CN107910523A - A kind of solid lithium battery anode composite and preparation method thereof - Google Patents
A kind of solid lithium battery anode composite and preparation method thereof Download PDFInfo
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- CN107910523A CN107910523A CN201711127414.0A CN201711127414A CN107910523A CN 107910523 A CN107910523 A CN 107910523A CN 201711127414 A CN201711127414 A CN 201711127414A CN 107910523 A CN107910523 A CN 107910523A
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/00—Electrodes
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01M4/485—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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Abstract
A kind of solid lithium battery anode composite and preparation method thereof, belongs to technical field of lithium ion.The anode composite is according to 1 ~ 5:1~5:1 mass ratio is prepared by lithium titanate, gas-phase growth of carbon fibre VGCFs and binary sulfide electrolyte LPSCI.The method is as follows：（1）10 ~ 100 mL 200# gasoline are taken first in measuring cup, and weighing lithium titanate powder, VGCFs and LPSCl electrolyte respectively in mass ratio, totally 10 ~ 50 g are added in measuring cup, and 12~24 h are mixed；（2）Obtained mixed solution is dried, temperature is 50~100 DEG C, and the time is 10~24h, and dry atmosphere is argon gas atmosphere, obtains Li4Ti5O12And Li6PS5Cl mixed powders；（3）Every 1 ~ the 30mg of obtained mixed powder is pressed into a potsherd, pressing pressure is 100~550MPa, and the pressing time is 1~60min, that is, obtains anode composite.It is an advantage of the invention that：Preparation method is simple, cost is low, and obtained composite positive pole particle uniformity is preferable, lithium ion conductivity is higher, electrochemical performance.
Description
Technical field
The invention belongs to technical field of lithium ion, and in particular to a kind of solid lithium battery anode composite and its preparation
Method.
Background technology
Secondary lithium battery because its voltage is high, energy density is big, have extended cycle life the advantages that, be widely used in portable
Electronics field.At present, secondary lithium battery is commercialized using organic solvent as electrolyte, and there are leakage, inflammable, easy
The shortcomings of quick-fried, limit its application in hybrid vehicle and electric automobile industry.Moreover, people are to the energy content of battery
The requirement of density is continuously improved, and two-shot liquid lithium battery density will reach the limit values, and urgent need opens up new battery system.
Secondary solid lithium battery is using lithium metal as anode, using all solid state electrolyte, while battery security is effectively improved,
The energy density of battery is greatly improved, meets the needs of hybrid vehicle and electric automobile industry development.
Solid electrolyte is divided into two major classes, is respectively solid polyelectrolyte and inorganic solid electrolyte.At present, to solid
The research of state lithium ion battery is mostly focused on solid electrolyte, and achieves significant achievement, many solid state electrolysis plastids
It is that ionic conductivity is reached 10-4S/m, has substantially met the requirement of application.And in the structure of all-solid-state battery, especially
The structure design of anode composite is still urgent problem.
Anode composite can be effectively increased the contact area of electrolyte and positive electrode, be conducive to electrolyte and cathode material
Material interface problem is studied, while can shorten migration of the lithium ion in the positive electrode of low lithium ion conductivity, is ensured
Positive active material can sufficiently carry out redox reaction in charge and discharge process.At present, grinding on anode composite
Study carefully and concentrate on sulfide electrolyte.Since sulfide electrolyte is very sensitive to the moisture in air, to sulfide electricity
The positive electrode design for composite of solution matter has certain challenge.
The content of the invention
The problem of the purpose of the invention is to improve anode of solid lithium battery and electrolyte interface contact area, there is provided
It is a kind of it is easy to operate, production cost is relatively low, the solid lithium battery anode composite that can produce in enormous quantities and preparation method thereof.
To achieve the above object, the technical solution that the present invention takes is as follows：
A kind of solid lithium battery anode composite, prepares the raw material of the anode composite according to 1 ~ 5:1~5:1 mass ratio is by titanium
Sour lithium, gas-phase growth of carbon fibre VGCFs and binary sulfide electrolyte LPSCI compositions.
