CN109360935A - A kind of lithium ion battery cellular hard carbon coated LiFePO 4 for lithium ion batteries positive electrode, preparation method, porous electrode and lithium battery - Google Patents
A kind of lithium ion battery cellular hard carbon coated LiFePO 4 for lithium ion batteries positive electrode, preparation method, porous electrode and lithium battery Download PDFInfo
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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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
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
The invention discloses a kind of lithium ion battery cellular hard carbon coated LiFePO 4 for lithium ion batteries positive electrode, preparation method, porous electrode and lithium batteries, lithium ion battery cellular hard carbon coated LiFePO 4 for lithium ion batteries positive electrode, including basestocks mixture and auxiliary material component, the basestocks mixture is lithium salts, molysite, phosphatic mixture；The auxiliary material component includes pore creating material and hard carbon presoma.Specific discharge capacity with higher of the invention and very excellent high rate performance.
Description
Technical field
The present invention relates to technical field of lithium ion more particularly to a kind of lithium ion battery cellular hard carbon to coat phosphorus
Sour iron lithium anode material, preparation method, porous electrode and lithium battery.
Background technique
As new generation of green environmental protection power supply, lithium ion battery is small in size with its, light-weight, discharge platform is high, cyclicity
Can good, pollution-free, memory-less effect the advantages that, be widely used in the products such as mobile phone, laptop, electric car.As just
The LiFePO4 of pole material due to safety, cycle life, in terms of have significant advantage, applied on a large scale
In new-energy automobile power supply.But due to the limitation of its own structure, the electronic conductivity of LiFePO4 and lithium ion is caused to expand
Scattered rate is all lower, and respectively only 10-9Cm/s and 10-16-10-13cm2/ s, cause the actual discharge specific capacity of LiFePO4 with
Theoretical capacity differs larger, theoretical capacity 170mAh/g, and actual discharge specific capacity can only achieve 140mAh/g or so, the big electricity of battery
It is poor to flow charging and discharging capabilities.Presently mainly led by grain diameter nanosizing, carbon coating and metal ion mixing to improve electronics
Electric rate and lithium ion diffusion rate, improve the large current discharging capability of LiFePO4 with this, improve its specific discharge capacity.Ferric phosphate
Lithium since its electronic conductivity and lithium ion diffusion rate are all lower, cause its practical specific discharge capacity differed with theoretical capacity compared with
Greatly, high rate performance is poor.Mainly improved at present by micronized particles partial size, bulk phase-doped and surface coated method, still
Effect is also extremely limited, and preparation process is more demanding.
Currently, patent CN105552431A improves anode material discharging specific capacity by doped graphene, anode is improved
Conductive capability.But graphene price is higher, product technology is immature, it is difficult to industrialized production.Patent CN105576220B is logical
It crosses and prepares porous structure LiFePO4 to improve lithium ion diffusion rate, increase material specific surface area, for the forthright again of material
It can have a distinct increment with cryogenic property.But the pore creating material ammonium salt used in preparation process has penetrating odor, volatile matter
It pollutes the environment.Patent application 201710399170.5 discloses a kind of lithium-manganese dioxide battery anode pore creating material, adopts
Porous anode and lithium-manganese dioxide battery are prepared with it.The pore creating material is fatty acid polyglycol of the relative molecular weight 200~750
Ethylene oxide esters, fatty alcohol polyethenoxy ether class and its isomer, any one in polyethenoxy ether class or at least two
The combination of kind.The present invention is dried at a suitable temperature by adding the pore creating material of suitable species, adjusting its additive amount, can
The porous anode with suitable hole is prepared, makes it have good intensity while improving the absorbent of anode, from
And promote the heavy-current discharge performance of lithium-manganese dioxide battery.But the porosity of anode is not uniform enough, forms channel and is easy damage
Wound, causes the promotion of performance not obvious enough.
Therefore, a kind of new lithium ion battery cellular hard carbon coated LiFePO 4 for lithium ion batteries positive electrode, preparation method, more is developed
Pore electrod and lithium battery not only have urgent researching value, it may have good economic benefit and commercial application potentiality, this is just
It is where the power that the present invention is accomplished and basis.
Summary of the invention
In order to overcome the defect of the prior art as indicated above, the present inventor has made intensive studies this, is paying
After a large amount of creative works, so as to complete the present invention.
