CN103326016A - Preparation method of layered lithium (Li)-rich manganese (Mn)-based anode material having multiple core-shell structures - Google Patents

Preparation method of layered lithium (Li)-rich manganese (Mn)-based anode material having multiple core-shell structures Download PDF

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CN103326016A
CN103326016A CN2013102830002A CN201310283000A CN103326016A CN 103326016 A CN103326016 A CN 103326016A CN 2013102830002 A CN2013102830002 A CN 2013102830002A CN 201310283000 A CN201310283000 A CN 201310283000A CN 103326016 A CN103326016 A CN 103326016A
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lithium
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shell structure
rich manganese
based anode
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何则强
熊利芝
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Jishou University
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Abstract

The invention discloses a preparation method of a layered lithium (Li)-rich manganese (Mn)-based anode material having multiple core-shell structures. The layered (1-t)LiNixCoyMn1-x-yO2@tLi2MnO3 having the multiple core-shell structures is prepared by taking LiNixCoyMn1-x-yO2 (the x is greater than or equal to 0 while the y is less than or equal to 1) as cores and Li2MnO3 with the concentration in gradient change as shells. According to the method, the core-shell structures are applied into the lithium (Li)-rich layered material, namely, the concept of the multiple core-shell structures is put forward, so that the defects reported in the literature that the simple core-shell structure material has poor performance and the concentration gradient material is complicated to operate and difficult to realize are overcome. In the method, the core-shell concentrations are in antigradient change according to a certain arithmetic progression, namely, from the cores to the outer shells, the concentrations of the core materials are in gradually-decreased arithmetic progression distribution while the concentrations of the shell material are in gradually-increased arithmetic progression distribution. During the design, the equal concentration of transition metal ions in every layer is ensured, so that the interfacial resistance of the materials is reduced as far as possible. As a result, the material performance is improved.

