CN107591514A - A kind of preparation method of iron-phosphate-based lithium-ion battery positive plate - Google Patents
A kind of preparation method of iron-phosphate-based lithium-ion battery positive plate Download PDFInfo
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- CN107591514A CN107591514A CN201710791043.XA CN201710791043A CN107591514A CN 107591514 A CN107591514 A CN 107591514A CN 201710791043 A CN201710791043 A CN 201710791043A CN 107591514 A CN107591514 A CN 107591514A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
A kind of preparation method of iron-phosphate-based lithium-ion battery positive plate, comprises the following steps：1) quality proportioning is pressed, LiFePO4, acetylene black and PVDF is weighed, is placed in container, and N methyl pyrrolidones are added into container, after adjusting viscosity, 8~10h is stirred, obtains anode sizing agent；2) anode sizing agent is formed into coated sample coated on aluminium foil；3) described coated sample is subjected to vacuum freeze drying processing, cryogenic temperature is 50~30 DEG C, and cooling time is 4~6h, the sample formed after freeze-drying；4) by the sample after freeze-drying, it is dried in vacuo, vacuum drying temperature is 85~100 DEG C, and drying time is 8~10h, sample after being dried；5) sample obtains iron-phosphate-based lithium-ion battery positive plate through tabletting and sectioning after drying.This method technological process is simple, and cost is low, and prepared battery anode slice is functional, after tested, has higher first discharge specific capacity and discharging efficiency.
Description
Technical field：
The invention belongs to cell positive material preparing technical field, and in particular to a kind of cathode of lithium iron phosphate lithium ion battery
The preparation method of piece.
Background technology：
LiFePO4 has that raw material sources are extensive, cheap, heat endurance is good, good cycle higher than energy, safety
The characteristics of performance protrudes and is environmentally safe.But the drying means of traditional positive electrode is all vacuum drying, using tradition
Be present phenomena such as poor uniformity, powder aggregation in iron-phosphate-based lithium-ion battery positive plate prepared by drying means, directly affect
The problems such as chemical property of material, the field of batteries for entering innovation day can not be satisfied with, so new dry technology is ground
It is imperative to study carefully.
The content of the invention：
The purpose of the present invention is to overcome above-mentioned the shortcomings of the prior art, there is provided a kind of high-cobalt hart metal cutter gradient
Film and preparation method thereof, it is not even variation to solve the structure of the diamond coatings of existing multilayer and composition, should in fatigue
The problem of being destroyed under power effect.
It is an object of the invention to provide a kind of preparation method of positive plate of iron phosphate lithium battery, this method can make after drying
Positive electrode is functional, and discharging efficiency is stable.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of iron-phosphate-based lithium-ion battery positive plate, comprises the following steps：
(1) quality proportioning is pressed, LiFePO4: acetylene black: PVDF=(4~6): (0.5~0.75): (0.5~0.75), claimed
LiFePO4, acetylene black and PVDF are taken, is placed in container, and 1-METHYLPYRROLIDONE is added into container, after adjusting viscosity, is stirred
8~10h is mixed, obtains anode sizing agent；
(2) anode sizing agent is formed into coated sample coated on aluminium foil；
(3) described coated sample is subjected to vacuum freeze drying processing, the sample formed after freeze-drying；Its
In：The cryogenic temperature of described vacuum freeze drying processing is -50~-30 DEG C, and cooling time is 4~6h；
(4) by the sample after freeze-drying, it is dried in vacuo, sample after obtained drying；Wherein：Described vacuum is done
Dry temperature is 85~100 DEG C, and drying time is 8~10h；
(5) dried sample is obtained into iron-phosphate-based lithium-ion battery positive plate through tabletting and sectioning.
In described step (1), agitating mode is magnetic agitation.
In described step (2), aluminium foil is attached on smooth surface and operated.
In described step (2), described smooth surface is glass plate.
In described step (3), vacuum freeze drying processing is carried out in vacuum freezing drying oven.
In described step (5), after the iron-phosphate-based lithium-ion battery positive plate assembling of preparation is made into button cell, lead to
Cross charge-discharge test, first discharge specific capacity >=146mAh/g, battery efficiency >=96%.With same batch positive electrode (ferric phosphate
Lithium) based lithium-ion battery positive plate is prepared, half-cell (button cell) first discharge specific capacity made using positive plate of the present invention
Discharging efficiency is above conventional vacuum and dries the positive plate made first.
Iron-phosphate-based lithium-ion battery positive plate performance is improved by freeze-drying method, vacuum freeze drying is also known as
Literization is freeze-dried, and its general principle is by the moisture sharp freezing in material, then makes ice crystal straight by way of vacuumizing
Switch through and turn to gaseous state, so that material dewatering.Expansive force of the water in phase transition process make it that original particle close to each other is opened
Open, while the generation of ice is fixed its position, prevents particle is assembled in the drying process from obtaining the uniform mixture of component, together
When be advantageous to lithium ion by, improve phase charge-discharge performance.In be dried in vacuo purpose and being further to slough slurry
Solvent and moisture.
