CN106450222A - Preparation method of hollow spherical lithium nickel manganese oxide capable of automatically regulating pore diameter - Google Patents
Preparation method of hollow spherical lithium nickel manganese oxide capable of automatically regulating pore diameter Download PDFInfo
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- 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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- 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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Abstract
The invention discloses a preparation method of hollow spherical lithium nickel manganese oxide capable of automatically regulating the pore diameter. The preparation method comprises the steps that 1, a mixed solution of manganese salt and nickel salt, a sodium carbonate solution and a sodium hydroxide solution are prepared with deionized water separately, wherein the molar ratio of manganese salt to nickel salt is 3:1, the molar concentration of the manganese salt ranges from 0.1 mol/L to 1 mol/L, the molar concentration of sodium carbonate ranges from 0.1 mol/L to 1 mol/L, and the molar concentration of sodium hydroxide ranges from 0.1 mol/L to 1 mol/L; 2, the sodium carbonate solution is dropwise added into the mixed solution of the manganese salt and the nickel salt, reacting is conducted for 0.5 h to 2 h, then the sodium hydroxide solution is dropwise added into the solution, reacting is conducted for 0.5 h to 2 h, and filtering, washing and drying are conducted in sequence; 3, obtained precipitates are calcined at the temperature of 350 DEG C to 600 DEG C to obtain a precursor, after the precursor and lithium salt are mixed according to the manganese-lithium molar ratio of 3:2, calcining is conducted for 2 h to 10 h at the temperature of 750 DEG C to 900 DEG C, and then lithium nickel manganese oxide can be obtained.
Description
Technical field
The present invention relates to the technology of preparing of nickel ion doped.
Background technology
Lithium ion battery has important application prospect in fields such as energy-storage systems.With lithium ion battery in electric motor car side
The fast development of face application, people propose further requirement to the specific energy density of battery, specific power density.
Spinel-type nickel ion doped has high-energy-density（Theoretical value 1100 Wh/kg, actual value approaches as 700
Wh/kg）And high working voltage（Electrode potential about 4.7 V, vs Li/Li+）, stable structure, abundant preparing raw material, Gao An
The features such as full performance, be high-energy-density, the contenders of high power density type anode material for lithium-ion batteries（Referring to：Cai
Y, Huang S Z, She F S, et al. Facile synthesis of well-shaped spinel
LiNi0.5Mn1.5O4nanoparticles as cathode materials for lithium ion batteries[J].
Rsc Advances, 2015, 6(4):2785-2792.）In recent years, the research and development of high-voltage electrolyte achieve rapid progress,
Make the exploitation prospect of nickel ion doped material more optimistic（Referring to：Kang Xu. Electrolytes and
interphases in Li-ion batteries and beyond[J]. Chem. Rev., 2014, 114: 11503–
11618）.
In order to improve the power density of nickel ion doped material further, need to be firstly placed on improving it by focus quickly to fill
Discharge capability, i.e. high rate capability.It is known that the key factor of impact lithium ion battery high rate performance is lithium ion and electronics
Migration rate in electrode material, and the main method increasing transport kinetics is to design and can make lithium ion and electronics
The material structure of fast transferring, or improve material morphology material minimizing lithium ion and electron transfer path.（Okubo M,
Mizuno Y, Yamada H, et al. Fast Li-Ion Insertion into Nanosized LiMn2O4
without Domai Boundaries[J]. Acs Nano, 2010, 4(2):741-52.）.
In pattern research, hollow structure has cavity, can increase the specific surface area of material, strengthens electrolyte and material
Contact area, increased Li+Diffusion, thus improve the high rate capability of positive electrode.Liu little Lin
（CN103915616A）Deng the preparation method also reporting the spherical nickel ion doped of similar associated hollow, invention is with water and a small amount of ethanol
For reaction dissolvent, the use of soluble manganese salt and sodium acid carbonate is raw material, prepares MnCO at room temperature3Presoma micron ball, with
MnCO3Presoma micron ball is spherical template, according to Kinkendal Effect, so that forerunner's surface layer is mixed in the reaction generation of lithium salts nickel salt
The obvious LiNi of hollow structure0.5Mn1.5O4Positive electrode.
Additionally, Wang Zhenbo (CN103474650A) etc. also discloses hollow pattern high-voltage anode material
LiNi0.5Mn1.5O4Preparation method, at a certain temperature calcine manganese carbonate, then dissolve manganese carbonate kernel with diluted acid, remain
Under manganese dioxide be shell, then obtain hollow pattern nickel ion doped with nickel source manganese source mixed calcining.
To sum up two methods also represent two big thinkings of present hollow structure preparation, during Kirkendall effect auxiliary is formed
Hollow structure presoma and with the manganese carbonate after pickling calcining and then form hollow structure presoma, but both approaches all cannot be adjusted
The size of section cavity.The chemical property of material is closely related with the size of cavity, so the preparation of hollow structure material also needs
Researcher is wanted to probe into further.
