CN109728273A - The preparation method of anode material of lithium-ion battery titanium phosphate sodium double nano carbon - Google Patents
The preparation method of anode material of lithium-ion battery titanium phosphate sodium double nano carbon Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of anode material of lithium-ion battery titanium phosphate sodium double nano carbon, prepare the NaTi with nano-scale using sol-gal process combination Freeze Drying Technique and rapid microwave radiant heating method2(PO4)3Particle, meanwhile, the NaTi with specific microscopic appearance has been designed and synthesized in conjunction with in-situ compositing2(PO4)3Compound nano material, improves NaTi with double nano carbon material (carbon film and sulfur doping graphene)2(PO4)3Storage sodium performance.The synthetic method large scale preparation can go out the NaTi of high quality in a short time2(PO4)3@double nano carbon composite electrode material, this synthetic route is in design construction nano-grade size NaTi2(PO4)3It is a kind of completely new and effective method in terms of@carbon composite electrode material.
Description
Technical field
The present invention relates to sodium ion battery electrode material preparation fields, and in particular to a kind of anode material of lithium-ion battery phosphorus
The preparation method of sour titanium sodium double nano carbon.
Background technique
The mankind have stimulated giving more sustained attention of supplying of global energy to a certain extent has recyclable charge and discharge, Gao Rong
The development of the energy reserves technology of the advantages that amount, long circulation life and low cost.Currently, lithium ion battery has been developed as most
One of promising energy technology, it has been obtained extensively in fields such as portable electronic product, hybrid vehicle, pure electric automobiles
General application.However, causing the further development of lithium ion battery to be limited due at high cost and lithium resource is deficient
System.In recent years, scientific research personnel always searched for a kind of competitive energy technology that can substitute lithium ion battery, sodium from
Sub- battery becomes the focus of people's research hot spot because of its low cost and sodium resource abundant and has obtained quick hair in a short time
Exhibition.However, insertion and abjection resistance of the sodium ion in electrode material lattice are big since sodium ion radius is larger, lead to electrode
The storage sodium performance of material is poor.Therefore, more and more researchers, which start to put into a large amount of energy, carrys out the high property of developmental research
Sodium-ion battery anode/negative electrode material of energy.
Polyanionic compound N aTi2(PO4)3Because having, security performance is prominent, thermal stability is good, theoretical specific capacity is high
The advantages that high with sodium ion conductivity, it is considered to be one of most promising anode material of lithium-ion battery.NaTi2
(PO4)3The quick transmission that the intracell of electrode material has biggish gap duct to be thus suitble to sodium ion is a kind of excellent
Fast ion conducting material.NaTi2(PO4)3Typical NASICON framework is by pinpointing shared PO4Tetrahedron and TiO6It is octahedra
It is composed that there is " beacon " unit to constitute, form Three-dimensional Open ion transport channel.This special Three-dimensional Open structural frames
Frame has high ionic conductivity and chemical stability, belongs to " zero strain " material, can satisfy to the electrode material long circulating longevity
The requirement of life.However, pure phase NaTi2(PO4)3Compound is due to TiO disconnected from each other6Octahedron cause in it electronics electricity
Conductance is poor, is similar to Li3V2(PO4)3And Na3V2(PO4)3.The disadvantage leads to NaTi2(PO4)3The charge and discharge of negative electrode material are reversible
The problems such as property is poor, high rate performance is undesirable, cyclical stability is poor, limits this electrode material in high-performance sodium-ion battery
Further practical application.In order to overcome NaTi2(PO4)3The above problem existing for negative electrode material, vast researcher investment
A large amount of energy has carried out to it positive modified attempt.It so far, can not also be by NaTi2(PO4)3The storage of negative electrode material
Sodium performance boost continually looks for significantly more efficient route of synthesis and modification mode to NaTi to actual application level2(PO4)3Electricity
Chemical property, which is regulated and controled and optimizes to be still, currently needs the research direction furtherd investigate.
