CN106207114A - A kind of preparation method of low ferrum lithium porous LiFePO4 positive electrode - Google Patents
A kind of preparation method of low ferrum lithium porous LiFePO4 positive electrode Download PDFInfo
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- CN106207114A CN106207114A CN201610566031.2A CN201610566031A CN106207114A CN 106207114 A CN106207114 A CN 106207114A CN 201610566031 A CN201610566031 A CN 201610566031A CN 106207114 A CN106207114 A CN 106207114A
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- positive electrode
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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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 the preparation method of a kind of low ferrum lithium porous LiFePO4 positive electrode, the method is the calcium alginate fibre and Fe3+ wet method spinned, and PO43, Li+ carry out ion exchange, alginic acid fibre after exchange is taken out and dries, then prepare after high-temperature roasting under tube furnace nitrogen.Alginate fibre used by this preparation method is biological material, it it is the new fiber materials of environmental protection, and preparation method is simple, the gained micro-Guan Yinqi of lotus-like porous LiFePO4 carbon low ferrum lithium antistructure defect and special one-dimensional loose structure and there is higher specific capacity, cyclical stability and high rate performance.It is widely used in electronic product, the field such as electric bicycle and electric automobile.
Description
Technical field
The invention belongs to field of lithium ion battery material, particularly relate to one low ferrum lithium porous prepared by ion exchange
The preparation method of LiFePO4 positive electrode.
Background technology
The LiFePO4 anode material for lithium-ion batteries of olivine-type, high owing to having reversible capacity, safety is high, to ring
The advantages such as border is pollution-free are it is considered to be the ideal chose of anode material for lithium-ion batteries.The conjunction of traditional LiFePO4 positive electrode
One-tenth method includes, coprecipitation, high temperature solid-state method, carbothermic method, hydro-thermal and solvent-thermal method etc..But, these methods obtain
Chunk products often ferrum lithium antistructure defect content many, hinder the efficiently fully diffusion of lithium ion, thus cause high rate performance not
Good, and duct is undeveloped, and the specific surface area of material is little, thus, the shortcomings such as specific capacity is relatively low, govern LiFePO4 large-scale
Extensive application in electrical equipment.
In view of with first-class problem, the present invention utilizes alginate fibre for masterplate, and first alginate fibre is to utilize from natural sea
The alginic acid extracted in algae is raw material, by the high-performance fiber of a kind of green that wet spinning prepares, secondly in alginate fibre
Carboxyl and hydroxyl can form stable Egg tray structure chelate with iron ion, the two embodies good binding ability, with
Time alginate fibre in carboxyl can utilize electrostatic interaction adsorb Li+, the carbon of fiber reinforcement after high-temperature process, nitrogen, hydrogen can heat
Decomposing, thus form lotus-like porous LiFePO4@carbon micro-pipe positive electrode, the porous lotus-like carbon micro-tubular structure of this material is not
Provide only more effective electrode and electrolyte liquor contact area, and the transmission for lithium ion provide shorter path, simultaneously by
In the chelation of Egg tray structure, effectively inhibit ferrum lithium antistructure defect in pyroprocess, thus be effectively improved LiFePO4@carbon
Micro-pipe the most forthright.Secondly, multiple structure provides passage and the short transmission path of more lithium ion transport, is favorably improved
The specific capacity of material and the most forthright.Loose structure on fibre wall can buffer due to generation during lithium ion deintercalation repeatedly simultaneously
Cause the pressure that material lattice change in volume produces, be conducive to improving the cyclical stability of material.Therefore, low ferrum lithium antistructure defect
Lotus-like porous LiFePO4@carbon micro-pipe positive electrode by be a feasible raising LiFePO4 positive electrode specific capacity, times
The forthright method with cyclical stability.
Summary of the invention
The deficiency existed for prior art, it is an object of the invention to overcome existing lithium ion battery LiFePO4 positive pole
The specific capacity that material exists is relatively low, and the shortcomings such as high rate performance is poor, less stable seek to prepare the height ratio of a kind of green
Capacity, the preparation method of the forthright low ferrum lithium porous LiFePO4 positive electrode with high stability of high power.
For solving above-mentioned technical problem, the technical solution used in the present invention is: a kind of low ferrum lithium porous LiFePO4 positive pole
The preparation method of material, use alginic acid fibre as masterplate, by ion exchange realize iron ion, phosphate anion and lithium from
Son is combined with alginate fibre, obtains load only iron ion, phosphate anion, the Precursors of Fibers of lithium ion；Pass through high-temperature hot
Process, Precursors of Fibers high temperature is bakeed, is dried, just obtaining the lotus-like porous LiFePO4 micro-pipe of@carbon of low ferrum lithium antistructure defect
Pole material.