Content of the invention
It is an object of the invention to provide a kind of can the autonomous hollow sphere nickel ion doped of adjustment aperture preparation method.
The present invention be can the autonomous hollow sphere nickel ion doped of adjustment aperture preparation method, its step is：
（1）Deionized water prepares mixed solution, sodium carbonate liquor and the sodium hydroxide solution of manganese salt/nickel salt, wherein manganese respectively
The mol ratio of salt and nickel salt is 3:1, the molar concentration 0.1-1 mol/L of manganese salt, the molar concentration of sodium carbonate is 0.1-1 mol/
L；The molar concentration of NaOH is 0.1-1 mol/L；
（2）After sodium carbonate liquor being added drop-wise to reaction 0.5-2h in the mixed solution of manganese salt/nickel salt, drip NaOH thereto
Solution, then react filtration/washing post-drying after 0.5-2h；
（3）The sediment obtaining is obtained presoma in 350 DEG C of -600 DEG C of calcinings, after presoma and lithium salts mixing, Mn and lithium
Mol ratio is 3:2, calcine 2-10 h at 750 DEG C -900 DEG C, you can obtain hollow pattern nickel ion doped.
The invention has benefit that：With respect to the preparation method of traditional hollow structure, the present invention does not use at acid
Reason, still for hollow structure, and the present invention can be adjusted by adjusting sodium carbonate and the addition sequence of NaOH and addition
The size of control cavity.And then form the hollow spheres nickel ion doped of cavity tuneable.
Brief description
Fig. 1 is the scanning electron microscope (SEM) photograph of embodiment 1 hollow spheres nickel ion doped.Fig. 2 is embodiment 2 hollow spheres nickel ion doped
Scanning electron microscope (SEM) photograph.
Specific embodiment
The present invention be can the autonomous hollow sphere nickel ion doped of adjustment aperture preparation method, its step is：
（1）Deionized water prepares mixed solution, sodium carbonate liquor and the sodium hydroxide solution of manganese salt/nickel salt, wherein manganese respectively
The mol ratio of salt and nickel salt is 3:1, the molar concentration 0.1-1 mol/L of manganese salt, the molar concentration of sodium carbonate is 0.1-1 mol/
L；The molar concentration of NaOH is 0.1-1 mol/L；
（2）After sodium carbonate liquor being added drop-wise to reaction 0.5-2h in the mixed solution of manganese salt/nickel salt, drip NaOH thereto
Solution, then react filtration/washing post-drying after 0.5-2h；
（3）The sediment obtaining is obtained presoma in 350 DEG C of -600 DEG C of calcinings, after presoma and lithium salts mixing, Mn and lithium
Mol ratio is 3:2, calcine 2-10 h at 750 DEG C -900 DEG C, you can obtain hollow pattern nickel ion doped.
Above-mentioned steps（1）Described in manganese salt be manganese sulfate, or manganese acetate, or manganese nitrate, or manganese chloride, or its
One of or two or more arbitrary proportion mixture；Described nickel salt is nickel sulfate, or nickel acetate, or nickel nitrate, or
Person's nickel chloride, or the mixture of one or more arbitrary proportions therein.
Above-mentioned steps（2）The dripping quantity of middle sodium carbonate liquor is 0.5-0.9 times of manganese nickel complete sedimentation theory amount；Hydroxide
The dripping quantity of sodium solution is 0.2-0.7 times of manganese nickel complete sedimentation theory amount, and sodium carbonate and NaOH add total amount to should be manganese
1.1-1.5 times of nickel complete sedimentation theory amount.
Above-mentioned steps（3）Described in lithium salts be lithium carbonate, or lithium acetate, or lithium nitrate, or lithium hydroxide, or
The mixture of one or more arbitrary proportions therein.
Resulting materials of the present invention have uniform spherical shapes, surface pore formation, and inside has special cavity structure.Overall
Nano particle group is had to become regular spherical hollow loose structure.Porous shell and special cavity increased the specific surface of material
Long-pending, strengthen the contact area of electrolyte and material, the diffusion for increasing lithium ion and electronics provides excellent dynamics and supports,
And decrease the intercalation/deintercalation resistance of lithium ion, reduce because of the stress of Lithium-ion embeding/abjection generation, battery can be significantly improved
High rate capability, and then lifted battery specific power density.
The present invention when after add a small amount of NaOH, by Ostwald ripening on carbonic acid sediment shelling, before exacerbating
Drive Kirkendall effect in roasting process for the body, simple is that solid porous knot is typically obtained during sediment using carbonate
Structure, and add a small amount of NaOH in the reaction so that the hydroxide producing is changed into oxide in roasting process, volume
Rapid contraction, increased the migration free path of manganese atom and nickle atom, thus producing obvious cavity structure.