A kind of preparation method of above-mentioned solid lithium battery anode composite, the method comprise the following steps that：
Step 1：10 ~ 100 mL 200# gasoline are taken to weigh metatitanic acid respectively in mass ratio in 40mm × 70mm measuring cups first
Totally 10 ~ 50 g are added in measuring cup for lithium powder, VGCFs and LPSCl electrolyte, and 12~24 h are mixed；
Step 2：The mixed solution that step 1 is obtained is dried, and drying temperature is 50~100 DEG C, and drying time is 10~24h,
Dry atmosphere is argon gas atmosphere, obtains Li4Ti5O12And Li6PS5Cl mixed powders；
Step 3：Every 1 ~ the 30mg of mixed powder that step 2 is obtained is pressed into a potsherd, pressing pressure for 100~
550MPa, pressing time are 1~60min, that is, obtain anode composite.
In above-mentioned steps one, preferably mixing time is 16~20 h, and optimal mixing time is 20 h；
In above-mentioned steps two, preferably drying temperature is 60~80 DEG C, and optimal drying temperature is 60 DEG C；
In above-mentioned steps two, preferably drying time is 14~20h, and optimal drying time is 20h；
In above-mentioned steps three, the preferred tablet quality of mixed powder is 5~20mg, optimum quality 10mg；
In above-mentioned steps three, preferably tableting pressure is 200~400MPa, optimal tableting pressure 330MPa.
In above-mentioned steps three, the preferably tabletting time is 20~50min, and the optimal tabletting time is 30min.
It is of the invention to be relative to the beneficial effect of the prior art：
（1）The method of the present invention prepares solid lithium battery composite positive pole using liquid phase method, and preparation method is simple, cost is low,
It is expected to realize the extensive preparation of LTO@LPSCl composite positive poles, there is practical value；
（2）Solid lithium battery composite positive pole particle uniformity prepared by the present invention preferably, electrochemical performance,
Capacity is 158.4mAh/g after lower 250 circulations of 0.05C, capacity retention ratio 94.3%.
Brief description of the drawings
Fig. 1 is LTO the and LPSCl materials and LPSCl electrolyte XRD diagram that embodiment 1 obtains；
Fig. 2 is that LTO the and LPSCl materials SEM and Mapping that embodiment 1 obtains schemes；
Fig. 3 is LTO the and LPSCl solid lithium battery first lap CV curve maps that embodiment 1 obtains；
Fig. 4 is that LTO the and LPSCl solid lithium batteries second that embodiment 1 obtains enclose CV curve maps；
Fig. 5 is that LTO the and LPSCl solid lithium batteries the 3rd that embodiment 1 obtains enclose CV curve maps；
Fig. 6 is the graph of a relation of electrolyte content and electrode capacity in combination electrode.
Embodiment
Technical scheme is further described with reference to the accompanying drawings and examples, but is not limited thereto,
It is every to technical solution of the present invention technical scheme is modified or replaced equivalently, without departing from the spirit and scope of technical solution of the present invention,
It should all cover in protection scope of the present invention.
Embodiment one：What present embodiment was recorded is a kind of solid lithium battery anode composite, is prepared described multiple
The raw material of cathode is closed according to 1 ~ 5:1~5:1 mass ratio is electrolysed by lithium titanate, gas-phase growth of carbon fibre VGCFs and binary sulfide
Matter LPSCI is formed.
Embodiment two：A kind of preparation side of solid lithium battery anode composite described in embodiment one
Method, is prepared using liquid phase method, and the method comprises the following steps that：
Step 1：10 ~ 100 mL200# gasoline are taken to weigh lithium titanate respectively in mass ratio in 40mm × 70mm measuring cups first
Totally 10 ~ 50 g are added in measuring cup for powder, VGCFs and LPSCl electrolyte, and 12~24 h are mixed；
Step 2：The mixed solution that step 1 is obtained is dried, and drying temperature is 50~100 DEG C, and drying time is 10~24h,
Dry atmosphere is argon gas atmosphere, obtains Li4Ti5O12And Li6PS5Cl（LTO@LPSCl）Mixed powder；
Step 3：Every 1 ~ the 30mg of mixed powder that step 2 is obtained is pressed into a potsherd, pressing pressure for 100~
550MPa, pressing time are 1~60min, that is, obtain anode composite.
