CN103400969B - A kind of preparation method of high-performance lithium battery anode material of lithium iron phosphate/carbon composite powder - Google Patents
A kind of preparation method of high-performance lithium battery anode material of lithium iron phosphate/carbon composite powder Download PDFInfo
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- CN103400969B CN103400969B CN201310373486.9A CN201310373486A CN103400969B CN 103400969 B CN103400969 B CN 103400969B CN 201310373486 A CN201310373486 A CN 201310373486A CN 103400969 B CN103400969 B CN 103400969B
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- phosphate
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- iron phosphate
- lithium iron
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- 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
Abstract
The present invention relates to the preparation method of a kind of high-performance lithium battery anode material of lithium iron phosphate/carbon composite powder.The method is that raw material mixes with trivalent iron salt with high energy phosphate compound, and then mixes with lithium source, through carbon source reductive heat treatment under nitrogen protection atmosphere, synthesizes the lithium iron phosphate /carbon composite powder obtained containing high energy quantum dot.The present invention utilizes the phosphate group in high energy phosphate compound structure to be hydrolyzed a large amount of free energys of release, iron ion absorption is made to be attached on the energy-rich phosphate bond in high energy phosphate compound large biological molecule chain, form energy-rich phosphate iron granule, the chemical property of lithium iron phosphate positive material can be significantly improved, for the preparation of high-capacity lithium-ion power battery etc.
Description
Technical field
The present invention relates to a kind of preparation method of the lithium iron phosphate /carbon composite powder containing high energy quantum dot, belong to technical field of function materials.
Background technology
LiFePO4 (LiFePO
4) because having Stability Analysis of Structures, fail safe and Heat stability is good, low price, non-environmental-pollution, advantages such as high temperature circulation good reversibility and be subject to people and pay close attention to greatly, are considered to the high-capacity lithium-ion power battery positive electrode having application potential.But it also has the inferior positions such as preparation is more difficult, chemical property is poor.
Current preparation LiFePO
4method mainly contain: high temperature solid-state method, hydro thermal method, sol-gel process, coprecipitation, carbothermic method etc.The people such as Choi adopt sol-gel processing to synthesize LiFePO
4(see: Choi D, Kumta P N, Surfactant based sol-gel approach to nanostructured LiFePO
4for high rate Li-ion batteries.Journal of the Power Sources, 2007,163 (2): 1064-1069), the method chemical uniformity is good, heat treatment temperature is low, particle diameter is little and narrowly distributing, be easy to control, but dry shrink large, suitability for industrialized production is difficult, synthesis cycle is long.Co deposited synthesis LiFePO
4component is even, synthesis temperature is low, particle is thin, but tap density is little, seriously polluted; Water heat transfer LiFePO
4have that thing is mutually homogeneous, diameter of particle is little, but be only limited to the preparation of a small amount of powder, need high-temperature high-pressure apparatus, cost high.The people such as Wang adopt carbothermic method to synthesize LiFePO
4(see: Wang L, Liang G C, Ou X Q, Zhi X K, Zhang J P, Cui J Y, Effect of synthesis temperature on the properties of LiFePO
4/ C composites prepared by carbothermal reduction, Journal of the Power Sources, 2009,189 (1): 423-428), the method overcome the shortcoming that solid phase method cost is high, can material conductivity be improved, but the reaction time is long, product uniformity is poor, and particle is thicker; Have for this reason and adopt high temperature solid-state method synthesis LiFePO
4report, simple to operation comparatively speaking, but still have that synthesis cycle is long, product batch quality stability is poor, high in cost of production shortcoming.In addition, CN1635648A discloses a kind of preparation method of high-density spherical ferric lithium phosphate as anode material of lithium-ion battery, the method is first by the spherical or class ball shape ferric phosphate precursor of wet-chemical Reactive Synthesis, then with lithium source, carbon source, doping metals compound Homogeneous phase mixing, reducing atmosphere heat treatment obtains spherical LiFePO
4; CN101339995A provides a kind of preparation method of lithium iron phosphate positive electrode material for lithium ion power cell, and the method by adding micro-nano-metal-oxide or slaine, and adopts water system Wet technique to synthesize LiFePO
4.
Up to now, prior art mainly concentrates on and improves and LiFePO existing synthetic technology
4modification aspect, does not make LiFePO
4the synthetic technology of material, aspect of performance produce significant substantial variation, therefore, and the LiFePO of synthesis
4being difficult to because its performance is undesirable meet the needs for high-capacity lithium-ion power batteries such as electric automobile, electric adjustment, Aero-Space and energy-storage batteries, being badly in need of having new breakthrough in synthetic technology, to significantly improving LiFePO
4chemical property, thus meet the needs of new energy field to high-capacity lithium-ion power battery positive electrode.