Its principle of the cavity tuneable of the present invention is：Generate carbonic acid sediment after sodium carbonate adds, NaOH adds
Generate hydrogen-oxygen sediment, form one kind with carbonate sediment as core through the principle of Ostwald ripening, hydrogen-oxygen sediment is shell
Spherical precipitation material.During roasting, oxygen atom slow transits through gas-solid interface and spreads to core center, and manganese, nickle atom are fast
Speed, to external diffusion, thus there occurs Kirkendall effect.Simultaneously as in last stage reaction, with air contact, hydrogen-oxygen nickel manganese
Sediment will become nickel manganese oxide material, and now lattice structure is acutely shunk（Due to water will be lost when changing）This structure both shrinks
On the one hand accelerate reaction speed, also increase the migration free path of manganese, nickle atom simultaneously, so when the consumption of NaOH increases
Added-time manganese, nickle atom migration free path are consequently increased so that Kirkendall effect is had an effect in bigger space,
Reach simultaneously and become big effect when hydroxyl consumption increases then cavity.So hollow structure cavity size can be controlled.
Embodiment 1：（1）By Mn (Ac)2·4H2O and Ni (Ac)2·6H2O is dissolved in deionized water, wherein the rubbing of manganese ion
Your concentration is 1mol/L, and wherein the mol ratio of manganese salt and nickel salt is 3:1.Sodium carbonate is dissolved in deionized water（Carbonate molar concentration
For 0.5mol/L）；
（2）Sodium carbonate liquor is added drop-wise in the mixed solution of manganese salt/nickel salt to react after 0.5 h, drips NaOH thereto
Solution（Hydroxyl molar concentration is 0.1mol/L）, then react filtration/washing post-drying after 2h；
（3）Obtained solids of sedimentation powder is mixed by hand lapping and lithium salts（Li:Mn=2:3）, by mixture
Calcine 10 hours at 800 DEG C, you can obtain the spherical nickel lithium manganate cathode material of hollow diameters about 600 nm.
As shown in figure 1, prepared nickel lithium manganate cathode material has hollow structure.
Embodiment 2：（1）By Mn (Ac)2·4H2O and Ni (Ac)2·6H2O is dissolved in deionized water, wherein the rubbing of manganese ion
Your concentration is 0.6 mol/L, and wherein the mol ratio of manganese and nickel is 3:1；,.Sodium carbonate is dissolved in deionized water（Carbonate molar concentration
For 0.5mol/L）；
（2）Sodium carbonate liquor is added drop-wise in the mixed solution of manganese salt/nickel salt to react after 0.5 h, drips NaOH thereto
Solution（Hydroxyl molar concentration is 0.4 mol/L）, then react filtration/washing post-drying after 1h；
（3）Obtained solids of sedimentation powder is mixed by hand lapping and lithium acetate（Li:Mn=2:3）, will mix
Thing calcines 10 hours at 800 DEG C, you can obtain the spherical nickel lithium manganate cathode material of hollow diameters about 800 nm, such as schemes
Shown in 2.
Embodiment 3：（1）By Mn (Ac)2·4H2O and Ni (Ac)2·6H2O is dissolved in deionized water, wherein the rubbing of manganese ion
Your concentration is 0.1 mol/L, and wherein the mol ratio of manganese and nickel is 3:1.Sodium carbonate is dissolved in deionized water（Carbonate molar concentration is
1mol/L）；
（2）Sodium carbonate liquor is added drop-wise in the mixed solution of manganese salt/nickel salt to react after 2 h, and dropping NaOH is molten thereto
Liquid（Hydroxyl molar concentration is 1 mol/L）, then react filtration/washing post-drying after 2h；
（3）Obtained solids of sedimentation powder is mixed by hand lapping and lithium carbonate（Li:Mn=2:3）, will mix
Thing calcines 10 hours at 750 DEG C, prepared nickel lithium manganate cathode material, has hollow structure.
Embodiment 4：（1）By MnSO4·2H2O and NiSO4·6H2O is dissolved in deionized water, and wherein manganese ion is mole dense
Spending the mol ratio for 0.1 mol/L, wherein manganese and nickel is 3:1.Sodium carbonate is dissolved in deionized water（Carbonate molar concentration is
1mol/L）；
（2）Sodium carbonate liquor is added drop-wise in the mixed solution of manganese salt/nickel salt to react after 2 h, and dropping NaOH is molten thereto
Liquid（Hydroxyl molar concentration is 1 mol/L）, then react filtration/washing post-drying after 2h；
（3）Obtained solids of sedimentation powder is mixed by hand lapping and lithium nitrate（Li:Mn=2:3）, will mix
Thing calcines 2 h at 800 DEG C, prepared nickel lithium manganate cathode material, has hollow structure.
