CN109802075A - A kind of preparation method of lithium battery high magnification PE film - Google Patents
A kind of preparation method of lithium battery high magnification PE film Download PDFInfo
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- CN109802075A CN109802075A CN201811609620.XA CN201811609620A CN109802075A CN 109802075 A CN109802075 A CN 109802075A CN 201811609620 A CN201811609620 A CN 201811609620A CN 109802075 A CN109802075 A CN 109802075A
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Abstract
The present invention provides a kind of preparation method of lithium battery high magnification PE film, including S1 prepares electrolytic solution, S2 chemical reaction, and S3 prepares lithium aluminate base-material, and S4 prepares aluminic acid powder for lithium, and S5 prepares ceramic coating, by the low nanometer LiAlO for being 15% with weight ratio2Powder is added in the acetone soln that weight ratio is 85%, is stirred 12h, obtains sticky slurry, sticky slurry is spread on PE diaphragm, carries out hot pressed sintering, finished product is prepared.Invention is combined using ceramic coating with PE film, according to enough isolations of nanometer aluminic acid lithium material electronic isolation, the effective mechanical isolation for guaranteeing positive and negative anodes and the migration for preventing active material, and there is certain aperture, have good permeability to lithium ion, guarantee low resistance and high ion conductivity, and use hot pressed sintering mode, promote substance to migrate, reduces hot pressing temperature, it is energy saving.
Description
Technical field
The present invention relates to the preparations of lithium battery diaphragm manufacturing technology field more particularly to a kind of lithium battery high magnification PE film
Method.
Background technique
Lithium ion battery has become the mainstream development direction of secondary cell with its excellent performance.Lithium ion battery mainly wraps
Four big critical materials are included, are positive electrode, negative electrode material, diaphragm and electrolyte respectively, diaphragm is as the important of lithium ion battery
Component part plays the effect for preventing positive and negative anodes short circuit in the battery；Overcharge or temperature increase when, diaphragm is obstructed by closed pore
Electric current conduction, prevents from exploding；In addition, being provided with the effect of ion transport channel in charge and discharge process septation.Diaphragm accounts for about lithium
The 25-30% of battery manufacturing cost has a major impact lithium ion battery safety, performance and cost, and performance superiority and inferiority determines
Interfacial structure, internal resistance of battery etc. directly affect battery capacity, cycle performance, charging and discharging currents density and security performance etc.
Key characteristic.Diaphragm is the highest a kind of high added value material of technical barrier in lithium battery material, accounts for about the 25- of lithium battery cost
30%, technological difficulties are engineering technology, basis material and the manufacturing equipment of pore-creating.Diaphragm holds at high price main
The reason is that the key technology and equipment of some production diaphragms are monopolized by Japan and the U.S., domestic diaphragm is especially high-end diaphragm
Index is also not up to the level of external product.Currently, lithium ion battery separator, is PE diaphragm and PP diaphragm, two such diaphragms
Isolation and electronic isolation, it is less good, be easy to cause positive and negative anodes short-circuit, and lithium ion to penetrate efficiency lower,
It is inadaptable to be used for a long time with lithium battery.
Therefore, it is necessary to solve the above problems with the preparation method of high magnification PE film to invent a kind of lithium battery
Summary of the invention
The purpose of the present invention is to provide a kind of lithium battery preparation methods of high magnification PE film, are asked with solving above-mentioned technology
Topic.
