CN106898745A - Lithium titanate/activated graphene nanosheet composite material preparation method and application - Google Patents
Lithium titanate/activated graphene nanosheet composite material preparation method and application Download PDFInfo
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- CN106898745A CN106898745A CN201710151138.5A CN201710151138A CN106898745A CN 106898745 A CN106898745 A CN 106898745A CN 201710151138 A CN201710151138 A CN 201710151138A CN 106898745 A CN106898745 A CN 106898745A
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Abstract
The present invention relates to lithium titanate/activated graphene nanosheet composite material preparation method and application.Graphene nanometer sheet and titanium dioxide mass ratio 1:5~20, it is added in LiOH solution, stir at room temperature, then ultrasound makes it be completely dispersed and mix；Mixed liquor is transferred in high pressure water heating kettle, is reacted at 140~220 DEG C；After being cooled to room temperature, black sample is obtained by centrifugation, washing and forced air drying；Sample is put into 500~1000 DEG C of calcinings in argon gas tube furnace, product is obtained.The present invention realizes that lithium titanate synthesis, graphene nanometer sheet activation and the synchronization of the two are compound, it is to avoid the use of organic titanium source and organic solvent by one step hydro thermal method.The materials application significantly improves battery performance in lithium ion battery negative, and 113mAh g have been remained under high magnification 100C‑1Specific capacity, charge and discharge cycles 2000 times under 10C, capability retention is 90.21%.
Description
Technical field
The present invention relates to electrochmical power source and energy storage material field, in more detail, it is related to a kind of lithium ion battery composite cathode
Material and preparation method thereof；Particularly lithium titanate/activated graphene nanosheet composite material preparation method and application.
Background technology
With economic and society development, people substitute oil etc. and pass to the quality requirement of living environment also more and more higher
The energy of system pollution environment is a development trend of the times.In recent years, lithium ion battery development is swift and violent, with voltage is high, energy
The many merits such as density is big, good cycle, the small, memory-less effect of self discharge, are developed rapidly over nearly 10 years, and with it
Remarkable high performance price ratio advantage is in mobile electricity such as mobile phone, notebook computer, mobile phone, arms equipment, video cameras
Sub- field of terminal equipment is widely used.The carbon materials such as lithium cell cathode material mostly graphite are now widely used for,
But the formation of Li dendrite is had in charge and discharge process, such lithium ion battery is there are major safety risks, therefore, improve lithium
Ion battery security and fast charging and discharging performance need the new negative material of exploitation.
Lithium titanate (Li with spinel structure4Ti5O12) material due to intercalation potential high (1.55V, relative to
Li/Li+Electrode), the advantages of Volume Changes are small in charge and discharge process and degree of reversibility is high, as lithium ion power cell cathode material
Material, is expected to solve the fast charging and discharging performance and security performance of lithium ion battery, with good development and application prospect.But it is low
Conductance and difference lithium ion diffusion coefficient seriously reduce its chemical property, so as to hinder its practical application.
Research shows to prepare lithium titanate/carbon (Li4Ti5O12/ C) composite be solve this problem effective ways, its preparation method
Mostly it is the lithium titanate for first synthesizing different-shape and size, then selects different carbon sources, is realized using various solid, liquid phase methods
Lithium titanate is compound with carbon.Graphene is constantly subjected to concern because of its application of unique property in electrode material, however, production
Quality individual layer high or form the few-layer graphene alkene, preparation technology are complicated and costly, greatly limit the industrialization production of Graphene
And application.And be produced on a large scale in commercially available graphene product and low production cost it is mostly be sandwich construction graphene nano
Piece, it is stacked by graphene sheet layer, and thickness is the two-dimentional graphitic nanomaterials of nanoscale.But its specific surface area
Smaller, porosity is also far away from individual layer and form the few-layer graphene alkene.There are some researches show[1], Graphene can be improved by activation process and received
The specific surface area and porosity of rice piece.But the high temeperature chemistry activation method condition of document report harshness process is numerous and diverse[2], study bar
Part is gentle, process is simple and can obtain preferable pore structure activation method it is very with practical value.
