CN108630913A - A kind of conduction electric double layer cladded type tertiary cathode material and preparation method thereof - Google Patents
A kind of conduction electric double layer cladded type tertiary cathode material and preparation method thereof Download PDFInfo
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- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- 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 present invention is suitable for field of lithium, a kind of conductive electric double layer cladded type tertiary cathode material and preparation method are provided, the present invention is coated by electric double layer, first layer is inorganic conductive clad, it is coated by wet method, inorganic conductive substance can be effectively and uniformly coated to material surface, constitute effective Li+ ion conductors, improve Li+ transmittabilities；The second layer is organic conductive layers, has good electronic conductance effect, it is effectively increased material electric conductivity, and organic conductive layers have " sponge " effect, it is broken in extrusion process that its flexibility can reduce material, the structural intergrity of effective protection material, pass through the cladding of electric double layer, reduce because the case where causing conductivity of material to decline because of clad under normal conditions, and the generation of surface side reaction can also be further reduced by organic conductive layers cladding, improve surface texture, and organic conductive layers cladding can be with the extruding between padded coaming, protection materials stable structure, pass through the above mechanism, the cycle performance of material has obtained larger improvement.
Description
Technical field
The invention belongs to anode material of lithium battery field more particularly to a kind of conductive electric double layer cladded type tertiary cathode materials
And preparation method thereof.
Background technology
Nickelic nickel cobalt aluminium (manganese) ternary anode material for lithium-ion batteries is due to higher energy density and relatively
Simple preparation process is widely used in IT product and new-energy automobile field.But simple nickle cobalt lithium manganate (LNCA
(M)) since structural stability is not good enough, in growth process charge and discharge process especially in the case of high voltage, it is easy to due to table
The side reaction in face causes cycle performance decaying fast, and safety is also easy to get great harm.It is general to use for these problems
The mode of cladding improves, but common cladding, due to the presence of the non-conductive performance of coating, leads to electronic conductance and ion-conductance
It leads and is weakened, influence electronics and ion transmission, electrical property is weakened.
Invention content
In view of the above problems, the purpose of the present invention is to provide a kind of conductive electric double layer cladded type tertiary cathode material and its
Preparation method, it is intended to which solving the clad of existing tertiary cathode material influences electronics and ion transmission, the poor technology of electrical property
Problem.
On the one hand, the preparation method of the conductive electric double layer cladded type tertiary cathode material includes the following steps：
Step S1, the once sintered semi-finished product of positive electrode are weighed, pure water, inorganic ions conductor object are weighed according to certain proportion
The once sintered semi-finished product of the positive electrode, pure water, inorganic ions conductive species are mixed matter, are then dehydrated, are dry
It is dry；
Step S2, the mixture after step S1 dryings is put into atmosphere furnace and is sintered；
Step S3, material after the sintering that step S2 is obtained is weighed, then weighs certain proportion organic solvent, organic conductive forerunner
Material, organic solvent and organic conductive presoma after the sintering weighed are mixed, are then put into ice bath, so by body
Oxidant is added afterwards and continues stirring a period of time；
Step S4, the obtained mixtures of step S3 are put into vacuum drying chamber and are dried, then by the object after drying
Matter carries out can be obtained conductive electric double layer cladded type tertiary cathode material except iron sieving.
Further, in step S1, the once sintered semi-finished product of positive electrode, pure water, the inorganic ions conductive species that weigh
Mass ratio be 1:(1~5):(0.0001~0.005) is mixed at being then 20~50 DEG C in water temperature, and incorporation time is
15~80min, the inorganic ions conductor are as a kind of or several in tungstate lithium, boron oxide lithium, lithium phosphate either lithium zirconate
Kind.
Further, the sintering time in step S2 is 2~15h, and sintering temperature is 300~800 DEG C.
Further, in step S3, the matter of material, organic solvent, organic conductive presoma after the step S2 sintering weighed
Amount is than being 1:(1~10):(0.001~0.01), is then mixed, and the mixing time is 2~5h, and the organic solvent is
Absolute ethyl alcohol, DMF, the one or several kinds in NMP, dimethylbenzene, dichloromethane, the organic precursor be pyrroles with to toluene
Azochlorosulfonate acid sodium mixture and aniline dodecyl benzene sulfonic acid and one kind of ammonium persulfate acid mixed solution or two kinds.
Further, oxidant is added in step S3, in ice bath and continues 1~15h of stirring, the organic conductive presoma with
The mass ratio of oxidant is 1：(0.02~0.1), the oxidant are FeCl3·6H2O、MnO2、ZnO2One or more of.
