CN104733731B - The method preparing uniform carbon coating vanadium phosphate sodium material - Google Patents
The method preparing uniform carbon coating vanadium phosphate sodium material Download PDFInfo
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- CN104733731B CN104733731B CN201510133080.2A CN201510133080A CN104733731B CN 104733731 B CN104733731 B CN 104733731B CN 201510133080 A CN201510133080 A CN 201510133080A CN 104733731 B CN104733731 B CN 104733731B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 28
- 239000000463 material Substances 0.000 title claims abstract description 28
- 239000011248 coating agent Substances 0.000 title claims abstract description 27
- 238000000576 coating method Methods 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 26
- ZMVMBTZRIMAUPN-UHFFFAOYSA-H [Na+].[V+5].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O Chemical compound [Na+].[V+5].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O ZMVMBTZRIMAUPN-UHFFFAOYSA-H 0.000 title claims abstract description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 25
- 239000011734 sodium Substances 0.000 claims abstract description 17
- 229910020657 Na3V2(PO4)3 Inorganic materials 0.000 claims abstract description 16
- 229910052786 argon Inorganic materials 0.000 claims abstract description 14
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 13
- NYHBQMYGNKIUIF-UUOKFMHZSA-N Guanosine Chemical compound C1=NC=2C(=O)NC(N)=NC=2N1[C@@H]1O[C@H](CO)[C@@H](O)[C@H]1O NYHBQMYGNKIUIF-UUOKFMHZSA-N 0.000 claims abstract description 12
- 239000008103 glucose Substances 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 9
- MIKUYHXYGGJMLM-GIMIYPNGSA-N Crotonoside Natural products C1=NC2=C(N)NC(=O)N=C2N1[C@H]1O[C@@H](CO)[C@H](O)[C@@H]1O MIKUYHXYGGJMLM-GIMIYPNGSA-N 0.000 claims abstract description 6
- NYHBQMYGNKIUIF-UHFFFAOYSA-N D-guanosine Natural products C1=2NC(N)=NC(=O)C=2N=CN1C1OC(CO)C(O)C1O NYHBQMYGNKIUIF-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000012153 distilled water Substances 0.000 claims abstract description 6
- 229940029575 guanosine Drugs 0.000 claims abstract description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 6
- 239000000725 suspension Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000013019 agitation Methods 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 4
- 229910017677 NH4H2 Inorganic materials 0.000 claims abstract description 3
- 229910003206 NH4VO3 Inorganic materials 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 3
- 239000002453 shampoo Substances 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 11
- 239000008187 granular material Substances 0.000 abstract description 5
- 238000005245 sintering Methods 0.000 abstract description 5
- 238000005054 agglomeration Methods 0.000 abstract description 3
- 230000002776 aggregation Effects 0.000 abstract description 3
- 229910001415 sodium ion Inorganic materials 0.000 description 7
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 6
- 238000005253 cladding Methods 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 4
- 239000002228 NASICON Substances 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 3
- 235000009392 Vitis Nutrition 0.000 description 2
- 241000219095 Vitis Species 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- OHVGNSMTLSKTGN-BTVCFUMJSA-N [C].OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O Chemical compound [C].OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O OHVGNSMTLSKTGN-BTVCFUMJSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005858 glycosidation reaction Methods 0.000 description 1
- 239000010416 ion conductor Substances 0.000 description 1
- 230000037427 ion transport Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
Classifications
-
- 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
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- Battery Electrode And Active Subsutance (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention provides a kind of method preparing uniform carbon coating vanadium phosphate sodium material；By V2O5、NH4H2PO4And Na2CO3Or NH4VO3、H3PO4And Na2CO3It is dissolved in distilled water；Na3V2(PO4)3Mol ratio with glucose is 2:3～4:3 mix homogeneously；Above-mentioned solution is transferred in hydrothermal reaction kettle, carries out reaction of guanosine；Drive kettle after cooling down under room temperature, so that it is uniformly dispersed by ultrasonic for the suspension obtaining, then magnetic agitation transpiring moisture obtains colloidal sol under water-bath, colloidal sol is dried to obtain gel in an oven；Above-mentioned gel is fully ground and pre-burning in argon；It is fully ground again, calcining in argon obtains the Na of uniform carbon coating3V2(PO4)3Material.Add carbon source glucose in water-heat process, make particle surface wrap up carbon-coating, improve the electric conductivity of material, agglomeration in sintering process for the granule can be suppressed simultaneously, obtain the product of size uniformity.