Description

A kind of preparation method of multi-kernel shell structure stratiform lithium-rich manganese-based anode material
Technical field
The present invention relates to a kind of preparation method of multi-kernel shell structure stratiform lithium-rich manganese-based anode material.
Background technology
Owing to can showing unusual chemical property, as height ratio capacity (specific discharge capacity surpasses 230mAh/g, reaches as high as 300mAh/g), high-specific-power (reaching 300Wh/kg) and new charge discharge mechanism, the rich lithium material Li of stratiform 1+X+m 1-xo 2(transition metal that M is one or more) becomes one of the study hotspot in anode material for lithium-ion batteries field in global range, also makes it become the most possible positive electrode candidate of high performance lithium ion battery technology of future generation.Research through nearly 20 years, researchers are for the defect of such material, many improved measures (as bulk phase-doped, that surface coats etc.) have been proposed, promoted widely the practicalization of the rich lithium material of stratiform, yet still there are some shortcomings at present in such material, as irreversible capacity is large, cycle performance is undesirable, the thermal stability of de-lithium material is poor, high rate performance is undesirable and cryogenic property is bad etc.Therefore, how to such material advance novelty structural design, its preparation technology is optimized promoting the practical still very necessary of such material.
For the research of anode material for lithium-ion batteries, except research is carried out, surface coating, the modified method such as bulk phase-doped, some material new preparation technologies, new method also frequently having occurred to existing material system.Wherein design of material being become to nucleocapsid structure (with the advantage of giving full play to nuclear material and shell material, overcome their shortcomings separately) is exactly a very promising method .su and Yoshio etc. adopt the co-precipitation mode to prepare the nucleocapsid structure presoma the earliest, and then form nucleocapsid structure raising stratiform LiNi 1-xco xmn yo 2performance.The rich manganese stratified material that rich nickel dam shape material, the shell material that the nuclear material that they adopt is high power capacity, low cyclicity and fail safe is high security, Stability Analysis of Structures, cyclicity is good, finally obtained the material of the excellent combination properties such as capacity, cycle performance, high rate performance and security performance.Sun etc. further designs and has prepared the core-shell material of concentration gradient subsequently, continuously change by increasing a constant displacement pump the continuous alternation of charging composition that the salting liquid composition is realized salt, to reduce the component difference between core and shell material, reduce the phase boundary resistance between material, further optimized the performance of material.But because experiment condition is restive, need accurate instrument and strictly control condition.Zhang Lianqi etc. find under study for action, the rich lithium material Li of stratiform 1.2co 0.4mn 0.4o 2-Li 1.2ni 0.2mn 0.6o 2-Li 1.2ni 0.4mn 0.4o 2can form in gamut, and the different charge-discharge mechanisms of composition may be different, thereby have caused great chemical property difference.2011, the success of U.S. Argonne laboratory was applied to the synthetic of the rich lithium material of stratiform to concentration gradient nucleocapsid structure designing material concept, has observed excellent chemical property.These studying enlightenments we: adopting coprecipitation to control the component gradient nucleocapsid structure of presoma, is feasible thereby prepare the rich lithium material of the stratiform with component gradient nucleocapsid structure.But the first nucleocapsid structure material that Sun proposes preparation is simple, controllability is strong, but the second nucleocapsid structure material that performance proposes than them is poor; And although the second nucleocapsid structure material property is excellent, the preparation difficulty, poor controllability, be difficult for suitability for industrialized production, causes homogeneity of product poor.And, from material essence, there is the structural mutation between nuclear material and shell material in the former, between latter's nuclear material and shell material, composition changes continuously, does not have structural mutation so excellent material performance.So, whether exist a kind of between the structure between the two, the preparation that had both taken into account the former is simple, the advantage that controllability is strong, can bring into play again the high performance advantage of material? under this thinking, we have proposed a kind of nucleocapsid structure with " the many shells of a core " type, it is the multi-kernel shell structure, in this structure, component gradient is the staged variation, in theory, step number (this research is called " multiple degree ") is larger, material structure more approaches concentration gradient nucleocapsid structure (the second), material property is also better, but in limited multiple degree, this structure specific concentration gradient core shell structure has more operability.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of multi-kernel shell structure stratiform lithium-rich manganese-based anode material, take into account to realize the perfection of this material at aspects such as high power capacity and cycle performance, security performance, high rate performances.
The objective of the invention is to realize as follows: with LiNi xco ymn 1-x-yo 2for core (0≤x, y≤1), the Li that changes with concentration in gradient 2mnO 3for shell, prepare multi-kernel shell structure stratiform (1-t) LiNi xco ymn 1-x-yo 2@tLi 2mnO 3.
Described multi-kernel shell structure stratiform (1-t) LiNi xco ymn 1-x-yo 2@tLi 2mnO 3the preparation that one of preparation process is core and shell precursor solution: by He Meng source, ,Gu source, nickel source according to metal ion n (Ni 2+): n (Co 2+): n (Mn 2+)=x:y:(1-x-y) the precursor solution that the even mixing salt solution of preparation finite concentration is nuclear material; The manganese source is mixed with to certain density Mn simultaneously 2+precursor solution as shell material.
Described multi-kernel shell structure stratiform (1-t) LiNi xco ymn 1-x-yo 2@tLi 2mnO 3the even mixing that two of preparation process is core and shell precursor solution: from the precursor solution of nuclear material and shell material, taking-up accounts for the solution of the volume that the volume fraction of overall solution volume separately is identical respectively.The core solution of taking-up is to certain arithmetic progression (successively decreasing) according to volume and is divided into some parts: A1, A2 ... An; Equally by the shell solution of taking-up according to volume be reverse arithmetic progression (increasing progressively) be divided into same umber: B1, B2 ... Bn.Then corresponding salting liquid is uniformly mixed to form salting liquid A1B1, A2B2 ... AnBn.