Specifically, the technical problems to be solved by the present invention are: providing a kind of lithium ion battery cellular hard carbon packet
Lithium iron phosphate positive material, preparation method, porous electrode and lithium battery are covered, to improve specific discharge capacity, high rate performance.
In order to solve the above technical problems, the technical scheme is that
In a first aspect, the present invention provides lithium ion battery cellular hard carbon coated LiFePO 4 for lithium ion batteries positive electrodes, including
Basestocks mixture and auxiliary material component,
The basestocks mixture is lithium salts, molysite, phosphatic mixture；
The auxiliary material component includes pore creating material and hard carbon presoma.
In the present invention, as a kind of perferred technical scheme, in the basestocks mixture, elemental lithium, ferro element, phosphorus member
The molar ratio of element is 1:1:1.
In the present invention, as a kind of perferred technical scheme, the lithium salts includes Li2CO3, one of LiOH.
In the present invention, as a kind of perferred technical scheme, the molysite includes Fe3(PO4)2·8H2O、Fe(NO3)3·
9H2O、FeC2O4·2H2One of O.
In the present invention, as a kind of perferred technical scheme, the phosphate includes NH4H2PO4、LiH2PO4One of.
In the present invention, as a kind of perferred technical scheme, the pore creating material is decomposing volatile object at a certain temperature
Matter, preferably one or more of PVA, PVB, PVP, PEG, the more preferably mixture of PVA, PVB, PEG, the weight of three
Amount is than being 1:0.7:0.3.
In the present invention, as a kind of perferred technical scheme, the hard carbon presoma includes but is not limited to resinae such as phenol
Urea formaldehyde, epoxy resin etc. or organic polymer species such as PFA, PVC, PVDF, PAN etc..The preferred hard carbon presoma is adopted
With the mixture of PFA, PVC, PVDF, the weight ratio of three is 3:1:1.
In the present invention, as a kind of perferred technical scheme, the mass ratio of the pore creating material and basestocks mixture is 1:
1.5-1:30。
Second aspect, the present invention provides the lithium ion battery preparations of cellular hard carbon coated LiFePO 4 for lithium ion batteries positive electrode
Method includes the following steps:
Lithium salts, molysite, phosphate are weighed according to the ratio of molar ratio Li:Fe:P=1:1:1 and obtains basestocks mixture, are added
Enter a certain proportion of pore creating material and a certain proportion of hard carbon presoma, mixing and ball milling after solvent is added, it is dry to ball-milled mixtures
After dry under inert atmosphere conditions Fractional Heat-treatment: first in 300~600 DEG C of 2~20h of heat preservation, pore creating material is decomposed with gas shape
Formula volatilization, achievees the purpose that pore-creating, obtains porous structure LiFePO4；Then 650~900 DEG C of 2~20h of heat preservation are warming up to, are made
The charing of hard carbon presoma is obtained, and fills and is coated in porous structure LiFePO4 surface and duct, it is hard to obtain cellular
Carbon-coated LiFePO 4 for lithium ion batteries positive electrode.
In the present invention, as a kind of perferred technical scheme, ball milling ratio is 6-10:1 in the step, and rotational speed of ball-mill is
300-450 revs/min；Ball-milling Time is 20-36 hours.
In the present invention, as a kind of perferred technical scheme, ball milling solvent for use is water, ethyl alcohol or two in the step
The mixture of person.
In the present invention, as a kind of perferred technical scheme, the inert atmosphere in the step is argon gas, nitrogen, helium
Or one of neon.
In the present invention, as a kind of perferred technical scheme, hard carbon covering amount is 2%~10% in the step.
The third aspect, the present invention provides porous electrode, to use active material produced above, and by itself and conductive charcoal
The ratio of black, PVDF 8:1:1 in mass ratio mixes, and uniformly coats on aluminium foil, is then made for 24 hours in 110 DEG C of vacuum drying
Lithium battery anode.
Fourth aspect, lithium ion battery provided by the invention, including lithium battery anode as described above.
After above-mentioned technical proposal, the beneficial effects of the present invention are:
The present invention carries out pore-creating processing by LiFePO4 of the pore creating material to synthesis, and obtained porous structure material increases
The contact area of material and electrolyte shortens the transmission path of lithium ion, simultaneously because any heaped-up structure of hard carbon has
Conducive to the insertion and abjection of lithium, therefore obtained cellular hard carbon coated LiFePO 4 for lithium ion batteries positive electrode electric discharge specific volume with higher
Amount and very excellent high rate performance.
