CN104347855A - Method for preparing phosphate-cladded lithium nickel manganese oxide and use of phosphate-cladded lithium nickel manganese oxide - Google Patents
Method for preparing phosphate-cladded lithium nickel manganese oxide and use of phosphate-cladded lithium nickel manganese oxide Download PDFInfo
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- CN104347855A CN104347855A CN201410522917.8A CN201410522917A CN104347855A CN 104347855 A CN104347855 A CN 104347855A CN 201410522917 A CN201410522917 A CN 201410522917A CN 104347855 A CN104347855 A CN 104347855A
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- 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
- H01M4/5805—Phosphides
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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Abstract
The invention discloses a method for preparing phosphate-cladded lithium nickel manganese oxide and use of the phosphate-cladded lithium nickel manganese oxide. The method for preparing the phosphate-cladded lithium nickel manganese oxide comprises the following steps: first, preparing spinel structure lithium nickel manganese oxide, and dispersing the spinel structure lithium nickel manganese oxide in metal nitrate to obtain a suspension; and then slowly dropwise adding a phosphate solution into the suspension, filtering, washing and drying to obtain the spinel structure phosphate-cladded lithium nickel manganese oxide positive electrode material. The preparing method disclosed by the invention is simple and easy to implement and has low requirements on equipment; and the obtained spinel structure phosphate-cladded lithium nickel manganese oxide positive electrode material has a relatively high specific capacity and a good prospect for industrial applications.
Description
Technical field
The invention belongs to technical field of nano material, be specifically related to a kind of preparation method and application of Phosphate coating nickel ion doped.
Background technology
Compared with lead-acid battery and nickel-cadmium cell, lithium ion battery has that operating voltage is high, energy density and power density is large, memory-less effect, have extended cycle life, environmental friendliness and the many merits such as self-discharge rate is low.As one of the battery of excellent performance in commercial secondary power supply, lithium ion battery is widely used in the middle-size and small-size transit equipment fields such as portable type electronic product and electric bicycle such as mobile phone, notebook computer, camera.But due to the restriction of power density and energy density aspect, it encounters a difficult problem in the application in the large-scale fields such as electric automobile, hybrid-electric car and intelligent grid.And the electrode material finding high-energy and power density becomes the key point addressed this problem.
The nickel ion doped of spinel structure has 4.7V high voltage platform, and its theoretical specific capacity is 147mAh g
-1, actual specific capacity is about 130mAh/g (A perspective on the high-voltage LiMn
1.5ni
0.5o
4spinel cathode for lithium-ion batteries, Manthiram, A., Chemelewski, K., Lee, E.-S., Energy & Environmental Science, 2014,7,1339-1350).With traditional LiCoO
2, LiFeO
4with LiMn
2o
4positive electrode is compared, and has higher energy density.Particularly it has the charging/discharging voltage platform of about 4.7V, under identical electric current, higher power density can be provided, thus favor by large-scale energy storage fields such as electric automobiles, developed into one of anode material for lithium-ion batteries of new generation most with application potential.And this material has three-dimensional diffusion passage, is conducive to Li
+fast transport (Spinel materials for high-voltage cathodes in Li-ion batteries, Liu, D., Zhu, W., Trottier, J., Gagnon, C., Barray, F., Guerfi, A., Mauger, A., Groult, H., Julien, C.M., Goodenough, J.B., Zaghib, K., RSC Advances, 2014,4,154-167).
But, because its discharge and recharge is interval close to 5V, exceed the stability window of the traditional electrolyte such as carbonates, in charge and discharge process, can there is oxidation Decomposition in electrolyte, and then cause the increase of battery impedance and decay (A Stable High-Voltage Cathode Material for Lithium-Ion Batteries., Chong, the J. of capacity, Xun, S., Zhang, J., Song, X., Xie, H., Battaglia, V., Wang, R., Li
3pO
4-Coated LiNi
0.5mn
1.5o
4, Chem.Eur.J., 2014,20,1-8).Under normal temperature condition, electrolyte decomposition speed is that slight fading phenomenon only appears in specific capacity relatively slowly.But when temperature continues to raise, as 55 DEG C of high temperature, decomposing phenomenon seriously aggravates, and in cyclic process, degradation appears in specific discharge capacity.