Embodiment 1：
50mL 200# gasoline is taken first in 40mm × 70mm measuring cups, is in mass ratio 5:4:1 weighs lithium titanate powder respectively
End, 5 g of VGCFs and LPSCl electrolyte, 4 g, 1 g are added in measuring cup, 20 h are stirred, by the mixed solution of acquisition in argon
Gas atmosphere, dry 20 h at 60 DEG C, the mixed-powder for weighing 10 mg dryings push 30min in 330 MPa, obtain anode composite.
XRD characterization is carried out to gained composite positive pole, as shown in Figure 1, it is seen that the characteristic peak of LTO and LPSCl it is sharp and
Independently of each other, do not lack.So during mixing, without side reaction occurs between two-phase, original crystal form is kept
With state.SEM characterizations are carried out to gained electrolyte, the results are shown in Figure 2, it can be seen that composite dielectrics grain diameter is 1 μm
Left and right, shape are more regular.Gas-phase growth of carbon fibre VGCFs inlays or through electrolyte granular.
CV tests are carried out to gained electrolyte, for acquired results as shown in Fig. 3 ~ Fig. 5, which clearly illustrates that redox is sent out
Life is in two steps：Oxidation peak is located at 1.65 V, and corresponding reduction peak has corresponded to Ti respectively near 1.42 V3+And Ti4+
Mutually convert.Compare second and the 3rd to enclose, it can be seen that cyclic voltammetry curve repeats substantially, this explanation is in follow-up charge and discharge
Battery can keep basic chemical stability and electrochemical stability in electricity circulation.
In combination electrode electrolyte content from the relation of electrode capacity as shown in fig. 6, the compound electric of different electrolyte contents
Pole carries out the specific capacity that discharge and recharge obtains at 80 DEG C and shows as capacity from 35mAhg-1（10% electrolyte content）Arrive
164mAh·g-1（40% electrolyte content）, when electrolyte content further increases, specific capacity is reduced therewith.
Embodiment 2：
50mL 200# gasoline is taken first in 40mm × 70mm measuring cups, is in mass ratio 5:4:1 weighs lithium titanate powder respectively
End, VGCFs and LPSCl electrolyte 5g, 4g, 1g are added in measuring cup, 20h are stirred, by the mixed solution of acquisition in argon gas gas
Atmosphere, dry 20h at 60 DEG C, the mixed-powder for weighing 10mg dryings push 10 ~ 60min in 500MPa, anode composite are made.
Embodiment 3：
50mL 200# gasoline is taken first in 40mm × 70mm measuring cups, is in mass ratio 5:4:1 weighs lithium titanate powder respectively
End, VGCFs and LPSCl electrolyte 5g, 4g, 1g are added in measuring cup, 20h are stirred, by the mixed solution of acquisition in argon gas gas
Atmosphere, dry 20h at 100 DEG C, the mixed-powder for weighing 10mg dryings push 30min in 330MPa, obtain anode composite.
Embodiment 4：
50mL 200# gasoline is taken first in 40mm × 70mm measuring cups, is in mass ratio 5:4:1 weighs lithium titanate powder respectively
End, VGCFs and LPSCl electrolyte 5g, 4g, 1g are added in measuring cup, 20h are stirred, by the mixed solution of acquisition in argon gas gas
Atmosphere, dry 20h at 60 DEG C, the mixed-powder for weighing 20mg dryings push 30min in 330MPa, obtain anode composite.
Embodiment 5:
50mL 200# gasoline is taken first in 40mm × 70mm measuring cups, is in mass ratio 5:4:1 weighs lithium titanate powder respectively
End, VGCFs and LPSCl electrolyte 5g, 4g, 1g are added in measuring cup, 20h are stirred, by the mixed solution of acquisition in argon gas gas
Atmosphere, dry 20h at 60 DEG C, the mixed-powder for weighing 10mg dryings push 10min in 330MPa, obtain anode composite.
