
Stannic oxide/graphene nanocomposite material lithium ion battery negative material.
Wherein:
It by condition that sediment thoroughly cleans up is to be washed respectively using deionized water and dehydrated alcohol described in step 1
It washs three times.
Described in step 2 with the condition that liquid nitrogen from top to bottom freezes it completely be cooling time at least 10 minutes with
On, it is ensured that no liquid phase exists.
The pressure of calcination processing described in step 3 is normal pressure, and atmosphere is argon gas.
The viscosity of the sodium carboxymethylcellulose is greater than 1.9 pascal seconds, and the molecular weight of polyvinyl alcohol is 89 000~98
Between 000, the mass ratio of sodium carboxymethylcellulose and polyvinyl alcohol is 1:1~1:2.
The utility model has the advantages that
1, the present invention makees solvent using water and ethanol solution, environmentally protective.It is multiple that stannic oxide/glycan is prepared using hydro-thermal method
Close object cluster, prepare three-dimensional porous structure with freeze-drying, technical process is easy to control, and the material property of preparation is good, cost compared with
It is low.
2, product of the present invention is three-dimensional porous structure, possesses hole abundant and inner space, restrained effectively dioxy
Change volume change of the tin in cyclic process, while substantially increasing the contact area of active material and electrolyte, and then contracts
Short diffusion length of the lithium ion in electrode material, this structure are conducive to improve the cyclical stability of material and forthright again
Energy.
3, product of the present invention is a kind of amorphous carbon/stannic oxide/graphene nanocomposite material, amorphous carbon and graphite
Alkene can not only alleviate the volume change of stannic oxide, but also greatly improve the electric conductivity of entire electrode.
Detailed description of the invention
Fig. 1 is that the amorphous carbon/stannic oxide/graphene nano for the three-dimensional porous structure that the embodiment of the present invention 1 obtains is multiple
X-ray diffraction (XRD) map of condensation material.
Fig. 2 is that the amorphous carbon/stannic oxide/graphene nano for the three-dimensional porous structure that the embodiment of the present invention 1 obtains is multiple
The photomacrograph of condensation material and the scanning electron microscopic picture of low range.
Fig. 3 is that the amorphous carbon/stannic oxide/graphene nano for the three-dimensional porous structure that the embodiment of the present invention 1 obtains is multiple
The high magnification scanning electron microscopic picture and transmission electron microscope picture of condensation material.
Fig. 4 is that the amorphous carbon/stannic oxide/graphene nano for the three-dimensional porous structure that the embodiment of the present invention 1 obtains is multiple
Cyclic voltammetry curve when condensation material is as negative electrode of lithium ion battery.
Fig. 5 is that the amorphous carbon/stannic oxide/graphene nano for the three-dimensional porous structure that the embodiment of the present invention 1 obtains is multiple
Cycle performance figure when condensation material is as negative electrode of lithium ion battery.Test condition is first to recycle 20 at current density 100mA/g
It is secondary, it is then recycled under current density 1A/g 680 times, voltage range is 0.01~3V.It is recycled by 700 times, specific capacity is maintained at
1458.8mAh/g, for coulombic efficiency close to 100%, capacity retention ratio is up to 98.8%.
