CN108767207A - A kind of high-performance oxide cladding nano SnO2The preparation method of negative material - Google Patents
A kind of high-performance oxide cladding nano SnO2The preparation method of negative material Download PDFInfo
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- CN108767207A CN108767207A CN201810372840.9A CN201810372840A CN108767207A CN 108767207 A CN108767207 A CN 108767207A CN 201810372840 A CN201810372840 A CN 201810372840A CN 108767207 A CN108767207 A CN 108767207A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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
The invention discloses a kind of high-performance oxides to coat nano SnO2The preparation method of negative material, includes the following steps：First to nano SnO2Particle carries out surface passivating treatment, then in nano SnO2Particle surface is oxide coated.Negative material prepared by the present invention not only has big specific capacity, but also can inhibit the Volumetric expansion of negative material in lithium ion battery charge and discharge process, has good charge-discharge performance, and preparation method of the present invention is simple, reproducible.
Description
Technical field
The present invention relates to technical field of lithium ion more particularly to a kind of high-performance oxide to coat nano SnO2Cathode
The preparation method of material.
Background technology
Lithium ion battery is electric by the main carrying as electric vehicle due to performance advantages such as high-energy-density and lasting stabilities
Source, using lithium ion battery as the chemical energy storage technology of representative also actively input research and development.Commercial lithium ion battery is negative at present
Pole material is graphite-like carbon material, but its theoretical capacity is only 372mAh/g；On the other hand, the intercalation potential master of this material
It concentrates in 0-0.1V (vs.Li/Li+) range, the deposition potential of very close lithium metal is unfavorable for the safety of battery.
To meet the needs of high-capacity lithium ion cell, research and development height ratio capacity, the reliable lithium ion cell electrode material of security performance
Material is very urgent and necessary.
In the lithium ion battery negative material studied at present, tin-based material increasingly attracts attention, because of its theory storage lithium
Capacity is 1494mAh/g, is to have now been found that the highest negative material of theoretical capacity close to ten times of carbon negative pole material；In addition, this
The intercalation potential (0.85V vs Li/Li+) of kind material is safer, and the rich content in the earth, makes it in lithium cell negative pole
There are very big potentiality in terms of material.However due to tin base cathode in charge and discharge process along with serious bulk effect
(the change rate of volume expansion and contraction>250%), this be easy to cause active material powder of detached on electrode, leads to lithium-ion electric
Tankage is decayed, to influence the cyclical stability of electrode.
For inhibit its volume expansion improve cycle performance, study at present it is more be, by tin-based material surface into
Row indefinite form carbon or oxide coat to inhibit the bulk effect in charge and discharge process.
In the prior art, liquid phase process is generally used to carry out the cladding of oxide to tin-based material, but liquid phase process produces
Raw coating thickness is thicker, influences the insertion and abjection of lithium ion, and the actual use specific capacity of tin-based material is caused to decline.
Also have been reported that the method by gas phase atomic layer deposition (ALD) carries out tin-based material the report of oxide coating decoration at present,
The characteristics of gas phase atomic layer deposition (ALD) method is can be with the thickness of finely regulating clad, if but the too thick meeting of clad
So that clad is dense, the performance of tin-based material actual specific capacity is influenced；If the thickness of clad is too thin, inhibit tinbase
The mechanical property of material expand is relatively low, does not have the problem of tin-based material expands in control charge and discharge process.Therefore one kind is needed
Method can realize that very thick clad inhibits the expansion in stannic oxide negative material charge and discharge process and influences lithium ion
In the insertion and abjection of stannic oxide particle, the big specific capacity feature of material is given full play to.
Invention content
Based on background technology there are the problem of, the present invention proposes a kind of high-performance oxide cladding nano SnO2Cathode material
The preparation method of material, negative material prepared by the present invention not only has big specific capacity, but also can inhibit lithium ion battery charge and discharge process
The Volumetric expansion of middle negative material has good charge-discharge performance, and preparation method of the present invention is simple, repeats
Property is good.
The present invention proposes a kind of high-performance oxide cladding nano SnO2The preparation method of negative material, including following steps
Suddenly：First to nano SnO2Particle carries out surface passivating treatment, then in nano SnO2Particle surface is oxide coated, obtains height
Performance oxide coats nano SnO2Negative material.
Preferably, using ethylene glycol to nano SnO2Particle carries out surface passivating treatment.
