CN102299285A - Porous inorganic membrane used for lithium ion battery diaphragm and preparation method thereof - Google Patents
Porous inorganic membrane used for lithium ion battery diaphragm and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a porous inorganic membrane used for lithium ion battery diaphragm and a preparation method thereof. The porous inorganic membrane comprises alumina, silicon dioxide or magnesium oxide. The preparation method comprises the following steps: mixing insulating inorganic material with pore-forming material and grinding, carrying out tabletting under the pressure of 2-20 MPa, repeating the calcinations of the pressed membrane twice at the temperature of 300-1600 DEG C, carrying out ultrasonic cleaning in deionized water and alcohol successively to obtain the porous inorganic membrane with stable structure and high porosity. The porous inorganic membrane disclosed in the invention used as the lithium ion battery diaphragm has substantial advantages of thermal stability and thermal safety. The battery which uses the porous inorganic membrane disclosed in the invention has good cycle performance, discharge rate and high and low temperature performance. The porous inorganic membrane disclosed in the invention can improve the thermal safety and electrochemical character of the lithium ion battery, and has stable property and low cost.
Description
Technical field
The invention belongs to field of chemical power source, relate to lithium rechargeable battery critical material and technology, be specifically related to a kind of inorganic porous membrane that is used as lithium ion battery separator and preparation method thereof.
Background technology
Along with the consumption of fossil fuel, the research of store energy and converting apparatus is more and more caused people's attention.Lithium ion battery owing to the energy density height, have extended cycle life, self-discharge rate is low etc., and advantage becomes the most noticeable secondary cell.Yet electrokinetic cell and the required main equipment of long-term energy storage require lithium ion battery to possess high rate capability, long-time stability energy and high-temperature behavior etc., and these all are lithium ion battery development problem demanding prompt solutions.Existing business-like lithium ion battery is extensive use of by the polymer nature in polyolefin and the colloidal sol type electrolyte as barrier film, however these organic barrier films exist usually problems such as fusing point is low, bad mechanical strength.Membrane for polymer is under higher temperature (~ 100
oC) obvious torsional deformation can appear, under big multiplying power, discharge and recharge and long-time cyclic process in can be pierced through by Li dendrite.Therefore, organic barrier film may cause some potential potential safety hazards.
Inorganic material has outstanding thermal stability and electrolyte wetting property, therefore is widely used in the modified polymer barrier film.Membrane for polymer after inorganic material is modified presents better thermodynamic stability, with the battery of its assembling more performance is arranged.Recently, in order further to improve the thermal stability of battery, it is main component and the anodic aluminium oxide membrane that adds the organic substance preparation that people have studied with the inorganic nano ceramic powder.On the other hand, there has been the report solid inorganic thing electrolyte can be, still, very difficultly between the solid electrolyte of non-liquid phase and the solid phase electrode material fully contacted simultaneously as barrier film and electrolyte.In battery winding assembly, anodic aluminium oxide membrane is not used owing to the pliability difference.But in prismatic battery and other rigidity battery design, inorganic diaphragm is feasible as barrier film, and using value is arranged very much.With respect to business-like membrane for polymer, anodic aluminium oxide membrane have " absolute " thermal stability, to the high adsorption capacity of electrolyte, can not be by advantages such as Li dendrite pierce through.Because the stability of anodic aluminium oxide membrane material, will obvious superior performance be arranged than the battery pack of forming by a lot of baby batteries with the large-scale monocell of anodic aluminium oxide membrane material preparation.In addition, pure inorganic matter barrier film might be used to design three-dimensional batteries.