Embodiment 5：（1）By MnSO4·2H2O and NiSO4·6H2O is dissolved in deionized water, and wherein manganese ion is mole dense
Spending the mol ratio for 1 mol/L, wherein manganese and nickel is 3:1.Sodium carbonate is dissolved in deionized water（Carbonate molar concentration is 1mol/
L）；
（2）Sodium carbonate liquor is added drop-wise in the mixed solution of manganese salt/nickel salt to react after 2 h, and dropping NaOH is molten thereto
Liquid（Hydroxyl molar concentration is 1 mol/L）, then react filtration/washing post-drying after 0.5 h；
（3）Obtained solids of sedimentation powder is mixed by hand lapping and lithium nitrate（Li:Mn=2:3）, will mix
Thing calcines 10 h at 900 DEG C, prepared nickel lithium manganate cathode material, has hollow structure.
Claims (4)
1. can the autonomous hollow sphere nickel ion doped of adjustment aperture preparation method it is characterised in that its step is：
（1）Deionized water prepares mixed solution, sodium carbonate liquor and the sodium hydroxide solution of manganese salt/nickel salt, wherein manganese respectively
The mol ratio of salt and nickel salt is 3:1, the molar concentration 0.1-1 mol/L of manganese salt, the molar concentration of sodium carbonate is 0.1-1 mol/
L；The molar concentration of NaOH is 0.1-1 mol/L；
（2）After sodium carbonate liquor being added drop-wise to reaction 0.5-2h in the mixed solution of manganese salt/nickel salt, drip NaOH thereto
Solution, then react filtration/washing post-drying after 0.5-2h；
（3）The sediment obtaining is obtained presoma in 350 DEG C of -600 DEG C of calcinings, after presoma and lithium salts mixing, Mn and lithium
Mol ratio is 3:2, calcine 2-10 h at 750 DEG C -900 DEG C, you can obtain hollow pattern nickel ion doped.
2. according to claim 1 can the autonomous hollow sphere nickel ion doped of adjustment aperture preparation method, its feature exists
In：Step（1）Described in manganese salt be manganese sulfate, or manganese acetate, or manganese nitrate, or manganese chloride, or one kind therein
Or the mixture of two or more arbitrary proportion；Described nickel salt is nickel sulfate, or nickel acetate, or nickel nitrate, or nickel chloride,
Or the mixture of one or more arbitrary proportions therein.
3. according to claim 1 can the autonomous hollow sphere nickel ion doped of adjustment aperture preparation method, its feature exists
In：Step（2）The dripping quantity of middle sodium carbonate liquor is 0.5-0.9 times of manganese nickel complete sedimentation theory amount；Sodium hydroxide solution
Dripping quantity is 0.2-0.7 times of manganese nickel complete sedimentation theory amount, and it is completely heavy that sodium carbonate and NaOH addition total amount should be manganese nickel
1.1-1.5 times of shallow lake theoretical amount.
4. according to claim 1 can the autonomous hollow sphere nickel ion doped of adjustment aperture preparation method, its feature exists
In：Step（3）Described in lithium salts be lithium carbonate, or lithium acetate, or lithium nitrate, or lithium hydroxide, or therein
Kind or the mixture of two or more arbitrary proportion.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109599553A (en) * | 2018-11-20 | 2019-04-09 | 湘潭大学 | A kind of hollow sphere nickel sodium manganate and preparation method thereof, sodium-ion battery positive plate and sodium-ion battery |
| CN114613986A (en) * | 2022-03-18 | 2022-06-10 | 北京卫蓝新能源科技有限公司 | Heterogeneous layered structure precursor and preparation method and application thereof |
| CN114772556A (en) * | 2022-06-20 | 2022-07-22 | 天津蓝天太阳科技有限公司 | Porous structure precursor, hollow structure oxide and application in anode material |
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| CN103187564A (en) * | 2011-12-28 | 2013-07-03 | 上海空间电源研究所 | Preparation method for battery anode material LiNi0.5Mn1.5O4 |
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| CN103187564A (en) * | 2011-12-28 | 2013-07-03 | 上海空间电源研究所 | Preparation method for battery anode material LiNi0.5Mn1.5O4 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109599553A (en) * | 2018-11-20 | 2019-04-09 | 湘潭大学 | A kind of hollow sphere nickel sodium manganate and preparation method thereof, sodium-ion battery positive plate and sodium-ion battery |
| CN114613986A (en) * | 2022-03-18 | 2022-06-10 | 北京卫蓝新能源科技有限公司 | Heterogeneous layered structure precursor and preparation method and application thereof |
| CN114772556A (en) * | 2022-06-20 | 2022-07-22 | 天津蓝天太阳科技有限公司 | Porous structure precursor, hollow structure oxide and application in anode material |
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