The preparation method of above-mentioned low ferrum lithium porous LiFePO4 positive electrode, specifically comprises the following steps that
Step one: be first immersed in the hydrochloric acid solution of 0.5mol/L-3mol/L by alginic acid fibre, alginic acid fibre is fallen in exchange
In calcium ion；
Step 2: subsequently alginic acid fibre is added iron ion/phosphate anion/lithium that concentration is 0.1mol/L-0.4mol/L
In the mixed salt solution of ion, obtain alginic acid fibre；
Step 3: the alginic acid fibre that step 2 prepares is placed in vacuum drying oven drying；
Step 4: the alginic acid fibre in step 3 is warmed up in tube furnace 650 DEG C 850 DEG C, heating rate in nitrogen
For 1-5 ° of C/min, baking times is 6-12h, is then cooled to room temperature, obtains low ferrum lithium porous LiFePO4 positive electrode.
The preparation method of above-mentioned low ferrum lithium porous LiFePO4 positive electrode, it is characterised in that: described hydrochloric acid solution can replace
Being changed to salpeter solution or sulfuric acid solution, concentration is 0.5mol/L-3mol/L.
The preparation method of above-mentioned low ferrum lithium porous LiFePO4 positive electrode, it is characterised in that: described iron ion/phosphoric acid
The mixed salt solution of radical ion/lithium ion is ferric nitrate, ammonium dihydrogen phosphate, lithium nitrate, and concentration is 0.1mol/L-0.4mol/L,
Ratio is 1:1:1.
The preparation method of above-mentioned low ferrum lithium porous LiFePO4 positive electrode, it is characterised in that: in described mixed salt solution
Ultrasonic disperse, ultrasonic power is 30w, and jitter time is 30min.
The preparation method of above-mentioned low ferrum lithium porous LiFePO4 positive electrode, it is characterised in that: described alginic acid fibre is
Wet spinning is made.
The advantage of the preparation method of the present invention low ferrum lithium porous LiFePO4 positive electrode is: use a kind of environmental protection
Alginate fibre as masterplate, utilizes the lotus-like porous of the low ferrum lithium antistructure defect that the chelation of alginic acid fibre obtains
The low ferrum lithium antistructure defect of LiFePO4@carbon micro-pipe positive electrode be conducive to the deintercalation of lithium ion, porous carbon structure be conducive to lithium from
Son and the diffusion of electronics and transmission, thus improve the charge/discharge capacity of LiFePO4, improve the most forthright.
Accompanying drawing explanation
Fig. 1 is the electron microscopic picture of the present invention, (a) 650 DEG C, (b) 750 DEG C, (c) 850 DEG C；
Fig. 2 is the XRD refine picture of the present invention；
Fig. 3 is the cycle performance curve of the present invention；
Fig. 4 is the rate discharge characteristic of the present invention；
Fig. 5 be the present invention different multiplying under charging and discharging curve.
Detailed description of the invention
Below in conjunction with the accompanying drawings, the present invention is described in further detail by technical scheme and embodiment.
A kind of preparation method of low ferrum lithium porous LiFePO4 positive electrode, use alginic acid fibre as masterplate, by from
Son exchange realizes iron ion, phosphate anion and lithium ion and is combined with alginate fibre, obtain loading only have iron ion, phosphate radical from
Son, the Precursors of Fibers of lithium ion；By high-temperature heat treatment, Precursors of Fibers high temperature is bakeed, is dried, obtain low ferrum lithium antiposition
Lotus-like porous LiFePO of defect4@carbon micro-pipe positive electrode.
The preparation method of above-mentioned low ferrum lithium porous LiFePO4 positive electrode, specifically comprises the following steps that
Step one: be first immersed in the hydrochloric acid solution of 0.5mol/L-3mol/L by alginic acid fibre, alginic acid fibre is fallen in exchange
In calcium ion；
Step 2: subsequently alginic acid fibre is added iron ion/phosphate anion/lithium that concentration is 0.1mol/L-0.4mol/L
In the mixed salt solution of ion, obtain alginic acid fibre；
Step 3: the alginic acid fibre that step 2 prepares is placed in vacuum drying oven drying；
Step 4: the alginic acid fibre in step 3 is warmed up in tube furnace 650 DEG C 850 DEG C, heating rate in nitrogen
For 1-5 ° of C/min, baking times is 6-12h, is then cooled to room temperature, obtains low ferrum lithium porous LiFePO4 positive electrode.
The preparation method of above-mentioned low ferrum lithium porous LiFePO4 positive electrode, it is characterised in that: described hydrochloric acid solution can replace
Being changed to salpeter solution or sulfuric acid solution, concentration is 0.5mol/L-3mol/L.
