CN107910512A - A kind of preparation method of multi-layer core-shell structure combination electrode material - Google Patents
A kind of preparation method of multi-layer core-shell structure combination electrode material Download PDFInfo
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- 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
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Abstract
The present invention relates to a kind of preparation method of multi-layer core-shell structure combination electrode material, including：By SiO2Microballoon is dispersed in Tris buffer solutions, is added DA stirring reactions, is obtained SiO2@PDA；It is dispersed in mixed liquor and stirs reaction, adding TBOT, the reaction was continued, obtains SiO2@PDA@TiO2；It is dispersed in Tris buffer solutions, adds DA stirring reactions, obtain SiO2@PDA@TiO2@PDA；Calcine under inert atmosphere, then etched with NaOH, obtain hollow C@TiO2@C；N is blended in sublimed sulfur2Calcined under atmosphere, up to multi-layer core-shell structure combination electrode material.The method of the present invention is simple, and raw material sources are convenient, and safety and environmental protection, cost is low, and suitable for large-scale production, obtained sandwich construction can effectively improve the electric conductivity of electrode material, while can inhibit shuttle effect, so as to strengthen the chemical property of lithium-sulfur cell.
Description
Technical field
The invention belongs to lithium sulphur battery electrode field of material technology, more particularly to a kind of multi-layer core-shell structure combination electrode material
The preparation method of material.
Background technology
Recently as the fast development of mobile electronic device, electric automobile and field of renewable energy, people are to storage
Energy equipment proposes the requirement of higher.Conventional lithium ion battery cannot increasingly meet to send out due to the limitation of energy density itself
The needs of exhibition, therefore it is very necessary to develop energy storage system of new generation.Using lithium sulphur of the elemental sulfur as cathode, lithium metal for anode
Battery is since it has higher energy density, overcharging resisting, and Sulphur ressource enriches, and the advantages such as cost is low are increasingly subject to close extensively
Note.But current lithium-sulfur cell there are problems that poorly conductive and stability is poor, coulombic efficiency is low caused by shuttle effect etc., this
A little problems hamper its commercial applications.Therefore how to further improve lithium-sulfur cell performance cause people research it is emerging
Interest.
Carbon material has excellent electric conductivity, big specific surface area and abundant duct.Internal gutter is beneficial to the entrance of sulphur,
The electric conductivity of electronics and ion is provided, while can also can effectively be pressed down as electrochemical reaction generator small one by one
The dissolving of polysulfide processed.And oxide has polysulfide good absorption property, it can effectively suppress shuttle effect.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of preparation method of multi-layer core-shell structure combination electrode material,
The method of the present invention is simple, and raw material sources are convenient, and safety and environmental protection, cost is low, suitable for large-scale production, obtained sandwich construction electrode
Material can be applied to the electrode material of lithium-sulfur cell, using suction-operated of the electric conductivity and oxide of carbon to polysulfide, carry
The comprehensive performance of high battery, makes it while with high-energy-density with excellent cycle performance.
A kind of preparation method of multi-layer core-shell structure combination electrode material of the present invention, including：
(1) by SiO2Microballoon is dispersed in Tris buffer solutions, adds Dopamine hydrochloride DA, stirring reaction, is washed through centrifugation
Wash, be dried in vacuo, obtain SiO2@PDA；Wherein SiO2Microballoon, the amount ratio of DA are 0.1~0.2g：0.2~0.3g；
(2) SiO for obtaining step (1)2@PDA are dispersed in the mixed liquor of absolute ethyl alcohol and ammonium hydroxide, and stirring reaction, adds
Enter butyl titanate TBOT, continue stirring reaction, through centrifuge washing, vacuum drying, obtains SiO2@PDA@TiO2；Wherein SiO2@
PDA, absolute ethyl alcohol, ammonium hydroxide, the amount ratio of TBOT are 0.1~0.3g：100mL：0.3mL：0.5~1.5mL；
(3) SiO for obtaining step (2)2@PDA@TiO2It is dispersed in Tris buffer solutions, adds Dopamine hydrochloride DA,
Stirring reaction, through centrifuge washing, vacuum drying, obtains SiO2@PDA@TiO2@PDA；Wherein SiO2@PDA@TiO2, DA dosage
Than for 0.1~0.15g：0.1~0.2g；
(4) SiO for obtaining step (3)2@PDA@TiO2@PDA are placed under inert atmosphere and calcine, and obtain SiO2@C@TiO2@
C is etched with NaOH solution, and through centrifuge washing, vacuum drying, obtains hollow-C@TiO2@C；
(5) hollow-C@TiO for obtaining step (4)2@C and sublimed sulfur in mass ratio 1：0.1~10 mixed grinding is uniform
Afterwards, in N2Calcined under atmosphere, obtain multi-layer core-shell structure combination electrode material S@C@TiO2@C。
SiO in the step (1)2Microballoon is to useMethod is anhydrous with 2.5mL ethyl orthosilicates TEOS, 27.5mL
The ammonium hydroxide that ethanol, 22.5mL deionized waters, 7.5mL mass fractions are 28% is raw material, 4~6h of stirring at normal temperature, through centrifuge washing,
Vacuum drying is made, for white, a diameter of 145~155nm.