The porous anodic aluminium oxide membrane of the present invention's preparation has the intensity that the battery assembling needs, as the enough big porosity of battery diaphragm.The present invention prepares porous anodic aluminium oxide membrane, and is assembled into battery as battery diaphragm, tests its chemical property.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of inorganic porous membrane that is used as lithium ion battery separator and preparation method thereof is provided.The present invention uses relatively inexpensive raw material, by comparatively simple equipment and technology, prepare a kind of inorganic porous membrane by double sintering as lithium ion battery separator, its absorption property to electrolyte is higher, resistance to elevated temperatures good, therefore can significantly improve cycle performance, high rate performance and the high temperature performance of battery; Product homogeneous, good reproducibility, not high to equipment requirements, with low cost, excellent performance.Inorganic porous membrane of the present invention is as lithium ion battery separator, make battery thermal stability and thermal safety significantly improve, the anodic aluminium oxide membrane conductivity of soaking into electrolyte simultaneously is far above business-like membrane for polymer, thereby make battery have better cycle ability, high rate performance and high temperature performance, and can effectively improve the Applicable temperature of battery.
A kind of inorganic porous membrane as lithium ion battery separator, it consists of: aluminium oxide, silicon dioxide or magnesium oxide.
The present invention also provides a kind of preparation method who is used as the inorganic porous membrane of lithium ion battery separator, may further comprise the steps:
(1) will insulate inorganic material and pore creating material is even with 1:10 ~ 10:1 mixed, grinds, and obtains mixture powder;
(2) mixture powder that step (1) is obtained is put into mould, is pressed into diaphragm under 2 ~ 20MPa pressure;
(3) diaphragm that step (2) is obtained is at 300 ~ 1600 ℃ of calcining 2 ~ 10h, and 2 ~ 10h is calcined once more at 300 ~ 1600 ℃ in the cooling back, cooling, the diaphragm after obtaining activating;
(4) diaphragm after the activation that step (3) is obtained immerses in the deionized water and carries out ultrasonic cleaning 1 ~ 10min, immerses after the taking-up in the ethanol again, carries out ultrasonic cleaning 1 ~ 10min under same frequency and the power, and 80 ℃ of vacuumize 6 ~ 24h obtain inorganic porous membrane.
In the step of the present invention (1), described insulation inorganic material is an insulation oxide, comprises in aluminium oxide, calcium oxide or the magnesium oxide one or both; Described insulation inorganic material is of a size of nanoscale and/or micron order.
In the step of the present invention (1), described pore creating material is ethylenediamine tetra-acetic acid, polyvinyl alcohol, carbon black or carbonic hydroammonium.
In the step of the present invention (4), the frequency of described ultrasonic cleaning is 35 ~ 50kHz, and power is 100W.
The present invention also provides the application of a kind of described inorganic porous membrane in lithium ion battery separator.
The present invention compared with prior art has following advantage:
(1) inorganic porous membrane high-temperature thermal stability of the present invention, thermal safety height as lithium ion battery separator, make battery thermal stability and thermal safety significantly improve, and have better high temperature performance, and can effectively improve the Applicable temperature of battery;
(2) inorganic porous membrane of the present invention is as lithium ion battery separator, absorption electrolyte ability is strong, soak into the porous anodic aluminium oxide membrane conductivity height of electrolyte,, thereby make battery have better cycle ability, high rate performance far above existing business-like membrane for polymer;
(3) product homogeneity of the present invention and good reproducibility, excellent performance;
(4) pressed powder and the pore creating material selected for use of the present invention is all cheap and easy to get, with low cost; Preparation method's technology is simple, and not high to equipment requirements, equipment investment is few, and the cycle is shorter, is beneficial to reduce cost and heavy industrialization.
Description of drawings
Fig. 1 is the sem photograph of the porous anodic aluminium oxide membrane of the embodiment of the invention 1 preparation.
Fig. 2 is that the anodic aluminium oxide membrane of the embodiment of the invention 1 preparation soaks into the conductivity of electrolyte and the conductivity contrast of electrolytic conductivity and traditional polymer barrier film infiltration electrolyte.
After Fig. 3 was the anodic aluminium oxide membrane and traditional polymer barrier film infiltration electrolyte of the embodiment of the invention 1 preparation, diaphragm quality is change curve in time.
Fig. 4 is the anodic aluminium oxide membrane of the embodiment of the invention 1 preparation and the LiFePO that the traditional polymer barrier film is respectively barrier film
4The cycle performance figure of the full battery of/C.