Summary of the invention
To solve the above problems, the present invention provides a kind of systems of anode material of lithium-ion battery titanium phosphate sodium double nano carbon
Preparation Method, with NaTi2(PO4)3Electrode material is main study subject, for the low disadvantage of the material electronics electrical conductivity, is used
Sol-gal process combination Freeze Drying Technique and rapid microwave radiant heating method prepare the NaTi with nano-scale2
(PO4)3Particle.In conjunction with in-situ compositing, the NaTi with specific microscopic appearance has been designed and synthesized2(PO4)3@double nano carbon (carbon
Film and sulfur doping graphene) compound nano material.The present invention is NaTi2(PO4)3Design, synthesis and the modification of negative electrode material are ground
Study carefully and a kind of new thinking and approach are provided, to NaTi2(PO4)3The further exploitation of material has important scientific guidance meaning:
The present invention is realized especially by following technical scheme:
The preparation method of anode material of lithium-ion battery titanium phosphate sodium double nano carbon passes through sol-gal process, freeze-drying
The mode of technology and rapid microwave radiant heating, quickly and effectively prepares composite nano-electrode material, comprising the following steps:
S1, graphene oxide preparation:
The crystalline flake graphite that 1.5g partial size is 300 mesh, 0.75g NaNO are added into 250mL beaker3, the 35mL concentrated sulfuric acid sets
After reacting 1.5~3 hours in 0~4 DEG C of ice-water bath, it is slowly added to 4.5g KMnO4, keep ice-water bath to handle 2 hours, then
It is transferred in 35 DEG C of water-bath, after reaction 2 hours, beaker is taken out from ice-water bath, 50mL is slowly added into beaker and steams
Then the hydrogen peroxide that 7.5~8mL mass fraction is 30% is added into beaker, obtains golden yellow precipitate, as oxygen for distilled water dilution
Graphite；
S2, beaker is stood into 1~2 hour, until graphite oxide is precipitated to below beaker, removes supernatant, take oxidation
It after aquadag is washed repeatedly with 5% hydrochloric acid solution, adopts and is washed with distilled water to solution and is in neutrality, be centrifugated, by what is obtained
Graphite oxide precipitating, which is placed in 80 DEG C of drying boxes, to be dried for 24 hours；
S3, take 100mg dry after graphene oxide the ethanol solution of 40mL is dispersed in through ultrasonic disperse and magnetic agitation
In, 50mg diphenyl disulfide dopant is added, magnetic agitation is incited somebody to action to mixture in after drying regime under conditions of 60~70 DEG C
It is placed in the tube furnace full of argon gas, 600 DEG C be heat-treated 2 hours, then by resulting sulfur doping graphite ene product spend from
Sub- water and ethyl alcohol cleaning are several times neutrality to filtrate, are placed in 50~60 DEG C of low temperature dryings in baking oven；
S3、NaTi2(PO4)3The preparation of@double nano carbon composite
By reactant sodium carbonate, butyl titanate, ammonium dihydrogen phosphate, citric acid, ethyl alcohol stoichiometrically 1: 4: 6: 1~
6: 100~3000 are mixed to form clear solution, and suitable sulfur doping graphene is then added, and sulfur doping graphene dosage is
NaTi2(PO4)35~20wt% of theoretical yield by above-mentioned mixed system ultrasonic vibration, and is sufficiently stirred and to form clear solution；
By resulting clear solution side magnetic agitation, while being progressively heated at 60~80 DEG C, keep ethyl alcohol and deionized water continuous
Volatilization, until forming gel to get sol precursor；
S4, it after by the sol precursor of above-mentioned preparation, low temperature is sufficiently dry under vacuum by the way of freeze-drying, sets
In NaTi can be obtained in 4~12 hours in 750~760 DEG C of sintering under conditions of argon gas is protected in microwave tube type oven2(PO4)3@is bis-
Nano-carbon material composite negative pole material.
The invention has the following advantages:
(1) sol-gal process combination Freeze Drying Technique and rapid microwave radiant heating method are used for the first time, and are combined
In-stiu coating method prepares NaTi2(PO4)3@double nano carbon composite electrode material.The synthetic method incorporates collosol and gel and is easy to
Prepare nano particle, freeze-drying destruction, microwave irradiation technology reaction time do not generated to presoma microstructure short, Yi Jiyuan
The advantage that position is evenly coated and interface cohesion is strong.Large scale preparation it can go out the NaTi of high quality in a short time2(PO4)3@is bis-
Nano Carbon electrode material, this synthetic route is in design construction nano-grade size NaTi2(PO4)3The carbon composite electrode material side@
Face is a kind of completely new and effective method.
(2) select the sulfur doping graphene with excellent electric conductivity, high chemical stability and bigger serface as carrier
And additive can form the space with high conductance in conjunction with the carbon film that electrode material surface coats in the composite
Network structure preferably resolves NaTi2(PO4)3The low problem of negative electrode material electronic conductivity, to substantially increase electrode
The high rate capability and cyclical stability of material are NaTi2(PO4)3The industrialization of negative electrode material is laid a good foundation.
Detailed description of the invention
Fig. 1 is NaTi2(PO4)3@double nano carbon composite electrode material preparation flow figure.
Fig. 2 is NaTi2(PO4)3The TEM photo (a, b, c) of@double nano carbon composite electrode material.