Further, in step S4, time for being dried in vacuum drying chamber is 5~10h, drying temperature is 60~
120℃。
Further, the once sintered semi-finished product nickel cobalt lithium aluminate of the positive electrode or nickel cobalt aluminium LiMn2O4.
On the other hand, the conductive electric double layer cladded type tertiary cathode material is prepared using the above method, pattern
For spherical shape, matrix composition is nickel cobalt lithium aluminate or nickle cobalt lithium manganate, and tertiary cathode material Components Chemical formula can be used
LixNi1-a-b-cCoaMbO2It indicates, 0.85≤x≤1.2,0≤a≤0.15,0.01≤b≤0.03, wherein M are Al or Mn.
The beneficial effects of the invention are as follows：The present invention carries out two layers of cladding to positive electrode, and first layer coats for inorganic conductive
Layer, is coated by wet method, can inorganic conductive substance be effectively and uniformly coated to material surface, constitute effective Li+ ions
Conductor improves Li+ transmittabilities；The second layer is organic conductive layers, has good electronic conductance effect, is effectively increased material electricity
Conductance, and organic conductive layers have " sponge " effect, and flexibility can reduce material being crushed in extrusion process, effectively protect
The structural intergrity of protective material is reduced by the cladding of electric double layer because under normal conditions because clad leads to conductivity of material
The case where decline, and the generation that can also be further reduced surface side reaction is coated by organic conductive layers, improve surface
Structure, and organic conductive layers cladding can pass through the above machine with the extruding between padded coaming, protection materials stable structure
Reason, the cycle performance of material have obtained larger improvement.
Description of the drawings
Fig. 1 is the Electronic Speculum of conductive electric double layer cladded type nickel cobalt lithium aluminate tertiary cathode material prepared by the embodiment of the present invention one
Figure；
Fig. 2 is the electrical property comparison diagram of the embodiment of the present invention one and comparative example lithium battery.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
The method of the present invention uses following steps：
Step S1, the once sintered semi-finished product of positive electrode are weighed, pure water, inorganic ions conductor object are weighed according to certain proportion
The once sintered semi-finished product of the positive electrode, pure water, inorganic ions conductive species are mixed matter, are then dehydrated, are dry
It is dry.
The once sintered semi-finished product of the positive electrode, pure water, inorganic ions conductive species mass ratio be 1:(1~5):
(0.0001~0.005), then water temperature be 20~50 DEG C at mixed, incorporation time be 15~80min, it is described it is inorganic from
Sub- conductor is such as the one or several kinds in tungstate lithium, boron oxide lithium, lithium phosphate or lithium zirconate.The positive electrode is once burnt
Tie semi-finished product nickel cobalt lithium aluminate or nickel cobalt aluminium LiMn2O4.
Step S2, the mixture after step S1 dryings is put into atmosphere furnace and is sintered；Sintering time is 2~15h, sintering
Temperature is 300~800 DEG C.
Step S3, material after the sintering that step S2 is obtained is weighed, then weighs certain proportion organic solvent, organic conductive forerunner
Material, organic solvent and organic conductive presoma after the sintering weighed are mixed, are then put into ice bath, so by body
Oxidant is added afterwards and continues stirring a period of time.
Material after the step S2 sintering weighed, organic solvent, organic conductive presoma mass ratio be 1:(1~10):
(0.001~0.01), is then mixed, the mixing time be 2~5h, the organic solvent be absolute ethyl alcohol, DMF,
One or several kinds in NMP, dimethylbenzene, dichloromethane, the organic precursor are pyrroles and paratoluenesulfonic acid sodium salt mixture,
And aniline dodecyl benzene sulfonic acid and ammonium persulfate acid mixed solution one kind or two kinds.Oxidant is added in ice bath to continue to stir
Mix 1~15h, the mass ratio of the organic conductive presoma and oxidant is 1：(0.02~0.1), the oxidant are
FeCl3·6H2O、MnO2、ZnO2One or more of.
Step S4, the obtained mixtures of step S3 are put into vacuum drying chamber and are dried, then by the object after drying
Matter carries out can be obtained conductive electric double layer cladded type tertiary cathode material except iron sieving.
The time being dried in vacuum drying chamber is 5~10h, and drying temperature is 60~120 DEG C.
The matrix composition for the conductive electric double layer cladded type tertiary cathode material being finally prepared is nickel cobalt lithium aluminate or nickel
Cobalt manganic acid lithium, pattern are spherical shape, and Components Chemical formula can use LixNi1-a-b-cCoaMbO2It indicates, 0.85≤x≤1.2,
0≤a≤0.15,0.01≤b≤0.03, wherein M are Al or Mn.