The technological parameter of stirring reaction is in the step (2)：Reaction temperature is 40~50 DEG C, the reaction time for 10~
40min。
The middle addition TBOT of the step (2) continues the technological parameter that stirring is reacted and is：Reaction temperature is 40~50 DEG C, reaction
Time is 20~24h.
The step (1) and pH=8~9 of the Tris buffer solutions in (3).
The time of stirring reaction is 9~12h in the step (1) and (3).
Scattered in the step (1), (2) and (3) is ultrasonic disperse, and the ultrasonic disperse time is 10~40min.
The process conditions of centrifuge washing are each with deionized water, absolute ethyl alcohol in the step (1), (2), (3) and (4)
Washing 3 times.
Inert atmosphere is nitrogen atmosphere or argon gas atmosphere in the step (4).
The technological parameter of calcining is in the step (4)：Calcining heat is 400~900 DEG C, and heating rate is 2 DEG C/min,
Calcination time is 2~4h.
The process conditions of NaOH etchings are in the step (4)：The NaOH for being 2~6mol/L with the concentration of 50~100mL
Solution etches 4~20h under the conditions of 40~100 DEG C.
The time of grinding is 10~40min in the step (5).
The technological parameter of calcining is in the step (5)：Calcining heat is 150~160 DEG C, and calcination time is 22~26h.
Multi-layer core-shell structure combination electrode material in the step (5) is applied to lithium as the conductive frame of sulfur loaded S
Sulphur battery electrode material.
Beneficial effect
(1) raw material sources of the invention are convenient, and cost is low, and preparation method is simple, Environmental Safety, suitable for large-scale production.
(2) the multi-layer core-shell structure lithium sulphur battery electrode material obtained using preparation method of the present invention, interior cavity diameters
About 150nm, has the volumetric expansion that sufficient space allows sulphur to be produced in charge and discharge process；Porous carbon materials@oxide@carbon materials
The sandwich construction of material can effectively improve the electric conductivity of electrode material, while can inhibit shuttle effect, and stable structure, so as to strengthen
The chemical property of lithium-sulfur cell.
Brief description of the drawings
Fig. 1 is the low power field emission scanning electron microscope of multi-layer core-shell structure combination electrode material prepared by the embodiment of the present invention 1
Picture；
Fig. 2 is the high power Flied emission transmission electron microscope of multi-layer core-shell structure combination electrode material prepared by the embodiment of the present invention 1
Picture；
Fig. 3 is the electrical performance testing result of multi-layer core-shell structure combination electrode material prepared by the embodiment of the present invention 1.
Embodiment
With reference to specific embodiment, the present invention is further explained.It is to be understood that these embodiments are merely to illustrate the present invention
Rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, people in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Scope.
Embodiment 1
(1) 27.5mL absolute ethyl alcohols, 22.5mL deionized waters, the ammonium hydroxide that 7.5mL mass fractions are 28% are weighed and pours into burning
In bottle, stir evenly, be then added dropwise 2.5mL ethyl orthosilicate TEOS, after stirring 4h under room temperature, with absolute ethyl alcohol, go from
Each centrifuge washing of sub- water 3 times, vacuum drying, obtains white SiO2Microballoon, a diameter of 145~155nm.
