CN110498449A - A kind of ferrous acid lithium material and preparation method thereof - Google Patents

A kind of ferrous acid lithium material and preparation method thereof Download PDF

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Publication number
CN110498449A
CN110498449A CN201910840485.8A CN201910840485A CN110498449A CN 110498449 A CN110498449 A CN 110498449A CN 201910840485 A CN201910840485 A CN 201910840485A CN 110498449 A CN110498449 A CN 110498449A
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acid lithium
ferrous acid
preparation
mixed liquor
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程光春
孙杰
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Hubei Rong Tong Hi Tech Advanced Materials Co Ltd
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Hubei Rong Tong Hi Tech Advanced Materials Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/58Selection 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
    • H01M4/5825Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624Electric conductive fillers
    • H01M4/625Carbon or graphite
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The present invention relates to electrochemical field, a kind of ferrous acid lithium material and preparation method thereof is disclosed.The described method includes: (1) mixes source of iron, lithium source, carbon source and deionized water, mixed liquor is obtained;(2) mixed liquor that step (1) obtains is ground, so that the granularity of solid particle is 0.4 μm or less in mixed liquor;(3) mixed liquor after grinding is spray-dried, obtains ferrous acid lithium presoma;(4) the ferrous acid lithium presoma is sintered, crushed, obtain ferrous acid lithium material;Wherein, the dosage of the carbon source makes the content of material with carbon-coated surface layer in prepared ferrous acid lithium material be 0.5-15 weight %;The molar ratio of Li/Fe is (5-25) in the lithium source and the source of iron: 1.There is ferrous acid lithium material prepared by the present invention preferable irreversibility and preferable capacity to play, so as to improve the energy density of battery.

