CN110165144A - A kind of preparation method and application of full-wood sulphur anode - Google Patents
A kind of preparation method and application of full-wood sulphur anode Download PDFInfo
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- CN110165144A CN110165144A CN201910299748.9A CN201910299748A CN110165144A CN 110165144 A CN110165144 A CN 110165144A CN 201910299748 A CN201910299748 A CN 201910299748A CN 110165144 A CN110165144 A CN 110165144A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- 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
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Abstract
The present invention relates to a kind of preparation method and applications of the cylindric sulphur anode of full-wood, belong to lithium sulfur battery anode material technical field.The present invention is and to provide a kind of completely new anode structure of lithium-sulfur cell and its preparation method and application to solve the anode of lithium-sulfur cell in the prior art and can generate the deficiencies of " shuttle effect " can occur between biggish bulk strain and positive and negative anodes in charge and discharge process.The present invention is remarkably improved the load capacity of sulphur with elongated microchannel abundant using the Round Porous column wooden unit carrier that carbonization treatment obtains, while also can be relieved the bulk effect generated in charge and discharge process, and reduction is destroyed caused by electrode structure;In addition, the conductivity of positive electrode can be improved as conductive network for carbon material skeleton, be conducive to the cyclical stability and high rate performance that improve battery;Protection sleeve pipe produced by the present invention both can be used as electrode diaphragm, while also have certain inhibiting effect to " the shuttle effect " of polysulfide.
Description
Technical field
The present invention relates to a kind of preparation method and applications of the cylindric sulphur anode of full-wood, belong to lithium-sulphur cell positive electrode material
Expect technical field.
Background technique
Lithium battery manufacturing expense is high at present, and the routine use demand of user is also not achieved in energy density.Wherein, lithium battery
Cost is heavily dependent on positive electrode, accounts for about the 30%~40% of total manufacturing cost.Therefore, it is high to find energy density,
Low-cost novel anode material is extremely urgent.
Lithium-sulfur cell is using lithium metal as cathode, and the compound of elemental sulfur or sulphur is secondary electricity composed by positive electrode
Pond.The theoretical specific capacity of sulphur is up to 1675mA h g-1, and the theoretical specific capacity of lithium metal is also up to 3860mA h g-1, therefore,
The theoretical specific energy of lithium-sulfur cell can achieve 2600Wh kg-1.However, the commercialization of lithium-sulfur cell is also faced with huge choose
War: sulphur simple substance and the lithium sulfide electric conductivity of generation are very poor, and biggish bulk strain can be generated in charge and discharge process, cause electricity
Pole structural damage;Migration caused " shuttle effect " can be serious back and forth between a positive electrode and a negative electrode for the more lithium sulfides of intermediate product
The utilization rate for influencing active material, ultimately causes active material loss, and the cycle life of battery shortens.Therefore, develop a kind of new
Type, efficient, low-cost sulphur positive electrode are of great significance to the practicalization application of lithium-sulfur cell.
Summary of the invention
The present invention is to solve the anode of lithium-sulfur cell in the prior art and can generate biggish body in charge and discharge process
The deficiencies of " shuttle effect " can occur between product strain and positive and negative anodes, and a kind of anode structure of completely new lithium-sulfur cell is provided
And its preparation method and application.The present invention also provides a kind of preparation methods of protection sleeve pipe, can not only be used for lithium-sulphur cell positive electrode
Diaphragm, moreover it is possible to alleviate " the shuttle effect " of polysulfide.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of preparation method of full-wood sulphur anode, described method includes following steps:
The pretreatment of S1, carrier
Take log as support material, one section for intercepting log is used as carrier, is processed into the cylindric of suitable diameter,
Then through dipping by lye, boil after with distilled water flushing, obtain the cylindric wooden unit carrier of removal organic matter, the cylindric carrier
Barrel it is consistent with the direction of growth of log;
The carbonization of S2, carrier
The resulting carrier of step S1 is placed in tube furnace, when being full of air atmosphere in tube furnace, by it with 5~20
DEG C/heating rate of min is warming up to 150~350 DEG C, temperature carries out pre- 1~12h of carbonization treatment to carrier after reaching;Then exist
When being full of inert atmosphere in tube furnace, it is warming up to 500~1500 DEG C with the heating rate of 5~20 DEG C/min, temperature reaches
1~12h of carbonization treatment is carried out to the carrier in tube furnace afterwards, obtains cylindric carbonization wooden unit carrier;
The preparation of S3, sulphur anode
Sulphur positive electrode is filled in the gap of wooden unit carrier in the carbonized, obtains cylindric sulphur anode;
The preparation of S4, protection sleeve pipe
By log along perpendicular to its direction of growth ring cutting at certain thickness annular shape, through dipping by lye, boil after with steam
Distilled water is rinsed, then places it in 80~120 DEG C of baking oven dry 1~10h to get protection sleeve pipe, the annular shape protection sleeve pipe
Barrel it is vertical with the direction of growth of log;
S5, protective case are chimeric with sulphur anode
In protection sleeve pipe made from sulphur anode Embedded step S4 made from step S3, the sulphur anode of full-wood will be obtained.