Overall process of the present invention is completed by high temperature solid-state method, and technical process is simple and easy to control, industrialization easy to accomplish.It is innovative
Use free of contamination being completely decomposed of volatile property substance under certain temperature to obtain porous structure at a certain temperature as pore creating material
Then LiFePO4 is warming up to certain temperature and carries out hard carbon carbon coating, it is uniform to obtain a kind of electrode interior porosity, and formed
Pore channel electrode material not easily damaged under hard carbon carbon coating so that cellular hard carbon coated LiFePO 4 for lithium ion batteries anode
Material discharging specific capacity is high, high rate performance is very excellent.
Detailed description of the invention
Fig. 1 is preparation flow schematic diagram of the invention；
Fig. 2 is the room temperature rate discharge curves figure of embodiment 1；
Fig. 3 is 20 DEG C of low temperature discharge curve graphs of ﹣ of embodiment 1.
Specific embodiment
Below with reference to specific embodiment, the present invention is further described.But the purposes and mesh of these exemplary embodiments
Be only used to enumerate the present invention, any type of any restriction not is constituted to real protection scope of the invention, it is more non-to incite somebody to action this
The protection scope of invention is confined to this.
Embodiment 1:
Li:Fe:P=1:1:1 weighs Li in molar ratio2CO3、FeC2O4·2H2O、NH4H2PO4Total 332g, weighs 80g's
PEG2000 and 5.2g phenolic resin is fitted into ball grinder, ratio of grinding media to material 6:1 jointly, and dehydrated alcohol is added as solvent, turns
Speed 400 turns/min ball milling 20h, then 100 DEG C of drying obtain precursor mixture；Mixture under Ar atmosphere protection, with 10 DEG C/
The heating rate of min is warming up to 400 DEG C of heat preservation 6h, is then warming up to 700 DEG C of heat preservation 8h with the heating rate of 10 DEG C/min, cooling
After obtain cellular hard carbon coated LiFePO 4 for lithium ion batteries positive electrode.
The charge-discharge performance of the present embodiment product is tested: active material, conductive black, the PVDF 8:1 in mass ratio of preparation:
1 ratio mixing, uniformly coats on aluminium foil, lithium battery anode is then made for 24 hours in 110 DEG C of vacuum drying.Cathode metal
Lithium, the LiPF of 1M6For electrolyte, CELL GARD 2003 is that diaphragm is assembled into button cell.To the lithium iron phosphate positive material
Electrochemical property test is carried out, charging/discharging voltage is 2.5V -4.2V.The electrochemical property test of this example product the results are shown in Table
1, room temperature rate discharge curves are shown in that Fig. 1,20 DEG C of low temperature discharge curves of ﹣ are shown in Fig. 2.
Embodiment 2:
Li:Fe:P=1:1:1 weighs LiOH, Fe (NO in molar ratio3)3·9H2O、NH4H2PO4Total 553g is packed into ball milling
In tank, PVC of the molecular weight of PVP and 50g that the K value for weighing 300g is 90 in 6~80,000 is fitted into ball grinder, ball jointly
Than being 10:1 dehydrated alcohol is added as solvent, for 24 hours, then 80 DEG C of drying obtain precursor mixing to 450 turns/min of revolving speed ball milling in material
Object；Mixture is in N2Under atmosphere protection, 500 DEG C of heat preservation 10h are warming up to the heating rate of 12 DEG C/min, then with 8 DEG C/min
Heating rate be warming up to 750 DEG C of heat preservation 6h, obtain cellular hard carbon coated LiFePO 4 for lithium ion batteries positive electrode after cooling.
The electrochemical property test method of the present embodiment product is same as Example 1, and test result is shown in Table 1.
Embodiment 3:
Li:Fe:P=1:1:1 weighs Li in molar ratio2CO3、Fe3(PO4)2·8H2O、LiH2PO4Total 690g, weighs
PAN of the molecular weight of the PVB and 40g of 200g 8~150,000, is fitted into ball grinder, ratio of grinding media to material 8:1 jointly, and quality is added
Than dehydrated alcohol: water=7:3 is as solvent, and revolving speed 300 turns/min ball milling 36h, then 100 DEG C of drying obtain precursor mixture；
Mixture is in N2450 DEG C of heat preservation 10h are warming up to the heating rate of 10 DEG C/min under atmosphere protection, then with the liter of 12 DEG C/min
Warm rate is warming up to 800 DEG C of heat preservation 8h, obtains cellular hard carbon coated LiFePO 4 for lithium ion batteries positive electrode after cooling.