Fig. 5 is the anodic aluminium oxide membrane of the embodiment of the invention 1 preparation and the LiFePO that the traditional polymer barrier film is respectively barrier film
4The discharge curve that the full battery of/C discharges and recharges in different multiplying.
Embodiment
Below in conjunction with embodiment the specific embodiment of the present invention is described further, but the scope of protection of present invention is not limited to this.
Take by weighing the 0.3g alumina in Nano level, 0.3g micron order aluminium oxide and 0.4g ethylenediamine tetra-acetic acid, grind behind the mixing and obtain mixture powder, take by weighing 0.25g said mixture powder and put into mould, under 16MPa pressure, be pressed into diaphragm, with the diaphragm that obtains in Muffle furnace with 1000 ℃ of sintering 5h, after naturally cooling to room temperature, 1600 ℃ of sintering 5h in Muffle furnace again, naturally cool to room temperature, in 35kHz, carry out ultrasonic cleaning 3min under the 100W in the immersion deionized water, immerse in the ethanol again after the taking-up, carry out ultrasonic cleaning 3min, 80 ℃ of dry 8h obtain inorganic porous membrane of the present invention in vacuum drying oven.
As shown in Figure 1, observe under ESEM, porous, inorganic membrane porosity of the present invention is greater than 70%.
Inorganic porous membrane of the present invention as lithium ion battery separator, is carried out battery performance test, and test condition is as follows: positive electrode is a commercialization LiFePO4 (chemical formula: LiFePO
4), negative material is a graphite, is conductive agent with Super P all, and binding agent is that Kynoar (is called for short: PVdF), (be called for short: NMP) make pole piece on aluminium foil and the Copper Foil for solvent furnishing slip is applied to respectively, electrolyte is the 1mol/L LiPF of 1:1 to the N-methyl pyrrolidone
6(lithium hexafluoro phosphate)/EC(ethylene carbonate)+the DEC(diethyl carbonate); Be the barrier film of battery with the Woelm Alumina of the present invention's preparation and traditional commercialization microporous polypropylene membrane respectively, be assembled into the test battery that model is CR2032.In being full of the glove box of argon gas, be assembled into the button electricity, carry out electro-chemical test.The test voltage scope is 2.4 ~ 4.3V.
In glove box, will seal with the CR2032 battery case behind multiaperture pellumina and the microporous polypropylene membrane infiltration electrolyte, test its conductivity by Zahner IM6ex electrochemical workstation, as shown in Figure 2, soak into Woelm Alumina membrane conductivity behind the electrolyte as can be seen apparently higher than the microporous polypropylene membrane that soaks into behind the electrolyte.
Multiaperture pellumina and microporous polypropylene membrane soaked into put into 55 ℃ of baking ovens behind the electrolyte and dry, test mass over time, as shown in Figure 3, multiaperture pellumina obviously is better than microporous polypropylene membrane to the absorption and the retention of electrolyte as can be seen.
Be barrier film with multiaperture pellumina and microporous polypropylene membrane respectively, positive pole is selected commercialization LiFePO for use
4, negative pole is selected graphite for use, and being assembled into model is the CR2032 test battery, tests its cycle performance and high rate performance respectively, and as shown in Figure 4, inorganic porous membrane of the present invention is used for lithium ion battery separator makes battery have excellent cycle performance; As shown in Figure 5, the inorganic porous membrane of the present invention battery that is used for lithium ion battery separator has more outstanding high rate performance than the battery of commodity in use microporous polypropylene membrane.
Embodiment 2
Take by weighing 0.3g nanoscale calcium oxide, 0.3g micron order calcium oxide and 0.4g carbonic hydroammonium, grind behind the mixing and obtain mixture powder, take by weighing 0.25g said mixture powder and put into mould, under 2MPa pressure, be pressed into diaphragm, with the diaphragm that obtains in Muffle furnace with 300 ℃ of sintering 10h, after naturally cooling to room temperature, 300 ℃ of sintering 10h in Muffle furnace again, naturally cool to room temperature, in 40kHz, carry out ultrasonic cleaning 1min under the 100W in the immersion deionized water, immerse in the ethanol again after the taking-up, carry out ultrasonic cleaning 1min, 80 ℃ of dry 6h obtain inorganic porous membrane of the present invention in vacuum drying oven.
