CN103066294B - Method for preparing lithium battery material by using plant fibers - Google Patents
Method for preparing lithium battery material by using plant fibers Download PDFInfo
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- CN103066294B CN103066294B CN201310030425.2A CN201310030425A CN103066294B CN 103066294 B CN103066294 B CN 103066294B CN 201310030425 A CN201310030425 A CN 201310030425A CN 103066294 B CN103066294 B CN 103066294B
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- cotton fiber
- ion battery
- lithium ion
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- cotton
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- 239000000463 material Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 38
- 239000000835 fiber Substances 0.000 title claims abstract description 16
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 13
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 41
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000003763 carbonization Methods 0.000 claims abstract description 5
- 239000007772 electrode material Substances 0.000 claims abstract description 4
- 238000010298 pulverizing process Methods 0.000 claims abstract description 3
- 229920000742 Cotton Polymers 0.000 claims description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 16
- 229910052799 carbon Inorganic materials 0.000 claims description 14
- 239000002305 electric material Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000011149 active material Substances 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000002086 nanomaterial Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 238000006253 efflorescence Methods 0.000 claims description 2
- 239000012634 fragment Substances 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 206010037844 rash Diseases 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 2
- 229910001887 tin oxide Inorganic materials 0.000 claims description 2
- 238000012546 transfer Methods 0.000 claims description 2
- 238000010335 hydrothermal treatment Methods 0.000 claims 2
- 239000002131 composite material Substances 0.000 abstract description 6
- 238000011161 development Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000000746 purification Methods 0.000 abstract description 2
- 239000013543 active substance Substances 0.000 abstract 1
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 238000011068 loading method Methods 0.000 abstract 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- AEMOLEFTQBMNLQ-BKBMJHBISA-N alpha-D-galacturonic acid Chemical compound O[C@H]1O[C@H](C(O)=O)[C@H](O)[C@H](O)[C@H]1O AEMOLEFTQBMNLQ-BKBMJHBISA-N 0.000 description 2
- 239000010406 cathode material Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000002733 tin-carbon composite material 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
Landscapes
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a method for preparing a lithium battery material by using plant fibers. According to the method, the lithium ion battery electrode material is produced through the processes of pulverization, purification, loading of lithium ion battery active substances and carbonization by using plant fibers as the raw material. Based on the scheme disclosed by the invention, the composite material with a micro-nano mosaic structure can be prepared conveniently, and the raw materials have wide sources. According to the method, a support is provided for improving lithium ion battery production technology and developing novel lithium ion battery materials, and is beneficial for the development of the lithium ion battery industry is facilitated.
Description
Technical field
The invention belongs to lithium electric material preparation field, be specifically related to a kind of method being prepared lithium electric material by string.
Background technology
Since the nineties in last century, lithium ion battery came out, show that specific energy is large, good cycle, operating voltage are high, the life-span is long as third generation rechargeable battery and polluted the excellent properties such as little and receive much attention, and be widely used in, in various light-duty portable equipment, there is very important status in the secondary battery.But, in recent years, along with the appearance of electric motor car, to high-power, high-capacity secondary battery demand aggravation, more and more higher to the requirement of lithium ion battery material and lithium ion battery production technology, continually develop and have high storage density, safe and feasible, cheap lithium ion battery material, one-step optimization production technology etc. of going forward side by side becomes the subject matter that lithium ion battery industry faces.
At present, business-like carbon negative electrode material of lithium ion cell mainly material with carbon element, other novel materials are also still in conceptual phase.Carbon anode lithium ion battery demonstrates good performance in safety and cycle life, and material with carbon element is inexpensive, nontoxic, and current commodity lithium ion battery extensively adopts carbon negative pole material.As everyone knows, material with carbon element is of a great variety, studies more at present and comparatively successfully carbon negative pole material has graphite, acetylene black, microballon carbon, petroleum coke and cracking carbon etc.But these materials exist the defects such as theoretical capacity is low, have impact on the development of lithium ion battery material.Therefore, research work for new type lithium ion battery material is in the ascendant, research shows have various metals alloy, metal oxide, multi-element composite material etc. in lithium ion battery negative material, have huge application scenario, and wherein portion of material is considered to the ideal material that may replace current carbon negative pole material.But because the existing many Novel anode materials studied in laboratory conditions exist number of drawbacks, as the problem such as Study of Volume Expansion, poorly conductive, these defects directly limit its extensive use in lithium ion battery.