The sulphur anode of the full-wood of method preparation of the present invention, wherein cylindric sulphur anode uses in the carbonized
The method that positive electrode is filled in wooden unit carrier can avoid the charge and discharge process in battery since the wooden unit support shapes are firm
The biggish bulk strain of middle generation, to cause the destruction to electrode structure, the raw material sources of full-wood sulphur anode are in day
Right timber is a kind of included diaphragm block structure of completely new integration, is different from previous powder structure;Meanwhile protection sleeve pipe
Design can be as the diaphragm of electrode, moreover it is possible to " the shuttle effect " for effectively reducing polysulfide improves the utilization of active material
Rate extends the service life of battery.
It is furthermore preferred that in step s 2, the resulting carrier of step S1 is placed in tube furnace, air is full of in tube furnace
When atmosphere, it is warming up to 200~300 DEG C with the heating rate of 5~10 DEG C/min, temperature is carbonized in advance to carrier after reaching
Handle 5~7h;When being then full of inert atmosphere in tube furnace, it is warming up to the heating rate of 5~10 DEG C/min
800~1200 DEG C, temperature carries out 5~7h of carbonization treatment to the carrier in tube furnace after reaching, and obtains cylindric carbon
Change wooden unit carrier.
Preferably, the log is in pine, China fir, oak, mahogany, willow, teak, beech, linden and maple
It is at least one.
Preferably, the fill method of sulphur positive electrode described in step S3 is high temperature thermal diffusion method, liquid phase synthesizing method, electricity
At least one of sedimentation, spray heating decomposition and supercritical fluid method.
Preferably, the protection sleeve pipe is the annular structure of sealed bottom, the internal diameter and cylinder of the protection sleeve pipe
The major diameter fit of shape sulphur anode.
Preferably, the top of the sulphur anode exposes to protection sleeve pipe when the sulphur anode is embedded in protection sleeve pipe
Height be 1~5mm.
Preferably, lye described in step S1 and step S4 is sodium hydroxide solution, potassium hydroxide solution, calcium hydroxide
At least one of solution and ammonia spirit, the concentration of the lye are 0.1~10mol/L.
It is furthermore preferred that the concentration of the lye is 1.5~4.5mol/L.
Preferably, the time that the log after cutting in step S1 and step S4 is boiled through lye is 5~20h, distilled water
The number of flushing is 2~5 times.
Preferably, sulphur positive electrode is positive electrode used in the anode of usual lithium-sulfur cell, circle made from step S3
The mass fraction of sulphur is 20~90% in column sulphur anode.
The invention also discloses full-wood sulphur anodes made from a kind of preparation method described herein for 18650,
21700 and 26650 type cylindrical batteries.,
The beneficial effects of the present invention are:
The present invention has elongated microchannel abundant using the Round Porous column wooden unit carrier that carbonization treatment obtains, can be significant
The load capacity of sulphur is improved, while also can be relieved the bulk effect generated in charge and discharge process, reduces and is broken caused by electrode structure
It is bad;In addition, the conductivity of positive electrode can be improved as conductive network for carbon material skeleton, the circulation for being conducive to improve battery is steady
Qualitative and high rate performance;Protection sleeve pipe produced by the present invention both can be used as electrode diaphragm, while also " shuttling to polysulfide
Effect " has certain inhibiting effect.Method and process of the invention is simple, processing is easily and fast efficient, raw material is easy to get, economical
Remarkable benefit is with a wide range of applications.