Bibliography：
[1]Kwang-Bum Kim,S.-H.Park et al.Self-assembly of Si entrapped
graphene architecture for high-performance Li-ion batteries.Electrochemistry
Communications 34(2013)117-120
[2]MichálkováM,SiarováM K,Tatarko P,et al.Effect of homogenization
treatment on the fracture behavior of silicon nitride/graphene nanoplatelets
composites.Journal of the European Ceramic Society,2014,34(14):3291-3299
The content of the invention
The present invention uses one step hydro thermal method, realizes the activation of graphene nanometer sheet, the generation of lithium titanate and is synchronously combined, mistake
The additives such as any surfactant need not be added in journey, the titanium source of use is enriched, and process is simple and easy to control, reduce pollution and
Cost.Lithium titanate/activated graphene nanosheet composite material is obtained for lithium ion battery negative material, it is shown that excellent electricity
Chemical property.
The present invention is achieved by following technical solution.
Lithium titanate of the invention/activated graphene nanosheet composite material preparation method, comprises the following steps that：
(1) graphene nanometer sheet and titanium dioxide mass ratio 1:5~20, it is added in LiOH solution, stir at room temperature, so
Ultrasound makes it be completely dispersed and mix afterwards；
(2) mixed liquor of step (1) is transferred in high pressure water heating kettle, 0.5h~24h is reacted at 140~220 DEG C；
(3) after the high pressure water heating kettle of step (2) naturally cools to room temperature, by being centrifuged and washing, then forced air drying
Obtain black sample；
(4) sample that step (3) is dried is put into 500~1000 DEG C of 1~10h of calcining in argon gas tube furnace, obtains product.
Step (1) the LiOH solution concentrations are 0.1M~10M.It is preferred that LiOH solution concentrations are 0.5M~4M.
The step (1) stirs 0.1~4h. at room temperature
Ultrasonic power is 300W in the step (1)；0.1~2h of ultrasound.
Reaction temperature is 160~200 DEG C in the autoclave of the step (2), and the reaction time is 0.5h~4h.
The forced air drying of the step (3) is in 50~70 DEG C of 4~8h of forced air drying.
Step (3) washing is preferred to wash 3~9 times.
Step (3) the forced air drying condition is：In 50~70 DEG C of 4~8h.
Lithium titanate/activated graphene nanometer sheet prepared by the present invention is applied to lithium ion battery negative material.
The synthesis of lithium titanate, the activation of graphene nanometer sheet are realized by one step hydro thermal method simultaneously and both is compound.
The additives such as any surfactant need not be added in the synthetic system.
The beneficial effects of the invention are as follows by one-step method while realizing the synthesis of lithium titanate and the work of graphene nanometer sheet
Change, while avoiding the use of organic titanium source and organic solvent in the synthetic system, reduce pollution and be conducive to environmental protection.In addition,
The materials application is drastically increased into battery performance in lithium ion battery negative, has been remained under high magnification 100C
113mAh g-1Specific capacity, charge and discharge cycles 2000 times under multiplying power 10C, capability retention is 90.21%.
Brief description of the drawings
Fig. 1 is the scanning electron microscopic picture of lithium titanate/activated graphene nanosheet composite material prepared by embodiment 1；
Fig. 2 is the high rate performance curve of lithium titanate/activated graphene nanosheet composite material prepared by embodiment 1；
Fig. 3 is the cycle life and coulombic efficiency of lithium titanate/activated graphene nanosheet composite material prepared by embodiment 1
Curve.
Specific embodiment
Embodiment 1
(1) (average grain diameter is 25 nanometers of anatase crystal and golden red for 10mg graphene nanometer sheets and 0.1g titanium dioxide
Stone crystal form titanium dioxide, trade names P25) it is added in 60mL 1M LiOH solution, 2h is stirred at room temperature, then ultrasound 1h
(ultrasonic power is 300W) makes it be completely dispersed and mix.
(2) mixed liquor is transferred in 100mL high pressure water heating kettles, 1h is reacted at 180 DEG C.
(3) after naturally cooling to room temperature, by being centrifuged and washing (washing six times), then 55 DEG C of forced air drying 6h obtain black
Tinctorial pattern product.