Specific embodiment
Embodiment 1:
The potassium stannate of the glucose of 8.87g and 3.93g is added sequentially in the container for filling 70mL deionized water, then
Above-mentioned mixed solution is stirred 1 hour, the mass ratio of glucose and potassium stannate is 2.25:1.Obtained colourless solution is packed into water
It in thermal response kettle, seals, and reaction kettle is placed in 180 DEG C of drying box and is heated 4 hours.To after reaction by product from
The heart outwells supernatant, and sediment is thoroughly cleaned up, and obtained sepia solid (stannic oxide/glycan) is placed in 80
DEG C vacuum oven in dry 12 hours；
Stannic oxide/glycan of 100mg is added in the container of the mixed solution of the water and ethyl alcohol that fill 10mL, ultrasound
Processing 1 hour, wherein the volume ratio of water and ethyl alcohol is 1:1.Being stated in solution then up successively adds 17.5mg to enter carboxymethyl cellulose
Plain sodium and 25mg polyvinyl alcohol stir 10 minutes, and the mass ratio of sodium carboxymethylcellulose and polyvinyl alcohol is 7:10.It then will be dense
Degree is that the graphene oxide water solution of 2mg/mL is added in above-mentioned solution, and container was placed at 50 DEG C and connects after 0.5 hour by ultrasound
Continuous stirring 12 hours.The solution stirred evenly is instilled in silica gel mould, is from top to bottom freezed it completely with liquid nitrogen, by sample
It is freeze-dried 72 hours after demoulding；
Dried product is subjected to calcination processing in tube furnace, wherein the temperature of calcination processing is 550 DEG C, heating speed
Rate is 3 DEG C/min, and soaking time is 4 hours, obtains three-dimensional porous amorphous carbon/stannic oxide/graphene nano composite wood
Expect lithium ion battery negative material.
X-ray diffraction point is carried out to three-dimensional porous amorphous carbon/stannic oxide/graphene nanocomposite material of preparation
Analysis does not observe the diffraction maximum of graphene as shown in Figure 1, product is stannic oxide, this may be the diffraction maximum because of graphene
Caused by being overlapped with the diffraction maximum of stannic oxide.
Take a picture to three-dimensional porous amorphous carbon/stannic oxide/graphene nanocomposite material and under low range into
Row scanning electron microscope characterization, as a result as shown in Fig. 2, visible product is three-dimensional porous structure, stannic oxide is in graphene nanometer sheet
It distributes very evenly.
Electricity is scanned to three-dimensional porous amorphous carbon/stannic oxide/graphene nanocomposite material under high magnification
Mirror and transmission electron microscope characterization, as seen from Figure 3, amorphous carbon and graphene nanometer sheet were tightly wrapped in stannic oxide cluster week
It encloses, which is about 70~80nm, and the tin dioxide nano-particle by many partial sizes in 5~8nm forms.
Electrode is made in three-dimensional porous amorphous carbon/stannic oxide/graphene nanocomposite material and is assembled into button
Battery carries out cyclic voltammetry in the case where sweep speed is 2mV/s, as a result as shown in figure 4, after recycling for the first time, cyclic voltammetric
Curve is almost overlapped, and shows that battery invertibity and repeatability are good.
The battery is recycled 20 times at current density 100mA/g, then then recycles 680 at current density 1A/g
Secondary, as shown in figure 5, capacity is maintained at 1458.8mAh/g after 700 circulations, coulombic efficiency is close to 100%, capacity retention ratio
Up to 98.8%.
Embodiment 2:
The potassium stannate of the glucose of 7.86g and 3.93g is added sequentially in the container for filling 80mL deionized water, then
Above-mentioned mixed solution is stirred 1.5 hours, the mass ratio of glucose and potassium stannate is 2:1；Obtained colourless solution is packed into water
It in thermal response kettle, seals, and reaction kettle is placed in 170 DEG C of drying box and is heated 6 hours；To after reaction by product from
The heart outwells supernatant, and sediment is thoroughly cleaned up, and will obtain sepia solid (stannic oxide/glycan) and is placed in 70 DEG C
Vacuum oven in dry 10 hours；
Stannic oxide/glycan of 200mg is added in the container of the mixed solution of the water and ethyl alcohol that fill 20mL, ultrasound
Processing 1.5 hours, wherein the volume ratio of water and ethyl alcohol is 3:2；Being stated in solution then up successively adds 20mg to enter carboxymethyl cellulose
Plain sodium and 28.6mg polyvinyl alcohol stir 20 minutes, and the mass ratio of sodium carboxymethylcellulose and polyvinyl alcohol is 7:10；Then will
Concentration is that the graphene oxide water solution of 3mg/mL is added in above-mentioned solution, and container was placed at 60 DEG C and connects after 1 hour by ultrasound
Continuous stirring 10 hours, the solution stirred evenly is instilled in silica gel mould, is from top to bottom freezed it completely with liquid nitrogen, by sample
It is freeze-dried 60 hours after demoulding；
Dried product is subjected to calcination processing in tube furnace, wherein the temperature of calcination processing is 450 DEG C, heating speed
Rate is 5 DEG C/min, and soaking time is 2 hours, obtains high performance amorphous carbon/stannic oxide/graphene nanocomposite material
Lithium ion battery negative material.