Beneficial effects of the present invention：
(1) method that the present invention prepares iron-phosphate-based lithium-ion battery positive plate, technological process is simple, and cost is low；
(2) iron-phosphate-based lithium-ion battery positive plate prepared using the method for the present invention has good performance, charge and discharge
Electrical efficiency is excellent, first discharge specific capacity >=146mAh/g, first discharging efficiency efficiency >=96%.
Embodiment：
With reference to embodiment, the present invention is described in further detail.
Embodiment 1
A kind of preparation method of iron-phosphate-based lithium-ion battery positive plate, comprises the following steps：
(1) quality proportioning is pressed, LiFePO4 0.6g is weighed respectively, acetylene black 0.075g and PVDF 0.075g, is placed in weighing
In bottle, and 1-METHYLPYRROLIDONE is added into measuring cup, after adjusting viscosity, magnetic agitation 10h, obtain anode sizing agent；
(2) by aluminium foil patch on a glass, anode sizing agent is formed into coated sample coated on aluminium foil；
(3) by described coated sample in vacuum freezing drying oven, vacuum freeze drying processing is carried out, is formed cold
Freeze dried sample；Wherein：The cryogenic temperature of described vacuum freeze drying processing is -40 DEG C, cooling time 6h；
(4) by the sample after freeze-drying, it is dried in vacuo, sample after obtained drying；Wherein：Described vacuum is done
Dry temperature is 100 DEG C, drying time 8h；
(5) iron-phosphate-based lithium-ion battery positive plate is made through tabletting and sectioning in dried sample；It will prepare
Iron-phosphate-based lithium-ion battery positive plate assembling button cell is made after, by charge-discharge test, first discharge specific capacity is
152mAh/g, discharging efficiency is 96% first.
Comparative example 1
A kind of preparation method of iron-phosphate-based lithium-ion battery positive plate, comprises the following steps：
(1) quality proportioning is pressed, LiFePO4 0.6g is weighed respectively, acetylene black 0.075g and PVDF 0.075g, is placed in weighing
In bottle, and 1-METHYLPYRROLIDONE is added into measuring cup, after adjusting viscosity, magnetic agitation 10h, obtain anode sizing agent；
(2) by aluminium foil patch on a glass, anode sizing agent is formed into coated sample coated on aluminium foil；
(3) described coated sample is dried in vacuo, sample after obtained drying；Wherein：Described vacuum
Drying temperature is 100 DEG C, drying time 8h；
(4) iron-phosphate-based lithium-ion battery positive plate is made through tabletting and sectioning in dried sample；It will prepare
Iron-phosphate-based lithium-ion battery positive plate assembling button cell is made after, by charge-discharge test, first discharge specific capacity is
145mAh/g, discharging efficiency is 93% first.
Embodiment 2
A kind of preparation method of iron-phosphate-based lithium-ion battery positive plate, comprises the following steps：
(1) quality proportioning is pressed, LiFePO4 0.4g is weighed respectively, acetylene black 0.05g and PVDF 0.05g, is placed in measuring cup
It is interior, and 1-METHYLPYRROLIDONE is added into measuring cup, after adjusting viscosity, magnetic agitation 8h, obtain anode sizing agent；
(2) by aluminium foil patch on a glass, anode sizing agent is formed into coated sample coated on aluminium foil；
(3) by described coated sample in vacuum freezing drying oven, vacuum freeze drying processing is carried out, is formed cold
Freeze dried sample；Wherein：The cryogenic temperature of described vacuum freeze drying processing is -50 DEG C, cooling time 4h；
(4) by the sample after freeze-drying, it is dried in vacuo, sample after obtained drying；Wherein：Described vacuum is done
Dry temperature is 85 DEG C, drying time 10h；
(5) iron-phosphate-based lithium-ion battery positive plate is made through tabletting and sectioning in dried sample；It will prepare
Iron-phosphate-based lithium-ion battery positive plate assembling button cell is made after, by charge-discharge test, first discharge specific capacity is
153mAh/g, discharging efficiency is 97% first.