(4) sample of drying is put into 750 DEG C of calcining 5h in argon gas tube furnace, obtains final products.
Fig. 1 is the scanning electron microscopic picture of lithium titanate/activated graphene nanosheet composite material prepared by embodiment 1.As schemed
It is shown, it can be seen that the pattern of graininess lithium titanate and graphene nanometer sheet；Embedded figure is the TEM pictures of activated graphene, can
To see the loose structure on graphene nanometer sheet.
Fig. 2 is the high rate performance curve of lithium titanate/activated graphene nanosheet composite material prepared by embodiment 1,1C=
175mA g-1.Using blue electricity battery comprehensive tester test (model LAND CT-2001A) in Wuhan, test voltage scope is
1.0V-2.5V is (to Li/Li+Electrode).As illustrated, under each multiplying power electric current, specific capacity keeps stabilization, even if in 100C super larges
Multiplying power electric current under, specific capacity remains to reach 113mAh g-1。
Fig. 3 is the cycle life and coulombic efficiency of lithium titanate/activated graphene nanosheet composite material prepared by embodiment 1
Curve.As illustrated, it is 90.21% that capability retention is enclosed in circulation 2000 under the multiplying power electric current of 10C.
Embodiment 2
(1) 5mg graphene nanometer sheets and 0.1g titanium dioxide are added in 60mL 4M LiOH solution, are stirred at room temperature
4h, then ultrasound 2h (ultrasonic power is 300W) it is completely dispersed and is mixed.
(2) mixed liquor is transferred in 100mL high pressure water heating kettles, 12h is reacted at 160 DEG C.
(3) after naturally cooling to room temperature, by being centrifuged and washing (washing three times), then 50 DEG C of forced air drying 8h obtain black
Tinctorial pattern product.
(4) sample of drying is put into 500 DEG C of calcining 10h in argon gas tube furnace, obtains final products.
By products application in specific capacity under lithium ion battery negative, the multiplying power electric current of 1C be 143.4mAh g-1, circulation 500
Capacity is reduced to 130.2mAh g after circle-1。
Embodiment 3
(1) 20mg graphene nanometer sheets and 0.1g titanium dioxide are added in 60mL 0.5M LiOH solution, are stirred at room temperature
0.1h is mixed, then ultrasound 0.1h (ultrasonic power is 300W) makes it be completely dispersed and mix.
(2) mixed liquor is transferred in 100mL high pressure water heating kettles, 4h is reacted at 200 DEG C.
(3) after naturally cooling to room temperature, by being centrifuged and washing (washing nine times), then 70 DEG C of forced air drying 4h obtain black
Tinctorial pattern product.
(4) sample of drying is put into 1000 DEG C of calcining 1h in argon gas tube furnace, obtains final products.
By products application in specific capacity under lithium ion battery negative, the multiplying power electric current of 1C be 155.3mAh g-1, circulation 500
Capacity is reduced to 144.7mAh g after circle-1。
Embodiment 4
(1) 15mg graphene nanometer sheets and 0.1g titanium dioxide are added in 60mL 0.1M LiOH solution, are stirred at room temperature
1h is mixed, then ultrasound 1h (ultrasonic power is 300W) makes it be completely dispersed and mix.
(2) mixed liquor is transferred in 100mL high pressure water heating kettles, 24h is reacted at 140 DEG C.
(3) after naturally cooling to room temperature, by being centrifuged and washing (washing six times), then 60 DEG C of forced air drying 6h obtain black
Tinctorial pattern product.
(4) sample of drying is put into 800 DEG C of calcining 4h in argon gas tube furnace, obtains final products.
By products application in specific capacity under lithium ion battery negative, the multiplying power electric current of 1C be 162.1mAh g-1, circulation 500
Capacity is reduced to 150.3mAh g after circle-1。
Embodiment 5
(1) 8mg graphene nanometer sheets and 0.1g titanium dioxide are added in 60mL 10M LiOH solution, are stirred at room temperature
3h, then ultrasound 0.5h (ultrasonic power is 300W) it is completely dispersed and is mixed.