Description
Technical field
The invention belongs to inorganic nano material synthesis field.In particular, it is related to hydro-thermal assisting sol gel method
Preparation appearance and size is homogeneous, uniformly the method for the vanadium phosphate sodium material of cladding carbon-coating
Background technology
Vanadium phosphate sodium (Na3V2(PO4)3) it is the electrode material being applied to sodium-ion battery, (sodium surpasses to belong to NASICON structure
Ion conductor).NASICON structural compounds Na3M2(PO4)3(M=Ti, Fe, V) is one kind of phosphate cathode material, has
Three-dimensional Open ion transport channel, typically has higher ion diffusion rates and ionic conductivity.Wherein Na3V2(PO4)3Tool
There are high-energy-density (400Wh/kg), good heat stability (450 DEG C) and excellent chemical property, receive widely
Concern.Na3V2(PO4)3There is hexagoinal lattice, belong to R-3c space group, by each VO6Octahedron and three PO4Tetrahedron corner-sharing
Connect and compose stable NASICON skeleton.Na+Positioned at two kinds of different positions, it is hexa-coordinate and eight-coordinate respectively, eight-coordinate
Two Na ions can with reversible deintercalation, corresponding theoretical specific capacity be 117.6mAh/g, volume deformation in its charge and discharge process
Less, about 8.3%.Additionally, Na3V2(PO4)3Respectively there is a charge and discharge platform in 1.6V and 3.4V, correspond respectively to V3+/V2+
And V4+/V3+Redox couple, therefore Na3V2(PO4)3Positive pole and the negative pole of sodium-ion battery can be applied simultaneously to, be prepared into symmetrical
Battery.It can be seen that, Na3V2(PO4)3It is a kind of promising sodium ion energy-storage battery electrode material.
But research finds due to Na3V2(PO4)3The reason this body structure, its electric conductivity is very poor, limits its Fabrication of High Specific Capacitance
The performance of amount, common modification mode is to add suitable carbon source to be modified to improve electric conductivity, because carbon source high temperature cabonization
The activated carbon obtaining has very strong electric conductivity, it is possible to increase the diffusivity of electronics and ion in material, so that material
Electric conductivity increases.Compared to being as substrate using carbon source, carbon-coating is coated on grain surface and forms nucleocapsid structure, can increase carbon
Layer and the contact area of crystal grain, shorten the evolving path of electronics and sodium ion, make material have more preferable electric conductivity and electrochemistry
Performance.Additionally, carbon-coating is coated on grain surface can also play buffer action, can effectively suppress granule that group occurs in sintering process
Poly- phenomenon.Na3V2(PO4)3The scantling of the traditional preparation method of the material such as preparation such as high temperature solid-state method, sol-gal process is all
Relatively large and material particle size distribution scope is also larger, and the cladding of carbon-coating is also uneven.So, how to prepare size equal
One, the Na of uniform carbon coating3V2(PO4)3, it is to prepare efficient Na3V2(PO4)3Urgently to be resolved hurrily the asking of sodium ion battery electrode material
Topic.
Content of the invention
The purpose of the present invention is as carbon source using glucose, by hydro-thermal assisting sol gel method, so that crystal grain is being given birth to
Obtain effective appearance and size in length to control and uniform carbon-coating cladding, there is provided one kind prepares single-size, uniform carbon coating
The method of vanadium phosphate sodium material.
The invention provides one kind prepares single-size, the method for uniform carbon coating vanadium phosphate sodium material, the method is molten
On the basis of sol-gel, make glucose carbon source, in water-heat process, reaction of guanosine occur using hydro-thermal method auxiliary, generation
High polymer is wrapped in granular precursor surface, and high polymer carbonization after high temperature sintering is evenly coated at particle surface life, is obtained
Grain diameter is less, pattern vanadium phosphate sodium material evenly.
Comprise the following steps that：
A kind of method preparing uniform carbon coating vanadium phosphate sodium material；Using glucose as carbon source, assisted by hydro-thermal
Sol-gal process, makes crystal grain obtain particle diameter about 50-100nm in growth, carbon-coating is evenly coated, and carbon layers having thicknesses are 8-10nm's
Na3V2(PO4)3Material.
Comprise the following steps that：
1). by V2O5、NH4H2PO4And Na2CO3Or NH4VO3、H3PO4And Na2CO3It is dissolved in distilled water, stir；
2). add glucose mix homogeneously, Na in above-mentioned solution3V2(PO4)3Mol ratio with glucose is 2:3～4:
3；
3). above-mentioned solution is transferred in hydrothermal reaction kettle, carries out reaction of guanosine；
4). drive kettle after cooling down under room temperature, so that it is uniformly dispersed by ultrasonic for the suspension obtaining, then magnetic force stirs under water-bath
Mix transpiring moisture and obtain colloidal sol, colloidal sol is dried to obtain gel in an oven；
5). above-mentioned gel is fully ground and pre-burning in argon；Pre-sintered sample is fully ground again, calcines in argon
Obtain the Na of uniform carbon coating3V2(PO4)3Material.