The electrochemical property test method of the present embodiment product is same as Example 1, and test result is shown in Table 1.
Comparative example 1
Li:Fe:P=1:1:1 weighs LiOH, Fe (NO in molar ratio3)3·9H2O、NH4H2PO4Total 553g is packed into ball milling
In tank, the molecular weight of the 60g PVC in 6~80,000, ratio of grinding media to material 10:1 is added, dehydrated alcohol is added as solvent, revolving speed 500
Turn/min ball milling 20h, then 80 DEG C of drying obtain precursor mixture；Mixture is in N2Under atmosphere protection, with the liter of 10 DEG C/min
Warm rate is warming up to 400 DEG C of heat preservation 10h, is then warming up to 750 DEG C of heat preservation 6h with the heating rate of 10 DEG C/min, obtains after cooling
Hard carbon coated LiFePO 4 for lithium ion batteries positive electrode.
The electrochemical property test method of the present embodiment product is same as Example 1, and test result is shown in Table 1.
Comparative example 2
Carbon-coated LiFePO 4 for lithium ion batteries positive electrode is prepared according to conventional high-temperature solid phase method, the 13 of 1% mass ratio are added
Alkyl polyoxyethylene ether mixes by stirring granulation, and then sample is made in tabletting, puts it into 200 DEG C of baking 10h in oven,
Sodium Trideceth decomposes removal, obtains porous carbon-coated LiFePO 4 for lithium ion batteries positive electrode.
The electrochemical property test method of the present embodiment product is same as Example 1, and test result is shown in Table 2.
It is tested in different multiplying discharge capacity specific capacity, test result is shown in Table 1.
Specific discharge capacity (mAh/g) of the battery under different multiplying under the conditions of each embodiment of table 1
| Embodiment title | 0.1C | 0.5C | 1C | 2C | 5C | 10C |
| Embodiment 1 | 158 | 153 | 148 | 146 | 130 | 116 |
| Embodiment 2 | 158 | 150 | 146 | 143 | 131 | 112 |
| Embodiment 3 | 155 | 148 | 145 | 143 | 128 | 113 |
| Comparative example 1 | 150 | 145 | 143 | 133 | 115 | 98 |
| Comparative example 2 | 153 | 148 | 144 | 138 | 121 | 105 |
It should be appreciated that the purposes of these embodiments is merely to illustrate the present invention and is not intended to limit protection model of the invention
It encloses.In addition, it should also be understood that, after reading the technical contents of the present invention, those skilled in the art can make the present invention each
Kind change, modification and/or variation, all these equivalent forms equally fall within guarantor defined by the application the appended claims
Within the scope of shield.
Claims (10)
1. lithium ion battery cellular hard carbon coated LiFePO 4 for lithium ion batteries positive electrode, it is characterised in that: including basestocks mixture
With auxiliary material component,
The basestocks mixture is lithium salts, molysite, phosphatic mixture；
The auxiliary material component includes pore creating material and hard carbon presoma.
2. lithium ion battery as described in claim 1 cellular hard carbon coated LiFePO 4 for lithium ion batteries positive electrode, it is characterised in that:
In the basestocks mixture, elemental lithium, ferro element, P elements molar ratio be 1:1:1.
3. lithium ion battery as described in claim 1 cellular hard carbon coated LiFePO 4 for lithium ion batteries positive electrode, it is characterised in that:
The lithium salts includes Li2CO3, one of LiOH.
4. lithium ion battery as described in claim 1 cellular hard carbon coated LiFePO 4 for lithium ion batteries positive electrode, it is characterised in that:
The molysite includes Fe3(PO4)2·8H2O、Fe(NO3)3·9H2O、FeC2O4·2H2One of O.
5. lithium ion battery as described in claim 1 cellular hard carbon coated LiFePO 4 for lithium ion batteries positive electrode, it is characterised in that:
The phosphate includes NH4H2PO4、LiH2PO4One of.
