CN101685861A - Method for preparing lithium titanate cathode size - Google Patents
Method for preparing lithium titanate cathode size Download PDFInfo
- Publication number
- CN101685861A CN101685861A CN200810216384A CN200810216384A CN101685861A CN 101685861 A CN101685861 A CN 101685861A CN 200810216384 A CN200810216384 A CN 200810216384A CN 200810216384 A CN200810216384 A CN 200810216384A CN 101685861 A CN101685861 A CN 101685861A
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- CN
- China
- Prior art keywords
- lithium titanate
- oxalic acid
- cathode size
- titanate cathode
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 64
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 63
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 12
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 129
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 43
- 239000000463 material Substances 0.000 claims abstract description 25
- 238000002360 preparation method Methods 0.000 claims abstract description 22
- 239000002002 slurry Substances 0.000 claims description 8
- 239000002033 PVDF binder Substances 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 5
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 4
- 230000000694 effects Effects 0.000 abstract description 6
- 238000000576 coating method Methods 0.000 description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 229910052596 spinel Inorganic materials 0.000 description 3
- 239000011029 spinel Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000005030 aluminium foil Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
Classifications
-
- 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
The invention relates to a method for preparing lithium titanate cathode size, belonging to the battery preparation method field. The method is characterized in that the lithium titanate cathode sizedis added with oxalic acid, wherein 1-6% of oxalic acid is added by taking the total weight of the cathode size as 100%. The method for adding oxalic acid includes: oxalic acid and lithium titanate are mixed in dry, fully mixed to be uniform and then added with other materials to be made into the lithium titanate cathode size; or materials except oxalic acid is firstly mixed into size, and then oxalic acid is added into the size and fully mixed to be uniform, so as to obtain the lithium titanate cathode size. The invention provides a method for preparing lithium titanate cathode size with highadhesive force with afflux surface and good bonding effect, thus being capable of effectively improving electrochemical performances of battery with lithium titanate as cathode such as capacity, cycle performance and the like.
Description
Affiliated technical field:
The invention belongs to the battery preparation method field, specifically is a kind of preparation method of lithium titanate cathode size.
Background technology:
Lithium ion battery is since the nineties in 20th century commercial applications, and lithium rechargeable battery has occupied more than 70% of global secondary cell market scale so far.Based on the security consideration of lithium ion battery, need to seek the novel negative material that substitutes material with carbon element.Spinel type lithium titanate is as lithium ion battery negative material, because it has with respect to Li
+The current potential that/Li is higher, the problem that does not exist lithium metal to separate out in charge and discharge process can improve the security performance of battery greatly; Spinel type lithium titanate still is a kind of zero strain material simultaneously, has excellent cycle performance, can be widely used in electric tool, HEV (hybrid electrically instrument), and EV fields such as (electric tools), thus become the focus that lithium ion battery negative material is studied.The spinel lithium titanate material is because itself conductivity is relatively poor, thereby need make sub-micron even nano level material could be used, and as everyone knows, the granularity of material is more little, Li
+In material, need the path passed through short more, also just be suitable for the system that discharges and recharges of big multiplying power more.Thereby each material maker positive and negative pole material that conductivity is the relatively poor especially granularity of phosphoric acid system positive electrode and lithium titanate anode material is controlled at nanoscale or submicron order more.Yet the material of small particle diameter has bigger specific area, higher specific surface energy, when adopting PVDF (polyvinylidene fluoride) oiliness system, relatively poor with the compatibility of collector, bond effect is bad, thereby caused material in the production application process, to apply difficulty, had a strong impact on the problems such as chemical property of battery.
Summary of the invention:
The objective of the invention is in order to remedy the compatibility that has lithium titanate cathode size and collector now relatively poor, the deficiency that bond effect is bad, for people provide a kind of and adhesive force height collection liquid surface, bond effect is good, thus the preparation method of the lithium titanate cathode size of chemical properties such as the capacity of the battery that effective raising is negative pole with the lithium titanate and cycle performance.