Described multi-kernel shell structure stratiform (1-t) LiNi xco ymn 1-x-yo 2@tLi 2mnO 3three of preparation process is the formation of core presoma: according to certain drop rate to stirring and add above-mentioned remaining core solution in reactor, add the pH value of certain density aqueous slkali regulator solution to certain value, coprecipitation reaction obtains the suspension of nuclear material presoma at a certain temperature, and its solid is the presoma (Ni of nuclear material xco ymn 1-x-y) (OH) 2.
Described multi-kernel shell structure stratiform (1-t) LiNi xco ymn 1-x-yo 2@tLi 2mnO 3four of preparation process is the formation of multiple shell presoma: in the suspension of above-mentioned nuclear material presoma, stir successively add salting liquid A1B1, A2B2 ... AnBn, finally add the above-mentioned remaining shell solution of claim, realizes repeatedly co-precipitation.
Described multi-kernel shell structure stratiform (1-t) LiNi xco ymn 1-x-yo 2@tLi 2mnO 3five of preparation process is the formation of the lithium-rich manganese-based material presoma of multi-kernel shell structure stratiform: stop reaction after all salting liquids all add reactor, dry 12-24h after Separation of Solid and Liquid, washing in 105 ℃ of vacuum drying ovens, obtain the lithium-rich manganese-based material presoma of multi-kernel shell structure stratiform (1-t) [Ni xco ymn 1-x-y(OH) 2]@t[Mn (OH) 2].
Described multi-kernel shell structure stratiform (1-t) LiNi xco ymn 1-x-yo 2@tLi 2mnO 3six of preparation process is the formation of the lithium-rich manganese-based material of multi-kernel shell structure stratiform: by the lithium-rich manganese-based material presoma of multi-kernel shell structure stratiform and lithium source evenly be blended according to a certain percentage in Muffle furnace according to cooling after certain roasting system roasting, grind and obtain multi-kernel shell structure stratiform (1-t) LiNi xco ymn 1-x-yo 2@tLi 2mnO 3.
Described source metal can be one or more in nitrate, sulfate, oxalates, halide or other organic metal salt of this metal.
Described alkali can be one or more in NaOH, ammoniacal liquor, sodium carbonate, sodium acid carbonate or other alkaline matter.
Described lithium source can be one or both in lithium carbonate, lithium hydroxide.
Described roasting system refers to the multistep roasting of steps such as comprising low temperature presintering and high temperature sintering, and roasting time can change from 0.5h to 48h.
Described multi-kernel shell structure stratiform (1-t) LiNi xco ymn 1-x-yo 2@tLi 2mnO 3in the scope of t value be 0≤t≤0.5, particularly 0≤t≤0.3.
The present invention applies to nucleocapsid structure in rich lithium stratified material, has proposed the concept of multi-kernel shell structure, has overcome that the simple nucleocapsid structure material property of bibliographical information is not good enough and the concentration gradient material operation complicated, be difficult to the shortcoming realized.The concentration of core and shell is antigradient according to certain arithmetic progression and changes, by core to shell, the nuclear material concentration arithmetic progression that tapers off distributes, shell material is the arithmetic progression that progressively increases and distributes.The transition metal ions concentration that guarantees each layer during design is the same, to reduce as far as possible the phase boundary resistance of storeroom, improves the performance of material.
Multi-kernel shell structure stratiform (1-t) LiNi that adopts the present invention to prepare xco ymn 1-x-yo 2@tLi 2mnO 3lithium ion battery as positive electrode is applicable to the equipment that various mobile electronic devices maybe need mobile driven by energy, such as mobile phone, notebook computer, portable camera, electric bicycle, electric automobile, hybrid-electric car and energy storage device etc.
embodiment:
the preparation of embodiment 1(triple core-shell structure material)
A. the preparation of nuclear material and shell material precursor solution: with amount of substance, than Ni:Co:Mn=5:2:3, prepare a certain amount of certain density nuclear material salting liquid A; Prepare certain density manganese salt solution as shell material salting liquid B.The ratio that control A, B GOLD FROM PLATING SOLUTION belong to ion is 9:1;
B. take out respectively 70% of total liquor capacity from salting liquid A and salting liquid B, the A solution and the B solution that take out part be divided into respectively to 2 parts, be designated as A1(40%), A2(30%) and B1(30%), B2(40%); Corresponding A solution is evenly mixed with B solution, form salting liquid A1B1, A2B2;
C. stir the salting liquid A that adds residue 30% according to certain drop rate in reactor, add the pH value of certain density sodium hydrate regulator solution to certain value 10-11, obtain the suspension of nuclear material presoma at 60 ℃ of lower coprecipitation reactions, its solid be nuclear material presoma ( ni 0.5 co 0.2 mn 0.3 ) (OH) 2 ;
D. conservation condition is constant, in above-mentioned suspension, stirs and adds salting liquid A1B1, A2B2 successively, finally adds the salting liquid B of residue 30%, realizes repeatedly co-precipitation;
E. all salting liquids stop reaction after all adding reactor, after Separation of Solid and Liquid, washing, in 105 ℃ of vacuum drying ovens, dry 18h, obtain the lithium-rich manganese-based material presoma of multi-kernel shell structure stratiform 0.9[Ni 0.5 co 0.2 mn 0.3 (OH) 2 ]@0.1[Mn (OH) 2 ];
F. by gained in e 0.9[Ni 0.5 co 0.2 mn 0.3 (OH) 2 ]@0.1[Mn (OH) 2 ]with lithium hydroxide, according to 1:1.2(, be the volatilization that prevents lithium, lithium hydroxide is suitably excessive) evenly be blended in Muffle furnace carry out cooling after two one-step bakings (first 400 ℃ low temperature presintering 3h after 950 ℃ of high temperature sintering 16h), grind and obtain multi-kernel shell structure stratiform 0.9LiNi 0.5 co 0.2 mn 0.3 o 2 @0.1Li 2 mnO 3 .
The chemical property of gained sample is measured as follows: the sample that is 80% by mass fraction, 10% acetylene black and 10% Kynoar (PVDF), and make electrode slice and be assembled into battery by embodiment 1.The loop test of electrode material adopts the charge-discharge magnification of 0.2C under room temperature to charge to 4.2V, is discharged to 3.0V.The sample discharge curve stable discharge voltage plateau occurs in the 3.6V left and right, and reversible specific capacity is about 192 mAh/g first, and the capability retention of 0.2C multiplying power after 50 circulations reaches 94.5%; The capability retention of 5C multiplying power after 50 circulations reaches 89.9%.