Fig. 3 is NaTi2(PO4)3The CV curve of@double nano carbon composite electrode.
Fig. 4 is NaTi2(PO4)3The charge-discharge performance of@double nano carbon composite electrode material.
Fig. 5 is NaTi2(PO4)3The high rate performance and cyclical stability of@double nano carbon composite electrode.
Specific embodiment
In order to which objects and advantages of the present invention are more clearly understood, the present invention is carried out with reference to embodiments further
It is described in detail.It should be appreciated that described herein, specific examples are only used to explain the present invention, is not intended to limit the present invention.
As shown in Figure 1, the embodiment of the invention provides a kind of anode material of lithium-ion battery titanium phosphate sodium double nano carbon
Preparation method includes the following steps:
(1) graphene oxide is prepared
Using high quality crystalline flake graphite as initial feed, graphene oxide is prepared using improved Hummers method.
(2) sulfur doping graphene is prepared
Resulting graphene oxide is dispersed in ethanol solution with a certain concentration, it is certain through ultrasonic disperse and magnetic agitation
After time be added diphenyl disulfide dopant, then under specific temperature conditions magnetic agitation to drying regime and in be full of argon gas
Tube furnace in high-temperature heat treatment certain time.Finally sulfur doping graphite ene product deionized water and ethyl alcohol are cleaned several
It is secondary, it is placed in low temperature drying in baking oven.
(3) preparation of Gel Precursor
Pure phase NaTi is prepared by sol-gal process combination Freeze Drying Technique and rapid microwave radiant heating method2
(PO4)3Electrode material realizes nanometer NaTi2(PO4)3Particle external sheath carbon film and the double of sulfur doping graphene conductive network receive
The preparation of rice carbon composite electrode material.Its specific synthetic route is as follows: by reactant sodium carbonate, butyl titanate, biphosphate
Ammonium, citric acid, ethyl alcohol stoichiometrically 1: 4: 6: 0.5~4: 100~1800 are mixed to form clear solution, are then added appropriate
Sulfur doping graphene, sulfur doping graphene dosage be NaTi2 (PO4) 3 theoretical yield 5~20wt%.By above-mentioned mixture
It is ultrasonic vibration, and is sufficiently stirred and to form clear solution；
(4) it fires
After low temperature is sufficiently dry under vacuum by the way of freeze-drying by resulting sol precursor, it is placed in microwave tube
NaTi can be obtained in 4~12 hours in 750~760 DEG C of sintering under conditions of argon gas protection in formula furnace2(PO4)3@double nano carbon materials
Expect composite negative pole material.
The present invention is in the NaTi with nano-scale2(PO4)3Material surface coats certain thickness carbon film and can significantly mention
The conductivity of high particle, by that can go out after introducing sulfur doping graphene in the internal build of composite material with carbon film and sulfur doping
High conductivity spatial network based on graphene, this will greatly promote NaTi2(PO4)3The multiplying power and cyclicity of negative electrode material
Energy.
Embodiment
S1, graphene oxide preparation:
The crystalline flake graphite that 1.5g partial size is 300 mesh, 0.75g NaNO are added into 250mL beaker3, the 35mL concentrated sulfuric acid sets
After reacting 1.5~3 hours in 0~4 DEG C of ice-water bath, it is slowly added to 4.5g KMnO4, keep ice-water bath to handle 2 hours, then
It is transferred in 35 DEG C of water-bath, after reaction 2 hours, the dilution of 50mL distilled water is slowly added into beaker, finally into beaker
The hydrogen peroxide that 7.5mL mass fraction is 30% is added, obtains golden yellow precipitate, as graphite oxide；
S2, beaker is stood into 1~2 hour, until graphite oxide is precipitated to below beaker, removes supernatant, take oxidation
It after aquadag is washed repeatedly with 5% hydrochloric acid solution, adopts and is washed with distilled water to solution and is in neutrality, be centrifugated, by what is obtained
Graphite oxide precipitating, which is placed in 80 DEG C of drying boxes, to be dried for 24 hours；
S3, take 100mg dry after graphene oxide the ethanol solution of 40mL is dispersed in through ultrasonic disperse and magnetic agitation
In, 50mg diphenyl disulfide dopant is added, under the conditions of 60~70 DEG C magnetic agitation to mixture in after drying regime, by it
It is placed in the tube furnace full of argon gas, 600 DEG C are heat-treated 2 hours, then by resulting sulfur doping graphite ene product deionization
Water and ethyl alcohol cleaning are several times neutrality to filtrate, are placed in 50~60 DEG C of low temperature dryings in baking oven；
S3、NaTi2(PO4)3The preparation of@double nano carbon composite
100mg sulfur doping graphene and 480mg citric acid are added in the ethyl alcohol of 150mL respectively, ultrasonic vibration 3 hours
Afterwards, the butyl titanate of 5.1mL is added to after 1.5h is sufficiently stirred in said mixture, by 25mL dissolved with 2588.3mg phosphoric acid
The aqueous solution of ammonium dihydrogen is slowly added to, then again by 15mL dissolved with the Na of 397.5mg2CO3Aqueous solution be slowly added to, sufficiently stir
It mixes to form clear solution；
Resulting clear solution is progressively heated at 60~80 DEG C in magnetic agitation, waves ethyl alcohol and deionized water constantly
Hair, until forming gel to get sol precursor；
S4, by the sol precursor of above-mentioned preparation, low temperature is sufficiently dry under vacuum by the way of freeze-drying；Finally
Presoma is placed in microwave tube type oven 750 DEG C of sintering under protection of argon gas and obtains NaTi within 12 hours2(PO4)3@double nano carbon materials
Expect composite negative pole material.
