CN106058195A - Double-coated lithium vanadium phosphate anode material and preparation method thereof - Google Patents
Double-coated lithium vanadium phosphate anode material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a double-coated lithium vanadium phosphate anode material and a preparation method thereof. The preparation method includes: performing ball mill mixing on a lithium source containing lithium carbonate, a vanadium source containing vanadium pentoxide, a phosphorus source containing ammonium dihydrogen phosphate and nano silicon dioxide according a certain proportion, and performing high-temperature thermal treatment on the evenly-mixed materials in a carbonization furnace to obtain the carbon-silicon dioxide double-coated lithium vanadium phosphate anode material with the particle size being 0.2-1.5 micrometers. The preparation method has the advantages that the preparation method is simple in synthesizing process and easy in process condition control; the prepared carbon-silicon dioxide double-coated lithium vanadium phosphate anode material is stable in structure and is good in circulation stability when being used as the anode material of a lithium-ion battery.
Description
Technical field
The present invention relates to a kind of vanadium phosphate cathode material, especially a kind of double cladded type vanadium phosphate cathode materials and
Preparation method, belongs to anode material for lithium-ion batteries technical field.
Background technology
Anode material for lithium ion battery currently mainly has cobalt acid lithium, nickle cobalt lithium manganate, LiMn2O4, LiFePO4 etc..?
In polyanionic lithium ion battery anode material, the positive electrode with LiFePO4 as representative has specific capacity height, raw material comes
Heat stability that source is abundant, cheap and excellent and charge-discharge performance.But the running voltage (3.4V of LiFePO4
vs.Li/Li+) relatively low, thus limit the performance of its energy density, and its one-dimensional lithium ion diffusion admittance seriously hinders
Its high rate performance and the performance of cryogenic property.Compared with LiFePO4, monoclinic phosphoric acid vanadium lithium (Li3V2(PO4)3) have
Higher discharge voltage plateau (3.6V, 3.68V, 4.08V, 4.55V vs.Li/Li+) make it have putting of up to 197mAh/g
Electricity specific capacity；Three-dimensional lithium ion diffusion admittance makes its high rate performance and cryogenic property be improved significantly.So phosphoric acid vanadium lithium
It it is a kind of lithium electricity positive electrode with fine development prospect.
But, when charging voltage is higher than 4.55V, three lithium ion all abjections of phosphoric acid vanadium lithium can cause the knot of material
Structure is unstable；And electrolyte can aggravate with the interfacial reaction of material surface under high voltage, so that cycle performance is deteriorated.
Summary of the invention
The technical problem to be solved is to provide a kind of double cladded type vanadium phosphate cathode material and preparation side thereof
Method, by phosphoric acid vanadium lithium coated with carbon bed and SiO2Improve electronic conductivity and the structural stability of material.This double-contracting
Cover type vanadium phosphate cathode material and there is good chemical property, and preparation process is simple.
In order to solve above-mentioned technical problem, the technical solution used in the present invention is: a kind of double cladded type phosphoric acid vanadium lithium positive poles
The preparation method of material, comprises the following steps:
1) it is Li:V:P=(3～3.15): 2:3 according to mol ratio, weighs lithium source, vanadium source, phosphorus source, carbon source and nanometer
SiO2, it is subsequently adding deionized water, deionized water quality: (lithium source quality+vanadium source quality+phosphorus source quality+carbon source quality+SiO2Matter
Amount)=(1～2): 1, final products carbon mass content is 1.5%～5%, SiO2Mass content is 0.5%～2%, will prepare
Material add in ball mill and carry out ball milling mixing 0.5～6h；
2) being dried by gained slurry in step (1), baking temperature is 60 DEG C～120 DEG C；
3) dried material in step (2) is placed in tube furnace, under the protection of nitrogen or argon inert atmosphere, with
The heating rate of 1 DEG C/min～5 DEG C/min rises to 700 DEG C～900 DEG C, and constant temp. heating processes 6h～24h, obtains double cladded type phosphoric acid
Vanadium lithium anode material.
The matter of particle diameter 0.2～1.5 μm of described pair of cladded type vanadium phosphate cathode material, carbon coating layer and phosphoric acid vanadium lithium core
Amount ratio is (0.015～0.05): (0.985～0.95), SiO2The mass ratio of clad and phosphoric acid vanadium lithium core be (0.005～
0.02): (0.995～0.98).