Research shows, prepare composite nano materials can effectively improve part Novel cathode material for lithium ion battery application feature.Effectively can suppress the change in volume phenomenon of tin material in lithium ion charge and discharge process as prepared tin carbon composite nano-material, improving the lithium electrical property of tin material.But the existing most complex process of method preparing composite material, and just limit in laboratory environments, and its cost of material is expensive, also has certain distance from real industrialization.
Summary of the invention
For promoting lithium ion battery material industry development, solve the problem that the low and Novel cathode material for lithium ion battery of existing commercial Li-ion battery negative material capacity is difficult to apply, the invention provides a kind of method being prepared lithium electric material by string, make full use of natural plant fibre source fully, there is micro-nano hole gap structure and can the advantages such as material with carbon element be converted into through high-temperature process, by other new type lithium ion battery active materials and string compound, prepare composite material, for improving the preparation technology of lithium ion battery, development of new lithium ion battery material provides support, be conducive to the development of lithium ion battery industry.
For achieving the above object, the present invention adopts following technical scheme:
Being prepared a method for lithium electric material by string, take string as raw material, prepares lithium ion battery electrode material by efflorescence, purifying, load lithium ion battery active material, carbonisation.
Described string comprises the string of natural formation and the later stage string through artificial, and its carbon elements mass fraction after the abundant high temperature cabonization process of inert gas is 95%-100%.
Described atomization process is pulverized by string as 10-104 object particle or the long fiber of 1-2000 micron.
Described purge process removes pectic substance, gumminess and the metal ion in string.
Described load lithium ion battery active material process is that this process is realized by the combination of one or more methods in hydro thermal method, vapour deposition process, sol-gal process, thermal decomposition method at string internal voids or fiber surface load lithium ion battery active material.
Described carbonisation carries out high-temperature heat treatment to material to make the abundant carbonization of organic principle finally obtain lithium ion battery electrode material.
The lithium electric material that a kind of method as above obtains has the material with dimension micro-nano structure that material with carbon element and other materials are inlayed mutually.
Remarkable advantage of the present invention is: prepare lithium ion battery material by method provided by the invention, the advantages such as the higher theoretical capacity of new type lithium ion battery, cycle performance be good can be given full play to, effectively can solve the problems such as the change of new type lithium ion battery material volume, poorly conductive, the material with micro-nano mechanism mutually inlayed finally prepared can ensure fully reacting in lithium ion battery charge and discharge process of material, and this invention has facilitation for the lithium electrical property improving new type lithium ion battery.This invention take string as primary raw material in addition, and this Feedstock treating is very abundant, facilitates feasible, pollution-free in process of production, and the present invention can provide a kind of method of simple possible for producing lithium ion battery material, have huge application prospect.
Accompanying drawing explanation
Fig. 1 is the pattern schematic diagram of string, and wherein 1 is string structure.
Fig. 2 is the pattern schematic diagram of other lithium ion battery active materials of string load, and wherein 2 is the lithium ion battery active material of plant fibre surface or internal load, and 3 is carbon fiber.
Fig. 3 is the SEM picture of the cotton fiber of tin supported sill.
Embodiment
More comprehensively the present invention is described below in conjunction with accompanying drawing, shown in the drawings of the preferred embodiments of the present invention.But the present invention can realize in different forms, and should not be construed as the embodiment being only limitted to this place and setting forth.
(1) choosing cotton fiber is raw material, and cotton fiber is main component is cellulose, and every root cotton fiber is all made up of multistage fibre structure, and its inside exists many pore structures.First to the fiber of natural maturity through deionized water, alcohol washes process, be aided with ultrasonic process in cleaning process.Then by cotton fiber dry process in 70 DEG C of convection oven.Finally cotton fibre powder is broken into the fiber fragments that length is about 1mm.
(2) by chemical method, purification process is carried out to cotton fiber, remove the material such as pectic substance, gumminess, metal ion in string.First the cotton fiber segment of pulverizing is immersed in the NaOH solution of 0.75M, under 80 DEG C of water bath condition, processes 5 hours, use deionized water rinsing afterwards.Then cotton fiber segment is soaked in the salpeter solution of 10%, stirring at room temperature process 5 hours.Finally cotton fiber segment is cleaned, dry process.