Surface coating modification is considered to can effectively improve one of its cycle performance mode.At present, the coating layer of this high potential positive pole is mainly concentrated as metal and nonmetal oxide.Such as, A.Manthiram etc. adopt electrostatic self-assembled method to realize Al
2o
3, ZnO, Bi
2o
3to LiMn
1.5ni
0.42zn
0.08o
4with LiMn
1.42ni
0.42co
0.16o
4evenly coated, the cycle performance of material significantly improves (Understanding the Improvement in the Electrochemical Properties of Surface Modified 5V LiMn
1.42ni
0.42co
0.16o
4spinel Cathodes in Lithium-ion Cells, Liu, J., Manthiram, A., Chemistry of Materials, 2009,21,1695-1707).For the positive electrode of Phosphate coating modified spinelle nickel ion doped, current report is relatively less, mainly contains AlPO
4, FePO
4with Li
3pO
4.Because all phosphate is all containing strong P=O double bond, effectively can suppress the generation of side reaction and the erosion of HF between electrolyte and electrode material, therefore other metal phosphates are also expected to as coating layer to improve the cyclical stability of nickel ion doped.Adopt Phosphate coating can improve the security performance of material simultaneously.
In order to improve the electrochemistry and security performance of improving nickel ion doped material, we adopt the coated nickel ion doped of lanthanum orthophosphate.
The preparation method and application of the coated nickel ion doped of lanthanum orthophosphate have not been reported.
Summary of the invention
The object of the invention is to the preparation method proposing the coated nickel ion doped of lanthanum orthophosphate.
Another object of the present invention is to provide the application of the coated nickel ion doped of the lanthanum orthophosphate of preparation in lithium rechargeable battery.
For deficiency of the prior art, the present invention adopts following technical scheme:
A preparations and applicatio for Phosphate coating nickel ion doped, its special character is: comprise the following steps:
1) by lithium acetate, nickel acetate, manganese acetate, acetate containing other doping X metal ions, citric acid and fluorine-containing, nitrogen or/and gel made by the ammonium salt of sulphur, then calcine, prepare LiNi
0.5mn
1.5-ax
ay
bo
4-bpositive electrode, wherein X be chromium, aluminium, cobalt, copper, zinc, rubidium, lanthanum, titanium, magnesium, iron, tungsten, sow, one or more in molybdenum, rhodium, niobium and vanadium, a is the ion populations summation of one or more metal ions X in this positive electrode molecular formula, 0≤a≤0.2; Y is one or more in fluorine, nitrogen and sulphur, and b is one or more in fluorine, nitrogen and the sulphur ion populations summations in this positive electrode molecular formula, wherein, and 0≤b≤0.2;
2) by LiNi
0.5mn
1.5-ax
ay
bo
4-bbe dispersed in metal nitrate, be made into the suspension-turbid liquid containing metal ions M, then drip the phosphate solution that mass percent concentration is metal nitrate 5 ~ 10 times, filtration product, calcines in atmosphere, prepares M
a(PO
4)
bcoated nickel lithium manganate cathode material, wherein M is magnesium, barium, copper, calcium, lanthanum, chromium, sows or the one of yttrium, and A is phosphate M
a(PO
4)
bthe number of middle metal ions M, B is phosphate M
a(PO
4)
bmiddle phosphate anion PO
4number; Phosphate accounts for M
a(PO
4)
bthe mass fraction of coated nickel lithium manganate cathode material is 1% ~ 5%.
Above-mentioned steps 2) in metal nitrate be one or more in magnesium nitrate, barium nitrate, copper nitrate, calcium nitrate, lanthanum nitrate, chromic nitrate, gallium nitrate and yttrium nitrate.
Above-mentioned steps 2) in phosphate be one or more in ammonium dihydrogen phosphate, diammonium hydrogen phosphate and triammonium phosphate.
Above-mentioned steps 2) calcination condition is: in air atmosphere, is warmed up to 400 ~ 950 DEG C with the speed of 2 ~ 5 DEG C/min, and keeps 0.5 ~ 9 hour at this temperature, after reaction terminates, in air atmosphere, naturally cool to room temperature.
The application in lithium ion secondary battery anode material of the Phosphate coating nickel ion doped prepared by said method.The invention has the beneficial effects as follows:
1, by preparation method of the present invention, a kind of new lithium ion secondary battery anode material is provided.
2, preparation method's preparation process of the present invention is simple, and equipment requirement is low, and course of reaction is pollution-free, and product uniformity is good, and the lanthanum orthophosphate prepared coated nickel ion doped material has better high gram volume, has good prospects for commercial application.