(2) mixed liquor is transferred in 100mL high pressure water heating kettles, 0.5h is reacted at 220 DEG C.
(3) after naturally cooling to room temperature, by being centrifuged and washing (washing seven times), then 55 DEG C of forced air drying 6h obtain black
Tinctorial pattern product.
(4) sample of drying is put into 600 DEG C of calcining 8h in argon gas tube furnace, obtains final products.
By products application in specific capacity under lithium ion battery negative, the multiplying power electric current of 1C be 158.5mAh g-1, circulation 500
Capacity is reduced to 141.3mAh g after circle-1。
The lithium titanate/activated graphene nanosheet composite material preparation method and application, ability that the present invention is disclosed and proposed
Field technique personnel can be by using for reference present disclosure, and the appropriate links such as condition route that change are realized, although the method for the present invention and system
Standby technology is described by preferred embodiment, and person skilled can substantially not depart from present invention, spirit
Final technology of preparing is realized with being modified to methods and techniques described herein route in scope or being reconfigured.It is special
Not it is pointed out that all similar replacements and apparent to those skilled in the art, the Ta Mendou of change
It is deemed to be included in spirit of the invention, scope and content.
Claims (10)
1. lithium titanate/activated graphene nanosheet composite material preparation method；It is characterized in that step is as follows：
(1) graphene nanometer sheet and titanium dioxide mass ratio 1:5~20, it is added in LiOH solution, stir at room temperature, Ran Houchao
Sound makes it be completely dispersed and mix；
(2) mixed liquor of step (1) is transferred in high pressure water heating kettle, 0.5h~24h is reacted at 140~220 DEG C；
(3) after the high pressure water heating kettle of step (2) naturally cools to room temperature, by being centrifuged and washing, then forced air drying is obtained
Black sample；
(4) sample that step (3) is dried is put into 500~1000 DEG C of 1~10h of calcining in argon gas tube furnace, obtains product.
2. the method for claim 1, it is characterized in that the step (1) LiOH solution concentrations are 0.1M~10M.
3. the method for claim 1, it is characterized in that the step (1) stirs 0.1~4h at room temperature.
4. the method for claim 1, it is characterized in that ultrasonic power is 300W, 0.1~2h of ultrasound in the step (1).
5. the method for claim 1, it is characterized in that LiOH solution concentrations are 0.5M~4M.
6. the method for claim 1, it is characterized in that in the autoclave of the step (2) reaction temperature be 160~
200 DEG C, the reaction time is 0.5h~4h.
7. the method for claim 1, it is characterized in that the forced air drying of the step (3) is in 50~70 DEG C of forced air dryings
4~8h.
8. the method for claim 1, it is characterized in that the step (3) is washed 3~9 times.
9. the method for claim 1, it is characterized in that the step (3) forced air drying condition is：50~70 DEG C 4~
8h。
10. lithium titanate/activated graphene nanosheet composite material that prepared by claim 1 is applied to lithium ion battery negative material
Material.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113753946A (en) * | 2021-09-01 | 2021-12-07 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of titanium dioxide @ graphene @ titanium dioxide anode material, product and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103151509A (en) * | 2013-03-18 | 2013-06-12 | 江苏悦达墨特瑞新材料科技有限公司 | Lithium titanate-graphene nano composite electrode material and preparation method thereof |
| CN105789582A (en) * | 2016-03-25 | 2016-07-20 | 华东理工大学 | Lithium titanate/porous carbon composite material and preparation method of lithium titanate/porous carbon composite material |
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2017
- 2017-03-14 CN CN201710151138.5A patent/CN106898745A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103151509A (en) * | 2013-03-18 | 2013-06-12 | 江苏悦达墨特瑞新材料科技有限公司 | Lithium titanate-graphene nano composite electrode material and preparation method thereof |
| CN105789582A (en) * | 2016-03-25 | 2016-07-20 | 华东理工大学 | Lithium titanate/porous carbon composite material and preparation method of lithium titanate/porous carbon composite material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113753946A (en) * | 2021-09-01 | 2021-12-07 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of titanium dioxide @ graphene @ titanium dioxide anode material, product and application |
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Application publication date: 20170627 |