Detailed description of the invention
Fig. 1 is the sectional view of the sulphur anode of full-wood prepared by method of the invention;
Fig. 2 is the top view of the sulphur anode of full-wood prepared by method of the invention;
Fig. 3 is the cycle performance figure of battery prepared by the embodiment of the present invention 1.
In figure: 1- sulphur positive electrode;2- carbonization wooden unit carrier;3- protection sleeve pipe.
Specific embodiment
Below by embodiment, in conjunction with attached drawing, explanation is further described to technical solution of the present invention.
Embodiment 1:
Step 1: the preparation of full-wood sulphur anode
The pretreatment of S1, carrier
One section of pine is taken as carrier, being processed into suitable diameter cylindric, (suitable diameter indicates the cylinder
The internal diameter of protection sleeve pipe made from the outer diameter and step S4 of shape carrier cooperates), it is then immersed in the sodium hydroxide of 2.5mol/L
In solution, fluidized state 12h is kept, is then used distilled water flushing 3 times, the cylindric wooden unit carrier of removal organic matter is obtained;
The carbonization of S2, carrier
Wooden unit carrier is placed in tube furnace, when being full of air atmosphere in tube furnace, by it with the heating speed of 5 DEG C/min
Rate is warming up to 250 DEG C, and temperature carries out pre- carbonization treatment 6h to carrier after reaching;When being then full of argon atmosphere in tube furnace,
It is warming up to 1000 DEG C with the heating rate of 5 DEG C/min, temperature carries out carbonization treatment 6h to the carrier in tube furnace after reaching,
Obtain cylindric carbonization wooden unit carrier;
The preparation of S3, sulphur anode
Sulphur positive electrode is filled with supercritical fluid method in the gap of wooden unit carrier in the carbonized, is obtaining cylindric sulphur just
Pole, wherein the mass fraction of sulphur is 40% in cylindric sulphur anode;
The preparation of S4, protection sleeve pipe
By oak along its direction of growth ring cutting at the annular shape of certain thickness sealed bottom, then by resulting annular shape
Timber immerses in the potassium hydroxide solution of 3.0mol/L, keeps fluidized state 10h, has with removal is obtained after distilled water flushing 2 times
Circular timber after machine object dries 6h in 100 DEG C of baking oven then to get protection sleeve pipe;
S5, protective case are chimeric with sulphur anode
By treated, circular protection sleeve pipe is nested in cylindric sulphur anode outside, the top of cylindric sulphur anode when nested
The height that portion exposes to protection sleeve pipe is 3mm, the major diameter fit of the internal diameter of protection sleeve pipe and cylindric sulphur anode;
Step 2: the assembling of battery
Cathode is sleeved on to the cylindric full-wood sulphur anode of the included diaphragm of integration obtained above in glove box
Outside, be then charged into battery case, be subsequently added into electrolyte, form cylindrical battery after encapsulation.Wherein, electrolyte 1M
LiTFSI/DOL+DME/4wt%LiNO3(volume ratio of DOL:DME is 1:1), cathode is lithium metal ring.
Step 3: performance test
Fig. 3 is battery manufactured in the present embodiment in 100mA g-1Current density under cycle performance figure, show to survey electricity
Pond have good cycle performance and close to 99% coulombic efficiency, the battery as made from the present embodiment exists as seen from the figure
100mA g-1Discharge capacity after circulation 300 times is 892mA h g-1, cycle performance is excellent.