(3) with SnCl
2for primary raw material, carrying tin oxide nano particle on cotton fiber.Get the cotton fiber segment 0.2g obtained in (2), be soaked in the SnCl of 0.5M
2in ethanolic solution, room temperature leaves standstill 24 hours.By the cotton fiber segment material transfer after immersion in the hydrothermal reaction kettle of 100ml, add the SnCl soaking cotton fibre material
2ethanolic solution, to about 60ml, added several ammoniacal liquor, with 180 DEG C of water bath processing 24 hours.
(4), after water bath processing, produced composite material is cleaned, dry process.Finally by material in tube furnace with 500 DEG C of argon shield heat treatments 2 hours.
The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (2)
1. prepared a method for lithium electric material by cotton fiber, it is characterized in that: take cotton fiber as raw material, prepare lithium ion battery electrode material by efflorescence, purifying, load lithium ion battery active material, carbonisation;
Comprise the following steps:
(1) choosing cotton fiber is raw material, every root cotton fiber is all made up of multistage fibre structure, there is many pore structures in its inside, through deionized water, alcohol washes process, ultrasonic process is aided with in cleaning process, then by cotton fiber dry process in 70 DEG C of convection oven, finally cotton fibre powder is broken into the fiber fragments of length 1mm;
(2) the cotton fiber segment of pulverizing is immersed in the NaOH solution of 0.75M, 5 hours are processed under 80 DEG C of water bath condition, use deionized water rinsing afterwards, then cotton fiber segment is soaked in the salpeter solution of 10wt.%, stirring at room temperature process 5 hours, finally carries out cleaning and dry process to cotton fiber segment;
(3) get the cotton fiber segment 0.2g obtained in step (2), be soaked in the SnCl of 0.5M
2ethanolic solution in, room temperature leave standstill 24 hours, by soak after cotton fiber segment material transfer in the hydrothermal reaction kettle of 100mL, add the SnCl soaking cotton fibre material
2ethanolic solution to 60mL, add ammoniacal liquor, with 180 DEG C of hydrothermal treatment consists 24 hours;
(4) after hydrothermal treatment consists, by material in tube furnace with 500 DEG C of argon shield heat treatments 2 hours.
2. the lithium electric material that the method for claim 1 is obtained, is characterized in that: described lithium electric material has the material with micro-nano structure that material with carbon element and tin oxide inlays mutually.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310030425.2A CN103066294B (en) | 2013-01-28 | 2013-01-28 | Method for preparing lithium battery material by using plant fibers |
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| CN201310030425.2A CN103066294B (en) | 2013-01-28 | 2013-01-28 | Method for preparing lithium battery material by using plant fibers |
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| CN103066294A CN103066294A (en) | 2013-04-24 |
| CN103066294B true CN103066294B (en) | 2015-02-04 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103441280B (en) * | 2013-09-13 | 2015-12-23 | 桂林理工大学 | The method of lithium ion battery negative material prepared by the sisal carbon fiber of hydro-thermal activation |
| CN104157832B (en) * | 2014-09-04 | 2016-09-28 | 湖北工程学院 | A kind of preparation method of ferroferric oxide/carbon composite lithium ion battery material |
| CN104393261B (en) * | 2014-10-21 | 2017-05-17 | 湖北工程学院 | Preparation method of Cox/(CoO)y/Cz composite lithium ion battery electrode material |
| CN104766963B (en) * | 2015-04-22 | 2017-03-08 | 安徽理工大学 | A kind of method preparing metal-oxide carbon fiber nanometer composite material |
| CN105845451A (en) * | 2016-01-08 | 2016-08-10 | 西北工业大学 | Supercapacitor electrode materials based on plant fiber base and preparation method thereof |
| CN106654267A (en) * | 2017-01-04 | 2017-05-10 | 华南理工大学 | Plant fiber three-dimensional structural carbon material used as cathode material of sodium-ion battery and lithium ion battery and preparation method thereof |
| CN108923047B (en) * | 2018-06-29 | 2020-09-25 | 中南林业科技大学 | Hollow carbon fiber negative electrode material for lithium ion battery and preparation method and application thereof |
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| CN101704504B (en) * | 2009-12-03 | 2012-08-22 | 中国科学院宁波材料技术与工程研究所 | In-situ synthesis method for nano tin dioxide/carbon nano tube composite material |
| CN101916845B (en) * | 2010-08-05 | 2012-12-05 | 深圳市贝特瑞新能源材料股份有限公司 | Hard carbon material for power and energy-storage battery and preparation method thereof |
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