CN106784823B - A kind of synthetic method of lithium vanadate as cathode material of lithium ion battery - Google Patents
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- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
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Abstract
The present invention discloses a kind of synthetic method of lithium vanadate as cathode material of lithium ion battery, comprising the following steps: after lithium source material is dried, obtains the lithium source substrate of surface passivation by atomic deposition technique；Again by the vanadic anhydride cyclic deposition reacted by ammonium metavanadate and oxygen in the lithium source substrate of passivation, the precursor A obtained from；Precursor A obtains presoma C after pre-burning, washing, suction filtration, drying；Last presoma C is sintered under protective atmosphere obtains lithium vanadate anode material.The presoma that the present invention is obtained by atomic deposition technique, then the lithium vanadate anode material being sintered by high temperature solid-state method, have the characteristics of crystallinity is high, stable structure, and the lithium vanadate anode material of production has good high rate performance and cycle performance.
Description
Technical field
The invention belongs to lithium battery material fields, and in particular to a kind of synthesis side of lithium vanadate as cathode material of lithium ion battery
Method.
Background technique
Currently, along with the rapid development of traffic, communication and the industrialization of information, electric car, laptop and movement
The products such as communication tool propose higher and very urgent requirement to Development of Novel electrochmical power source.Lithium ion battery is as a kind of
Novel green battery, since its operating voltage is high, light-weight, specific energy is big, self-discharge rate is small, has extended cycle life, memoryless
The advantages that effect, non-environmental-pollution, has at home and abroad formed one Study on Li-ion batteries upsurge.
And lamellar compound LiV3O8With excellent embedding lithium ability, there is specific capacity as cell positive material
High, the advantages that having extended cycle life；And lithium ion is in LiV3O8In diffusion ratio in V3O5 、V6O13Middle diffusion is fast.Along with
Up to the average voltage of 2.63V when, every mole of barium oxide LiV3O8Reversible lithium-inserting amount reach 3mol or more, so theoretically
LiV3O8Gram volume can achieve 372mAh/g.Due to these features, LiV3O8As into over year most it is promising just
One of pole material.
The preparation method of lithium vanadate includes solid phase method, liquid phase method etc. at present, and lithium vanadate capacity is in 200mAh/ in practical application
G or so, and atomic deposition technique is deposited into V on lithium source surface2O5Afterwards, then after pre-burning, calcining the lithium vanadate prepared, in state
It is inside and outside to have no relevant report.
Summary of the invention
The present invention provides a kind of synthetic method of lithium vanadate as cathode material of lithium ion battery.
The solution of the present invention is as follows:
A kind of synthetic method of lithium vanadate as cathode material of lithium ion battery comprising following steps:
(1) it pre-processes: lithium source material is dried；
(2) lithium source active site controls: dry lithium source material is put into the atomic layer deposition chamber that temperature is 120-160 DEG C
In body, then it is passed through pulse gas source into atomic layer deposition cavity, after then blowing extra pulse gas source off with high pure nitrogen, obtains
The lithium source substrate of surface passivation；
(3) atomic layer deposition cavity is carried out after being warming up to 200 DEG C, by ammonium metavanadate steam into atomic layer deposition cavity
Lithium source substrate carry out pulse 50-100s after, purged with high pure nitrogen；Then pulse 30-60s is carried out to lithium source substrate with oxygen
Afterwards, it is purged with high pure nitrogen；The pulse of repetitive cycling ammonium metavanadate steam, purging, pulse of oxygen, purging each 5-30 times, obtain five
V 2 O is uniformly deposited on the precursor A in passivation lithium source substrate；
(4) processing of precursor A: by precursor A in the 500-600 DEG C of pre-burning 5-10h under protective atmosphere, lithium vanadate is obtained
Then precursor B carries out deionized water washing to precursor B, filters, is dried, obtains after washing away extra lithium source material
Presoma C；
(5) lithium vanadate anode material is obtained after being put into protective atmosphere by presoma C, be sintered 8-16h under the conditions of 800-1000 DEG C
Material.
Further scheme, the lithium source material in the step (1) are one or both of lithium hydroxide, lithium acetate；Lithium
The drying of source material is to put it into 80-100 DEG C of baking 1-10h in baking oven.