(2) SiO for obtaining 0.2g steps (1)2Microballoon is added in the Tris buffer solutions (pH=8.5) of 100mL, ultrasound
30min is uniformly dispersed, and adds 0.2g Dopamine hydrochloride DA, stirring reaction 9h, with absolute ethyl alcohol, each centrifuge washing 3 of deionized water
Secondary, vacuum drying, obtains brownish black SiO2@PDA。
(3) SiO for obtaining 0.14g steps (2)2@PDA add the mixed liquor of 100mL absolute ethyl alcohols and 0.3mL ammonium hydroxide
In, ultrasonic 30min is uniformly dispersed, and stirring reaction 30min, adds 0.75mL butyl titanate TBOT at 45 DEG C, and it is anti-to continue stirring
20h is answered, with absolute ethyl alcohol, each centrifuge washing of deionized water 3 times, vacuum drying, obtains brown SiO2@PDA@TiO2。
(4) SiO for obtaining 0.1g steps (3)2@PDA@TiO2Add in the Tris buffer solutions (pH=8.5) of 100mL,
Ultrasonic 30min is uniformly dispersed, and adds 0.1g Dopamine hydrochloride DA, stirring reaction 9h, respectively centrifugation is washed with absolute ethyl alcohol, deionized water
Wash 3 times, be dried in vacuo, obtain brownish black SiO2@PDA@TiO2@PDA。
(5) SiO for obtaining step (4)2@PDA@TiO2@PDA are placed in tube furnace, in inert atmosphere (N2Or Ar) under
750 DEG C of calcining 2h, 2 DEG C/min of heating rate, obtains black SiO2@C@TiO2@C, the NaOH for being 4mol/L with concentration are etched, and 60
After stirring 6h at DEG C, with absolute ethyl alcohol, each centrifuge washing of deionized water 3 times, vacuum drying, obtains the hollow-C@TiO of black2@C。
(6) hollow-C@TiO for obtaining step (5)2@C, with sublimed sulfur in mass ratio 1：4 grinding 30min are uniformly mixed
Afterwards, in N2The lower 155 DEG C of calcinings 24h of atmosphere, obtains black multi-layer core-shell structure combination electrode material S@C@TiO2@C。
The multi-layer core-shell structure combination electrode material S@C@TiO that the present embodiment obtains2The low power field emission scanning electron microscope of@C
Picture as shown in Figure 1, high power Flied emission transmission electron microscope picture as shown in Fig. 2, understanding with internal cavities, diameter about 150nm, tool
There is the volumetric expansion that sufficient space allows sulphur to be produced in charge and discharge process.
The multi-layer core-shell structure combination electrode material S@C@TiO obtained to the present embodiment2@C carry out electrical performance testing, knot
Fruit is as shown in Figure 3, it is known that first circle specific discharge capacity is 1184mAh g under 0.1C-1, in 0.2C, 0.5C, 1C, 2C, under 5C multiplying powers
Specific discharge capacity is respectively 801mAh g-1, 614mAh g-1, 503mAh g-1, 397mAh g-1, 336mAh g-1。
Embodiment 2
(1) SiO for obtaining 1 step of 0.2g embodiments (1)2Microballoon adds the Tris buffer solutions (pH=8.5) of 100mL
In, ultrasonic 30min is uniformly dispersed, add 0.2g Dopamine hydrochloride DA, stirring reaction 9h, with absolute ethyl alcohol, deionized water respectively from
The heart washs 3 times, and vacuum drying, obtains brownish black SiO2@PDA。
(2) SiO for obtaining 0.14g steps (1)2@PDA add the mixed liquor of 100mL absolute ethyl alcohols and 0.3mL ammonium hydroxide
In, ultrasonic 30min is uniformly dispersed, and stirring reaction 30min, adds 0.75mL butyl titanate TBOT at 45 DEG C, and it is anti-to continue stirring
20h is answered, with absolute ethyl alcohol, each centrifuge washing of deionized water 3 times, vacuum drying, obtains brown SiO2@PDA@TiO2。
(3) SiO for obtaining 0.12g steps (2)2@PDA@TiO2Add the Tris buffer solutions (pH=8.5) of 100mL
In, ultrasonic 30min is uniformly dispersed, add 0.1g Dopamine hydrochloride DA, stirring reaction 9h, with absolute ethyl alcohol, deionized water respectively from
The heart washs 3 times, and vacuum drying, obtains brownish black SiO2@PDA@TiO2@PDA。
(4) SiO for obtaining step (3)2@PDA@TiO2@PDA are placed in tube furnace, in inert atmosphere (N2Or Ar) under
750 DEG C of calcining 2h, 2 DEG C/min of heating rate, obtains black SiO2@C@TiO2@C, the NaOH for being 4mol/L with concentration are etched, and 60
After stirring 6h at DEG C, with absolute ethyl alcohol, each centrifuge washing of deionized water 3 times, vacuum drying, obtains the hollow-C@TiO of black2@C。
(5) hollow-C@TiO for obtaining step (4)2@C, with sublimed sulfur in mass ratio 1：4 grinding 30min are uniformly mixed
Afterwards, in N2The lower 155 DEG C of calcinings 24h of atmosphere, obtains black multi-layer core-shell structure combination electrode material S@C@TiO2@C。