Described lithium source is the one in Lithium hydrate, lithium carbonate, Quilonorm (SKB), lithium dihydrogen phosphate.
Described vanadium source is the one in vanadic anhydride, ammonium metavanadate.
Phosphorus source is the one in phosphoric acid, ammonium dihydrogen phosphate, lithium dihydrogen phosphate.
Described carbon source is one or more in organic carbon and simple substance carbon.
Described organic carbon is glucose, sucrose, citric acid, Polyethylene Glycol, starch, simple substance carbon is Super P, Ensaco,
ECP600。
Described Nano-meter SiO_22Particle size be 10～200nm.
Double cladded type phosphoric acid vanadium lithium positive pole materials that the preparation method of above-mentioned double cladded type vanadium phosphate cathode materials prepares
Material.
The invention has the beneficial effects as follows: synthesis technique is simple, and process conditions are easily controllable；The method using in-stiu coating,
Make carbon cladding, SiO2Cladding and precursor synthesis complete in the lump；Carbon coating layer can well improve the electronic conduction energy of material
Power, SiO2Cladding can effectively improve the structural stability of material；The specific capacity of products obtained therefrom is high, good cycling stability.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of double cladded type vanadium phosphate cathode materials of the embodiment of the present invention 1 preparation.
Fig. 2 is the SEM photograph of double cladded type vanadium phosphate cathode materials of the embodiment of the present invention 1 preparation.
Fig. 3 is the charging and discharging curve figure of double cladded type vanadium phosphate cathode materials of the embodiment of the present invention 1 preparation.
Fig. 4 is the cycle performance figure of double cladded type vanadium phosphate cathode materials of the embodiment of the present invention 1 preparation.
Detailed description of the invention
The invention will be further described with embodiment below in conjunction with the accompanying drawings.Following example be intended to illustrate the present invention and not
It it is limitation of the invention further.
The preparation method of double cladded type vanadium phosphate cathode materials of the present invention, comprises the following steps:
1) it is Li:V:P=(3～3.15): 2:3 according to mol ratio, weighs lithium source, vanadium source, phosphorus source, carbon source and nanometer
SiO2, it is subsequently adding deionized water, deionized water quality: (lithium source quality+vanadium source quality+phosphorus source quality+carbon source quality+SiO2Matter
Amount)=(1～2): 1, final products carbon mass content is 1.5%～5%, SiO2Mass content is 0.5%～2%, will prepare
Material add in ball mill and carry out ball milling mixing 0.5～6h；
2) being dried by gained slurry in step (1), baking temperature is 60 DEG C～120 DEG C；
3) dried material in step (2) is placed in tube furnace, under the protection of nitrogen or argon inert atmosphere, with
The heating rate of 1 DEG C/min～5 DEG C/min rises to 700 DEG C～900 DEG C, and constant temp. heating processes 6h～24h, obtains double cladded type phosphoric acid
Vanadium lithium anode material.
The matter of particle diameter 0.2～1.5 μm of described pair of cladded type vanadium phosphate cathode material, carbon coating layer and phosphoric acid vanadium lithium core
Amount ratio is (0.015～0.05): (0.985～0.95), SiO2The mass ratio of clad and phosphoric acid vanadium lithium core be (0.005～
0.02): (0.995～0.98).
Described lithium source is the one in Lithium hydrate, lithium carbonate, Quilonorm (SKB), lithium dihydrogen phosphate.
Described vanadium source is the one in vanadic anhydride, ammonium metavanadate.
Phosphorus source is the one in phosphoric acid, ammonium dihydrogen phosphate, lithium dihydrogen phosphate.
Described carbon source is one or more in organic carbon and simple substance carbon.
Described organic carbon is glucose, sucrose, citric acid, Polyethylene Glycol, starch, simple substance carbon is Super P, Ensaco,
ECP600。
Described Nano-meter SiO_22Particle size be 10～200nm.
Double cladded type phosphoric acid vanadium lithium positive pole materials that the preparation method of above-mentioned double cladded type vanadium phosphate cathode materials prepares
Material.
Embodiment 1
The preparation method of a kind of pair of cladded type vanadium phosphate cathode material, comprises the following steps:
1) weigh respectively 115.1g lithium carbonate, 181.9g vanadic anhydride, 345g ammonium dihydrogen phosphate, 38.8g glucose,
38.8g PEG-4000,3.9g Nano-meter SiO_22(particle size about 100nm) and 1085g deionized water, add in ball mill
Carry out ball milling mixing 4h；
2) being dried by gained slurry in step (1), baking temperature is 80 DEG C；
3) dried material in step (2) is placed in tube furnace, under the protection of nitrogen atmosphere, with 2 DEG C/min's
Heating rate rises to 800 DEG C, and constant temperature processes 10h, obtains final products.