Embodiment 2:
Step 1: the preparation of full-wood sulphur anode
The pretreatment of S1, carrier
One section of teak is taken as carrier, being processed into suitable diameter cylindric, (suitable diameter indicates the cylinder
The internal diameter of protection sleeve pipe made from the outer diameter and step S4 of shape carrier cooperates), it is then immersed in the sodium hydroxide of 1.5mol/L
In solution, fluidized state 10h is kept, is then used distilled water flushing 2 times, the cylindric wooden unit carrier of removal organic matter is obtained;
The carbonization of S2, carrier
Wooden unit carrier is placed in tube furnace, when being full of air atmosphere in tube furnace, by it with the heating speed of 5 DEG C/min
Rate is warming up to 300 DEG C, and temperature carries out pre- carbonization treatment 7h to carrier after reaching;When being then full of nitrogen atmosphere in tube furnace,
It is warming up to 1200 DEG C with the heating rate of 5 DEG C/min, temperature carries out carbonization treatment 5h to the carrier in tube furnace after reaching,
Obtain cylindric carbonization wooden unit carrier;
The preparation of S3, sulphur anode
Sulphur positive electrode is filled with electrodeposition process in the gap of wooden unit carrier in the carbonized, obtains cylindric sulphur anode,
Wherein, the mass fraction of sulphur is 40% in cylindric sulphur anode;
The preparation of S4, protection sleeve pipe
By beech along its direction of growth ring cutting at the annular shape of certain thickness sealed bottom, then by resulting annular shape
Timber immerses in the ammonia spirit of 3.0mol/L, keeps fluidized state 10h, with obtaining removal organic matter after distilled water flushing 3 times
Circular timber afterwards dries 5h in 120 DEG C of baking oven then to get protection sleeve pipe;
S5, protective case are chimeric with sulphur anode
By treated, circular protection sleeve pipe is nested in cylindric sulphur anode outside, the top of cylindric sulphur anode when nested
The height that portion exposes to protection sleeve pipe is 4mm, the major diameter fit of the internal diameter of protection sleeve pipe and cylindric sulphur anode;
Step 2: the assembling of battery
Cathode is sleeved on to the cylindric full-wood sulphur anode of the included diaphragm of integration obtained above in glove box
Outside, be then charged into battery case, be subsequently added into electrolyte, form cylindrical battery after encapsulation.Wherein, electrolyte 1M
LiTFSI/DOL+DME/4wt%LiNO3(volume ratio of DOL:DME is 1:1), cathode is lithium metal ring.
Step 3: performance test
Cylindrical battery made from the present embodiment is in 100mA g-1Current density under recycle 300 times after discharge capacity be
865mA h g-1, cycle performance is good.
Embodiment 3:
Step 1: the preparation of full-wood sulphur anode
The pretreatment of S1, carrier
One section of maple is taken as carrier, being processed into suitable diameter cylindric, (suitable diameter indicates the cylinder
The internal diameter of protection sleeve pipe made from the outer diameter and step S4 of shape carrier cooperates), it is then immersed in the potassium hydroxide of 4.5mol/L
In solution, fluidized state 10h is kept, is then used distilled water flushing 3 times, the cylindric wooden unit carrier of removal organic matter is obtained;
The carbonization of S2, carrier
Wooden unit carrier is placed in tube furnace, when being full of air atmosphere in tube furnace, by it with the heating speed of 5 DEG C/min
Rate is warming up to 200 DEG C, and temperature carries out pre- carbonization treatment 5h to carrier after reaching;When being then full of argon atmosphere in tube furnace,
It is warming up to 900 DEG C with the heating rate of 5 DEG C/min, temperature carries out carbonization treatment 7h to the carrier in tube furnace after reaching,
Obtain cylindric carbonization wooden unit carrier;
The preparation of S3, sulphur anode
Sulphur positive electrode is filled with spray pyrolysis in the gap of wooden unit carrier in the carbonized, is obtaining cylindric sulphur just
Pole, wherein the mass fraction of sulphur is 40% in cylindric sulphur anode;
The preparation of S4, protection sleeve pipe
By mahogany along its direction of growth ring cutting at the annular shape of certain thickness sealed bottom, then by resulting annular shape
Timber immerses in the calcium hydroxide solution of 2.0mol/L, keeps fluidized state 8h, organic with removal is obtained after distilled water flushing 3 times
Circular timber after object dries 8h in 80 DEG C of baking oven then to get protection sleeve pipe;
S5, protective case are chimeric with sulphur anode
By treated, circular protection sleeve pipe is nested in cylindric sulphur anode outside, the top of cylindric sulphur anode when nested
The height that portion exposes to protection sleeve pipe is 2mm, the major diameter fit of the internal diameter of protection sleeve pipe and cylindric sulphur anode;
Step 2: the assembling of battery
Cathode is sleeved on to the cylindric full-wood sulphur anode of the included diaphragm of integration obtained above in glove box
Outside, be then charged into battery case, be subsequently added into electrolyte, form cylindrical battery after encapsulation.Wherein, electrolyte 1M
LiTFSI/DOL+DME/4wt%LiNO3(volume ratio of DOL:DME is 1:1), cathode is lithium metal ring.