Embodiment 3
Take by weighing 0.5g micron order aluminium oxide and 0.5g ethylenediamine tetra-acetic acid, grind behind the mixing and obtain mixture powder, take by weighing 0.25g said mixture powder and put into mould, under 16MPa pressure, be pressed into diaphragm, with the diaphragm that obtains in Muffle furnace with 1000 ℃ of sintering 5h, after naturally cooling to room temperature, 1600 ℃ of sintering 5h in Muffle furnace again, naturally cool to room temperature, in 45kHz, carry out ultrasonic cleaning 3min under the 100W in the immersion deionized water, immerse in the ethanol again after the taking-up, carry out ultrasonic cleaning 3min, 80 ℃ of dry 8h obtain inorganic porous membrane of the present invention in vacuum drying oven.
Embodiment 4
Take by weighing 0.5g micron order magnesium oxide and 0.5g carbon black, grind behind the mixing and obtain mixture powder, take by weighing 0.25g said mixture powder and put into mould, under 10MPa pressure, be pressed into diaphragm, with the diaphragm that obtains in Muffle furnace with 800 ℃ of sintering 6h, after naturally cooling to room temperature, 800 ℃ of sintering 6h in Muffle furnace again, naturally cool to room temperature, in 50kHz, carry out ultrasonic cleaning 5min under the 100W in the immersion deionized water, immerse in the ethanol again after the taking-up, carry out ultrasonic cleaning 5min, 80 ℃ of dry 16h obtain inorganic porous membrane of the present invention in vacuum drying oven.
Take by weighing 0.1g micron order calcium oxide and 1.0g carbonic hydroammonium, grind behind the mixing and obtain mixture powder, take by weighing 0.25g said mixture powder and put into mould, under 20MPa pressure, be pressed into diaphragm, with the diaphragm that obtains in Muffle furnace with 1200 ℃ of sintering 4h, after naturally cooling to room temperature, 1200 ℃ of sintering 4h in Muffle furnace again, naturally cool to room temperature, in 35kHz, carry out ultrasonic cleaning 8min under the 100W in the immersion deionized water, immerse in the ethanol again after the taking-up, carry out ultrasonic cleaning 8min, 80 ℃ of dry 20h obtain inorganic porous membrane of the present invention in vacuum drying oven.
Take by weighing 0.5g nanoscale magnesium oxide, 0.5g micron order calcium oxide and 0.1g polyvinyl alcohol, grind behind the mixing and obtain mixture powder, take by weighing 0.25g said mixture powder and put into mould, under 8MPa pressure, be pressed into diaphragm, with the diaphragm that obtains in Muffle furnace with 600 ℃ of sintering 8h, after naturally cooling to room temperature, 600 ℃ of sintering 8h in Muffle furnace again, naturally cool to room temperature, in 50kHz, carry out ultrasonic cleaning 10min under the 100W in the immersion deionized water, immerse in the ethanol again after the taking-up, carry out ultrasonic cleaning 10min, 80 ℃ of dry 18h obtain inorganic porous membrane of the present invention in vacuum drying oven.
Embodiment 7
Take by weighing 0.5g micron order magnesium oxide, 0.5g alumina in Nano level and 0.1g carbon black, grind behind the mixing and obtain mixture powder, take by weighing 0.25g said mixture powder and put into mould, under 12MPa pressure, be pressed into diaphragm, with the diaphragm that obtains in Muffle furnace with 300 ℃ of sintering 10h, after naturally cooling to room temperature, 300 ℃ of sintering 10h in Muffle furnace again, naturally cool to room temperature, in 50kHz, carry out ultrasonic cleaning 6min under the 100W in the immersion deionized water, immerse in the ethanol again after the taking-up, carry out ultrasonic cleaning 6min, 80 ℃ of dry 12h obtain inorganic porous membrane of the present invention in vacuum drying oven.