Embodiment 2
The preparation method of a kind of pair of cladded type vanadium phosphate cathode material, comprises the following steps:
1) weigh respectively 115.1g lithium carbonate, 181.9g vanadic anhydride, 345g ammonium dihydrogen phosphate, 38.8g glucose,
38.8g PEG-4000,5.8g Nano-meter SiO_22(particle size about 100nm) and 1088g deionized water, add in ball mill
Carry out ball milling mixing 4h；
2) being dried by gained slurry in step (1), baking temperature is 80 DEG C；
3) dried material in step (2) is placed in tube furnace, under the protection of nitrogen atmosphere, with 2 DEG C/min's
Heating rate rises to 800 DEG C, and constant temperature processes 10h, obtains final products.
Embodiment 3
The preparation method of a kind of pair of cladded type vanadium phosphate cathode material, comprises the following steps:
1) weigh respectively 115.1g lithium carbonate, 181.9g vanadic anhydride, 345g ammonium dihydrogen phosphate, 38.8g glucose,
38.8g PEG-4000,2.1g Nano-meter SiO_22(particle size about 100nm) and 1082g deionized water, add in ball mill
Carry out ball milling mixing 4h；
2) being dried by gained slurry in step (1), baking temperature is 80 DEG C；
3) dried material in step (2) is placed in tube furnace, under the protection of nitrogen atmosphere, with 2 DEG C/min's
Heating rate rises to 800 DEG C, and constant temperature processes 10h, obtains final products.
Embodiment 4
The preparation method of a kind of pair of cladded type vanadium phosphate cathode material, comprises the following steps:
1) 115.1g lithium carbonate, 181.9g vanadic anhydride, 345g ammonium dihydrogen phosphate, 48.5g starch, 3.9g are weighed respectively
Nano-meter SiO_22(particle size about 100nm) and 849g deionized water, add in ball mill and carry out ball milling mixing 4h；
2) being dried by gained slurry in step (1), baking temperature is 80 DEG C；
3) dried material in step (2) is placed in tube furnace, under the protection of nitrogen atmosphere, with 2 DEG C/min's
Heating rate rises to 850 DEG C, and constant temperature processes 8h, obtains final products.
Embodiment 5
The preparation method of a kind of pair of cladded type vanadium phosphate cathode material, comprises the following steps:
1) weigh respectively 37g Lithium hydrate, 90.9g vanadic anhydride, 172.5g ammonium dihydrogen phosphate, 25.5g glucose,
2.0g Nano-meter SiO_22(particle size about 100nm) and 472g deionized water, add in ball mill and carry out ball milling mixing 4h；
2) being dried by gained slurry in step (1), baking temperature is 80 DEG C；
3) dried material in step (2) is placed in tube furnace, under the protection of nitrogen atmosphere, with 3 DEG C/min's
Heating rate rises to 800 DEG C, and constant temperature processes 10h, obtains final products.
Embodiment 6
The preparation method of a kind of pair of cladded type vanadium phosphate cathode material, comprises the following steps:
1) 156g lithium dihydrogen phosphate, 90.9g vanadic anhydride, 4.9g KJ600,2.0g Nano-meter SiO_2 are weighed respectively2(granule
Size about 100nm) and 405g deionized water, add in ball mill and carry out ball milling mixing 6h；
2) being dried by gained slurry in step (1), baking temperature is 80 DEG C；
3) dried material in step (2) is placed in tube furnace, under the protection of nitrogen atmosphere, with 1 DEG C/min's
Heating rate rises to 800 DEG C, and constant temperature processes 10h, obtains final products.
Experimental conditions:
Table 1 lists the double cladded type vanadium phosphate cathode materials utilizing above-described embodiment to prepare and makes the head of button cell
Secondary cycle charge-discharge specific capacity.The test condition of button cell is: 23 DEG C ± 2 DEG C, LR2032, I=0.1C, 2.0～4.8V
vs.Li/Li+。
Electricity first charge-discharge capacity comparison table buckled by table 1
By data in table 1 it can be seen that double cladded type lithium vanadium phosphate material of preparing of the present invention, specific capacity has reached about
165mAh/g, coulombic efficiency has reached more than 94%, hence it is evident that higher than the phosphoric acid vanadium lithium blank sample not carrying out double-coating.