Claims (12)

1. the preparation method of a multi-kernel shell structure stratiform lithium-rich manganese-based anode material, it is characterized in that: this material is with LiNi xco ymn 1-x-yo 2for core (0≤x, y≤1), the Li that changes with concentration in gradient 2mnO 3for shell.
2. the preparation method of a kind of multi-kernel shell structure stratiform lithium-rich manganese-based anode material according to claim 1 is characterized in that: by He Meng source, ,Gu source, nickel source according to metal ion n (Ni 2+): n (Co 2+): n (Mn 2+)=x:y:(1-x-y) the precursor solution that the even mixing salt solution of preparation finite concentration is nuclear material; The manganese source is mixed with to certain density Mn simultaneously 2+precursor solution as shell material.
3. the preparation method of a kind of multi-kernel shell structure stratiform lithium-rich manganese-based anode material according to claim 1 is characterized in that: the solution that takes out respectively the volume that the volume fraction that accounts for overall solution volume separately is identical from the precursor solution of nuclear material and shell material; The core solution of taking-up is to certain arithmetic progression (successively decreasing) according to volume and is divided into some parts: A1, A2 ... An; Equally by the shell solution of taking-up according to volume be reverse arithmetic progression (increasing progressively) be divided into same umber: B1, B2 ... Bn; Then corresponding salting liquid is uniformly mixed to form salting liquid A1B1, A2B2 ... AnBn.
4. the preparation method of a kind of multi-kernel shell structure stratiform lithium-rich manganese-based anode material according to claim 1, it is characterized in that: according to certain drop rate to stirring and add the described remaining core solution of claim 3 in reactor, add the pH value of certain density aqueous slkali regulator solution to certain value, coprecipitation reaction obtains the suspension of nuclear material presoma at a certain temperature, and its solid is the presoma (Ni of nuclear material xco ymn 1-x-y) (OH) 2.
5. the preparation method of a kind of multi-kernel shell structure stratiform lithium-rich manganese-based anode material according to claim 1, it is characterized in that: in the described suspension of claim 4, stir successively add salting liquid A1B1, A2B2 ... AnBn, finally add the described remaining shell solution of claim 3, realize repeatedly co-precipitation.
6. the preparation method of a kind of multi-kernel shell structure stratiform lithium-rich manganese-based anode material according to claim 1, it is characterized in that: stop reaction after all salting liquids all add reactor, dry 12-24h after Separation of Solid and Liquid, washing in 105 ℃ of vacuum drying ovens, obtain the lithium-rich manganese-based material presoma of multi-kernel shell structure stratiform (1-t) [Ni xco ymn 1-x-y(OH) 2]@t[Mn (OH) 2].
7. the preparation method of a kind of multi-kernel shell structure stratiform lithium-rich manganese-based anode material according to claim 1 is characterized in that: by the presoma of gained in claim 6 and lithium source evenly be blended according to a certain percentage in Muffle furnace according to cooling after certain roasting system roasting, grind and obtain multi-kernel shell structure stratiform (1-t) LiNi xco ymn 1-x-yo 2@tLi 2mnO 3.
8. the preparation method of a kind of multi-kernel shell structure stratiform lithium-rich manganese-based anode material according to claim 1 is characterized in that: the source metal described in claim 2 can be one or more in nitrate, sulfate, oxalates, halide or other organic metal salt of this metal.
9. the preparation method of a kind of multi-kernel shell structure stratiform lithium-rich manganese-based anode material according to claim 1, it is characterized in that: the alkali described in claim 4 can be one or more in NaOH, ammoniacal liquor, sodium carbonate, sodium acid carbonate or other alkaline matter.
10. the preparation method of a kind of multi-kernel shell structure stratiform lithium-rich manganese-based anode material according to claim 1, it is characterized in that: the lithium source described in claim 7 can be one or both in lithium carbonate, lithium hydroxide.
11. the preparation method of a kind of multi-kernel shell structure stratiform lithium-rich manganese-based anode material according to claim 1, it is characterized in that: the roasting system described in claim 7 refers to the multistep roasting of steps such as comprising low temperature presintering and high temperature sintering, and roasting time can change from 0.5h to 48h.
12. the preparation method of a kind of multi-kernel shell structure stratiform lithium-rich manganese-based anode material according to claim 1 is characterized in that: the scope of the t value in claim 6 and claim 7 is 0≤t≤0.5, particularly 0≤t≤0.3.
CN2013102830002A 2013-07-08 2013-07-08 Preparation method of layered lithium (Li)-rich manganese (Mn)-based anode material having multiple core-shell structures Pending CN103326016A (en)

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US20150155556A1 (en) * 2013-11-29 2015-06-04 Semiconductor Energy Laboratory Co., Ltd. Lithium-manganese composite oxide and secondary battery
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Application publication date: 20130925