Embodiment 3:
The potassium stannate of the glucose of 11.79g and 3.93g is added sequentially in the container for filling 80mL deionized water, so
Above-mentioned mixed solution is stirred 0.5 hour afterwards, the mass ratio of glucose and potassium stannate is 3:1；Obtained colourless solution is packed into
It in hydrothermal reaction kettle, seals, and reaction kettle is placed in 160 DEG C of drying box and is heated 8 hours；To after reaction by product from
The heart outwells supernatant, and sediment is thoroughly cleaned up, and will obtain sepia and consolidate (stannic oxide/glycan) body being placed in 60 DEG C
Vacuum oven in dry 8 hours；
Stannic oxide/glycan of 50mg is added in the container of the mixed solution of the water and ethyl alcohol that fill 15mL, ultrasound
Processing 1.5 hours, wherein the volume ratio of water and ethyl alcohol is 2:3；Being stated in solution then up successively adds 15mg to enter carboxymethyl cellulose
Plain sodium and 21.4mg polyvinyl alcohol stir 20 minutes, and the mass ratio of sodium carboxymethylcellulose and polyvinyl alcohol is 7:10；Then will
Concentration is that the graphene oxide water solution of 1mg/mL is added in above-mentioned solution, and container is placed at 70 DEG C by ultrasound after 1.5 hours
It continuously stirs 8 hours, the solution stirred evenly is instilled in silica gel mould, is from top to bottom freezed it completely with liquid nitrogen, by sample
It is freeze-dried 48 hours after pint mould；
Dried product is subjected to calcination processing in tube furnace, wherein the temperature of calcination processing is 350 DEG C, heating speed
Rate is 4 DEG C/min, and soaking time is 3 hours, obtains high performance amorphous carbon/stannic oxide/graphene nanocomposite material
Lithium ion battery negative material.
Claims (5)
1. a kind of preparation method of the lithium ion battery negative material of three-dimensional porous structure, which is characterized in that this method includes such as
Lower step:
Step 1: glucose, potassium stannate are added sequentially to fill in the container of deionized water, it is small then to stir 0.5~1.5
When, the mass ratio of glucose and potassium stannate is 2:1~3:1；Obtained colourless solution is fitted into hydrothermal reaction kettle, is sealed, and
Reaction kettle is placed in 160~180 DEG C of drying box and is heated 4~8 hours, to after reaction be centrifuged product, outwells supernatant
Liquid, and sediment is thoroughly cleaned up, the vacuum drying for stannic oxide/glycan sepia solid will be obtained being placed in 60~80 DEG C
It is 8~12 hours dry in case；
Step 2: product obtained in step 1 is added in the container of the mixed solution of the water and ethyl alcohol that fill, at ultrasound
Reason 0.5~1.5 hour, wherein the volume ratio of water and ethyl alcohol is 2:3~3:2, states successively add carboxylic first in mixed solution then up
Base sodium cellulosate and polyvinyl alcohol stir 5~20 minutes, then add the graphene oxide water solution that concentration is 1~3mg/mL
Enter into above-mentioned solution, container was placed at 50~70 DEG C and continuously stirs 8~12 hours, will stir after 0.5~1.5 hour by ultrasound
It mixes uniform solution to instill in silica gel mould, it is freezed from top to bottom completely with liquid nitrogen, is freeze-dried 48 after sample is demoulded
~72 hours；
Step 3: product obtained in step 2 is carried out calcination processing in tube furnace, wherein the temperature of calcination processing is 350
~550 DEG C, heating rate is 3~5 DEG C/min, and soaking time is 2~4 hours, obtains three-dimensional porous amorphous carbon/titanium dioxide
Tin/graphene nanocomposite material lithium ion battery negative material.