As can be seen from Figure 1 the phosphoric acid vanadium lithium prepared does not has dephasign.
As can be seen from Figure 2 obtained product particle size about 1 μm, even size distribution.Particle surface is thicker
Rough, SiO has been described2Cladding with carbon.
The first discharge specific capacity that can be obtained material by curve in Fig. 3 is 165.4mAh/g, and coulombic efficiency reaches 94.9%.
The material prepared as seen from Figure 4 has preferable cycle performance, the capability retention of 100 circulations to reach
91.7%.
In sum, present disclosure is not limited in the above embodiments, and the knowledgeable people in same area can
Can propose other embodiment within technological guidance's thought of the present invention easily, but this embodiment is included in this
Within the scope of bright.
Claims (9)
1. the preparation method of double cladded type vanadium phosphate cathode materials, it is characterised in that comprise the following steps:
1) it is Li:V:P=(3～3.15): 2:3 according to mol ratio, weighs lithium source, vanadium source, phosphorus source, carbon source and Nano-meter SiO_22, then
Add deionized water, deionized water quality: (lithium source quality+vanadium source quality+phosphorus source quality+carbon source quality+SiO2Quality)=(1
～2): 1, final products carbon mass content is 1.5%～5%, SiO2Mass content is 0.5%～2%, is added by the material prepared
Ball mill carries out ball milling mixing 0.5～6h；
2) being dried by gained slurry in step (1), baking temperature is 60 DEG C～120 DEG C；
3) dried material in step (2) is placed in tube furnace, under the protection of nitrogen or argon inert atmosphere, with 1 DEG C/
The heating rate of min～5 DEG C/min rises to 700 DEG C～900 DEG C, and constant temp. heating processes 6h～24h, obtains double cladded type phosphoric acid vanadium lithium
Positive electrode.
The preparation method of the most according to claim 1 pair of cladded type vanadium phosphate cathode material, it is characterised in that described double
Particle diameter 0.2～1.5 μm of cladded type vanadium phosphate cathode material, the mass ratio of carbon coating layer and phosphoric acid vanadium lithium core be (0.015～
0.05): (0.985～0.95), SiO2The mass ratio of clad and phosphoric acid vanadium lithium core is (0.005～0.02): (0.995～
0.98)。
The preparation method of the most according to claim 1 pair of cladded type vanadium phosphate cathode material, it is characterised in that described lithium
Source is the one in Lithium hydrate, lithium carbonate, Quilonorm (SKB), lithium dihydrogen phosphate.
The preparation method of the most according to claim 1 pair of cladded type vanadium phosphate cathode material, it is characterised in that described vanadium
Source is the one in vanadic anhydride, ammonium metavanadate.
The preparation method of the most according to claim 1 pair of cladded type vanadium phosphate cathode material, it is characterised in that described phosphorus
Source is the one in phosphoric acid, ammonium dihydrogen phosphate, lithium dihydrogen phosphate.
The preparation method of the most according to claim 1 pair of cladded type vanadium phosphate cathode material, it is characterised in that described carbon
Source is one or more in organic carbon and simple substance carbon.
The preparation method of the most according to claim 6 pair of cladded type vanadium phosphate cathode material, it is characterised in that described in have
Machine carbon is glucose, sucrose, citric acid, Polyethylene Glycol, starch, and simple substance carbon is Super P, Ensaco, ECP600.
The preparation method of the most according to claim 1 pair of cladded type vanadium phosphate cathode material, it is characterised in that described in receive
Rice SiO2Particle size be 10～200nm.
9. the double-contracting that the preparation method of the double cladded type vanadium phosphate cathode materials as described in any one of claim 1-8 prepares is covered
Type vanadium phosphate cathode material.
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| CN114420466A (en) * | 2021-12-24 | 2022-04-29 | 湖北文理学院 | Preparation method of modified cobalt vanadate material and supercapacitor |
| CN115020687A (en) * | 2022-08-08 | 2022-09-06 | 深圳市华宝新能源股份有限公司 | Positive electrode material and preparation method and application thereof |
| CN115020687B (en) * | 2022-08-08 | 2022-11-18 | 深圳市华宝新能源股份有限公司 | Positive electrode material and preparation method and application thereof |
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