Existing lithium battery is in growth process charge and discharge process especially in the case of high voltage, it is easy to due to surface
Side reaction causes cycle performance decaying fast, and safety is also easy to get great harm.It is general using cladding for these problems
Mode improve, but common cladding causes electronic conductance and ionic conductance to have due to the presence of the non-conductive performance of coating
Weakened, influence electronics and ion transmission, electrical property is weakened.And the present invention is coated by electric double layer, can effectively be solved
Certainly this problem, first layer are inorganic conductive layer, are coated by wet method, coat ion conductor proximate matter material, such as tungstate lithium, oxygen
Change boron lithium, lithium phosphate or lithium zirconate etc., second layer cladding is organic conductive layers, has the characteristics that flexibility, passes through electric double layer
Cladding, the conduction for increasing material lead lithium performance, reduce the side reaction on surface, can effectively improve nickelic tertiary cathode material
Cycle performance and security performance.
This product performance is verified below by specific embodiment and test example.
Embodiment one：
1) the once sintered semi-finished product of 100g nickel cobalt lithium aluminates, the pure water of 150mL, 0.5g boron oxide lithiums are weighed.By nickel cobalt
The once sintered semi-finished product of lithium aluminate, pure water, boron oxide lithium stir 30min, are then dehydrated, are dried at 25 DEG C.
2) mixture after drying step 1 is put into atmosphere furnace, at 300 DEG C, calcines 10h.
3) the sintered material 100g that step 2 obtains is weighed, then weighs absolute ethyl alcohol 200mL, pyrroles and to toluene sulphur
Sour sodium (1:3)1g.The substance weighed is subjected to mixing 5h, is then put into ice bath, 0.1g FeCl are then added3·
6H2O is stirred for 15h.
4) substance prepared by step 3 is put into vacuum drying chamber 80 DEG C, dry 10h, then by the substance after drying into
Row is conductive electric double layer cladded type nickel cobalt lithium aluminate tertiary cathode material except iron sieving, and electron microscope is as shown in Figure 1.
Embodiment two：
1) the once sintered semi-finished product of 100g nickel cobalt lithium aluminates, the pure water of 300mL, 0.2g tungstate lithiums are weighed.By nickel cobalt aluminium
The once sintered semi-finished product of sour lithium, pure water, tungstate lithium stir 30min, are then dehydrated, are dried at 45 DEG C.
2) mixture after drying step 1 is put into atmosphere furnace, at 600 DEG C, calcines 6h.
3) the sintered material 100g that step 2 obtains is weighed, then weighs absolute ethyl alcohol 200mL, aniline detergent alkylate
Sulfonic acid and ammonium persulfate acid mixed solution (1:1)1mL.The substance weighed is subjected to mixing 5h, is then put into ice bath, so
0.09g MnO are added afterwards2, it is stirred for 10h.
4) substance prepared by step 3 is put into vacuum drying chamber 60 DEG C, dry 15h, then by the substance after drying into
Row is except the nickel cobalt lithium aluminate tertiary cathode material that iron sieving is conductive electric double layer cladded type.
Comparative example one：
Take 100g nickel cobalt lithium aluminate finished products.
By the positive electrode of embodiment one and comparative example and conductive agent acetylene carbon black, binder PVDF is according to mass ratio 80：
12：8 ratios are uniformly mixed, and -2 pyrrolidones ball milling of suitable 1- methyl is added is made into slurry within 1 hour and be evenly coated on aluminium flake, are dried
Positive plate is made in dry, tabletting.2032 button cells are assembled by cathode of metal lithium sheet, electricity is carried out using Siken test systems
Performance test (charging/discharging voltage is 2.75~4.3V, and high voltage charging/discharging voltage is 2.75~4.4V).
From the point of view of cycle performance comparison diagram shown in Fig. 2, the lithium battery of one material preparation of the embodiment of the present invention follows performance
Far superior to common nickel cobalt lithium aluminate, after 50 circle cycles, the capacity retention ratio decline of one lithium battery of embodiment is very slow,
And existing common nickel cobalt lithium aluminate has dropped nearly 13%.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (9)
1. a kind of preparation method of conduction electric double layer cladded type tertiary cathode material, which is characterized in that the method includes following
Step：
Step S1, the once sintered semi-finished product of positive electrode are weighed, pure water, inorganic ions conductive species are weighed according to certain proportion,
The once sintered semi-finished product of the positive electrode, pure water, inorganic ions conductive species are mixed, is then dehydrated, is dry；
Step S2, the mixture after step S1 dryings is put into atmosphere furnace and is sintered；
Step S3, material after the sintering that step S2 is obtained is weighed, then weighs certain proportion organic solvent, organic conductive presoma,
Material, organic solvent and organic conductive presoma after the sintering weighed are mixed, are then put into ice bath, is then added
Enter oxidant and continues stirring a period of time；
Step S4, the obtained mixtures of step S3 are put into vacuum drying chamber and are dried, then by the substance after drying into
Row can be obtained conductive electric double layer cladded type tertiary cathode material except iron sieving.