Description

A kind of ferrous acid lithium material and preparation method thereof
Technical field
The present invention relates to electrochemical fields, and in particular to a kind of ferrous acid lithium material and preparation method thereof.
Background technique
With the development in market, the continuous promotion of material, battery technology, terminal enterprise is to lithium ion battery energy density It is required that being also continuously improved.Currently, the method for common promotion lithium ion battery energy density includes the height using height ratio capacity Nickel ternary material as positive electrode, use the higher silicon substrate of specific capacity as negative electrode material, promoted positive electrode work electricity The compacted density etc. of pressure and material.
However, lithium ion battery is de- along with the structure change of positive electrode, active material during first charge-discharge It falls, the generation of solid electrolyte interface film etc., can all make reversible capacity and the first charge discharge efficiency decline of battery, lead to battery energy Metric density decline.
Ferrous acid lithium (Li5FeO4) material has antifluorite structure, and every part of Li5FeO4Contain five parts of lithiums in material, makes its reason 867mAh/g, and Li are up to by specific capacity5FeO4Material operating voltage is moderate, and has preferable irreversibility, in charge and discharge for the first time Inert substance is produced after electricity, is not involved in subsequent electrochemical process, can be used for caused by solving first charge-discharge The problem of battery reversible capacity and first charge discharge efficiency decline.
However, Li5FeO4Material is easy to get the material (Li of a variety of crystal form mixing during the preparation process5Fe5O8、LiFeO2、 Li5FeO4), the charge-discharge performance of material is influenced, and the performance of its capacity is also a problem to be solved.
Summary of the invention
The purpose of the invention is to overcome the Li of the existing technology for being difficult to prepare single crystal form5FeO4Material provides A kind of Li5FeO4Material and preparation method thereof.
To achieve the goals above, one aspect of the present invention provides a kind of Li5FeO4The preparation method of material, the preparation Method the following steps are included:
(1) source of iron, lithium source, carbon source and deionized water are mixed, obtains mixed liquor;
(2) mixed liquor that step (1) obtains is ground so that in mixed liquor solid particle granularity be 0.4 μm with Under;
(3) mixed liquor after grinding is spray-dried, obtains Li5FeO4Presoma;
(4) by the Li5FeO4Presoma is sintered, crushes, and obtains Li5FeO4Material;
Wherein, the dosage of the carbon source makes prepared Li5FeO4The content of material with carbon-coated surface layer is 0.5-15 in material Weight %;
Preferably, the lithium source and the molar ratio of Li/Fe in the source of iron are (5-25): 1.
It is further preferred that the molar ratio of Li/Fe is (6-12) in the lithium source and the source of iron: 1.
Preferably, in step (1), the source of iron is Fe2O3、Fe3O4, FeOOH, in ferric nitrate and ironic citrate extremely Few one kind.
Preferably, in step (1), the lithium source is Li2CO3And/or LiOHH2O。
Preferably, in step (1), the carbon source be phenolic resin, polyvinyl alcohol, citric acid, stearic acid, glucose, At least one of sucrose, polyvinyl chloride and polyethylene glycol.
Preferably, in step (3), the spray drying condition includes: that spray inlet temperature is 110-180 DEG C, preferably It is 120-160 DEG C;Spray outlet temperature is 70-120 DEG C, preferably 80-100 DEG C.
Preferably, in step (4), the sintering condition includes: that temperature is 650-1000 DEG C, preferably 800-900 DEG C; Time is 3-72h, preferably 24-48h.
On the other hand, the present invention provides the Li that the above method is prepared5FeO4Material.
Preferably, the Li5FeO4Material is single crystal form, and surface is also wrapped on amorphous carbon layer.
Preferably, the amorphous carbon layer is in Li5FeO4Content in material is 0.5-15 weight %.
The technical solution provided through the invention can be prepared with single crystal form, the Li of no miscellaneous phase5FeO4Material, while its Surface is also wrapped on amorphous carbon layer, improves Li5FeO4The electrical property of material promotes the performance of its capacity.
Detailed description of the invention
Fig. 1 is the XRD diagram of material S1 made from embodiment 1.
Specific embodiment
Below in conjunction with attached drawing, detailed description of the preferred embodiments.It should be understood that this place is retouched The specific embodiment stated is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more New numberical range, these numberical ranges should be considered as specific open herein.
One aspect of the present invention provides a kind of Li5FeO4The preparation method of material, the preparation method comprises the following steps:
(1) source of iron, lithium source, carbon source and deionized water are mixed, obtains mixed liquor;
(2) mixed liquor that step (1) obtains is ground so that in mixed liquor solid particle granularity be 0.4 μm with Under;
(3) mixed liquor after grinding is spray-dried, obtains Li5FeO4Presoma;
(4) by the Li5FeO4Presoma is sintered, crushes, and obtains Li5FeO4Material;
Wherein, the dosage of the carbon source makes prepared Li5FeO4The content of material with carbon-coated surface layer is 0.5-15 in material Weight %, specifically, for example can be 0.5 weight %, 1 weight %, 3 weight %, 5 weight %, 7 weight %, 9 weight %, 11 Weight %, 13 weight % and 15 weight %.In the present invention, by introducing carbon source in Li5FeO4Material surface forms carbon coating Layer, and provide Li5FeO4The content of carbon coating layer in material, helps to improve the electric conductivity of the material.
In the present invention, the grinding is carried out in grinder, by grinding so that solid particle in mixed liquor Granularity is 0.4 μm hereinafter, reducing the granularity of solid particle in script mixed liquor, facilitates the Li for obtaining single crystal form5FeO4 Material, in a preferred embodiment, the granularity of solid particle is 0.02-0.3 μm in the mixed liquor.
In the present invention, the lithium source and the molar ratio of Li/Fe in the source of iron can be (5-25): 1, specifically, example It such as can be 5:1,6:1,9:1,12:1,15:1,18:1,21:1,24:1 or 25:1, in a preferred embodiment, the lithium The molar ratio of Li/Fe is (6-12) in source and the source of iron: 1.
In the present invention, in step (1), the source of iron can be the conventional selection of this field, in preferred embodiment party In formula, the source of iron is Fe2O3、Fe3O4, FeOOH, at least one of ferric nitrate and ironic citrate, preferably Fe2O3
In the present invention, in step (1), the lithium source can be the conventional selection of this field, in preferred embodiment party In formula, the lithium source is Li2CO3And/or LiOHH2O。