Accompanying drawing explanation
Fig. 1 is the embodiment of the present invention 1 step 1) gained pure phase LiNi
0.5mn
1.5o
4the XRD spectra of the spinel structure of sample;
Fig. 2 is the embodiment of the present invention 1 step 2) gained LaPO
4coated LiNi
0.5mn
1.5o
4the XRD spectra of the spinel structure of sample;
Fig. 3 is the embodiment of the present invention 1 step 1) gained pure phase LiNi
0.5mn
1.5o
4the SEM photo of sample;
Fig. 4 is the embodiment of the present invention 1 step 2) gained LaPO
4coated LiNi
0.5mn
1.5o
4the SEM photo of sample;
Fig. 5 is the embodiment of the present invention 1 step 1) gained pure phase LiNi
0.5mn
1.5o
4the X-ray energy scattering EDS spectrum of sample;
Fig. 6 is the embodiment of the present invention 1 step 2) gained LaPO
4coated LiNi
0.5mn
1.5o
4the X-ray energy scattering EDS spectrum of sample.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated, but the present invention is not limited thereto.
Embodiment raw materials, is analysis pure, content >=99.9%.
Embodiment 1
The preparation method of the coated nickel ion doped of lanthanum orthophosphate, comprises the following steps:
Step 1) preparation of nickel ion doped
Take two hydration lithium acetate 4.285g (0.042mol), four hydration nickel acetate 4.977g (0.02mol), four hydration manganese acetate 14.705g (0.06mol), be dissolved in 100mL deionized water, obtain green transparent solution one; Take monohydrate potassium 42.028g (0.2mol), be dissolved in 100mL deionized water, obtain colourless transparent solution two;
Under stirring, slowly solution one is added drop-wise in solution two, then ultrasonic 40min; Continue to stir under 90 DEG C of conditions, slowly boil off solvent, obtain light green color colloidal sol, then 120 DEG C of oven dry 10h obtain gel;
Gel is put into alumina crucible, at 400 DEG C of calcining 4h, then at 750 DEG C of sintering 10h, obtains brownish black spinel structure LiNi
0.5mn
1.5o
4positive electrode.
Step 2) the coated nickel ion doped of lanthanum orthophosphate
Take 0.518g lanthanum nitrate hexahydrate (5% mass ratio LaPO4), be dissolved in 50mL water, add 5.546g positive electrode, ultrasonic disperse 30min, form suspension-turbid liquid;
Claim 1.58g diammonium hydrogen phosphate, be dissolved in 30mL water, dropwise add suspension-turbid liquid under vigorous stirring, continue ultrasonic 20min, then suction filtration, solid is at 100 DEG C of dry 3h;
Dried solid is put into crucible, keeps 3h with the ramp of 5 DEG C/min to 500 DEG C, after cooling, namely obtain brownish black spinel structure LaPO
4coated LiNi
0.5mn
1.5o
4positive electrode.
Embodiment 2
The preparation method of lanthanum orthophosphate coated chromium doping nickel ion doped, comprise the following steps: the reaction environment of embodiment 2 and condition are with embodiment 1, difference is, in step 1) in, take two hydration lithium acetate 4.285g (0.042mol), four hydration nickel acetate 4.977g (0.02mol), four hydration manganese acetate 14.2152g (0.058mol), six water acetic acid chromium 0.67442g (0.002mol) are dissolved in 100mL deionized water.All the other steps are with embodiment 1.
Prepare LaPO
4coated LiNi
0.5mn
1.45cr
0.05o
4positive electrode.
Method of the present invention is applicable to equally being applicable to other metal-doped nickel ion doped, such as in step 1) the middle acetate of one or more adopting aluminium, cobalt, copper, zinc, rubidium, lanthanum, titanium, magnesium, iron and tungsten.
Material property characterizes
1) crystal structure test is carried out on Japanese Shimadzu X-ray diffractometer XRD-7000, adopts copper target, sweep speed 2 °/minute, measuring accuracy ± 0.04 °, sweep limits 5 ~ 90 °.
Embodiment 1 step 1) gained pure phase LiNi
0.5mn
1.5o
4the XRD spectra of the spinel structure of sample is shown in Fig. 1.
Embodiment 1 step 2) gained LaPO
4coated LiNi
0.5mn
1.5o
4the XRD spectra of the spinel structure of sample is shown in Fig. 2.