The present invention using following technical scheme in order to solve the above technical problems, realized: a kind of lithium battery high magnification PE
The preparation method of film, comprising the following steps:
S1 prepares electrolytic solution: in dry undivided cell, the ethyl alcohol for preparing 0.035mol/L (Bu4N) Br is molten
Liquid 100mL is charged with 0.18g metal lithium sheet as electrolyte, and lithium alkoxide solution is made；
S2 chemical reaction: accelerate hydrolysis since heat release increases solution temperature in reaction process, reaction need to be protected in argon gas
Under conditions of carry out, and be stirred continuously, while carrying out cooling processing with liquid nitrogen, acquired solution be concentrated as 85mL；
S3 prepares lithium aluminate base-material: by cleaned aluminium flake through precise, moving into the molten of step S2 as anode
In liquid, after electrolysis time continues 120min, the acetylacetone,2,4-pentanedione of 0.1mL is added with micro syringe at this time, control electric current is 0.2A,
It is electrolysed aluminium flake 6h under protection of argon gas, a nanometer LiAlO can be obtained2Presoma；
S4 prepares aluminic acid powder for lithium: the weak aqua ammonia of 1mL or so, ammonium hydroxide and nanometer LiAlO is slowly added dropwise2Presoma percentage
Than being 9.0 for 1:10, control PH, it is stirred continuously, gel after solution 6h, by the gel after aluminium, the hydrolysis of lithium complex alkoxide at 60 degree
Xerogel powder is made in dry 12h, and powder is put into smelting furnace at 550 degree and calcines 2h, obtains corresponding nanometer LiAlO2Powder；
S5 prepares ceramic coating: by the low nanometer LiAlO matched2Powder is added in acetone soln, is stirred 12h, obtains
Sticky slurry is spread on PE diaphragm, is sintered, finished product is prepared by sticky slurry.
Preferably, the metal lithium sheet purity in the step S1 is 99.90%, and is activated through polishing.
Preferably, the smelting furnace in the step S4 uses Muffle furnace.
Preferably, it is bonded between ceramic coating and PE diaphragm using polyacrylate binder in the step S5.
Preferably, nanometer LiAlO in the step S52The weight ratio of powder is 10-20%, and the weight ratio of acetone soln is
80-90%.
Preferably, sintering processing is hot pressed sintering in the step S5.
Preferably, the method that the step S5 prepares ceramic coating is wet chemistry method.
The beneficial effects of the present invention are:
The present invention is compared with existing lithium battery PE film, and the present invention is combined using ceramic coating with PE film, according to nanometer
Enough isolations of aluminic acid lithium material electronic isolation, the effective mechanical isolation for guaranteeing positive and negative anodes and prevents active matter
The migration of matter, and there is certain aperture, there is good permeability to lithium ion, guarantee low resistance and high ion conductivity,
And hot pressed sintering mode is used, substance is promoted to migrate, reduces hot pressing temperature, it is energy saving, and manufactured by wet chemistry method,
It is set to have equipment simple, without exacting terms such as vacuum states, convenient for the manufacturing to coating.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Specific embodiment is closed, the present invention is further explained, and however, the following embodiments are merely preferred embodiments of the present invention, and not all.
Based on the implementation example in the implementation mode, those skilled in the art's obtained other realities without making creative work
Example is applied, protection scope of the present invention is belonged to.Experimental method in following embodiments is unless otherwise specified conventional method,
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Embodiment one:
S1 prepares electrolytic solution: in dry undivided cell, the ethyl alcohol for preparing 0.035mol/L (Bu4N) Br is molten
Liquid 100mL is charged with the metal lithium sheet that 0.18g purity is 99.90% as electrolyte, and lithium alkoxide solution is made；
S2 chemical reaction: accelerate hydrolysis since heat release increases solution temperature in reaction process, reaction need to be protected in argon gas
Under conditions of carry out, and be stirred continuously, while carrying out cooling processing with liquid nitrogen, acquired solution be concentrated as 85mL；
S3 prepares lithium aluminate base-material: by cleaned aluminium flake through precise, moving into the molten of step S2 as anode
In liquid, after electrolysis time continues 120min, the acetylacetone,2,4-pentanedione of 0.1mL is added with micro syringe at this time, control electric current is 0.2A,
It is electrolysed aluminium flake 6h under protection of argon gas, a nanometer LiAlO can be obtained2Presoma；
S4 prepares aluminic acid powder for lithium: the weak aqua ammonia of 1mL or so, ammonium hydroxide and nanometer LiAlO is slowly added dropwise2Presoma percentage
Than being 9.0 for 1:10, control PH, it is stirred continuously, gel after solution 6h, by the gel after aluminium, the hydrolysis of lithium complex alkoxide at 60 degree
Xerogel powder is made in dry 12h, and powder is put into Muffle furnace at 550 degree and calcines 2h, obtains corresponding nanometer LiAlO2Powder
Body；
S5 prepares ceramic coating: by the low nanometer LiAlO for being 10% with weight ratio2Third that weight ratio is 90% is added in powder
In ketone solution, it is stirred 12h, obtains sticky slurry, sticky slurry is spread on PE diaphragm, carries out hot pressing burning
Knot, is prepared finished product.