Step 3: performance test
Cylindrical battery made from the present embodiment is in 100mA g-1Current density under recycle 300 times after discharge capacity be
858mAh g-1, cycle performance is good.
Embodiment described above is preferred version of the invention, is not intended to limit the present invention in any form,
There are also other variants and remodeling on the premise of not exceeding the technical scheme recorded in the claims.
Claims (10)
1. a kind of preparation method of full-wood sulphur anode, which is characterized in that described method includes following steps:
The pretreatment of S1, carrier
Take log as support material, one section for intercepting log is used as carrier, is processed into the cylindric of suitable diameter, then
Through dipping by lye, boil after with distilled water flushing, obtain the cylindric wooden unit carrier of removal organic matter;
The carbonization of S2, carrier
The resulting carrier of step S1 is placed in tube furnace, when being full of air atmosphere in tube furnace, by it with 5~20 DEG C/min
Heating rate be warming up to 150~350 DEG C, temperature carries out pre- 1~12h of carbonization treatment to carrier after reaching;Then in tube furnace
It is interior that it is warming up to 500~1500 DEG C with the heating rate of 5~20 DEG C/min when being full of inert atmosphere, temperature reach after to pipe
Carrier in formula furnace carries out 1~12h of carbonization treatment, obtains cylindric carbonization wooden unit carrier;
The preparation of S3, sulphur anode
Sulphur positive electrode is filled in the gap of wooden unit carrier in the carbonized, obtains cylindric sulphur anode;
The preparation of S4, protection sleeve pipe
By log along perpendicular to its direction of growth ring cutting at certain thickness annular shape, through dipping by lye, boil after use distilled water
It rinses, then places it in 80~120 DEG C of baking oven dry 1~10h to get protection sleeve pipe;
S5, protection sleeve pipe are chimeric with sulphur anode
In protection sleeve pipe made from sulphur anode Embedded step S4 made from step S3, the sulphur anode of full-wood will be obtained.
2. the preparation method of full-wood sulphur anode according to claim 1, which is characterized in that the log be pine,
At least one of China fir, oak, mahogany, willow, teak, beech, linden and maple.
3. the preparation method of full-wood sulphur anode according to claim 1, which is characterized in that sulphur described in step S3 is just
The fill method of pole material is high temperature thermal diffusion method, liquid phase synthesizing method, electrodeposition process, spray heating decomposition and supercritical fluid method
At least one of.
4. the preparation method of full-wood sulphur anode according to claim 1, which is characterized in that the protection sleeve pipe is bottom
The annular structure of portion's sealing, the major diameter fit of the internal diameter of the protection sleeve pipe and cylindric sulphur anode.
5. the preparation method of full-wood sulphur anode according to claim 1, which is characterized in that the sulphur anode to be embedded in
When in protection sleeve pipe, the height that the top of the sulphur anode exposes to protection sleeve pipe is 1~5mm.
6. the preparation method of full-wood sulphur anode according to claim 1, which is characterized in that in step S1 and step S4
The lye is at least one of sodium hydroxide solution, potassium hydroxide solution, calcium hydroxide solution and ammonia spirit, the alkali
The concentration of liquid is 0.1~10mol/L.
7. the preparation method of full-wood sulphur anode according to claim 1, which is characterized in that in step S1 and step S4
The time that log after cutting is boiled through lye is 5~20h, and the number of distilled water flushing is 2~5 times.
8. the preparation method of full-wood sulphur anode according to claim 1, which is characterized in that cylinder made from step S3
The mass fraction of sulphur is 20~90% in shape sulphur anode.
9. the preparation method of full-wood sulphur anode according to claim 1, which is characterized in that in step s 2, will walk
The rapid resulting carrier of S1 is placed in tube furnace, when being full of air atmosphere in tube furnace, by it with the heating speed of 5~10 DEG C/min
Rate is warming up to 200~300 DEG C, and temperature carries out pre- 5~7h of carbonization treatment to carrier after reaching;Then inertia is full of in tube furnace
When atmosphere, it is warming up to 800~1200 DEG C with the heating rate of 5~10 DEG C/min, to the load in tube furnace after temperature arrival
Body carries out 5~7h of carbonization treatment, obtains cylindric carbonization wooden unit carrier.
10. a kind of full-wood sulphur anode of preparation method according to any one of claims 1 to 9 preparation for 18650,
21700 and 26650 type cylindrical batteries.
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