Summary of the invention
For the deficiencies in the prior art, in order to solve the anode material for lithium-ion batteries LiFePO that prior art exists
4conductivity and the problem such as charging capacity is low, the invention provides a kind of preparation method of the lithium iron phosphate /carbon composite powder containing high energy quantum dot.Prepare a kind of lithium iron phosphate /carbon composite powder that there is high performance anode material of lithium battery and contain high energy quantum dot.
Term illustrates:
High energy quantum dot: the high energy quantum dot described in the present invention refers in lithium iron phosphate /carbon composite powder particle have that particle diameter is 1 ~ 6nm, its structure is in metastable high-energy nano particle-LiFePO4 particle.
High energy phosphate compound: refer to the phosphate cpd storing higher-energy is generally that release free energy is called high energy phosphate compound more than 5.0 kilocalories (20.9 kilojoule) when being hydrolyzed.
Technical scheme of the present invention is as follows:
A preparation method for the lithium iron phosphate /carbon composite powder of high-performance lithium cell positive material, step is as follows:
(1) by PO
4 3-concentration is that the high energy phosphate compound solution of 0.1 ~ 0.5mol/L cultivates 20 ~ 40min under 30 DEG C ~ 70 DEG C conditions, for subsequent use after chilling, is designated as solution A.
(2) according to FePO
4stoichiometric proportion, adds Fe in solution A
3+concentration is the ferric salt solution of 0.4 ~ 0.8mol/L, is 2.5 ~ 3.5 by watery hydrochloric acid adjust ph, fully stirs and ageing 3 ~ 5h, makes it produce sediment, after being separated washing at 100 ~ 120 DEG C dry 2h, obtain ferric phosphate powder.
(3) by LiFePO
4stoichiometric proportion, adds lithium source, then adds appropriate glucose or ascorbic acid in above-mentioned ferric phosphate powder, and abundant ground and mixed is even, obtains lithium iron phosphate/carbon composite precursor.
(4) by gained lithium iron phosphate/carbon composite precursor under nitrogen protection through 300 ~ 400 DEG C of heat treatment 1 ~ 2h, and then be warming up to 500 ~ 800 DEG C of heat treatment 2 ~ 4h, obtain lithium iron phosphate /carbon composite powder.
Gained lithium iron phosphate /carbon composite powder, granular size 50 ~ 220 nanometer, in meso-hole structure, mesoporous pore size is 10 ~ 40nm, and containing metastable energy-rich phosphate iron lithium particle in particle, size is 1 ~ 6nm.
According to the present invention, preferably, the high energy phosphate compound in step (1) is trinosin (ATP), PEP or amine formyl phosphoric acid.
According to the present invention, preferably, the chilling described in step (1) adopts liquid nitrogen chilling 6 ~ 20min.
According to the present invention, preferably, the watery hydrochloric acid mass concentration described in step (2) is 15 ~ 20wt%.
According to the present invention, preferably, the trivalent iron salt in step (2) is iron chloride or ferric nitrate.
According to the present invention, preferably, described in step (3), lithium source is lithium carbonate.
According to the present invention, preferably, Fe is pressed in step (3)
3+: C mol ratio is (24 ~ 25): (1 ~ 1.5) adds glucose or ascorbic acid; Preferred Fe further
3+: C mol ratio is 24:1.
The present invention is using the technical scheme of embodiment 1 as most preferably scheme.
Adopt the inventive method, key technology is combined with chemical synthesising technology at biotechnology, utilize the feature of the macromolecular chain of high energy phosphate compound itself and contained three energy-rich phosphate bonds, source of iron is mixed with high energy phosphate compound solution, the phosphate group in high energy phosphate compound structure is utilized to be hydrolyzed a large amount of free energys of release, iron ion absorption is made to be attached on the energy-rich phosphate bond in high energy phosphate compound large biological molecule chain, form energy-rich phosphate iron granule, and then with lithium source solid phase mixing, through carbon source reductive heat treatment under nitrogen protection atmosphere, formed in lithium iron phosphate/carbon complex matrix and be in metastable state and the special high energy quantum dot of its Structure and Properties, realize the thermochemical study of biomass energy.High energy phosphate compound is at LiFePO
4building-up process in, not only serve nanostructure template effect, also for preparation LiFePO
4provide phosphorus source and carbon source, and the different high energy quantum dot of Structure and Properties can be formed, be conducive to Li+ transmission, thus can LiFePO be improved
4the chemical property of positive electrode.