Embodiment two:
S1 prepares electrolytic solution: in dry undivided cell, the ethyl alcohol for preparing 0.035mol/L (Bu4N) Br is molten
Liquid 100mL is charged with the metal lithium sheet that 0.18g purity is 99.90% as electrolyte, and lithium alkoxide solution is made；
S2 chemical reaction: accelerate hydrolysis since heat release increases solution temperature in reaction process, reaction need to be protected in argon gas
Under conditions of carry out, and be stirred continuously, while carrying out cooling processing with liquid nitrogen, acquired solution be concentrated as 85mL；
S3 prepares lithium aluminate base-material: by cleaned aluminium flake through precise, moving into the molten of step S2 as anode
In liquid, after electrolysis time continues 120min, the acetylacetone,2,4-pentanedione of 0.1mL is added with micro syringe at this time, control electric current is 0.2A,
It is electrolysed aluminium flake 6h under protection of argon gas, a nanometer LiAlO can be obtained2Presoma；
S4 prepares aluminic acid powder for lithium: the weak aqua ammonia of 1mL or so, ammonium hydroxide and nanometer LiAlO is slowly added dropwise2Presoma percentage
Than being 9.0 for 1:10, control PH, it is stirred continuously, gel after solution 6h, by the gel after aluminium, the hydrolysis of lithium complex alkoxide at 60 degree
Xerogel powder is made in dry 12h, and powder is put into Muffle furnace at 550 degree and calcines 2h, obtains corresponding nanometer LiAlO2Powder
Body；
S5 prepares ceramic coating: by the low nanometer LiAlO for being 15% with weight ratio2Third that weight ratio is 85% is added in powder
In ketone solution, it is stirred 12h, obtains sticky slurry, sticky slurry is spread on PE diaphragm, carries out hot pressing burning
Knot, is prepared finished product.
Embodiment three:
S1 prepares electrolytic solution: in dry undivided cell, the ethyl alcohol for preparing 0.035mol/L (Bu4N) Br is molten
Liquid 100mL is charged with the metal lithium sheet that 0.18g purity is 99.90% as electrolyte, and lithium alkoxide solution is made；
S2 chemical reaction: accelerate hydrolysis since heat release increases solution temperature in reaction process, reaction need to be protected in argon gas
Under conditions of carry out, and be stirred continuously, while carrying out cooling processing with liquid nitrogen, acquired solution be concentrated as 85mL；
S3 prepares lithium aluminate base-material: by cleaned aluminium flake through precise, moving into the molten of step S2 as anode
In liquid, after electrolysis time continues 120min, the acetylacetone,2,4-pentanedione of 0.1mL is added with micro syringe at this time, control electric current is 0.2A,
It is electrolysed aluminium flake 6h under protection of argon gas, a nanometer LiAlO can be obtained2Presoma；
S4 prepares aluminic acid powder for lithium: the weak aqua ammonia of 1mL or so, ammonium hydroxide and nanometer LiAlO is slowly added dropwise2Presoma percentage
Than being 9.0 for 1:10, control PH, it is stirred continuously, gel after solution 6h, by the gel after aluminium, the hydrolysis of lithium complex alkoxide at 60 degree
Xerogel powder is made in dry 12h, and powder is put into Muffle furnace at 550 degree and calcines 2h, obtains corresponding nanometer LiAlO2Powder
Body；
S5 prepares ceramic coating: by the low nanometer LiAlO for being 20% with weight ratio2Third that weight ratio is 80% is added in powder
In ketone solution, it is stirred 12h, obtains sticky slurry, sticky slurry is spread on PE diaphragm, carries out hot pressing burning
Knot, is prepared finished product.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
For personnel it should be appreciated that the present invention is not limited to the above embodiments, described in the above embodiment and specification is only the present invention
Preference, be not intended to limit the invention, without departing from the spirit and scope of the present invention, the present invention also has various
Changes and improvements, these changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by institute
Attached claims and its equivalent thereof.