Further scheme, the pulse gas source in the step (2) is ethyl alcohol or formaldehyde, and the burst length of pulse gas source is
30-50s。
Further scheme, lithium source material and ammonium metavanadate are the amounts by elemental lithium and vanadium substance in the step (3)
Than for (3-10): 1.
Further scheme, in the step (4) it is dry refer to the precursor B after washing is put into 80-100 DEG C of dry 1-
10h。
Further scheme, the protective atmosphere in the step (4), (5) is high pure nitrogen or high-purity argon gas.
Beneficial effects of the present invention:
Barium oxide is deposited on lithium source surface by the method for atomic deposition (ALD) by the present invention, due to atomic deposition
(ALD) the intrinsic deposition uniformity of technology is the chemisorption of saturation, so the growth of controllable vanadium source thickness, reaches accurate
Atomic ratio is controlled, and can be adulterated easily and interface correction.
The presoma obtained by atomic deposition (ALD) technology, then the lithium vanadate being sintered by high temperature solid-state method is just
Pole material, has the characteristics of crystallinity is high, stable structure, and the lithium vanadate anode material of production has good high rate performance and follows
Ring performance.
Detailed description of the invention
Fig. 1 is the SEM spectrum for the vanadic acid lithium material that embodiment 1 synthesizes；
Fig. 2 is 50 weeks cyclic curves of the electric battery of button that the vanadic acid lithium material that embodiment 1 synthesizes is assembled into.
Specific embodiment
Embodiment 1
(1) it pre-processes: lithium hydroxide material being put into 80 DEG C of baking 8h in baking oven, is put into after taking-up in dry reagent bottle
It seals spare；
(2) lithium source active site controls: lithium source material dry in step (1) is put into the atomic layer that temperature is 120 DEG C
It deposits in (ALD) cavity, then after 30s, is blown off into atomic layer deposition cavity with high pure nitrogen more using ethyl alcohol as pulse gas source
Remaining pulse gas source obtains the lithium hydroxide substrate of surface passivation；
(3) the ald chamber body that the lithium hydroxide substrate of passivation is loaded in step (2) is warming up to 200 DEG C, by ammonium metavanadate plus
Heat, as pulse gas source, after the burst length is 50s, purges 100s with high pure nitrogen to 145.8 DEG C of its vapour pressure temperature；Again by oxygen
Then gas purges 100s with high pure nitrogen, obtains five oxidations an of cycle period as pulse gas source, burst length 30s
Two vanadium are uniformly deposited in passivation lithium hydroxide substrate；Obtain the vanadic anhydride of 5 cycle periods the repetitive cycling period 5 times
The precursor A being deposited on lithium hydroxide；
(4) processing of precursor A: by precursor A in 500 DEG C of pre-burning 5h under high pure nitrogen, lithium vanadate presoma is obtained
B；Precursor B is washed with deionized water, is filtered, after washing away extra lithium hydroxide material, filter cake is put into 80 DEG C and is done
Dry 8h obtains dry presoma C；
(5) presoma C is put into after being sintered 8h at lower 800 DEG C of high pure nitrogen and obtains lithium vanadate anode material.
In conjunction with attached drawing, illustrate that lithium vanadate anode material object that the present invention is prepared mutually characterizes and electrochemistry with embodiment 1
Performance:
Fig. 1 is the SEM spectrum for the lithium vanadate anode material that embodiment 1 synthesizes, as can be seen from the figure the particle of lithium vanadate
It is uniform in size, do not occur agglomeration；And its grain diameter exists substantially in 100nm or so to be conducive to raising lithium vanadate
Electron transfer rate in charge and discharge process improves the performance of material electrochemical performance.
Fig. 2 is the cyclic curve figure for the electric battery of button that the lithium vanadate anode material that embodiment 1 synthesizes is assembled into, can from figure
To find out, under 0.2C multiplying power, capacity retention ratio is still maintained at 85.28% after experienced 50 weeks circulations, illustrates by the present invention
Atomic deposition (ALD) lithium vanadate anode material have good cyclical stability.