Embodiment 8
Take by weighing 0.1g micron order calcium oxide, 0.1g alumina in Nano level and 2.0g polyvinyl alcohol, grind behind the mixing and obtain mixture powder, take by weighing 0.25g said mixture powder and put into mould, under 6MPa pressure, be pressed into diaphragm, with the diaphragm that obtains in Muffle furnace with 1600 ℃ of sintering 2h, after naturally cooling to room temperature, 1600 ℃ of sintering 2h in Muffle furnace again, naturally cool to room temperature, in 35kHz, carry out ultrasonic cleaning 3min under the 100W in the immersion deionized water, immerse in the ethanol again after the taking-up, carry out ultrasonic cleaning 3min, 80 ℃ of dry 24h obtain inorganic porous membrane of the present invention in vacuum drying oven.
Claims (6)
1. the inorganic porous membrane as lithium ion battery separator is characterized in that, the consisting of of described inorganic porous membrane: aluminium oxide, silicon dioxide or magnesium oxide.
2. the preparation method of the described inorganic porous membrane of claim 1 is characterized in that may further comprise the steps:
(1) be 10:(100 ~ 1 with mass ratio) insulation inorganic material and pore creating material mix, grind, obtain mixture powder;
(2) mixture powder that step (1) is obtained is put into mould, is pressed into diaphragm under 2 ~ 20MPa pressure;
(3) diaphragm that step (2) is obtained is at 300 ~ 1600 ℃ of calcining 2 ~ 10h, and 2 ~ 10h is calcined once more at 300 ~ 1600 ℃ in the cooling back, cooling, the diaphragm after obtaining activating;
(4) diaphragm after the activation that step (3) is obtained immerses in the deionized water and carries out ultrasonic cleaning 1 ~ 10min, immerses after the taking-up in the ethanol again, carries out ultrasonic cleaning 1 ~ 10min under same frequency and the power, and 80 ℃ of vacuumize 6 ~ 24h obtain inorganic porous membrane.
3. preparation method according to claim 2 is characterized in that, in the step (1), described insulation inorganic material is an insulation oxide, comprises in aluminium oxide, calcium oxide or the magnesium oxide one or both; Described insulation inorganic material is of a size of nanoscale and/or micron order.
4. preparation method according to claim 3 is characterized in that, in the step (1), described pore creating material is ethylenediamine tetra-acetic acid, polyvinyl alcohol, carbon black or carbonic hydroammonium.
5. preparation method according to claim 4 is characterized in that, in the step (4), the frequency of described ultrasonic cleaning is 35 ~ 50kHz, and power is 100W.
6. the described inorganic porous membrane of one of claim 1 ~ 5 is characterized in that, the application in lithium ion battery separator.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103904273A (en) * | 2012-12-28 | 2014-07-02 | 海洋王照明科技股份有限公司 | Electrochemical power source diaphragm and preparation method thereof, and electrochemical cell or capacitor |
| CN103964821A (en) * | 2013-01-28 | 2014-08-06 | 海洋王照明科技股份有限公司 | Aluminum oxide solid diaphragm, preparing method of aluminum oxide solid diaphragm, electrochemical battery or capacitor |
| CN103972447A (en) * | 2013-01-28 | 2014-08-06 | 海洋王照明科技股份有限公司 | Electrochemical power diaphragm and preparation method thereof, and electrochemical battery or capacitor |
| CN104993082A (en) * | 2015-06-01 | 2015-10-21 | 常州大学 | Preparation method for nano-alumina particle modified ceramic diaphragm |
| CN105514326A (en) * | 2015-01-16 | 2016-04-20 | 万向A一二三系统有限公司 | Composite separator and power lithium titanate battery containing composite separator |
| CN106601965A (en) * | 2016-12-21 | 2017-04-26 | 张家港智电芳华蓄电研究所有限公司 | Preparation method of high-strength and high-tenacity composite ceramic partition plate |