The lithium iron phosphate /carbon composite powder containing high energy quantum dot prepared by the inventive method, its particle is meso-hole structure, and mesoporous pore size is about 10 ~ 40nm; Powder granule is flake, granular size 50 ~ 220 nanometer, and thickness is 1 ~ 5 nanometer; Containing energy-rich phosphate iron lithium granule (high energy quantum dot) in lithium iron phosphate /carbon composite powder particle, its size is 1 ~ 6nm; Its structure different from lithium iron phosphate/carbon matrix (see encircled portion in Fig. 1 b), lattice fringe is different and unintelligible, illustrates that lattice distorts, is in metastable state (energy is high).The conductance of the lithium iron phosphate/carbon composite material containing high energy quantum dot prepared by the inventive method is 2.3 ~ 2.8 × 10
-3s/cm, 0.1C initial charge specific capacity is up to 197 ~ 208mAh/g, and its coulombic efficiency is 95% ~ 100%; When after circulation 100 times, 0.1C specific discharge capacity still can reach 157 ~ 179mAh/g, and its most high charge-discharge specific capacity has all exceeded LiFePO
4specific capacity theoretical value (170mAh/g).
Compared with the prior art, advantage of the present invention is to take high energy phosphate compound as stay in place form, phosphorus source and carbon source, iron ion is combined with energy-rich phosphate bond and forms energy-rich phosphate iron granule, realize the thermochemical study of biomass energy, in lithium iron phosphate/carbon complex matrix, define high energy quantum dot, effectively improve the chemical property of lithium iron phosphate positive material.The lithium iron phosphate /carbon composite powder prepared with the present invention can be used for preparing high-capacity lithium-ion power battery etc. as positive electrode.
Accompanying drawing explanation
Fig. 1 is the HRTEM photo of embodiment 1 synthetic powder, and b is the high multiple enlarged photograph in local of a.
Fig. 2 is the XRD spectra of embodiment 1 synthetic powder.
Fig. 3 is nitrogen adsorption desorption spectrogram (a) and the graph of pore diameter distribution (b) of embodiment 1 synthetic powder.
Embodiment
Below in conjunction with embodiment, the present invention will be further described, but be not limited thereto.
Embodiment 1,
By PO
4 3-concentration is that the trinosin solution of 0.2mol/L is incubated 30min at 40 DEG C, for subsequent use after then putting into rapidly liquid nitrogen chilling 10min, is designated as solution A.According to FePO
4stoichiometric proportion, adds the ferric chloride solution of 0.6mol/L in solution A, regulates its pH value to be 3 with 15wt% watery hydrochloric acid, abundant stirring ageing 4 hours, make it produce sediment, after being separated washing at 120 DEG C dry 2 hours, obtain the ferric phosphate powder of ecru.Then, by LiFePO
4stoichiometric proportion, adds lithium carbonate, then presses Fe in phosphoric acid iron powder
3+: C mol ratio is that 24:1 ratio adds ascorbic acid, and ground and mixed is even, obtains lithium iron phosphate/carbon presoma; Nitrogen atmosphere protection under by it in 350 DEG C of heat treatment 1.5h, then be warmed up to 700 DEG C insulation 3h, obtaining black lithium iron phosphate /carbon composite powder, is olivine-type LiFePO through its crystalline phase of X-ray diffraction analysis
4, as shown in Figure 2.Products therefrom powder granule is meso-hole structure, and as shown in Figure 3, mesoporous pore size is about 10 ~ 37nm; Lithium iron phosphate particles in structure is flake, granular size 50 ~ 200 nanometer, and thickness is 1 ~ 4 nanometer; Containing high energy quantum dot in lithium iron phosphate /carbon composite powder particle, its size is 1 ~ 3nm, as shown in encircled portion in Fig. 1 b; The conductance of this lithium iron phosphate/carbon composite material is 2.8 × 10
-3s/cm, 0.1C initial charge specific capacity is 197mAh/g, and first discharge specific capacity is 197mAh/g, and its coulombic efficiency is 100%; When after circulation 100 times, 0.1C specific discharge capacity reaches 179mAh/g.