Embodiment 2
(1) it pre-processes: acetic acid lithium material being put into 100 DEG C of baking 10h in baking oven, is put into after taking-up in dry reagent bottle
It seals spare；
(2) lithium source active site controls: acetic acid lithium material dry in step (1) is put into 140 DEG C of temperature of atomic layer
It deposits in (ALD) cavity；It using formaldehyde as pulse gas source 50s, then blows extra pulse gas source off with high pure nitrogen, it is blunt to obtain surface
The lithium acetate substrate of change；
(3) the ald chamber body for being loaded with the lithium acetate substrate of passivation in step (2) is warming up to 200 DEG C, ammonium metavanadate is heated
100s pulse 80s, is purged with high pure nitrogen as pulse gas source to 145.8 DEG C of its vapour pressure temperature；Again using oxygen as arteries and veins
Qi of chong channel ascending adversely source purges 100s with high pure nitrogen after pulse 50s, obtain a cycle period vanadic anhydride be uniformly deposited on it is blunt
In the lithium acetate substrate of change；The repetitive cycling period, 15 vanadic anhydrides for obtaining 15 cycle periods were deposited on acetic acid lithium material
On precursor A；
(4) processing of precursor A: by the precursor A of step (3) in 600 DEG C of pre-burning 8h under high-purity argon gas, vanadic acid is obtained
Precursor B is washed with deionized water, is filtered by lithium precursor B, washes away extra lithium source material, and filter cake is put into 100 DEG C
Dry 8h obtains the dry presoma C of lithium vanadate；
(5) presoma C is put into after being sintered 12h at lower 900 DEG C of high-purity argon gas and obtains lithium vanadate anode material.
Capacity retention ratio is 89.01% after the lithium vanadate anode material 50 weeks circulations that the present embodiment 2 synthesizes.
Embodiment 3
(1) it pre-processes: lithium hydroxide material being put into 90 DEG C of baking 10h in baking oven, dry reagent bottle is put into after taking-up
Middle sealing is spare；
(2) lithium source active site controls: lithium source material dry in step (1) is put into atomic layer deposition (ALD) cavity
In, cavity temperature is heated to 160 DEG C, and using ethyl alcohol as pulse gas source, using high pure nitrogen as carrier gas, the burst length of pulse gas source is
30s, then blow extra pulse gas source off with high pure nitrogen, obtain the lithium hydroxide substrate of surface passivation；
(3) the ald chamber body that the lithium hydroxide substrate of passivation is loaded in step (2) is warming up to 200 DEG C, by ammonium metavanadate plus
Burst length 50s, heat purges 100s with high pure nitrogen as pulse gas source to 145.8 DEG C of its vapour pressure temperature；Again by oxygen
Burst length 50s, gas purges 100s with high pure nitrogen, obtains the vanadic anhydride of a cycle period as pulse gas source
It is uniformly deposited in passivation lithium hydroxide substrate；The repetitive cycling period 20 times the vanadic anhydride for obtaining 20 cycle periods sinks
Precursor A of the product on lithium hydroxide；
(4) processing of precursor A: by the precursor A of step (3) in 600 DEG C of pre-burning 9h under high pure nitrogen, vanadic acid is obtained
Precursor B is washed with deionized water, is filtered by lithium precursor B, washes away extra lithium hydroxide material, filter cake is put into
90 DEG C of dry 10h obtain the dry presoma C of lithium vanadate；
(5) presoma C is put into after being sintered 16h at lower 900 DEG C of high pure nitrogen and obtains lithium vanadate anode material.
Capacity retention ratio is 90.34% after the lithium vanadate anode material 50 weeks circulations that the present embodiment 3 synthesizes.