The objective of the invention is to realize by following technical proposals.
The preparation method of lithium titanate cathode size of the present invention is characterized in that being added with in the lithium titanate cathode size oxalic acid, is 100% in the cathode size total weight, and the addition of oxalic acid is 1%～6%.
In the such scheme, the adding method of described oxalic acid is: oxalic acid is done with the lithium titanate material earlier and is mixed, and fully mixes, and adds other material again and makes lithium titanate cathode size.
In the such scheme, the adding method of described oxalic acid is: earlier the material outside the oxalic acid is made into slurry, oxalic acid is joined in the above-mentioned slurry again, fully mix, make lithium titanate cathode size.
In the such scheme, the proportioning of described lithium titanate cathode size is by weight: lithium titanate+oxalic acid: 85%～91%, and PVDF (polyvinylidene fluoride): 3.6%～6%, super conductive carbon black: 5.4%～9%.
Improve the compatibility and the bond effect of lithium titanate cathode size and collector, need to consider following factor: 1, surface cleanness; 2, wetability; 3, the selection of adhesive; 4, design of bonded joint etc.Inventor of the present invention is by discovering in a large number, owing to the processing technology reason, collector (Copper Foil or aluminium foil) in process of production its remained on surface have surface tension bigger roll oil, be to cause the uncleanly main cause of collection liquid surface, obviously reduced the wetability of lithium titanate cathode size simultaneously for collector.Therefore, the present invention only is used in the existing lithium titanate cathode size and adds oxalic acid, just can dispose the greasy dirt of collection liquid surface, reduce its surface tension, lithium titanate cathode size can be sprawled fully at collection liquid surface to come, improved the wetability of slurry for collector, thereby effectively raise the surface density and the adhesive force of the lithium titanate after the coating, improved the foil-covering effect of slurry, and can effectively to improve with the lithium titanate be chemical properties such as the capacity of battery of negative pole and cycle performance, remedied the deficiencies in the prior art.
Embodiment:
The invention is further illustrated by the following examples, and the present invention is not limited only to described embodiment.
Embodiment one
The preparation method of the lithium titanate cathode size that this is routine is as follows:
The proportioning of lithium titanate cathode size is 100% to count with the cathode size total weight: (lithium titanate+oxalic acid): PVDF: super conductive carbon black=90%: 4%: 6%, wherein, the consumption of oxalic acid is 1%.Oxalic acid is done with the lithium titanate material earlier and is mixed, and fully mixes, and adds other material again and makes lithium titanate cathode size.According to normal coating process coating identical faces density (20.1mg/cm
2) the lithium titanate anode sheet, and at identical compacted density (1.7g/cm
3) under be rolled into pole piece.
Hinge (production of 3M company) is sticked on the negative plate, and compress, hold one side of gummed paper and spend angles into about 150 with desktop to discharge the air of the inside, the gummed paper of tearing fast, the test peel strength is 0.11N.
Embodiment two
The preparation method of the lithium titanate cathode size that this is routine is 2% except that the consumption of oxalic acid, and all the other are with embodiment one.
Peel strength is 0.15N.
Embodiment three
The preparation method of the lithium titanate cathode size that this is routine is 3% except that the consumption of oxalic acid, and all the other are with embodiment one.
Peel strength is 0.30N.
Embodiment four
The preparation method of the lithium titanate cathode size that this is routine is 4% except that the consumption of oxalic acid, and all the other are with embodiment one.
Peel strength is 0.25N.
Embodiment five
The preparation method of the lithium titanate cathode size that this is routine is 5% except that the consumption of oxalic acid, and all the other are with embodiment one.
Peel strength is 0.20N.
Embodiment six
The preparation method of the lithium titanate cathode size that this is routine is 6% except that the consumption of oxalic acid, and all the other are with embodiment one.
Peel strength is 0.15N.