Preferably, the concrete operations of the Passivation Treatment are as follows：Using atomic layer deposition method, by nano SnO2Particle is put into
In atomic layer deposition cavity, cavity heating is passivated processing by pulse presoma of ethylene glycol.
Preferably, the cavity is warming up to 120-150 DEG C.
Preferably, the cavity is warming up to 140-150 DEG C.
Preferably, the time of Passivation Treatment is 35-65s.
Preferably, the time of the Passivation Treatment is 40-60s.
Preferably, the nano SnO2Particle is pre-processed in the following way using preceding：By nano SnO2Particle is in temperature
10-12h is dried under 80-100 DEG C of vacuum condition, be put into after taking-up in brown reagent bottle seal it is spare.
Preferably, using the ethylene glycol that carrier gas purge is extra after Passivation Treatment.
Preferably, the carrier gas is inert gas；It is further preferable that the carrier gas is argon gas.
Preferably, using atomic layer deposition method in nano SnO2Particle surface is oxide coated.
Preferably, the oxide is TiO2。
Preferably, in nano SnO2Particle surface coats TiO2Mode be：Using atomic layer deposition method, with five ethyoxyls
Titanium is precursor A, using deionized water as precursor B, to the nano SnO of passivation2Particle carries out cyclic deposition plating, and high property is made
It can oxide cladding nano SnO2Negative material.
Preferably, cycle-index is 45-55 times.
Preferably, the ball shaped nano SnO of passivation2The heating temperature of particle is 250-350 DEG C.
Preferably, the heating temperature of the precursor A is 130-140 DEG C, and the time for depositing plating every time is 80-120s.
Preferably, the heating temperature of the precursor B is 5-40 DEG C, and the time for depositing plating every time is 50-80s.
Preferably, in S2, precursor A and precursor B use carrier gas purge 140-160s after depositing plating every time.
Preferably, the carrier gas is argon gas.
Advantage is the present invention compared with prior art：
Due to the method for conventional atomic layer deposition oxide cladding, after some cycles cladding, often clad can become
Must be dense, influence the insertion of lithium ion so that the specific capacity of material, which plays, to be reduced.And the present invention uses atomic layer deposition skill
Art, by ball shaped nano SnO2Particle surface is passivated processing and carrys out the number of control surface active specy, then carries out atom
Layer deposition oxide cladding, the oxide cladding layers that such method is grown be nanoporous grade, can both provide in this way lithium from
The duct of son insertion and abjection, while clad can inhibit the expansion in tin dioxide material charge and discharge process again, increase battery
Cycle performance.
Preparation method of the present invention is simple, reproducible, and the lithium ion battery stannic oxide negative material of preparation had both had greatly
Specific capacity, and the expansion of stannic oxide negative material in lithium ion battery charge and discharge process can be inhibited so that height of the invention
Performance coats nano SnO2Negative material has good charge-discharge performance.
Description of the drawings
Fig. 1 is that the high-performance oxide that the present invention obtains coats nano SnO2The low range TEM electron microscopes of negative material；
Fig. 2 is that the high-performance oxide that the present invention obtains coats nano SnO2The high magnification TEM electron microscopes of negative material；
Fig. 3 is that the high-performance oxide that the present invention obtains coats nano SnO2Charge and discharge of the negative material under 0.1C multiplying powers
Cycle performance curve graph.
Specific implementation mode
Technical solution of the present invention is described in detail with reference to specific embodiment.
Embodiment 1
A kind of high-performance oxide cladding nano SnO2The preparation method of negative material, includes the following steps：
S1 is by ball shaped nano SnO2Particle is put into vacuum drying oven dries 12h under the conditions of 80 DEG C, and brown examination is put into after taking-up
It is sealed in agent bottle spare；
S2, using atomic layer deposition method, by dry ball shaped nano SnO2Particle is put into atomic layer deposition cavity, cavity
Temperature is heated to 120 DEG C, is passivated by pulse presoma of ethylene glycol, and passivation time 65s uses carrier gas purge later；
S3, using atomic layer deposition method, the ball shaped nano SnO of passivation will be loaded with2The atomic layer deposition cavity of particle heats up
To 250 DEG C, using five ethanolato-titaniums as precursor A, using deionized water as precursor B, to the ball shaped nano SnO of passivation2Particle into
Row cyclic deposition plating recycles 50 stoppings, and high-performance oxide is made and coats nano SnO2Negative material；The precursor A
Heating temperature be 140 DEG C, time of each plating is 80s；The heating temperature of the precursor B is 40 DEG C, each plating
Time is 50s；The precursor A and precursor B deposit purge 160s with argon gas after plating every time.