Embodiment 3
A kind of preparation method of iron-phosphate-based lithium-ion battery positive plate, comprises the following steps：
(1) quality proportioning is pressed, LiFePO4 0.5g is weighed respectively, acetylene black 0.062g and PVDF 0.062g, is placed in weighing
In bottle, and 1-METHYLPYRROLIDONE is added into measuring cup, after adjusting viscosity, magnetic agitation 9h, obtain anode sizing agent；
(2) by aluminium foil patch on a glass, anode sizing agent is formed into coated sample coated on aluminium foil；
(3) by described coated sample in vacuum freezing drying oven, vacuum freeze drying processing is carried out, is formed cold
Freeze dried sample；Wherein：The cryogenic temperature of described vacuum freeze drying processing is -30 DEG C, cooling time 5h；
(4) by the sample after freeze-drying, it is dried in vacuo, sample after obtained drying；Wherein：Described vacuum is done
Dry temperature is 90 DEG C, drying time 9h；
(5) iron-phosphate-based lithium-ion battery positive plate is made through tabletting and sectioning in dried sample；It will prepare
Iron-phosphate-based lithium-ion battery positive plate assembling button cell is made after, by charge-discharge test, first discharge specific capacity is
146mAh/g, battery efficiency 96%.
Claims (5)
1. a kind of preparation method of iron-phosphate-based lithium-ion battery positive plate, it is characterised in that comprise the following steps：
(1) quality proportioning, LiFePO4 are pressed：Acetylene black：PVDF=(4~6):(0.5~0.75):(0.5~0.75), weighs phosphorus
Sour iron lithium, acetylene black and PVDF, are placed in container, and 1-METHYLPYRROLIDONE is added into container, after adjusting viscosity, stirring 8
~10h, obtain anode sizing agent；
(2) anode sizing agent is formed into coated sample coated on aluminium foil；
(3) described coated sample is subjected to vacuum freeze drying processing, the sample formed after freeze-drying；Wherein：Institute
The cryogenic temperature for the vacuum freeze drying processing stated is -50~-30 DEG C, and cooling time is 4~6h；
(4) by the sample after freeze-drying, it is dried in vacuo, sample after obtained drying；Wherein：Described vacuum drying temperature
Spend for 85~100 DEG C, drying time is 8~10h；
(5) dried sample is obtained into iron-phosphate-based lithium-ion battery positive plate through tabletting and sectioning.
2. the preparation method of iron-phosphate-based lithium-ion battery positive plate according to claim 1, it is characterised in that described
In step (1), agitating mode is magnetic agitation.
3. the preparation method of iron-phosphate-based lithium-ion battery positive plate according to claim 1, it is characterised in that described
In step (2), aluminium foil is attached on smooth surface and operated.
4. the preparation method of iron-phosphate-based lithium-ion battery positive plate according to claim 1, it is characterised in that described
In step (3), vacuum freeze drying processing is carried out in vacuum freezing drying oven.
5. the preparation method of iron-phosphate-based lithium-ion battery positive plate according to claim 1, it is characterised in that described
In step (5), after the assembling of the iron-phosphate-based lithium-ion battery positive plate of preparation is made into button cell, by charge-discharge test,
First discharge specific capacity >=146mAh/g, battery efficiency >=96%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109873123A (en) * | 2019-02-14 | 2019-06-11 | 嘉兴市得高电源科技有限公司 | One kind having finely dispersed anode production technology |
| CN113451551A (en) * | 2021-07-05 | 2021-09-28 | 焦作伴侣纳米材料工程有限公司 | Modification method and application of lithium ion battery electrode material |
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| CN101399329A (en) * | 2007-09-26 | 2009-04-01 | 北京化工大学 | Positive pole plate of lithium-sulfur cell and manufacturing method thereof |
| CN102185129A (en) * | 2011-01-28 | 2011-09-14 | 厦门钨业股份有限公司 | Lithium iron phosphate lithium ion battery and machining method thereof |
| CN106654195A (en) * | 2016-11-23 | 2017-05-10 | 深圳市山木新能源科技股份有限公司 | Lithium ion battery and preparation method therefor |
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- 2017-09-05 CN CN201710791043.XA patent/CN107591514A/en active Pending
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| CN1734825A (en) * | 2005-08-08 | 2006-02-15 | 河南环宇集团有限公司 | Preparation method for high rate phosphate lithium ion battery and battery prepared thereby |
| CN101399329A (en) * | 2007-09-26 | 2009-04-01 | 北京化工大学 | Positive pole plate of lithium-sulfur cell and manufacturing method thereof |
| CN102185129A (en) * | 2011-01-28 | 2011-09-14 | 厦门钨业股份有限公司 | Lithium iron phosphate lithium ion battery and machining method thereof |
| CN106654195A (en) * | 2016-11-23 | 2017-05-10 | 深圳市山木新能源科技股份有限公司 | Lithium ion battery and preparation method therefor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109873123A (en) * | 2019-02-14 | 2019-06-11 | 嘉兴市得高电源科技有限公司 | One kind having finely dispersed anode production technology |
| CN113451551A (en) * | 2021-07-05 | 2021-09-28 | 焦作伴侣纳米材料工程有限公司 | Modification method and application of lithium ion battery electrode material |
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