Described step 1) in, according to Na3V2(PO4)3Chemical formula in each element ratio, preferably make Na:V:P mole
Than for 3:2:3.
Described step 3) in, preferably reaction of guanosine condition is 180 DEG C of thermotonuses 12-40h under hydrothermal condition.
Described step 4) in, preferably bath temperature is 70-95 DEG C；In baking oven, drying condition is 6-12h to be dried at 60-80 DEG C
Obtain gel.
Described step 5) in, preferably in 650-800 DEG C of argon, calcining 6-8h obtains the Na of uniform carbon coating3V2(PO4)3
Material.
The invention provides one kind prepares single-size, the method for uniform carbon coating vanadium phosphate sodium material.Other systems relatively
Preparation Method, the method being assisted using hydro-thermal is simultaneously used glucose as carbon source, makes glucose occur glycosidation anti-under hydrothermal conditions
Should, the high polymer of generation is coated on granular precursor surface, and sintered rear high polymer carbonization becomes activated carbon and uniformly coats
On crystalline particle surface, form the product with nucleocapsid structure.Additionally, presoma Surface coating high polymer in water-heat process,
Serve mutually isolated effect between granule, restrained effectively agglomeration in sintering process for the granule, make prepared product
Thing size is more homogeneous.
The effect of the present invention is：Size uniformity can be prepared, particle diameter about 50-100nm, carbon-coating is evenly coated, and carbon layers having thicknesses are about
The Na of 8-10nm3V2(PO4)3Material, by adding carbon source glucose in water-heat process, makes particle surface wrap up uniform carbon
Layer, improves the electric conductivity of material, can suppress agglomeration in sintering process for the granule simultaneously, obtain the product of size uniformity
Thing.
Brief description
Fig. 1 is Na prepared by embodiment 13V2(PO4)3Stereoscan photograph, illustrates that prepared product has homogeneous chi
Very little.
Fig. 2 is Na prepared by embodiment 23V2(PO4)3X-ray diffractogram, illustrate that prepared product has pure group
Become.
Fig. 3 is Na prepared by embodiment 33V2(PO4)3Transmission electron microscope photo, prepared product surface cladding is described all
Even carbon-coating.
Specific embodiment
Embodiment 1：
By 4mmolV2O5, 12mmolNH4H2PO4, 6mmolNa2CO3It is dissolved in 70ml distilled water, add 6mmol Fructus Vitis viniferae
Sugar stirs, and above-mentioned solution is transferred in reactor, hydro-thermal 12h at a temperature of 180 DEG C, drives kettle after cooling down under room temperature, will
The ultrasonic 90min of suspension obtaining, then under 70 DEG C of water-baths, magnetic agitation transpiring moisture obtains colloidal sol, and colloidal sol is in 60 DEG C of baking ovens
In 12h be dried obtain gel.Above-mentioned gel is fully ground and pre-burning 4h in 350 DEG C of argon；Pre-sintered sample fully grinds again
Mill, in 650 DEG C of argon, calcining 8h obtains product, prepared Na3V2(PO4)3The stereoscan photograph of material as shown in figure 1,
Illustrate that prepared product has homogeneous size.
Embodiment 2：
By 4mmolV2O5, 12mmolNH4H2PO4, 6mmolNa2CO3It is dissolved in 70ml distilled water, add 3mmol Fructus Vitis viniferae
Sugar stirs, and above-mentioned solution is transferred in reactor, hydro-thermal 40h at a temperature of 180 DEG C, drives kettle after cooling down under room temperature, will
The ultrasonic 90min of suspension obtaining, then under 95 DEG C of water-baths, magnetic agitation transpiring moisture obtains colloidal sol, and colloidal sol is in 80 DEG C of baking ovens
In 6h be dried obtain gel.Above-mentioned gel is fully ground and pre-burning 4h in 350 DEG C of argon；Pre-sintered sample fully grinds again
Mill, in 800 DEG C of argon, calcining 6h obtains product, prepared Na3V2(PO4)3The X ray diffracting spectrum of material such as Fig. 2 institute
Show, illustrate that prepared product has pure composition.