High-performance oxide manufactured in the present embodiment is coated into nano SnO2Negative material does low range TEM electron microscopes, knot
Fruit is as shown in Figure 1；Again by a kind of high-performance oxide cladding nano SnO manufactured in the present embodiment2Negative material is high magnification TEM
Electron microscope, as shown in Fig. 2, arrow meaning is titania oxide clad in figure.
Embodiment 2
A kind of high-performance oxide cladding nano SnO2The preparation method of negative material, includes the following steps：
S1, by ball shaped nano SnO2Particle is put into vacuum drying oven dries 10h under the conditions of 100 DEG C, and brown is put into after taking-up
It is sealed in reagent bottle spare；
S2, using atomic layer deposition method, by dry ball shaped nano SnO2Particle is put into atomic layer deposition cavity, cavity
Temperature is heated to 150 DEG C, is passivated by pulse presoma of ethylene glycol, and passivation time 35s uses carrier gas purge later；
S3, using atomic layer deposition method, the ball shaped nano SnO of passivation will be loaded with2The atomic layer deposition cavity of particle heats up
To 350 DEG C, using five ethanolato-titaniums as precursor A, using deionized water as precursor B, to the ball shaped nano SnO of passivation2Particle into
Row cyclic deposition plating recycles 45 stoppings, and high-performance oxide is made and coats nano-SnO2 anode material；The precursor A
Heating temperature be 130 DEG C, time of each plating is 120s；The heating temperature of the precursor B is 5 DEG C, each plating
Time is 80s；The precursor A and precursor B deposit purge 140s with argon gas after plating every time.
Embodiment 3
A kind of high-performance oxide cladding nano SnO2The preparation method of negative material, includes the following steps：
S1, by ball shaped nano SnO2Particle is put into vacuum drying oven dries 11h under the conditions of 90 DEG C, and brown examination is put into after taking-up
It is sealed in agent bottle spare；
S2, by dry ball shaped nano SnO2Particle is put into atomic layer deposition cavity, and cavity temperature is heated to 140 DEG C,
It is passivated by pulse presoma of ethylene glycol, passivation time 40s uses carrier gas purge later；
S3, using atomic layer deposition method, the ball shaped nano SnO of passivation will be loaded with2The atomic layer deposition cavity of particle heats up
To 270 DEG C, using five ethanolato-titaniums as precursor A, using deionized water as precursor B, to the ball shaped nano SnO of passivation2Particle into
Row cyclic deposition plating recycles 55 stoppings, and high-performance oxide is made and coats nano-SnO2 anode material；The precursor A
Heating temperature be 132 DEG C, time of each plating is 90s；The heating temperature of the precursor B is 10 DEG C, each plating
Time is 55s；The precursor A and precursor B deposit purge 145s with argon gas after plating every time.
Embodiment 4
A kind of high-performance oxide cladding nano SnO2The preparation method of negative material, includes the following steps：
S1, by ball shaped nano SnO2Particle is put into vacuum drying oven dries 11h under the conditions of 95 DEG C, and brown examination is put into after taking-up
It is sealed in agent bottle spare；
S2, by dry ball shaped nano SnO2Particle is put into atomic layer deposition cavity, and cavity temperature is heated to 150 DEG C,
It is passivated by pulse presoma of ethylene glycol, passivation time 60s uses carrier gas purge later；
S3, using atomic layer deposition method, the ball shaped nano SnO of passivation will be loaded with2The atomic layer deposition cavity of particle heats up
To 330 DEG C, using five ethanolato-titaniums as precursor A, using deionized water as precursor B, to the ball shaped nano SnO of passivation2Particle into
Row cyclic deposition plating recycles 52 stoppings, and high-performance oxide is made and coats nano SnO2Negative material；The precursor A
Heating temperature be 138 DEG C, time of each plating is 110s；The heating temperature of the precursor B is 30 DEG C, each plating
Time is 70s；The precursor A and precursor B deposit purge 155s with argon gas after plating every time.