Embodiment 6:
50mL 200# gasoline is taken first in 40mm × 70mm measuring cups, is in mass ratio 5:1:1 weighs lithium titanate powder respectively
End, VGCFs and LPSCl electrolyte 10g, 2g, 2g are added in measuring cup, 20h are stirred, by the mixed solution of acquisition in argon gas gas
Atmosphere, dry 20h at 60 DEG C, the mixed-powder for weighing 10mg dryings push 30min in 330MPa, obtain anode composite.
Embodiment 7:
50mL 200# gasoline is taken first in 40mm × 70mm measuring cups, is in mass ratio 5:4:1 weighs lithium titanate powder respectively
End, VGCFs and LPSCl electrolyte 5g, 4g, 1g are added in measuring cup, 1h are stirred, by the mixed solution of acquisition in argon gas gas
Atmosphere, dry 20h at 60 DEG C, the mixed-powder for weighing 10mg dryings push 30min in 330MPa, obtain anode composite.
Claims (2)
- A kind of 1. solid lithium battery anode composite, it is characterised in that：The raw material of the anode composite is prepared according to 1 ~ 5:1~5:1 Mass ratio be made of lithium titanate, gas-phase growth of carbon fibre VGCFs and binary sulfide electrolyte LPSCI.
- A kind of 2. preparation method of the solid lithium battery anode composite described in claim 1, it is characterised in that：The method has Body step is as follows：Step 1：10 ~ 100 mL 200# gasoline are taken to weigh metatitanic acid respectively in mass ratio in 40mm × 70mm measuring cups first Totally 10 ~ 50 g are added in measuring cup for lithium powder, VGCFs and LPSCl electrolyte, and 12~24 h are mixed；Step 2：The mixed solution that step 1 is obtained is dried, and drying temperature is 50~100 DEG C, and drying time is 10~24h, Dry atmosphere is argon gas atmosphere, obtains Li4Ti5O12And Li6PS5Cl mixed powders；Step 3：Every 1 ~ the 30mg of mixed powder that step 2 is obtained is pressed into a potsherd, pressing pressure for 100~ 550MPa, pressing time are 1~60min, that is, obtain anode composite.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109360966A (en) * | 2018-11-13 | 2019-02-19 | 成都市银隆新能源有限公司 | A kind of manufacturing method and battery of battery pole piece |
| CN109638240A (en) * | 2018-11-27 | 2019-04-16 | 华中科技大学 | A kind of all solid state lithium-sulfur cell and preparation method thereof |
| US11682792B2 (en) | 2019-12-09 | 2023-06-20 | Corning Incorporated | Composite cathodes for solid-state lithium sulfur batteries and methods of manufacturing thereof |
| CN116711094A (en) * | 2021-11-17 | 2023-09-05 | 三井金属矿业株式会社 | Battery cell |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103972464A (en) * | 2013-01-24 | 2014-08-06 | 华为技术有限公司 | Positive electrode of all-solid-state lithium battery and manufacturing method thereof, and all-solid-state lithium battery |
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2017
- 2017-11-15 CN CN201711127414.0A patent/CN107910523A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103972464A (en) * | 2013-01-24 | 2014-08-06 | 华为技术有限公司 | Positive electrode of all-solid-state lithium battery and manufacturing method thereof, and all-solid-state lithium battery |
Non-Patent Citations (1)
| Title |
|---|
| AILING HWANG等: ""Fabrication and Electrochemical Properties of Li4Ti5O12@Li6PS5Cl for All-soild-state Lithium Batteries using Simple Mechanical Method"", 《INT.J.ELECTROCHEM.SCI.》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109360966A (en) * | 2018-11-13 | 2019-02-19 | 成都市银隆新能源有限公司 | A kind of manufacturing method and battery of battery pole piece |
| CN109638240A (en) * | 2018-11-27 | 2019-04-16 | 华中科技大学 | A kind of all solid state lithium-sulfur cell and preparation method thereof |
| US11682792B2 (en) | 2019-12-09 | 2023-06-20 | Corning Incorporated | Composite cathodes for solid-state lithium sulfur batteries and methods of manufacturing thereof |
| CN116711094A (en) * | 2021-11-17 | 2023-09-05 | 三井金属矿业株式会社 | Battery cell |
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