In the present invention, in step (1), the carbon source can be the conventional selection of this field, in preferred embodiment party In formula, the carbon source is phenolic resin, polyvinyl alcohol, citric acid, stearic acid, glucose, sucrose, polyvinyl chloride and polyethylene glycol At least one of, preferably glucose, sucrose and polyethylene glycol.
In the present invention, in step (3), the mixed liquor after grinding need to carry out spray drying treatment, described spraying dry Dry treatment conditions are not particularly limited.In a preferred embodiment, the spray inlet temperature is 110-180 DEG C, preferably 120-160 DEG C, further preferably 130-140 DEG C;The spray outlet temperature be 70-120 DEG C, preferably 80-110 DEG C, into One step is preferably 85-95 DEG C.
In the present invention, in step (4), the sintering method is well known to those skilled in the art.Preferred real It applies in mode, the sintering is in N2It protects under atmosphere, is heated up in van-type furnace with 1-6 DEG C/min, the sintering temperature It is 650-1000 DEG C, preferably 700-950 DEG C, further preferably 850-900 DEG C;The sintering time is 3-72h, preferably 10-60h, further preferably 24-48h.
Another aspect of the present invention provides the Li that the above method is prepared5FeO4Material.
In the present invention, in situations where it is preferred, the Li5FeO4Material is single crystal form, and surface is also wrapped on without fixed Type carbon-coating.
In the present invention, in situations where it is preferred, the amorphous carbon layer is in Li5FeO4Content in material is 0.5-15 Weight %.
In the present invention, first charge discharge efficiency=first discharge specific capacity/initial charge specific capacity × 100%, in half electricity In the experiment of pond, initial charge specific capacity is higher, and first discharge specific capacity is lower, shows that the irreversibility of the material is better, more has Conducive to solve the problems, such as battery reversible capacity caused by first charge-discharge and first charge discharge efficiency decline.
In the present invention, pass through carbon coating layer in the granularity of solid particle in regulation mixed liquor, Li/Fe molar ratio, material Content so that preparation Li5FeO4Material has single crystal form, and no miscellaneous phase further promotes its appearance while improving electrical property The performance of amount.
The present invention will be described in detail by way of examples below, but scope of protection of the present invention is not limited thereto.
Embodiment 1
(1) by 1548g LiOHH2O、500g Fe2O3, 105g glucose and deionized water mixing, obtain mixed liquor.
(2) grinder is added in mixed liquor that step (1) obtains to grind so that in mixed liquor solid particle granularity For 150nm or less.
(3) mixed liquor after grinding is spray-dried, obtains Li5FeO4Presoma, wherein spray inlet temperature It is 135 DEG C, outlet temperature is 90 DEG C.
(4) by the Li5FeO4Presoma is placed in saggar, is placed into van-type furnace, in N2Protect atmosphere under, with 2 DEG C/ Min is warming up to 850 DEG C and is sintered, and sintering time is for 24 hours, to be crushed to obtain target Li later5FeO4Material S1.
Embodiment 2
(1) by 924g Li2CO3、196g Fe2O3, 200g sucrose and deionized water mixing, obtain mixed liquor.
(2) grinder is added in mixed liquor that step (1) obtains to grind so that in mixed liquor solid particle granularity For 200nm or less.
(3) mixed liquor after grinding is spray-dried, obtains Li5FeO4Presoma, wherein spray inlet temperature It is 140 DEG C, outlet temperature is 95 DEG C.
(4) by the Li5FeO4Presoma is placed in saggar, is placed into van-type furnace, in N2Protect atmosphere under, with 5 DEG C/ Min is warming up to 900 DEG C and is sintered, sintering time 48h, is crushed to obtain target Li later5FeO4Material S2.
Embodiment 3
(1) by 2000g LiOHH2O、317g Fe2O3, 150g polyethylene glycol and deionized water mixing, obtain mixed liquor.
(2) grinder is added in mixed liquor that step (1) obtains to grind so that in mixed liquor solid particle granularity For 300nm or less.
(3) mixed liquor after grinding is spray-dried, obtains Li5FeO4Presoma, wherein spray inlet temperature It is 130 DEG C, outlet temperature is 85 DEG C.
(4) by the Li5FeO4Presoma is placed in saggar, is placed into van-type furnace, in N2Protect atmosphere under, with 3 DEG C/ Min is warming up to 870 DEG C and is sintered, sintering time 30h, is crushed to obtain target Li later5FeO4Material S3.
Comparative example 1
With embodiment 1, the difference is that not having process of lapping, Li is obtained5FeO4Material D1.
Comparative example 2
With embodiment 1, the difference is that the granularity of solid particle is 1 μm hereinafter, obtaining in mixed liquor in step (2) Li5FeO4Material D2.
Test case 1
Material S1 made from embodiment 1 is measured using X-ray diffractometer, as a result as shown in Figure 1.
As shown in Figure 1, the peak type of the diffraction maximum of embodiment matches with PDF card (PCPDF:24-0623), out peak position It is consistent, no dephasign peak, shows the Li obtained5FeO4Material is single crystal form, without miscellaneous phase.
Test case 2
By acid lithium material made from embodiment 1-3 and comparative example 1-2 respectively with conductive agent, bonding agent according to mass ratio 8: 1:1 prepares Li5FeO4Slurry, adjusting slurry solid content using N-Methyl pyrrolidone is 40%, the Li that will be regulated5FeO4Slurry Material is respectively coated on aluminium foil after drying, roll-in, punching, and the assembly of 2032 battery of button is carried out in glove box, and electrolyte is The LiPF of 1.2mol/L6, using ethylene carbonate: methyl ethyl carbonate=3:7 (volume ratio) is used as solvent, is made using metal lithium sheet For reference electrode, diaphragm is Celgard polypropylene screen.
Above-mentioned 5 kinds of lithium ion batteries are taken to carry out volume test on new prestige tester respectively, charging is 4.5V by voltage, Discharge cut-off voltage is 2.0V, charge-discharge magnification 0.05C, and test result is as shown in table 1.
Table 1
As 1 test result of table it is found that using Li made from technical solutions according to the invention5FeO4Material is assembled into Battery, blanking voltage be 4.5V when, charge specific capacity is up to 749.2mAh/g, while specific discharge capacity is lower than 150mAh/g shows that there is the material preferable irreversibility and preferable capacity to play, so as to improve the energy of battery Metric density.
The preferred embodiment of the present invention has been described above in detail, and still, the present invention is not limited thereto.In skill of the invention In art conception range, can with various simple variants of the technical solution of the present invention are made, including each technical characteristic with it is any its Its suitable method is combined, and it should also be regarded as the disclosure of the present invention for these simple variants and combination, is belonged to Protection scope of the present invention.