Embodiment 2,
By PO
4 3-concentration is that the trinosin solution of 0.1mol/L is incubated 40min at 30 DEG C, for subsequent use after then putting into rapidly liquid nitrogen chilling 6min, is designated as solution A.According to FePO
4stoichiometric proportion, adds the ferric chloride solution of 0.4mol/L in solution A, regulates its pH value to be 2.5 with 20wt% watery hydrochloric acid, abundant stirring ageing 5 hours, make it produce sediment, after being separated washing at 120 DEG C dry 2 hours, obtain the ferric phosphate powder of ecru.Then, by LiFePO
4stoichiometric proportion, adds lithium carbonate, then presses Fe in phosphoric acid iron powder
3+: C mol ratio is that 25:1.5 ratio adds ascorbic acid, and ground and mixed is even, obtains lithium iron phosphate/carbon presoma; Nitrogen atmosphere protection under by it in 300 DEG C of heat treatment 2h, then be warmed up to 800 DEG C insulation 2h, obtain black lithium iron phosphate /carbon composite powder.Analyze after tested, powder granule mesoporous pore size is about 16 ~ 34nm; Lithium iron phosphate particles in structure is flake, granular size 70 ~ 180 nanometer, and thickness is 2 ~ 4 nanometers; Containing high energy quantum dot in lithium iron phosphate /carbon composite powder particle, its size is 2 ~ 5nm.The conductance of this lithium iron phosphate/carbon composite material is 2.4 × 10
-3s/cm, 0.1C initial charge specific capacity is 202mAh/g, and first discharge specific capacity is 199mAh/g, and its coulombic efficiency is 98.5%; When after circulation 100 times, 0.1C specific discharge capacity reaches 162mAh/g.
Embodiment 3,
By PO
4 3-concentration is that the trinosin solution of 0.5mol/L is incubated 20min at 70 DEG C, takes out for subsequent use, be designated as solution A after then putting into rapidly liquid nitrogen chilling 20min.According to FePO
4stoichiometric proportion, adds the ferric chloride solution of 0.8mol/L in solution A, regulates its pH value to be 3.5 with 17wt% watery hydrochloric acid, abundant stirring ageing 3 hours, make it produce sediment, after being separated washing at 100 DEG C dry 2 hours, obtain the ferric phosphate powder of ecru.Then, by LiFePO
4stoichiometric proportion, adds lithium carbonate, then presses Fe in phosphoric acid iron powder
3+: C mol ratio is that 23:1.2 ratio adds ascorbic acid, and ground and mixed is even, obtains lithium iron phosphate/carbon presoma; Nitrogen atmosphere protection under by it in 400 DEG C of heat treatment 1h, then be warmed up to 600 DEG C insulation 4h, obtain black lithium iron phosphate /carbon composite powder.Analyze after tested, powder granule mesoporous pore size is about 12 ~ 39nm; Lithium iron phosphate particles in structure is flake, granular size 65 ~ 210 nanometer, and thickness is 3 ~ 5 nanometers; Containing high energy quantum dot in lithium iron phosphate /carbon composite powder particle, its size is 3 ~ 6nm; The conductance of this lithium iron phosphate/carbon composite material is 2.3 × 10
-3s/cm, 0.1C initial charge specific capacity is 197mAh/g, and first discharge specific capacity is 193mAh/g, and its coulombic efficiency is 98%; When after circulation 100 times, 0.1C specific discharge capacity reaches 157mAh/g.
Embodiment 4,
As described in Example 1, difference is that high energy phosphate compound trinosin solution is changed to PEP solution, and other condition is with embodiment 1.Products therefrom lithium iron phosphate /carbon composite powder is analyzed after tested, and powder granule mesoporous pore size is about 11 ~ 36nm; Lithium iron phosphate particles in structure is flake, granular size 85 ~ 220 nanometer, and thickness is 1 ~ 3 nanometer; Containing high energy quantum dot in lithium iron phosphate /carbon composite powder particle, its size is 1 ~ 4nm; The conductance of this lithium iron phosphate/carbon composite material is 2.5 × 10
-3s/cm, 0.1C initial charge specific capacity is 208mAh/g, and first discharge specific capacity is 197mAh/g, and its coulombic efficiency is 94.9%; When after circulation 100 times, 0.1C specific discharge capacity reaches 159mAh/g.