2. the preparation method of the lithium ion battery negative material of three-dimensional porous structure according to claim 1, feature exist
In by condition that sediment thoroughly cleans up being to wash three respectively using deionized water and dehydrated alcohol described in step 1
It is secondary.
3. the preparation method of the lithium ion battery negative material of three-dimensional porous structure according to claim 1, feature exist
In with the condition that liquid nitrogen from top to bottom freezes it being completely cooling time at least at 10 minutes or more described in step 2, really
It protects and exists without liquid phase.
4. the preparation method of the lithium ion battery negative material of three-dimensional porous structure according to claim 1, feature exist
In the pressure of calcination processing described in step 3 is normal pressure, and atmosphere is argon gas.
5. the preparation method of the lithium ion battery negative material of three-dimensional porous structure according to claim 1, feature exist
Be greater than 1.9 pascal seconds in the viscosity of, the sodium carboxymethylcellulose, the molecular weight of polyvinyl alcohol 89 000~98 000 it
Between, the mass ratio of sodium carboxymethylcellulose and polyvinyl alcohol is 1:1~1:2.
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| CN108447695B (en) * | 2018-02-02 | 2020-01-03 | 北京理工大学 | Preparation method of foldable paper-based micro supercapacitor |
| CN108346789B (en) * | 2018-02-05 | 2020-07-31 | 东南大学 | Multi-contact core-shell cavity structure sodium ion battery cathode material and preparation method thereof |
| CN108717974A (en) * | 2018-06-07 | 2018-10-30 | 深圳市梅莎新能源科技有限公司 | A kind of preparation method of lithium ion battery material |
| CN109037611B (en) * | 2018-07-03 | 2021-11-09 | 上海交通大学 | Graphene-based flexible self-supporting adhesive-free electrode composite material and preparation method thereof |
| CN109817944A (en) * | 2019-02-18 | 2019-05-28 | 山东星火科学技术研究院 | Lithium ion battery cathode silica/graphene nano material preparation method |
| CN110391419B (en) * | 2019-07-26 | 2022-07-05 | 广东工业大学 | Porous carbon and application thereof in lithium-sulfur battery anode |
| CN111115618A (en) * | 2019-12-02 | 2020-05-08 | 深圳石墨烯创新中心有限公司 | Graphene/carbon/tin oxide nano composite material and preparation method and application thereof |
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| CN105047890A (en) * | 2015-07-08 | 2015-11-11 | 东南大学 | Three-dimensional porous lithium ion battery anode material of graphene composite material and preparation method of three-dimensional porous lithium ion battery anode material |
| CN105390675A (en) * | 2015-10-29 | 2016-03-09 | 陕西科技大学 | Preparation method of Sn/SnO<2>/C composite material for negative electrode of sodium-ion battery |
| CN105742635A (en) * | 2016-01-01 | 2016-07-06 | 三峡大学 | Stannic oxide/graphene/carbon composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105047890A (en) * | 2015-07-08 | 2015-11-11 | 东南大学 | Three-dimensional porous lithium ion battery anode material of graphene composite material and preparation method of three-dimensional porous lithium ion battery anode material |
| CN105390675A (en) * | 2015-10-29 | 2016-03-09 | 陕西科技大学 | Preparation method of Sn/SnO<2>/C composite material for negative electrode of sodium-ion battery |
| CN105742635A (en) * | 2016-01-01 | 2016-07-06 | 三峡大学 | Stannic oxide/graphene/carbon composite material and preparation method thereof |
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