2. the preparation method of conduction electric double layer cladded type tertiary cathode material as described in claim 1, which is characterized in that step S1
In, the once sintered semi-finished product of positive electrode that weigh, pure water, inorganic ions conductive species mass ratio be 1:(1~5):
(0.0001~0.005), then water temperature be 20~50 DEG C at mixed, incorporation time be 15~80min, it is described it is inorganic from
Sub- conductor is such as the one or several kinds in tungstate lithium, boron oxide lithium, lithium phosphate or lithium zirconate.
3. the preparation method of conduction electric double layer cladded type tertiary cathode material as described in claim 1, which is characterized in that step S2
In sintering time be 2~15h, sintering temperature be 300~800 DEG C.
4. the preparation method of conduction electric double layer cladded type tertiary cathode material as described in claim 1, which is characterized in that step S3
In, material after the step S2 sintering weighed, organic solvent, organic conductive presoma mass ratio be 1:(1~10):(0.001~
0.01), then mixed, the mixing time be 2~5h, the organic solvent be absolute ethyl alcohol, DMF, NMP, dimethylbenzene,
One or several kinds in dichloromethane, the organic precursor are pyrroles and paratoluenesulfonic acid sodium salt mixture and aniline ten
Dialkyl benzene sulfonic acids and one kind of ammonium persulfate acid mixed solution or two kinds.
5. the preparation method of conduction electric double layer cladded type tertiary cathode material as claimed in claim 4, which is characterized in that step S3
In, oxidant is added in ice bath and continues 1~15h of stirring, the mass ratio of the organic conductive presoma and oxidant is 1：(0.02
~0.1), the oxidant is FeCl3·6H2O、MnO2、ZnO2One or more of.
6. the preparation method of conduction electric double layer cladded type tertiary cathode material as described in claim 1, which is characterized in that step S4
In, the time being dried in vacuum drying chamber is 5~10h, and drying temperature is 60~120 DEG C.
7. the preparation method of conductive electric double layer cladded type tertiary cathode material, feature exist as described in claim any one of 1-6
In the once sintered semi-finished product nickel cobalt lithium aluminate of the positive electrode or nickel cobalt aluminium LiMn2O4.
8. a kind of conduction electric double layer cladded type tertiary cathode material, which is characterized in that the conduction electric double layer cladded type ternary is just
Pole material uses any one of claim 1-6 the method to be such as prepared, and pattern is spherical shape.
9. conduction electric double layer cladded type tertiary cathode material as claimed in claim 7, which is characterized in that the conduction electric double layer packet
The matrix composition for covering type tertiary cathode material is nickel cobalt lithium aluminate or nickle cobalt lithium manganate, and Components Chemical formula can be used
LixNi1-a-b-cCoaMbO2It indicates, 0.85≤x≤1.2,0≤a≤0.15,0.01≤b≤0.03, wherein M are Al or Mn.
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| CN109244428B (en) * | 2018-11-05 | 2022-06-14 | 桑顿新能源科技(长沙)有限公司 | Coating modification method of high-nickel ternary material |
| CN109244439A (en) * | 2018-11-27 | 2019-01-18 | 宁波容百新能源科技股份有限公司 | A kind of ternary cathode material of lithium ion battery and preparation method thereof and lithium ion battery of multistage layer cladding |
| CN109888252A (en) * | 2019-03-29 | 2019-06-14 | 荆门市格林美新材料有限公司 | It is a kind of to coat nickel-cobalt-manganese ternary anode material and preparation method altogether |
| CN109888252B (en) * | 2019-03-29 | 2021-12-07 | 荆门市格林美新材料有限公司 | Co-coated nickel-cobalt-manganese ternary positive electrode material and preparation method thereof |
| CN112133904A (en) * | 2020-09-24 | 2020-12-25 | 江西普瑞美新材料科技有限公司 | High-nickel ternary cathode material of lithium ion battery and preparation method thereof |
| CN113363477A (en) * | 2021-03-26 | 2021-09-07 | 万向一二三股份公司 | Preparation method of multilayer coated ternary cathode material |
| CN114975935A (en) * | 2022-06-02 | 2022-08-30 | 长沙理工大学 | Tungsten-modified high-nickel ternary lithium ion battery positive electrode material and preparation method thereof |
| CN114975935B (en) * | 2022-06-02 | 2024-02-13 | 长沙理工大学 | Tungsten-modified high-nickel ternary lithium ion battery positive electrode material and preparation method thereof |
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