Product is tested by multiple means, is analyzed.And electrode material is assembled into the research of CR2032 coin battery
NaTi2(PO4)3@double nano carbon electrode and battery performance.Contain NaTi by coating on copper foil2(PO4)3@double nano carbon is multiple
The slurry of composite electrode material (85wt%), carbon black (8wt%) and PVDF (7wt%) carrys out preparation work electrode.Then, electrode is existed
It is 24 hours dry at 110 DEG C, and it is cut into the disk that diameter is 12mm.NaTi2(PO4)3The dosage of@double nano carbon is 1.9mg.cm-2.Finally, using Na as to electrode, the NaClO of 1M in glove box4(EC: DEC volume ratio is 1: 1) is used as electrolyte.By
CHI600a type electrochemical workstation and Land battery test system test electrode and battery performance.NaTi2(PO4)3@double nano carbon
Cathode is in 1.5 and 3.0V voltage range, 0.2mVs-1Chemical property under sweep speed is as shown in Fig. 2, oxidation peak and reduction
The voltage difference at peak is about 0.17V, shows that double nano carbon coating network has satisfactory electrical conductivity, NaTi2(PO4)3@double nano carbon is negative
Pole shows the electrode polarization and good invertibity of very little.Gap very little in Fig. 3 between charge and discharge also illustrates compound pair
Nano-sized carbon may advantageously facilitate electronics and Na+Transmission.NaTi2(PO4)3The coin battery of@double nano carbon composite electrode material assembling
High rate performance and cycle performance test results are shown in figure 5.In 0.2,0.5,1,2,4,6 and 8C, cathode specific capacity difference
For 124,122,119,116,111,104 and 96mAh g-1, show excellent high rate performance.Even if in 10C, NaTi2
(PO4)3@double nano carbon composite remains to show 88mAhg-1Specific capacity.Furthermore, it is possible to find, NaTi2(PO4)3@is bis-
Nano-sized carbon also shows stable cycle characteristics under each current rate.Therefore NaTi2(PO4)3@double nano carbon negative pole material
The high rate performance and cyclical stability being excellent in.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the principle of the present invention, it can also make several improvements and retouch, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (2)
1. the preparation method of anode material of lithium-ion battery titanium phosphate sodium double nano carbon, which comprises the following steps:
S1, graphene oxide preparation:
The crystalline flake graphite that 1.5g partial size is 300 mesh, 0.75g NaNO are added into 250mL beaker3, the 35mL concentrated sulfuric acid is placed in 0~4
DEG C ice-water bath in react 1.5~3 hours after, be slowly added to 4.5g KMnO4, keep ice-water bath to handle 2 hours, transfer to
In 35 DEG C of water-bath, after reaction 2 hours, beaker is taken out from ice-water bath, it is dilute that 50mL distilled water is slowly added into beaker
It releases, the hydrogen peroxide that 7.5~8mL mass fraction is 30% is then added into beaker, obtains golden yellow precipitate, as oxidation stone
Ink；
S2, beaker is stood into 1~2 hour, until graphite oxide is precipitated to below beaker, removes supernatant, take graphite oxide
Precipitating with 5% hydrochloric acid solution wash it is multiple after, adopt and be washed with distilled water to solution and be in neutrality, centrifuge separation, the oxidation that will be obtained
Aquadag is placed in 80 DEG C of drying boxes and dries for 24 hours；
S3, it takes the graphene oxide after 100mg drying to be dispersed in the ethanol solution of 40mL through ultrasonic disperse and magnetic agitation, adds
Enter 50mg diphenyl disulfide dopant, magnetic agitation is set to mixture in after drying regime under conditions of 60~70 DEG C
In in the tube furnace full of argon gas, 600 DEG C are heat-treated 2 hours, then by resulting sulfur doping graphite ene product deionized water
It is several times neutrality to filtrate with ethyl alcohol cleaning, is placed in 50~60 DEG C of low temperature dryings in baking oven；
S3、NaTi2(PO4)3The preparation of@double nano carbon composite
By reactant sodium carbonate, butyl titanate, ammonium dihydrogen phosphate, citric acid, ethyl alcohol stoichiometrically 1: 4: 6: 1~6:
100~3000 are mixed to form clear solution, and suitable sulfur doping graphene is then added, by above-mentioned mixed system ultrasonic vibration,
And it is sufficiently stirred and to form clear solution；
By resulting clear solution side magnetic agitation, while being progressively heated at 60~80 DEG C, ethyl alcohol and deionized water is made constantly to volatilize,
Until forming gel to get sol precursor；
S4, it after by the sol precursor of above-mentioned preparation, low temperature is sufficiently dry under vacuum by the way of freeze-drying, is placed in micro-
NaTi can be obtained in 4~12 hours in 750~760 DEG C of sintering under conditions of argon gas protection in wave tube furnace2(PO4)3@double nano
Carbon material composite negative pole material.