Embodiment seven
The preparation method of the lithium titanate cathode size that this is routine is as follows:
The proportioning of lithium titanate cathode size is 100% to count with the cathode size total weight: (lithium titanate+oxalic acid): PVDF: super conductive carbon black=85%: 6%: 9%, wherein, the consumption of oxalic acid is 1%.Earlier the material outside the oxalic acid is made into slurry, again oxalic acid is joined in the above-mentioned slurry, fully mix, make lithium titanate cathode size.According to normal coating process coating identical faces density (20.1mg/cm
2) the lithium titanate anode sheet, and at identical compacted density (1.7g/cm
3) under be rolled into pole piece.
Hinge (production of 3M company) is sticked on the negative plate, and compress, hold one side of gummed paper and spend angles into about 150 with desktop to discharge the air of the inside, the gummed paper of tearing fast, the test peel strength is 0.12N.
Embodiment eight
The preparation method of the lithium titanate cathode size that this is routine removes (lithium titanate+oxalic acid): PVDF: super conductive carbon black=91%: 3.6%: 5.4%, and wherein, the consumption of oxalic acid is outside 2%, all the other are with embodiment seven.
Peel strength is 0.20N.
Embodiment nine
The preparation method of the lithium titanate cathode size that this is routine is 3% except that the consumption of oxalic acid, and all the other are with embodiment seven.
Peel strength is 0.25N.
Embodiment ten
The preparation method of the lithium titanate cathode size that this is routine is 4% except that the consumption of oxalic acid, and all the other are with embodiment seven.
Peel strength is 0.25N.
Embodiment 11
The preparation method of the lithium titanate cathode size that this is routine is 5% except that the consumption of oxalic acid, and all the other are with embodiment seven.
Peel strength is 0.20N.
Embodiment 12
The preparation method of the lithium titanate cathode size that this is routine is 6% except that the consumption of oxalic acid, and all the other are with embodiment seven.
Peel strength is 0.20N.
Embodiment 13
This example is a reference examples, and except that not adding the oxalic acid, all the other are with embodiment one.As a result, do not add oxalic acid and fall material seriously after coating, peel strength is 0.
Claims (4)
1. the preparation method of a lithium titanate cathode size is characterized in that being added with in the lithium titanate cathode size oxalic acid, is 100% in the cathode size total weight, and the addition of oxalic acid is 1%～6%.
2. the preparation method of lithium titanate cathode size according to claim 1 is characterized in that the adding method of described oxalic acid is: oxalic acid is done with the lithium titanate material earlier and is mixed, and fully mixes, and adds other material again and makes lithium titanate cathode size.
3. the preparation method of lithium titanate cathode size according to claim 1, the adding method that it is characterized in that described oxalic acid is: earlier the material outside the oxalic acid is made into slurry, again oxalic acid is joined in the above-mentioned slurry, fully mix, make lithium titanate cathode size.