Embodiment 3：
By 4mmolV2O5, 12mmolNH4H2PO4, 6mmolNa2CO3It is dissolved in 70ml distilled water, add 4.5mmol Portugal
Grape sugar stirs, and above-mentioned solution is transferred in reactor, hydro-thermal 24h at a temperature of 180 DEG C, drives kettle after cooling down under room temperature,
By ultrasonic for the suspension obtaining 90min, then under 80 DEG C of water-baths, magnetic agitation transpiring moisture obtains colloidal sol, and colloidal sol dries at 70 DEG C
9h is dried in case and obtains gel.Above-mentioned gel is fully ground and pre-burning 4h in 350 DEG C of argon；Pre-sintered sample fully grinds again
Mill, in 750 DEG C of argon, calcining 7h obtains product, prepared Na3V2(PO4)3The transmission electron microscope photo of material as shown in figure 3,
The carbon-coating that prepared product surface is evenly coated is described.
To sum up implement arrange accompanying drawing can also clearly find out, the product prepared by the present invention have homogeneous particle size and
The uniformly carbon-coating of cladding.
Claims (5)
1. a kind of method preparing uniform carbon coating vanadium phosphate sodium material；Using glucose as carbon source, assisted molten by hydro-thermal
Sol-gel, makes crystal grain obtain particle diameter 50-100nm in growth, carbon-coating is evenly coated, and carbon layers having thicknesses are the Na of 8-10nm3V2
(PO4)3Material；Comprise the following steps that：
1). by V2O5、NH4H2PO4And Na2CO3Or NH4VO3、H3PO4And Na2CO3It is dissolved in distilled water, stir；
2). add glucose mix homogeneously, Na in above-mentioned solution3V2(PO4)3Mol ratio with glucose is 2:3～4:3；
3). above-mentioned solution is transferred in hydrothermal reaction kettle, carries out reaction of guanosine；
4). drive kettle after cooling down under room temperature, so that it is uniformly dispersed by ultrasonic for the suspension obtaining, then magnetic agitation is steamed under water-bath
Shampoo gets colloidal sol, and colloidal sol is dried to obtain gel in an oven；
5). above-mentioned gel is fully ground and pre-burning in argon；Pre-sintered sample is fully ground again, calcines and obtain in argon
The uniformly Na of carbon coating3V2(PO4)3Material.
2. the method for claim 1, is characterized in that described step 1) in, according to Na3V2(PO4)3Chemical formula in each unit
The ratio of element, makes Na:V:The mol ratio of P is 3:2:3.
3. the method for claim 1, is characterized in that described step 3) in, reaction of guanosine condition is under hydrothermal condition 180
DEG C thermotonuses 12-40h.
4. the method for claim 1, is characterized in that described step 4) in, bath temperature is 70-95 DEG C；It is dried in baking oven
Condition is 6-12h to be dried at 60-80 DEG C to obtain gel.
5. the method for claim 1, is characterized in that described step 5) in, in 650-800 DEG C of argon, calcining 6-8h obtains
Na to uniform carbon coating3V2(PO4)3Material.
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| CN105140468A (en) * | 2015-06-26 | 2015-12-09 | 武汉大学 | Preparation method for cathode material Na3V2(PO4)3/C of sodium ion battery |
| CN105336924A (en) * | 2015-09-25 | 2016-02-17 | 中南大学 | Preparation method of carbon coated vanadium sodium phosphate positive electrode material |
| CN105552328A (en) * | 2015-12-24 | 2016-05-04 | 华中科技大学 | Sodium vanadium phosphate sodium ion battery positive electrode material and preparation method therefor |
| CN105680041B (en) * | 2016-01-18 | 2017-12-29 | 武汉理工大学 | Three-dimensional Na3V2(PO4)3Nanometer line network electrode material and its preparation method and application |
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| CN108123108A (en) * | 2016-11-28 | 2018-06-05 | 中国科学院大连化学物理研究所 | The preparation method and positive electrode of a kind of vanadium phosphate cathode material and application |
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| CN110518214B (en) * | 2019-09-02 | 2020-08-04 | 齐鲁工业大学 | Nitrogen-hydrogen in-situ double-doped soft carbon/sodium vanadium phosphate composite material and preparation method and application thereof |
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| CN103474662A (en) * | 2013-09-13 | 2013-12-25 | 上海大学 | High-temperature solid phase synthesis method for lithium ion battery anode material Na3V2(PO4)3 |
| CN103594716A (en) * | 2013-11-21 | 2014-02-19 | 天津工业大学 | Method for preparing cathode material of sodium-ion battery, namely sodium vanadium fluorophosphates |
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