6. lithium ion battery as described in claim 1 cellular hard carbon coated LiFePO 4 for lithium ion batteries positive electrode, it is characterised in that:
The pore creating material is one or more of PVA, PVB, PVP, PEG.
7. lithium ion battery as described in claim 1 cellular hard carbon coated LiFePO 4 for lithium ion batteries positive electrode, it is characterised in that:
The hard carbon presoma uses the mixture of PFA, PVC, PVDF, and the weight ratio of three is 3:1:1.
In the present invention, as a kind of perferred technical scheme, the mass ratio of the pore creating material and basestocks mixture is 1:1.5-
1:30。
8. the lithium ion battery preparation method of cellular hard carbon coated LiFePO 4 for lithium ion batteries positive electrode, it is characterised in that: including such as
Lower step:
Lithium salts, molysite, phosphate are weighed according to the ratio of molar ratio Li:Fe:P=1:1:1 and obtains basestocks mixture, are added one
Mixing and ball milling after solvent is added in the pore creating material of certainty ratio and a certain proportion of hard carbon presoma, after dry to ball-milled mixtures
The Fractional Heat-treatment under inert atmosphere conditions: first in 300~600 DEG C of 2~20h of heat preservation, pore creating material decomposition is waved in gaseous form
Hair, achievees the purpose that pore-creating, obtains porous structure LiFePO4；Then 650~900 DEG C of 2~20h of heat preservation are warming up to, so that firmly
Carbon matrix precursor charing, and fill and be coated in porous structure LiFePO4 surface and duct, obtain cellular hard carbon packet
Cover lithium iron phosphate positive material.
9. porous electrode, to press matter with conductive black, PVDF using the active material such as the preparation of claim 8 method, and by it
Measure than 8:1:1 ratio mixing, uniformly coated on aluminium foil, then in 110 DEG C vacuum drying for 24 hours and manufactured lithium battery just
Pole.
10. lithium ion battery, including porous electrode as claimed in claim 9 is as lithium battery anode.
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Cited By (6)
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| CN109860569A (en) * | 2019-02-28 | 2019-06-07 | 蜂巢能源科技有限公司 | Positive electrode of lithium ion battery and preparation method thereof |
| CN110112352A (en) * | 2019-06-17 | 2019-08-09 | 合肥国轩高科动力能源有限公司 | A kind of polyimide diaphragm and its preparation method and application |
| CN110247036A (en) * | 2019-06-10 | 2019-09-17 | 张雪花 | A kind of LiFePO based on lithium ion battery4Base composite positive pole and preparation method |
| CN113506865A (en) * | 2021-06-28 | 2021-10-15 | 山东玉皇新能源科技有限公司 | Battery negative electrode material and preparation method thereof |
| CN113506866A (en) * | 2021-06-28 | 2021-10-15 | 山东玉皇新能源科技有限公司 | Carbon-coated Fe2O3Hard carbon composite material and preparation method thereof |
| CN115050582A (en) * | 2022-06-20 | 2022-09-13 | 天津科技大学 | Porous carbon support composite lithium extraction electrode and preparation method thereof |
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| CN110247036A (en) * | 2019-06-10 | 2019-09-17 | 张雪花 | A kind of LiFePO based on lithium ion battery4Base composite positive pole and preparation method |
| CN110112352A (en) * | 2019-06-17 | 2019-08-09 | 合肥国轩高科动力能源有限公司 | A kind of polyimide diaphragm and its preparation method and application |
| CN113506865A (en) * | 2021-06-28 | 2021-10-15 | 山东玉皇新能源科技有限公司 | Battery negative electrode material and preparation method thereof |
| CN113506866A (en) * | 2021-06-28 | 2021-10-15 | 山东玉皇新能源科技有限公司 | Carbon-coated Fe2O3Hard carbon composite material and preparation method thereof |
| CN113506866B (en) * | 2021-06-28 | 2023-11-14 | 山东玉皇新能源科技有限公司 | Carbon-coated Fe 2 O 3 Hard carbon composite material and preparation method thereof |
| CN113506865B (en) * | 2021-06-28 | 2024-03-22 | 山东玉皇新能源科技有限公司 | Battery negative electrode material and preparation method thereof |
| CN115050582A (en) * | 2022-06-20 | 2022-09-13 | 天津科技大学 | Porous carbon support composite lithium extraction electrode and preparation method thereof |
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