The multi-layer core-shell structure combination electrode material S@C@TiO obtained to the present embodiment2@C carry out electrical performance testing, can
Know that first circle specific discharge capacity is 1100mAh g under 0.1C-1, in 0.2C, 0.5C, 1C, 2C, specific discharge capacity is distinguished under 5C multiplying powers
For 805mAh g-1, 632mAh g-1, 517mAh g-1, 426mAh g-1, 325mAh g-1。
Embodiment 3
(1) SiO for obtaining 1 step of 0.2g embodiments (1)2Microballoon adds the Tris buffer solutions (pH=8.5) of 100mL
In, ultrasonic 30min is uniformly dispersed, add 0.2g Dopamine hydrochloride DA, stirring reaction 9h, with absolute ethyl alcohol, deionized water respectively from
The heart washs 3 times, and vacuum drying, obtains brownish black SiO2@PDA。
(2) SiO for obtaining 0.14g steps (1)2@PDA add the mixed liquor of 100mL absolute ethyl alcohols and 0.3mL ammonium hydroxide
In, ultrasonic 30min is uniformly dispersed, and stirring reaction 30min, adds 0.75mL butyl titanate TBOT at 45 DEG C, and it is anti-to continue stirring
20h is answered, with absolute ethyl alcohol, each centrifuge washing of deionized water 3 times, vacuum drying, obtains brown SiO2@PDA@TiO2。
(3) SiO for obtaining 0.15g steps (2)2@PDA@TiO2Add the Tris buffer solutions (pH=8.5) of 100mL
In, ultrasonic 30min is uniformly dispersed, add 0.1g Dopamine hydrochloride DA, stirring reaction 9h, with absolute ethyl alcohol, deionized water respectively from
The heart washs 3 times, and vacuum drying, obtains brownish black SiO2@PDA@TiO2@PDA。
(4) SiO for obtaining step (3)2@PDA@TiO2@PDA are placed in tube furnace, in inert atmosphere (N2Or Ar) under
750 DEG C of calcining 2h, 2 DEG C/min of heating rate, obtains black SiO2@C@TiO2@C, the NaOH for being 4mol/L with concentration are etched, and 60
After stirring 6h at DEG C, with absolute ethyl alcohol, each centrifuge washing of deionized water 3 times, vacuum drying, obtains the hollow-C@TiO of black2@C。
(5) hollow-C@TiO for obtaining step (4)2@C, with sublimed sulfur in mass ratio 1：4 grinding 30min are uniformly mixed
Afterwards, in N2The lower 155 DEG C of calcinings 24h of atmosphere, obtains black multi-layer core-shell structure combination electrode material S@C@TiO2@C。
The multi-layer core-shell structure combination electrode material S@C@TiO obtained to the present embodiment2@C carry out electrical performance testing, can
Know that first circle specific discharge capacity is 891mAh g under 0.1C-1, in 0.2C, 0.5C, 1C, 2C, specific discharge capacity is distinguished under 5C multiplying powers
For 652mAh g-1, 400mAh g-1, 298mAh g-1, 277mAh g-1, 215mAh g-1。
Claims (10)
1. a kind of preparation method of multi-layer core-shell structure combination electrode material, including：
(1) by SiO2Microballoon is dispersed in Tris buffer solutions, adds Dopamine hydrochloride DA, stirring reaction, through centrifuge washing, very
Sky is dry, obtains SiO2@PDA；Wherein SiO2Microballoon, the amount ratio of DA are 0.1~0.2g：0.2~0.3g；
(2) SiO for obtaining step (1)2@PDA are dispersed in the mixed liquor of absolute ethyl alcohol and ammonium hydroxide, and stirring reaction, adds metatitanic acid
Four butyl ester TBOT, continue stirring reaction, and through centrifuge washing, vacuum drying, obtains SiO2@PDA@TiO2；Wherein SiO2@PDA, nothing
Water-ethanol, ammonium hydroxide, the amount ratio of TBOT are 0.1~0.3g：100mL：0.3mL：0.5~1.5mL；
(3) SiO for obtaining step (2)2@PDA@TiO2It is dispersed in Tris buffer solutions, adds Dopamine hydrochloride DA, stirring
Reaction, through centrifuge washing, vacuum drying, obtains SiO2@PDA@TiO2@PDA；Wherein SiO2@PDA@TiO2, DA amount ratio be
0.1~0.15g：0.1~0.2g；
(4) SiO for obtaining step (3)2@PDA@TiO2@PDA are placed under inert atmosphere and calcine, and obtain SiO2@C@TiO2@C are used
NaOH solution etches, and through centrifuge washing, vacuum drying, obtains hollow-C@TiO2@C；
(5) hollow-C@TiO for obtaining step (4)2@C and sublimed sulfur in mass ratio 1：After 0.1~10 mixed grinding is uniform,
N2Calcined under atmosphere, obtain multi-layer core-shell structure combination electrode material S@C@TiO2@C。
A kind of 2. preparation method of multi-layer core-shell structure combination electrode material according to claim 1, it is characterised in that：Institute
State the SiO in step (1)2Microballoon is to useMethod is with 2.5mL ethyl orthosilicate TEOS, 27.5mL absolute ethyl alcohol, 22.5mL
The ammonium hydroxide that deionized water, 7.5mL mass fractions are 26~30% is raw material, and 4~6h of stirring at normal temperature, through centrifuge washing, vacuum is done
It is dry to be made.