| CN108183189A (en) * | 2017-12-07 | 2018-06-19 | 常州市沃兰特电子有限公司 | A kind of preparation method of high temp resistance lithium ion cell diaphragm |
| CN110416632A (en) * | 2019-06-20 | 2019-11-05 | 合肥国轩高科动力能源有限公司 | A method of improving electrodes of lithium-ion batteries wellability |
| CN110729494A (en) * | 2019-10-30 | 2020-01-24 | 无锡威孚高科技集团股份有限公司 | Catalyst slurry for proton exchange membrane fuel cell and preparation method thereof |
| CN111584806A (en) * | 2019-02-18 | 2020-08-25 | 三星Sdi株式会社 | Separator and lithium battery including the same |
| CN112332022A (en) * | 2020-11-03 | 2021-02-05 | 贵州梅岭电源有限公司 | Porous vermiculite sheet and application method thereof in lithium ion battery |
| CN112928325A (en) * | 2021-02-05 | 2021-06-08 | 清华大学深圳国际研究生院 | Preparation method of solid-liquid mixed electrolyte and electrochemical device using same |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103904273A (en) * | 2012-12-28 | 2014-07-02 | 海洋王照明科技股份有限公司 | Electrochemical power source diaphragm and preparation method thereof, and electrochemical cell or capacitor |
| CN103904273B (en) * | 2012-12-28 | 2016-03-23 | 海洋王照明科技股份有限公司 | Electrochemical power source separation membrane and preparation method thereof, electrochemical cell or capacitor |
| CN103972447B (en) * | 2013-01-28 | 2017-02-08 | 海洋王照明科技股份有限公司 | Electrochemical power diaphragm and preparation method thereof, and electrochemical battery or capacitor |
| CN103964821A (en) * | 2013-01-28 | 2014-08-06 | 海洋王照明科技股份有限公司 | Aluminum oxide solid diaphragm, preparing method of aluminum oxide solid diaphragm, electrochemical battery or capacitor |
| CN103972447A (en) * | 2013-01-28 | 2014-08-06 | 海洋王照明科技股份有限公司 | Electrochemical power diaphragm and preparation method thereof, and electrochemical battery or capacitor |
| CN105514326B (en) * | 2015-01-16 | 2018-02-13 | 万向一二三股份公司 | A kind of composite diaphragm and the power lithium titanate battery containing the composite diaphragm |
| CN105514326A (en) * | 2015-01-16 | 2016-04-20 | 万向A一二三系统有限公司 | Composite separator and power lithium titanate battery containing composite separator |
| CN104993082A (en) * | 2015-06-01 | 2015-10-21 | 常州大学 | Preparation method for nano-alumina particle modified ceramic diaphragm |
| CN106601965A (en) * | 2016-12-21 | 2017-04-26 | 张家港智电芳华蓄电研究所有限公司 | Preparation method of high-strength and high-tenacity composite ceramic partition plate |
| CN108183189A (en) * | 2017-12-07 | 2018-06-19 | 常州市沃兰特电子有限公司 | A kind of preparation method of high temp resistance lithium ion cell diaphragm |
| CN111584806A (en) * | 2019-02-18 | 2020-08-25 | 三星Sdi株式会社 | Separator and lithium battery including the same |
| CN111584806B (en) * | 2019-02-18 | 2023-04-07 | 三星Sdi株式会社 | Separator and lithium battery including the same |
| CN110416632A (en) * | 2019-06-20 | 2019-11-05 | 合肥国轩高科动力能源有限公司 | A method of improving electrodes of lithium-ion batteries wellability |
| CN110416632B (en) * | 2019-06-20 | 2022-03-11 | 合肥国轩高科动力能源有限公司 | Method for improving wettability of lithium ion battery pole piece |
| CN110729494A (en) * | 2019-10-30 | 2020-01-24 | 无锡威孚高科技集团股份有限公司 | Catalyst slurry for proton exchange membrane fuel cell and preparation method thereof |
| CN112332022A (en) * | 2020-11-03 | 2021-02-05 | 贵州梅岭电源有限公司 | Porous vermiculite sheet and application method thereof in lithium ion battery |
| CN112928325A (en) * | 2021-02-05 | 2021-06-08 | 清华大学深圳国际研究生院 | Preparation method of solid-liquid mixed electrolyte and electrochemical device using same |
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Application publication date: 20111228 |