2) material surface pattern carries out on Zeiss, Germany company EV018 type scanning electron microscopy SEM, and X-ray energy scattering EDS spectrum and Element area profile carry out on Oxford X-MAX 20 type energy disperse spectroscopy.
Embodiment 1 step 1) the pure phase LiNi for preparing
0.5mn
1.5o
4the SEM image of particle is shown in Fig. 3.Fig. 5 is pure phase LiNi
0.5mn
1.5o
4x-ray energy scattering EDS spectrum, measure nickeliferous, manganese, oxygen and carbon.
Fig. 4 is embodiment 1 step 2) obtained LaPO
4coated LiNi
0.5mn
1.5o
4the SEM figure of particle.Fig. 6 is LaPO
4coated LiNi
0.5mn
1.5o
4x-ray energy scattering EDS spectrum, measure containing lanthanum, phosphorus, nickel, manganese, oxygen and carbon.Lanthanum and P elements derive from lanthanum orthophosphate, can determine that lanthanum orthophosphate is coated on LiNi
0.5mn
1.5o
4surface, generates LaPO
4coated LiNi
0.5mn
1.5o
4particle.
Electrochemical property test
90:2:8 gets LaPO in mass ratio
4coated LiNi
0.5mn
1.5o
4, super P and PVDF (HSV900), add appropriate 1-METHYLPYRROLIDONE as solvent, in glove box under argon shield, by magnetic stirrer 15 hours, prepare the required slurry of button electricity.Coating machine is Shenzhen Ke Jingzhida Science and Technology Ltd. MSK-AFA-III automatic spray dryer, coating clearance 25 microns, speed 5 cm per minute, slurry is evenly coated in 9 micron thickness that Jinxiang Copper Foil Co., Ltd., Mei County produces, on purity 99.8% shiny copper foil, vacuumize 12 hours at 120 DEG C, then strikes out at Shenzhen section brilliant MSK-T06 button cell sheet-punching machine the electrode foil that diameter is about 16 millimeter.CR2032 button cell is assembled in and carries out homemade being full of in 99.9% high-purity argon gas glove box, adopts Shenzhen section brilliant MSK-110 small-sized hydraulic button cell packaging machine.Negative pole is the high purity lithium sheet of purity 99.99% diameter 15.8 millimeters, and barrier film is thickness 16 microns of U.S. ENTEK LP16 type PE barrier films, and electrolyte is DMC:EMC (50:50, volume ratio), adds 1%VC (volume ratio), 1.3M LiPF
6.Button cell circulation and multiplying power test are carried out on the CT2001A tester of Wuhan Lan electricity Electronics Co., Ltd..
Electrochemistry cyclic voltammetry experiment carries out on the Huachen CHI604E of Shanghai, and work electrode is the LaPO prepared
4coated LiNi
0.5mn
1.5o
4, be lithium sheet to electrode and reference electrode, sweep speed is 200 μ V/s.
Through test, LaPO
4coated LiNi
0.5mn
1.5o
4discharge capacity is 108mAh/g first.
The coated nickel ion doped of the lanthanum orthophosphate prepared by the present invention has high gram volume, has a good application prospect at lithium rechargeable battery.
Claims (5)
1. a preparation method for Phosphate coating nickel ion doped, is characterized in that: comprise the following steps:
1) by lithium acetate, nickel acetate, manganese acetate, acetate containing other doping X metal ions, citric acid and fluorine-containing, nitrogen or/and gel made by the ammonium salt of sulphur, then calcine, prepare LiNi
0.5mn
1.5-ax
ay
bo
4-bpositive electrode, wherein X be chromium, aluminium, cobalt, copper, zinc, rubidium, lanthanum, titanium, magnesium, iron, tungsten, sow, one or more in molybdenum, rhodium, niobium and vanadium, a is the ion populations summation of one or more metal ions X in this positive electrode molecular formula, 0≤a≤0.2; Y is one or more in fluorine, nitrogen and sulphur, and b is one or more in fluorine, nitrogen and the sulphur ion populations summations in this positive electrode molecular formula, 0≤b≤0.2;
2) by LiNi
0.5mn
1.5-ax
ay
bo
4-bbe dispersed in metal nitrate, be made into the suspension-turbid liquid containing metal ions M, then drip the phosphate solution that mass percent concentration is metal nitrate 5 ~ 10 times, filtration product, calcines in atmosphere, prepares phosphate M
a(PO
4)
bcoated nickel lithium manganate cathode material, wherein M is magnesium, barium, copper, calcium, lanthanum, chromium, sows and one or more in yttrium, and A is phosphate M
a(PO
4)
bthe number of middle metal ions M, B is phosphate M
a(PO
4)
bmiddle phosphate anion PO
4number; Phosphate accounts for M
a(PO
4)
bthe mass percent of coated nickel lithium manganate cathode material is 1% ~ 5%.