2. the preparation method of anode material of lithium-ion battery titanium phosphate sodium double nano carbon as described in claim 1, feature exist
In in the step S3, sulfur doping graphene dosage is NaTi2(PO4)35~20wt% of theoretical yield.
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| CN110649242A (en) * | 2019-09-27 | 2020-01-03 | 广东工业大学 | Sodium titanium phosphate composite electrode material, preparation method thereof and battery |
| CN110880590A (en) * | 2019-11-26 | 2020-03-13 | 福州大学 | Carbon nitride and carbon-coated NASICON type electrode material and preparation method thereof |
| CN111547731A (en) * | 2020-05-20 | 2020-08-18 | 西安工业大学 | Three-dimensional carbon nano tube composite lithium iron silicate microsphere and preparation method thereof |
| CN113247962A (en) * | 2021-06-26 | 2021-08-13 | 深圳中科精研科技有限公司 | Battery anode material and method for rapidly synthesizing battery anode material |
| CN113764620A (en) * | 2021-09-13 | 2021-12-07 | 合肥国轩高科动力能源有限公司 | Preparation method of carbon-coated sodium titanium phosphate material, prepared carbon-coated sodium titanium phosphate material and application |
| CN114824207A (en) * | 2022-04-18 | 2022-07-29 | 中国科学技术大学 | Preparation method of hollow nano cube for cathode material of water system sodium ion battery |
| CN115504447A (en) * | 2022-09-22 | 2022-12-23 | 浙江格派钴业新材料有限公司 | Preparation method of lithium titanate coated ferric sodium pyrophosphate composite material |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110649242A (en) * | 2019-09-27 | 2020-01-03 | 广东工业大学 | Sodium titanium phosphate composite electrode material, preparation method thereof and battery |
| CN110880590A (en) * | 2019-11-26 | 2020-03-13 | 福州大学 | Carbon nitride and carbon-coated NASICON type electrode material and preparation method thereof |
| CN110880590B (en) * | 2019-11-26 | 2022-10-28 | 福州大学 | Carbon nitride and carbon-coated NASICON type electrode material and preparation method thereof |
| CN111547731A (en) * | 2020-05-20 | 2020-08-18 | 西安工业大学 | Three-dimensional carbon nano tube composite lithium iron silicate microsphere and preparation method thereof |
| CN113247962A (en) * | 2021-06-26 | 2021-08-13 | 深圳中科精研科技有限公司 | Battery anode material and method for rapidly synthesizing battery anode material |
| CN113764620A (en) * | 2021-09-13 | 2021-12-07 | 合肥国轩高科动力能源有限公司 | Preparation method of carbon-coated sodium titanium phosphate material, prepared carbon-coated sodium titanium phosphate material and application |
| CN114824207A (en) * | 2022-04-18 | 2022-07-29 | 中国科学技术大学 | Preparation method of hollow nano cube for cathode material of water system sodium ion battery |
| CN115504447A (en) * | 2022-09-22 | 2022-12-23 | 浙江格派钴业新材料有限公司 | Preparation method of lithium titanate coated ferric sodium pyrophosphate composite material |
| CN115504447B (en) * | 2022-09-22 | 2023-06-20 | 乐普钠电(上海)技术有限公司 | Preparation method of lithium titanate coated sodium ferric pyrophosphate composite material |
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