The preparation method of above-mentioned low ferrum lithium porous LiFePO4 positive electrode, it is characterised in that: described iron ion/phosphoric acid
The mixed salt solution of radical ion/lithium ion is ferric nitrate, ammonium dihydrogen phosphate, lithium nitrate, and concentration is 0.1mol/L-0.4mol/L,
Ratio is 1:1:1.
The preparation method of above-mentioned low ferrum lithium porous LiFePO4 positive electrode, it is characterised in that: in described mixed salt solution
Ultrasonic disperse, ultrasonic power is 30w, and jitter time is 30min.
The preparation method of above-mentioned low ferrum lithium porous LiFePO4 positive electrode, it is characterised in that: described alginic acid fibre is
Wet spinning is made.
Embodiment one: weigh 2g alginic acid fibre, by deionized water soaking and washing once, by cleaned alginic acid fibre
It is immersed in the hydrochloric acid solution that concentration is 1mol/L that 200mL deionized water is configured to, supersound process 40 minutes, ultrasonic completes
Rear filtration, then be dipped in hydrochloric acid, in triplicate.What alginic acid fibre joined 200mL deionized water is configured to subsequently is dense
Degree is for, in the ferric nitrate of 0.1mol/L, ammonium dihydrogen phosphate and lithium nitrate mixed solution, impregnating 30 minutes, afterwards in vacuum drying oven
Dry.Alginic acid fibre is warmed up in tube furnace 650 ° of C, and heating rate is 2 ° of C/min, roasting 8h in nitrogen, cools down afterwards
To room temperature, obtain low ferrum lithium porous LiFePO4 positive electrode.
Embodiment two: weigh 2g alginic acid fibre, by deionized water soaking and washing once, by cleaned alginic acid fibre
It is immersed in the hydrochloric acid solution that concentration is 1mol/L that 200mL deionized water is configured to, supersound process 40 minutes, ultrasonic completes
Rear filtration, then be dipped in hydrochloric acid, in triplicate.What alginic acid fibre joined 200mL deionized water is configured to subsequently is dense
Degree is for, in the ferric nitrate of 0.2mol/L, ammonium dihydrogen phosphate and lithium nitrate mixed solution, impregnating 30 minutes, afterwards in vacuum drying oven
Dry.Alginic acid fibre is warmed up in tube furnace 750 ° of C, and heating rate is 2 ° of C/min, roasting 10h in nitrogen, cools down afterwards
To room temperature, obtain low ferrum lithium porous LiFePO4 positive electrode.
Embodiment three: weigh 2g alginic acid fibre, by deionized water soaking and washing once, by cleaned alginic acid fibre
It is immersed in the hydrochloric acid solution that concentration is 1mol/L that 200mL deionized water is configured to, supersound process 40 minutes, ultrasonic completes
Rear filtration, then be dipped in hydrochloric acid, in triplicate.What alginic acid fibre joined 200mL deionized water is configured to subsequently is dense
Degree is for, in the ferric nitrate of 0.3mol/L, ammonium dihydrogen phosphate and lithium nitrate mixed solution, impregnating 30 minutes, afterwards in vacuum drying oven
Dry.Alginic acid fibre is warmed up in tube furnace 850 ° of C, and heating rate is 2 ° of C/min, roasting 12h in nitrogen, cools down afterwards
To room temperature, obtain low ferrum lithium porous LiFePO4 positive electrode.
Embodiment four: weigh 2g alginic acid fibre, by deionized water soaking and washing once, by cleaned alginic acid fibre
It is immersed in the hydrochloric acid solution that concentration is 1mol/L that 200mL deionized water is configured to, supersound process 40 minutes, ultrasonic completes
Rear filtration, then be dipped in hydrochloric acid, in triplicate.What alginic acid fibre joined 200mL deionized water is configured to subsequently is dense
Degree is for, in the ferric nitrate of 0.4mol/L, ammonium dihydrogen phosphate and lithium nitrate mixed solution, impregnating 30 minutes, afterwards in vacuum drying oven
Dry.Alginic acid fibre is warmed up in tube furnace 750 ° of C, and heating rate is 2 ° of C/min, roasting 6h in nitrogen, cools down afterwards
To room temperature, obtain low ferrum lithium porous LiFePO4 positive electrode.
Above in conjunction with accompanying drawing, the present invention is exemplarily described, it is clear that the present invention implements not by above-mentioned reality
Execute the restriction of mode.The present invention can be made various on the premise of conceiving without departing from the technology of the present invention by those skilled in the art
Amendment or modification, within these amendments or modification also fall into protection scope of the present invention certainly.