Embodiment 4
(1) it pre-processes: acetic acid lithium material being put into 90 DEG C of baking 10h in baking oven, is put into after taking-up in dry reagent bottle
It seals spare；
(2) lithium source active site controls: acetic acid lithium material dry in step (1) is put into atomic layer deposition (ALD) chamber
In body, cavity temperature is heated to 150 DEG C, using formaldehyde as pulse gas source, using high pure nitrogen as carrier gas, and the burst length of pulse gas source
It for 50s, then blows extra pulse gas source off with high pure nitrogen, obtains the lithium acetate substrate of surface passivation；
(3) the ald chamber body for being loaded with the lithium acetate substrate of passivation in step (2) is warming up to 200 DEG C, ammonium metavanadate is heated
100s burst length 80s, is purged with high pure nitrogen as pulse gas source to 145.8 DEG C of its vapour pressure temperature；Again by oxygen
As pulse gas source, 100s burst length 40s, is purged with high pure nitrogen, the vanadic anhydride for obtaining a cycle period is equal
Even is deposited in passivation lithium source substrate；The repetitive cycling period, 25 vanadic anhydrides for obtaining 25 cycle periods were deposited on vinegar
The precursor A of sour lithium material；
(4) processing of precursor A: by the precursor A of step (3) in 550 DEG C of pre-burning 10h under protective atmosphere, vanadium is obtained
Precursor B is washed with deionized water, is filtered by sour lithium precursor B, washes away extra lithium source material, filter cake is put into 100
DEG C dry 10h, obtains the dry presoma C of lithium vanadate；
(5) presoma C is put into after being sintered 12h at lower 1000 DEG C of protective atmosphere and obtains lithium vanadate anode material.
Capacity retention ratio is 86.06% after the lithium vanadate anode material synthesized by embodiment 4 50 weeks circulations.
Embodiment 5
(1) it pre-processes: lithium hydroxide material being put into 100 DEG C of baking 10h in baking oven, dry reagent bottle is put into after taking-up
Middle sealing is spare；
(2) lithium source active site controls: lithium hydroxide material dry in step (1) is put into atomic layer deposition (ALD)
In cavity, cavity temperature is heated to 160 DEG C, using formaldehyde as pulse gas source, using high pure nitrogen as carrier gas, when the pulse of pulse gas source
Between be 50s, then blow extra pulse gas source off with high pure nitrogen, obtain the lithium hydroxide substrate of surface passivation；
(3) the ald chamber body that the lithium hydroxide substrate of passivation is loaded in step (2) is warming up to 200 DEG C, by ammonium metavanadate plus
Burst length 100s, heat purges 100s with high pure nitrogen as pulse gas source to 145.8 DEG C of its vapour pressure temperature；Again by oxygen
Burst length 60s, gas purges 100s with high pure nitrogen, obtains the vanadic anhydride of a cycle period as pulse gas source
It is uniformly deposited in passivation lithium source substrate；The repetitive cycling period, 30 vanadic anhydrides for obtaining 30 cycle periods were deposited on
The precursor A of lithium hydroxide material；
(4) processing of precursor A: by the precursor A of step (3) in 600 DEG C of pre-burning 10h under protective atmosphere, vanadium is obtained
Precursor B is washed with deionized water, is filtered by sour lithium precursor B, washes away extra lithium source material, filter cake is put into 100
DEG C dry 10h, obtains the dry presoma C of lithium vanadate；
(5) presoma C is put into after being sintered 16h at lower 1000 DEG C of protective atmosphere and obtains lithium vanadate anode material.
Capacity retention ratio is 84.78% after the lithium vanadate anode material 50 weeks circulations that the present embodiment 5 synthesizes.
Above content is only to structure of the invention example and explanation, affiliated those skilled in the art couple
Described specific embodiment does various modifications or additions or is substituted in a similar manner, without departing from invention
Structure or beyond the scope defined by this claim, is within the scope of protection of the invention.