Embodiment 5,
As described in Example 1, difference is that high energy phosphate compound trinosin solution is changed to amine formyl phosphoric acid solution, and source of iron iron chloride is changed to ferric nitrate, and reducing agent ascorbic acid is changed to glucose, and other condition is with embodiment 1.Products therefrom lithium iron phosphate /carbon composite powder is analyzed after tested, and powder granule mesoporous pore size is about 10 ~ 40nm; Lithium iron phosphate particles in structure is flake, granular size 100 ~ 210 nanometer, and thickness is 2 ~ 5 nanometers; Containing high energy quantum dot in lithium iron phosphate /carbon composite powder particle, its size is 2 ~ 6nm; The conductance of this lithium iron phosphate/carbon composite material is 2.3 × 10
-3s/cm, 0.1C initial charge specific capacity is 199mAh/g, and first discharge specific capacity is 190mAh/g, and its coulombic efficiency is 95.5%; When after circulation 100 times, 0.1C specific discharge capacity reaches 158mAh/g.
Claims (7)
1. a preparation method for high-performance lithium battery anode material of lithium iron phosphate/carbon composite powder, step is as follows:
(1) by PO
4 3-concentration is that the high energy phosphate compound solution of 0.1 ~ 0.5 mol/L cultivates 20 ~ 40 min under 30 DEG C ~ 70 DEG C conditions, for subsequent use after chilling, is designated as solution A;
Described high energy phosphate compound is trinosin (ATP), PEP or amine formyl phosphoric acid;
(2) according to FePO
4stoichiometric proportion, adds Fe in solution A
3+concentration is the ferric salt solution of 0.4 ~ 0.8 mol/L, is 2.5 ~ 3.5 by watery hydrochloric acid adjust ph, fully stirs and ageing 3 ~ 5 h, makes it produce sediment, after being separated washing at 100 ~ 120 DEG C dry 2 h, obtain ferric phosphate powder;
(3) by LiFePO
4stoichiometric proportion, adds lithium source, then adds appropriate glucose or ascorbic acid in above-mentioned ferric phosphate powder, and abundant ground and mixed is even, obtains lithium iron phosphate/carbon composite precursor;
(4) by gained lithium iron phosphate/carbon composite precursor under nitrogen protection through 300 ~ 400 DEG C of heat treatment 1 ~ 2 h, and then be warming up to 500 ~ 800 DEG C of heat treatment 2 ~ 4 h, obtain lithium iron phosphate /carbon composite powder.
2. the preparation method of high-performance lithium battery anode material of lithium iron phosphate/carbon composite powder according to claim 1, uses liquid nitrogen chilling 6 ~ 20min after it is characterized in that the high energy phosphate compound solution heat treated in step (1).
3. the preparation method of high-performance lithium battery anode material of lithium iron phosphate/carbon composite powder according to claim 1, is characterized in that the trivalent iron salt in step (2) is iron chloride or ferric nitrate.
4. the preparation method of high-performance lithium battery anode material of lithium iron phosphate/carbon composite powder according to claim 1, is characterized in that the watery hydrochloric acid mass concentration described in step (2) is 15 ~ 20wt%.
5. the preparation method of high-performance lithium battery anode material of lithium iron phosphate/carbon composite powder according to claim 1, is characterized in that described in step (3), lithium source is lithium carbonate.
6. the preparation method of high-performance lithium battery anode material of lithium iron phosphate/carbon composite powder according to claim 1, is characterized in that in step (3) by Fe
3+: C mol ratio is (24 ~ 25): (1 ~ 1.5) adds glucose or ascorbic acid.
7. the preparation method of high-performance lithium battery anode material of lithium iron phosphate/carbon composite powder according to claim 1, is characterized in that in step (3) by Fe
3+: C mol ratio is that 24:1 adds glucose or ascorbic acid.
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| CN104393256B (en) * | 2014-09-30 | 2017-03-15 | 齐鲁工业大学 | The preparation method of LiFePO4 phosphoric acid vanadium lithium/carbon In-situ reaction positive electrode |
| CN105720247B (en) * | 2016-02-03 | 2018-01-05 | 齐鲁工业大学 | A kind of preparation method of lithium sodium hybrid ionic battery composite anode material |
| CN108598418B (en) * | 2018-04-24 | 2021-01-26 | 齐鲁工业大学 | Amorphous NaVOPO (sodium VOPO) as negative electrode material of sodium ion battery4/C and preparation method and application thereof |
| CN111525102B (en) * | 2019-12-04 | 2023-01-03 | 南通鼎鑫电池有限公司 | Carbon quantum dot modified LiFePO 4 Preparation method of positive electrode material |
| CN111056544B (en) * | 2019-12-16 | 2022-11-04 | 合肥国轩高科动力能源有限公司 | Sodium iron phosphate composite material and preparation method and application thereof |
| CN114275755B (en) * | 2021-12-14 | 2023-07-04 | 河源职业技术学院 | Method for preparing lithium iron phosphate by taking eggshell inner membrane as template |
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