Experimental example 1
High-performance oxide prepared by embodiment 1 coats nano SnO2Negative material, in fastening lithium ionic cell into
Row electrochemistry cycle performance is tested.The results are shown in Figure 3, it can be seen from the figure that after 50 charge and discharge cycles, system of the present invention
Standby high-performance oxide coats nano SnO2The capacity of negative material still can reach 800mAh/g, and the 50th time capacity retention ratio can
Up to 31%, this illustrates that nanometer titanium dioxide titanium oxide cladding can inhibit the expansion of tin dioxide material, while can provide lithium
The channel of ion insertion and abjection.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of high-performance oxide coats nano SnO2The preparation method of negative material, which is characterized in that include the following steps：
First to nano SnO2Particle carries out surface passivating treatment, then in nano SnO2Particle surface is oxide coated, obtains high-performance
Oxide coats nano SnO2Negative material.
2. preparation method according to claim 1, which is characterized in that using ethylene glycol to nano SnO2Particle carries out surface
Passivation Treatment.
3. preparation method according to claim 1 or 2, which is characterized in that the concrete operations of the Passivation Treatment are as follows：It adopts
With atomic layer deposition method, by nano SnO2Particle is put into atomic layer deposition cavity, cavity heating, using ethylene glycol as pulse forerunner
Body is passivated processing.
4. preparation method according to claim 3, which is characterized in that the cavity is warming up to 120-150 DEG C；Preferably,
The cavity is warming up to 140-150 DEG C；Preferably, the time of Passivation Treatment is 35-65s；Preferably, the Passivation Treatment when
Between be 40-60s.
5. preparation method according to claim 1, which is characterized in that the nano SnO2Particle is using preceding using such as lower section
Formula pre-processes：By nano SnO2Particle dries 10-12h in the case where temperature is 80-100 DEG C of vacuum condition.
6. preparation method according to claim 3, which is characterized in that extra using carrier gas purge after Passivation Treatment
Ethylene glycol；Preferably, the carrier gas is inert gas；It is further preferable that the carrier gas is argon gas.
7. according to claim 1-6 any one of them preparation methods, which is characterized in that using atomic layer deposition method in nanometer
SnO2Particle surface is oxide coated.
8. preparation method according to claim 7, which is characterized in that the oxide is TiO2。
9. preparation method according to claim 8, which is characterized in that in nano SnO2Particle surface coats TiO2Mode
For：Using atomic layer deposition method, using five ethanolato-titaniums as precursor A, using deionized water as precursor B, to the nanometer of passivation
SnO2Particle carries out cyclic deposition plating.
10. preparation method according to claim 9, which is characterized in that cycle-index is 45-55 times.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112164781A (en) * | 2020-09-25 | 2021-01-01 | 贵港益乐科技发展有限公司 | Porous SiO2Coated multi-shell hollow SnO2Lithium ion battery cathode material |
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| CN106129344A (en) * | 2016-06-06 | 2016-11-16 | 重庆大学 | A kind of tin ash/Titanium dioxide spherical granule and the preparation method of graphene nano belt composite |
| CN106299294A (en) * | 2016-09-13 | 2017-01-04 | 天津大学 | A kind of preparation method of tin dioxide nanocrystal/titania nanotube composite |
| CN106784763A (en) * | 2016-12-03 | 2017-05-31 | 合肥国轩高科动力能源有限公司 | A kind of porous oxide wraps up the preparation method of battery silicium cathode material |
| CN107180952A (en) * | 2017-05-03 | 2017-09-19 | 昆明理工大学 | A kind of SnO2‑TiO2The preparation method of negative material |
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2018
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102881881A (en) * | 2012-10-25 | 2013-01-16 | 中国科学院宁波材料技术与工程研究所 | Negative pole material of lithium ion battery, preparation method of material and lithium ion battery |
| CN106129344A (en) * | 2016-06-06 | 2016-11-16 | 重庆大学 | A kind of tin ash/Titanium dioxide spherical granule and the preparation method of graphene nano belt composite |
| CN106299294A (en) * | 2016-09-13 | 2017-01-04 | 天津大学 | A kind of preparation method of tin dioxide nanocrystal/titania nanotube composite |
| CN106784763A (en) * | 2016-12-03 | 2017-05-31 | 合肥国轩高科动力能源有限公司 | A kind of porous oxide wraps up the preparation method of battery silicium cathode material |
| CN107180952A (en) * | 2017-05-03 | 2017-09-19 | 昆明理工大学 | A kind of SnO2‑TiO2The preparation method of negative material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112164781A (en) * | 2020-09-25 | 2021-01-01 | 贵港益乐科技发展有限公司 | Porous SiO2Coated multi-shell hollow SnO2Lithium ion battery cathode material |
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