Claims (7)
1. a kind of lithium battery preparation method of high magnification PE film, it is characterised in that: the following steps are included:
S1 prepares electrolytic solution: in dry undivided cell, preparing the ethanol solution of 0.035mol/L (Bu4N) Br
100mL is charged with 0.18g metal lithium sheet as electrolyte, and lithium alkoxide solution is made；
S2 chemical reaction: accelerate hydrolysis since heat release increases solution temperature in reaction process, the item that reaction need to be protected in argon gas
It carries out, and is stirred continuously under part, while carrying out cooling processing with liquid nitrogen, acquired solution is concentrated as 85mL；
S3 prepares lithium aluminate base-material: by cleaned aluminium flake through precise, moved into as anode in the solution of step S2,
After electrolysis time continues 120min, the acetylacetone,2,4-pentanedione of 0.1mL is added with micro syringe at this time, control electric current is 0.2A, in argon
It is electrolysed aluminium flake 6h under gas shielded, a nanometer LiAlO can be obtained2Presoma；
S4 prepares aluminic acid powder for lithium: the weak aqua ammonia of 1mL or so, ammonium hydroxide and nanometer LiAlO is slowly added dropwise2Presoma percentage be
1:10, control PH are 9.0, are stirred continuously, gel after solution 6h, by the gel after aluminium, the hydrolysis of lithium complex alkoxide in 60 degree of dryings
Xerogel powder is made in 12h, and powder is put into smelting furnace at 550 degree and calcines 2h, obtains corresponding nanometer LiAlO2Powder；
S5 prepares ceramic coating: by the low nanometer LiAlO matched2Powder is added in acetone soln, is stirred 12h, obtains sticky
Sticky slurry is spread on PE diaphragm, is sintered, finished product is prepared by slurry.
2. a kind of preparation method of lithium battery high magnification PE film according to claim 1, it is characterised in that: the step
Metal lithium sheet purity in S1 is 99.90%, and activates through polishing.
3. a kind of preparation method of lithium battery high magnification PE film according to claim 1, it is characterised in that: the step
Smelting furnace in S4 uses Muffle furnace.
4. a kind of preparation method of lithium battery high magnification PE film according to claim 1, it is characterised in that: the step
It is bonded between ceramic coating and PE diaphragm using polyacrylate binder in S5.
5. a kind of preparation method of lithium battery high magnification PE film according to claim 1, it is characterised in that: the step
Nanometer LiAlO in S52The weight ratio of powder is 10-20%, and the weight ratio of acetone soln is 80-90%.
6. a kind of preparation method of lithium battery high magnification PE film according to claim 1, it is characterised in that: the step
Sintering processing is hot pressed sintering in S5.
7. a kind of preparation method of lithium battery high magnification PE film according to claim 1, it is characterised in that: the step
The method that S5 prepares ceramic coating is wet chemistry method.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811609620.XA CN109802075A (en) | 2018-12-27 | 2018-12-27 | A kind of preparation method of lithium battery high magnification PE film |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111900308A (en) * | 2020-08-04 | 2020-11-06 | 中国科学院物理研究所 | Battery diaphragm with novel nano material coating and preparation method and application thereof |
| CN112117416A (en) * | 2019-06-19 | 2020-12-22 | 通用汽车环球科技运作有限责任公司 | Ceramic coated separator for lithium-containing electrochemical cells and method of making same |
-
2018
- 2018-12-27 CN CN201811609620.XA patent/CN109802075A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112117416A (en) * | 2019-06-19 | 2020-12-22 | 通用汽车环球科技运作有限责任公司 | Ceramic coated separator for lithium-containing electrochemical cells and method of making same |
| CN112117416B (en) * | 2019-06-19 | 2023-10-17 | 通用汽车环球科技运作有限责任公司 | Ceramic coated separator for lithium-containing electrochemical cells and method of making same |
| CN111900308A (en) * | 2020-08-04 | 2020-11-06 | 中国科学院物理研究所 | Battery diaphragm with novel nano material coating and preparation method and application thereof |
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