Claims (6)
1. the preparation method of one kind low ferrum lithium porous LiFePO4 positive electrode, it is characterised in that: use alginic acid fibre as mould
Version, is realized iron ion, phosphate anion and lithium ion is combined with alginate fibre by ion exchange, obtain loading only have ferrum from
Son, phosphate anion, the Precursors of Fibers of lithium ion；By high-temperature heat treatment, Precursors of Fibers high temperature is bakeed, is dried, i.e.
Obtain lotus-like porous LiFePO of low ferrum lithium antistructure defect4@carbon micro-pipe positive electrode.
The preparation method of low ferrum lithium porous LiFePO4 positive electrode the most according to claim 1, it is characterised in that: concrete
Step is as follows:
Step one: be first immersed in the hydrochloric acid solution of 0.5mol/L-3mol/L by alginic acid fibre, alginic acid fibre is fallen in exchange
In calcium ion；
Step 2: subsequently alginic acid fibre is added iron ion/phosphate anion/lithium that concentration is 0.1mol/L-0.4mol/L
In the mixed salt solution of ion, obtain alginic acid fibre；
Step 3: the alginic acid fibre that step 2 prepares is placed in vacuum drying oven drying；
Step 4: the alginic acid fibre in step 3 is warmed up in tube furnace 650 DEG C 850 DEG C, heating rate in nitrogen
For 1-5 ° of C/min, baking times is 6-12h, is then cooled to room temperature, obtains low ferrum lithium porous LiFePO4 positive electrode.
The preparation method of low ferrum lithium porous LiFePO4 positive electrode the most according to claim 2, it is characterised in that: described
Hydrochloric acid solution can be replaced salpeter solution or sulfuric acid solution, and concentration is 0.5mol/L-3mol/L.
The preparation method of low ferrum lithium porous LiFePO4 positive electrode the most according to claim 3, it is characterised in that: described
The mixed salt solution of iron ion/phosphate anion/lithium ion is ferric nitrate, ammonium dihydrogen phosphate, lithium nitrate, and concentration is 0.1mol/
L-0.4mol/L, ratio is 1:1:1.
The preparation method of low ferrum lithium porous LiFePO4 positive electrode the most according to claim 4, it is characterised in that: described
Ultrasonic disperse in mixed salt solution, ultrasonic power is 30w, and jitter time is 30min.
The preparation method of low ferrum lithium porous LiFePO4 positive electrode the most according to claim 5, it is characterised in that: described
Alginic acid fibre is that wet spinning is made.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106814111A (en) * | 2017-02-13 | 2017-06-09 | 山东旭晟东阳新材料科技有限公司 | A kind of hollow porous SnO2Micro-pipe gas sensor and preparation method thereof |
| CN109244379A (en) * | 2017-09-14 | 2019-01-18 | 太原理工大学 | A kind of LiFePO4The preparation method of ultrathin nanometer piece@graphene aerogel positive electrode |
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| CN105185987A (en) * | 2014-05-29 | 2015-12-23 | 宁德新能源科技有限公司 | Positive electrode material and lithium ion secondary battery |
| CN105576217A (en) * | 2016-03-17 | 2016-05-11 | 齐鲁工业大学 | Preparation method of three-dimensional carbon in-situ coated phosphate positive electrode material |
| CN105609753A (en) * | 2015-12-14 | 2016-05-25 | 青岛大学 | Preparation method for one-dimensional multi-layer porous fibrous positive electrode material of lithium ion battery |
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2016
- 2016-07-19 CN CN201610566031.2A patent/CN106207114A/en active Pending
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|---|---|---|---|---|
| CN103553015A (en) * | 2013-09-29 | 2014-02-05 | 东华大学 | Preparation method of carbon-nanotube-modified lithium iron phosphate lithium ion battery positive electrode material |
| CN105185987A (en) * | 2014-05-29 | 2015-12-23 | 宁德新能源科技有限公司 | Positive electrode material and lithium ion secondary battery |
| CN105609753A (en) * | 2015-12-14 | 2016-05-25 | 青岛大学 | Preparation method for one-dimensional multi-layer porous fibrous positive electrode material of lithium ion battery |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106814111A (en) * | 2017-02-13 | 2017-06-09 | 山东旭晟东阳新材料科技有限公司 | A kind of hollow porous SnO2Micro-pipe gas sensor and preparation method thereof |
| CN109244379A (en) * | 2017-09-14 | 2019-01-18 | 太原理工大学 | A kind of LiFePO4The preparation method of ultrathin nanometer piece@graphene aerogel positive electrode |
| CN109244379B (en) * | 2017-09-14 | 2021-06-22 | 太原理工大学 | LiFePO4Preparation method of ultrathin nanosheet @ graphene aerogel positive electrode material |
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Application publication date: 20161207 |