Claims (6)
1. a kind of synthetic method of lithium vanadate as cathode material of lithium ion battery, it is characterised in that: the following steps are included:
(1) it pre-processes: lithium source material is dried；Lithium source material is one or both of lithium hydroxide, lithium acetate；
(2) lithium source active site controls: dry lithium source material is put into the atomic layer deposition cavity that temperature is 120-160 DEG C
In, then pulse gas source is passed through into atomic layer deposition cavity, after then blowing extra pulse gas source off with high pure nitrogen, obtain table
The lithium source substrate of face passivation；The pulse gas source be ethyl alcohol or formaldehyde,
(3) atomic layer deposition cavity is carried out after being warming up to 200 DEG C, by ammonium metavanadate steam to the intracorporal lithium of atomic layer deposition chamber
After source substrate carries out pulse 50-100s, purged with high pure nitrogen；Then after carrying out pulse 30-60s to lithium source substrate with oxygen,
It is purged with high pure nitrogen；The pulse of repetitive cycling ammonium metavanadate steam, purging, pulse of oxygen, purging each 5-30 times, obtain five oxidations
Two vanadium are uniformly deposited on the precursor A in passivation lithium source substrate；
(4) processing of precursor A: by precursor A in the 500-600 DEG C of pre-burning 5-10h under protective atmosphere, lithium vanadate forerunner is obtained
Then body B carries out deionized water washing to precursor B, filters, is dried after washing away extra lithium source material, obtains drying
Presoma C；
(5) lithium vanadate anode material is obtained after being put into protective atmosphere by presoma C, be sintered 8-16h under the conditions of 800-1000 DEG C.
2. the synthetic method of lithium vanadate as cathode material of lithium ion battery according to claim 1, it is characterised in that: the step
Suddenly the drying of the lithium source material in (1) is to put it into 80-100 DEG C of baking 1-10h in baking oven.
3. the synthetic method of lithium vanadate as cathode material of lithium ion battery according to claim 1, it is characterised in that: the step
Suddenly the burst length of the pulse gas source in (2) is 30-50s.
4. the synthetic method of lithium vanadate as cathode material of lithium ion battery according to claim 1, it is characterised in that: the step
Suddenly it is (3-10) that lithium source material and ammonium metavanadate, which are by elemental lithium and vanadium the mass ratio of the material, in (3): 1.
5. the synthetic method of lithium vanadate as cathode material of lithium ion battery according to claim 1, it is characterised in that: the step
Suddenly in (4) it is dry refer to the precursor B after washing is put into 80-100 DEG C of dry 1-10h.
6. according to the synthetic method of lithium vanadate as cathode material of lithium ion battery described in claim 1, it is characterised in that: the step
(4), the protective atmosphere in (5) is high pure nitrogen or high-purity argon gas.
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| CN107799754A (en) * | 2017-10-31 | 2018-03-13 | 湖南国盛石墨科技有限公司 | A kind of preparation method of fluorophosphoric acid vanadium lithium/fluorinated graphene composite positive pole |
| CN109888269A (en) * | 2018-12-29 | 2019-06-14 | 广东邦普循环科技有限公司 | A kind of pretreated method of ternary material mixing |
| CN110643973B (en) * | 2019-11-13 | 2021-11-23 | 西安近代化学研究所 | NaV2O5Preparation method of crystal film |
| CN114142035A (en) * | 2021-11-23 | 2022-03-04 | 万华化学(四川)有限公司 | Cobalt-free ternary cathode material, and preparation method and application thereof |
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| CN104681784A (en) * | 2015-02-10 | 2015-06-03 | 华中科技大学 | Lithium vanadate anode material, anode, battery and anode material preparation method |
| CN105870445A (en) * | 2016-05-06 | 2016-08-17 | 合肥国轩高科动力能源有限公司 | Method for synthesizing lithium vanadate/carbon/nitrogen-doped graphene serving as lithium ion battery cathode composite material |
| CN105958029A (en) * | 2016-06-24 | 2016-09-21 | 合肥国轩高科动力能源有限公司 | Preparation method for Li<3>VO<4>/carbon nano tube/carbon anode composite material of lithium ion battery |
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| CN104681784A (en) * | 2015-02-10 | 2015-06-03 | 华中科技大学 | Lithium vanadate anode material, anode, battery and anode material preparation method |
| CN105870445A (en) * | 2016-05-06 | 2016-08-17 | 合肥国轩高科动力能源有限公司 | Method for synthesizing lithium vanadate/carbon/nitrogen-doped graphene serving as lithium ion battery cathode composite material |
| CN105958029A (en) * | 2016-06-24 | 2016-09-21 | 合肥国轩高科动力能源有限公司 | Preparation method for Li<3>VO<4>/carbon nano tube/carbon anode composite material of lithium ion battery |
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