A kind of 3. preparation method of multi-layer core-shell structure combination electrode material according to claim 1, it is characterised in that：Institute
Stating the technological parameter that stirring is reacted in step (2) is：Reaction temperature is 40~50 DEG C, and the reaction time is 10~40min；Add
TBOT continues the technological parameter that stirring is reacted：Reaction temperature is 40~50 DEG C, and the reaction time is 20~24h.
A kind of 4. preparation method of multi-layer core-shell structure combination electrode material according to claim 1, it is characterised in that：Institute
State pH=8~9 of the Tris buffer solutions in step (1) and (3)；The time of stirring reaction is 9~12h.
A kind of 5. preparation method of multi-layer core-shell structure combination electrode material according to claim 1, it is characterised in that：Institute
State in step (1), (2) and (3) it is scattered be ultrasonic disperse, the ultrasonic disperse time is 10~40min.
A kind of 6. preparation method of multi-layer core-shell structure combination electrode material according to claim 1, it is characterised in that：Institute
The process conditions for stating centrifuge washing in step (1), (2), (3) and (4) are respectively to be washed 3 times with deionized water, absolute ethyl alcohol.
A kind of 7. preparation method of multi-layer core-shell structure combination electrode material according to claim 1, it is characterised in that：Institute
It is nitrogen atmosphere or argon gas atmosphere to state inert atmosphere in step (4)；The technological parameter of calcining is：Calcining heat is 400~900
DEG C, heating rate is 2 DEG C/min, and calcination time is 2~4h.
A kind of 8. preparation method of multi-layer core-shell structure combination electrode material according to claim 1, it is characterised in that：Institute
Stating the process conditions that NaOH is etched in step (4) is：With the NaOH solution that the concentration of 50~100mL is 2~6mol/L 40~
4~20h is etched under the conditions of 100 DEG C.
A kind of 9. preparation method of multi-layer core-shell structure combination electrode material according to claim 1, it is characterised in that：Institute
The time for stating grinding in step (5) is 10~40min；The technological parameter of calcining is：Calcining heat is 150~160 DEG C, during calcining
Between be 22~26h.
A kind of 10. preparation method of multi-layer core-shell structure combination electrode material according to claim 1, it is characterised in that：
Multi-layer core-shell structure combination electrode material in the step (5) is applied to lithium-sulfur cell electricity as the conductive frame of sulfur loaded S
Pole material.
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| CN111092211A (en) * | 2019-12-31 | 2020-05-01 | 青岛科技大学 | Micro-cavity liquid state vulcanization preparation method of carbon and sulfide composite electrode material |
| CN111312998A (en) * | 2020-02-13 | 2020-06-19 | 渤海大学 | TiO modified by KOH for potassium-sulfur cell positive electrode2/V2O5Preparation method and application of/S composite material |
| CN111312998B (en) * | 2020-02-13 | 2021-03-19 | 渤海大学 | TiO modified by KOH for potassium-sulfur cell positive electrode2/V2O5Preparation method and application of/S composite material |
| CN111834636A (en) * | 2020-07-21 | 2020-10-27 | 陕西师范大学 | Preparation method of nitrogen-doped TiO lithium-sulfur battery positive electrode carrier with large specific surface area |
| CN111834636B (en) * | 2020-07-21 | 2021-11-02 | 陕西师范大学 | Preparation method of nitrogen-doped TiO lithium-sulfur battery positive electrode carrier with large specific surface area |
| CN113479931A (en) * | 2020-08-26 | 2021-10-08 | 中南大学 | Titanium oxide @ C hollow composite framework and preparation method and application thereof |
| CN113410579A (en) * | 2021-05-18 | 2021-09-17 | 北京化工大学 | Monoatomic metal/nitrogen co-doped hollow carbon sphere photo/electro-catalytic material and preparation method and application thereof |
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