Claims (10)

1. a kind of preparation method of ferrous acid lithium material, which is characterized in that the preparation method comprises the following steps:
(1) source of iron, lithium source, carbon source and deionized water are mixed, obtains mixed liquor;
(2) mixed liquor that step (1) obtains is ground, so that the granularity of solid particle is 0.4 μm or less in mixed liquor;
(3) mixed liquor after grinding is spray-dried, obtains ferrous acid lithium presoma;
(4) the ferrous acid lithium presoma is sintered, crushed, obtain ferrous acid lithium material;
Wherein, the dosage of the carbon source makes the content of material with carbon-coated surface layer in prepared ferrous acid lithium material for 0.5-15 weight Measure %;
The molar ratio of Li/Fe is (5-25) in the lithium source and the source of iron: 1.
2. preparation method according to claim 1, which is characterized in that mole of Li/Fe in the lithium source and the source of iron Than for (6-12): 1.
3. preparation method according to claim 1 or 2, which is characterized in that in step (1), the source of iron is Fe2O3、 Fe3O4, FeOOH, at least one of ferric nitrate and ironic citrate.
4. preparation method according to claim 1 or 2, which is characterized in that in step (1), the lithium source is Li2CO3 And/or LiOHH2O。
5. preparation method according to claim 1, which is characterized in that in step (1), the carbon source be phenolic resin, At least one of polyvinyl alcohol, citric acid, stearic acid, glucose, sucrose, polyvinyl chloride and polyethylene glycol.
6. preparation method according to claim 1, which is characterized in that in step (3), the spray drying condition packet Include: spray inlet temperature is 110-180 DEG C, preferably 120-160 DEG C;Spray outlet temperature is 70-120 DEG C, preferably 80- 100℃。
7. preparation method according to claim 1, which is characterized in that in step (4), the sintering condition includes: temperature Degree is 650-1000 DEG C, preferably 800-900 DEG C;Time is 3-72h, preferably 24-48h.
8. the ferrous acid lithium material that preparation method according to any one of claims 1-7 obtains.
9. ferrous acid lithium material according to claim 8, which is characterized in that the ferrous acid lithium material is single crystal form, and table Face is also wrapped on amorphous carbon layer.
10. ferrous acid lithium material according to claim 9, which is characterized in that the amorphous carbon layer is in ferrous acid lithium material Content be 0.5-15 weight %.
CN201910840485.8A 2019-09-06 2019-09-06 A kind of ferrous acid lithium material and preparation method thereof Pending CN110498449A (en)

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CN112186143A (en) * 2020-08-14 2021-01-05 安徽德亚电池有限公司 Modified lithium iron oxide positive electrode material, preparation method thereof and positive plate
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WO2022007021A1 (en) * 2020-07-09 2022-01-13 湖北融通高科先进材料有限公司 Carbon-coated lithium-rich oxide composite material and preparation method therefor
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