2. the preparation method of Phosphate coating nickel ion doped according to claim 1, is characterized in that: step 2) in metal nitrate be one or more in magnesium nitrate, barium nitrate, copper nitrate, calcium nitrate, lanthanum nitrate, chromic nitrate, gallium nitrate and yttrium nitrate.
3. the preparation method of Phosphate coating nickel ion doped according to claim 1, is characterized in that: step 2) in phosphate be one or more in ammonium dihydrogen phosphate, diammonium hydrogen phosphate and triammonium phosphate.
4. the preparation method of Phosphate coating nickel ion doped according to claim 1, it is characterized in that: step 2) calcination condition is: in air atmosphere, 400 ~ 950 DEG C are warmed up to the speed of 2 ~ 5 DEG C/min, and keep 0.5 ~ 9 hour at this temperature, in air atmosphere, naturally cool to room temperature after reaction terminates.
5. the application in lithium ion secondary battery anode material of the Phosphate coating nickel ion doped prepared by any one of Claims 1 to 4.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105958054A (en) * | 2016-06-23 | 2016-09-21 | 中南大学 | Method for lanthanum phosphate coated lithium ion battery cathode material nickel cobalt lithium manganate |
| CN107516730A (en) * | 2016-06-17 | 2017-12-26 | 珠海泰坦储能科技有限公司 | A kind of preparation of the lithium sulfur battery anode material of phosphoric acid iron and the lithium-sulfur cell containing this positive electrode |
| CN109728285A (en) * | 2019-01-03 | 2019-05-07 | 清远佳致新材料研究院有限公司 | Anode material for lithium-ion batteries and preparation method thereof, lithium ion battery and electrical equipment |
| CN109888248A (en) * | 2019-03-26 | 2019-06-14 | 湖北锂诺新能源科技有限公司 | Manganese phosphate coats the preparation method of rich oxidate for lithium positive electrode |
| CN112151773A (en) * | 2019-06-26 | 2020-12-29 | 中国科学院物理研究所 | Positive active material, preparation method thereof and lithium battery |
| CN112186177A (en) * | 2019-07-04 | 2021-01-05 | 丰田自动车株式会社 | Nonaqueous electrolyte secondary battery and positive electrode active material |
| CN113488620A (en) * | 2021-06-28 | 2021-10-08 | 恒大新能源技术(深圳)有限公司 | Ternary positive electrode precursor and preparation method thereof, ternary positive electrode material and preparation method thereof, and lithium ion battery |
| CN113629229A (en) * | 2021-08-03 | 2021-11-09 | 浙江帕瓦新能源股份有限公司 | Phosphate-coated wet-method-doped ternary cathode material and preparation method thereof |
| CN114506877A (en) * | 2020-11-17 | 2022-05-17 | 松山湖材料实验室 | Method for preparing positive electrode active material, positive electrode, and lithium ion secondary battery |
| CN114512659A (en) * | 2020-11-17 | 2022-05-17 | 松山湖材料实验室 | Modified spinel-structured positive electrode active material, preparation method thereof, positive electrode and lithium ion secondary battery |
| CN114506830A (en) * | 2020-11-17 | 2022-05-17 | 松山湖材料实验室 | Preparation method of phosphate coated positive electrode active material |
| CN114566647A (en) * | 2022-02-09 | 2022-05-31 | 武汉理工大学 | Calcium phosphate coated high-nickel ternary cathode material and preparation method and application thereof |
| WO2023216672A1 (en) * | 2022-05-11 | 2023-11-16 | 宁波容百新能源科技股份有限公司 | Lithium nickel manganese oxide positive electrode material, preparation method therefor and application thereof |
| WO2024059980A1 (en) * | 2022-09-19 | 2024-03-28 | 宁德时代新能源科技股份有限公司 | Lithium-containing nickel-manganese composite oxide, preparation method therefor, positive electrode sheet containing same, secondary battery, and electrical apparatus |
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