4. the preparation method of lithium titanate cathode size according to claim 1, the proportioning that it is characterized in that described lithium titanate cathode size is by weight: lithium titanate+oxalic acid: 85%～91%, polyvinylidene fluoride: 3.6%～6%, super conductive carbon black: 5.4%～9%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810216384A CN101685861A (en) | 2008-09-25 | 2008-09-25 | Method for preparing lithium titanate cathode size |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810216384A CN101685861A (en) | 2008-09-25 | 2008-09-25 | Method for preparing lithium titanate cathode size |
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| CN101685861A true CN101685861A (en) | 2010-03-31 |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101924199A (en) * | 2010-07-29 | 2010-12-22 | 江苏双登集团有限公司 | Oily cathode material of lithium ion battery and manufacturing method thereof |
| CN102034981A (en) * | 2010-10-26 | 2011-04-27 | 东莞新能源科技有限公司 | Collector used for negative pole of lithium ion battery |
| CN102709602A (en) * | 2012-05-22 | 2012-10-03 | 株洲市高远电池有限公司 | Manufacturing method of high energy-density lithium-ion secondary battery |
| CN104134780A (en) * | 2014-07-18 | 2014-11-05 | 奇瑞汽车股份有限公司 | Lithium ion battery pole piece and preparation method thereof |
| CN105206819A (en) * | 2014-05-30 | 2015-12-30 | 河南科隆新能源有限公司 | Lithium-ion-battery negative electrode slurry, preparing method thereof and preparing method of negative electrode plate |
| CN105336943A (en) * | 2015-11-24 | 2016-02-17 | 四川省有色冶金研究院有限公司 | Lithium battery formed on basis of lithium nickel manganese oxide and lithium titanate and preparation method of lithium battery |
| CN105428636A (en) * | 2015-11-24 | 2016-03-23 | 四川省有色冶金研究院有限公司 | Lithium ion battery anode material based on lithium titanate and preparation method thereof |
| CN105529430A (en) * | 2015-11-20 | 2016-04-27 | 河北银隆新能源有限公司 | Preparation method of nano lithium titanate anode slurry |
| CN105552355A (en) * | 2015-12-16 | 2016-05-04 | 山东精工电子科技有限公司 | High-rate lithium-ion battery and preparation method thereof |
| CN106602050A (en) * | 2015-10-18 | 2017-04-26 | 深圳市沃特玛电池有限公司 | Preparation method of slurry for lithium titanate battery |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101154720A (en) * | 2006-09-29 | 2008-04-02 | 深圳市比克电池有限公司 | Cathode slurry of lithium battery, its producing method and lithium battery |
-
2008
- 2008-09-25 CN CN200810216384A patent/CN101685861A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101154720A (en) * | 2006-09-29 | 2008-04-02 | 深圳市比克电池有限公司 | Cathode slurry of lithium battery, its producing method and lithium battery |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101924199A (en) * | 2010-07-29 | 2010-12-22 | 江苏双登集团有限公司 | Oily cathode material of lithium ion battery and manufacturing method thereof |
| CN102034981A (en) * | 2010-10-26 | 2011-04-27 | 东莞新能源科技有限公司 | Collector used for negative pole of lithium ion battery |
| CN102709602A (en) * | 2012-05-22 | 2012-10-03 | 株洲市高远电池有限公司 | Manufacturing method of high energy-density lithium-ion secondary battery |
| CN102709602B (en) * | 2012-05-22 | 2014-08-06 | 株洲市高远电池有限公司 | Manufacturing method of high energy-density lithium-ion secondary battery |
| CN105206819A (en) * | 2014-05-30 | 2015-12-30 | 河南科隆新能源有限公司 | Lithium-ion-battery negative electrode slurry, preparing method thereof and preparing method of negative electrode plate |
| CN104134780A (en) * | 2014-07-18 | 2014-11-05 | 奇瑞汽车股份有限公司 | Lithium ion battery pole piece and preparation method thereof |
| CN106602050A (en) * | 2015-10-18 | 2017-04-26 | 深圳市沃特玛电池有限公司 | Preparation method of slurry for lithium titanate battery |
| CN105529430A (en) * | 2015-11-20 | 2016-04-27 | 河北银隆新能源有限公司 | Preparation method of nano lithium titanate anode slurry |
| CN105529430B (en) * | 2015-11-20 | 2018-08-21 | 河北银隆新能源有限公司 | The preparation method of nano lithium titanate negative electrode slurry |
| CN105336943A (en) * | 2015-11-24 | 2016-02-17 | 四川省有色冶金研究院有限公司 | Lithium battery formed on basis of lithium nickel manganese oxide and lithium titanate and preparation method of lithium battery |
| CN105428636A (en) * | 2015-11-24 | 2016-03-23 | 四川省有色冶金研究院有限公司 | Lithium ion battery anode material based on lithium titanate and preparation method thereof |
| CN105552355A (en) * | 2015-12-16 | 2016-05-04 | 山东精工电子科技有限公司 | High-rate lithium-ion battery and preparation method thereof |
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Application publication date: 20100331 |
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