CN109216685A - Rice hulls prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method - Google Patents
Rice hulls prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method Download PDFInfo
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Abstract
A kind of rice hulls prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, belong to the field of lithium ion battery.The preparation method will be used as raw material after rice hulls cleaning, drying, it is carbonized to it, carbonized rice husks ash ball is clayed into power, tabletting, sintering, using tabletting as cathode, graphite rod is as anode, in calcium chloride fused salt, apply voltage, potentiostatic deposition under high temperature, make the reducing silica silicon in rice hulls, restore the core-shell structure that obtained silicon is formed carbon coating silicon by the carbon coating in husk, tabletting lift-off fused salt is cooling, cleaning except desalt, chlorohydric acid pickling, drying, realize the preparation of lithium ion battery silicon-carbon negative pole material.This method can be made lithium ion battery silicon-carbon negative pole material of function admirable, environmental-friendly, cost is relatively low, easy to operate.
Description
Technical field
The present invention relates to the fields of lithium ion battery, and in particular to a kind of rice hulls prepare lithium ion battery silicon-Carbon anode
The melten salt electriochemistry method of material.
Background technique
The advantages that lithium ion battery is highly-safe due to big with specific energy, long service life, environmental pollution is small,
It is widely used in the numerous areas such as various portable electronic devices and new-energy automobile.The progress of lithium ion battery is very big
The performance of electrode material is depended in degree.Currently, commercialized lithium ion battery mainly uses graphite as negative electrode material.So
And lower theoretical capacity (372mAh/g) is difficult to meet the strict demand of next-generation lithium ion battery.Therefore, searching has
The lithium ion battery negative material of new generation of high capacity, high power density and excellent rate capacity seems extremely urgent.
In various negative electrode materials of new generation, silicon materials are due to high theoretical capacity (4200mAh/g) and rich
Rich resource, it is considered to be the next-generation lithium ion battery negative material of great future.However, due to the embedding de- lithium in charge and discharge
In the process, silicon materials volume expansion is shunk big, be will cause the fracture and dusting of silicon materials itself, is led to its poor circulation, library
The problems such as human relations low efficiency.Furthermore silicon itself does not have good electric conductivity.In view of the above problems, specifically how buffer cycles mistake
The volume expansion of silicon materials in journey enhances its electric conductivity, becomes the hot spot studied in the industry.
Summary of the invention
The object of the present invention is to provide a kind of rice hulls to prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry side
Method, the preparation method are carbonized to it using cheap rice hulls as raw material, after the rice hull ash ball that carbonization obtains is clayed into power
Tabletting, using tabletting as cathode, graphite rod is as anode, in calcium chloride fused salt, applies voltage, potentiostatic deposition one under high temperature
The section time, make the reducing silica silicon in rice hulls, the silicon restored forms carbon coating silicon by the carbon coating in husk
Core-shell structure, tabletting lift-off fused salt is cooling, cleaning except desalt, chlorohydric acid pickling, drying, realize that lithium ion battery silicon-carbon is negative
The preparation of pole material.Lithium ion battery silicon-carbon negative pole material of function admirable, environment friend can be made using method of the invention
Well, cost is relatively low, easy to operate.
A kind of rice hulls of the invention prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, including with
Lower step:
Step 1: the carbonization of rice hulls
(1) by after rice hulls cleaning, drying, cooling, dry rice hulls are obtained；
(2) dry rice hulls are fitted into crucible, are placed in Muffle furnace by crucible, is carbonized in 300~400 DEG C of constant temperature
10~15h obtains carbonized rice husks ash；
Step 2: the preparation of carbonized rice husks ash tabletting
Carbonized rice husks ash is placed in ball mill, ball milling, obtains rice husk ash powder；Wherein, the partial size of rice husk ash powder is
10nm~1000nm；
Rice husk ash powder is subjected to tabletting, sintering obtains rice husk ash pressed powder；
Step 3: preparing before electrolysis
(1) rice husk ash pressed powder is fixed on metal molybdenum rod collector with thin molybdenum filament, cathode is made；
Graphite rod is connect with metal molybdenum rod collector, anode is made；
(2) moisture removal is removed into calcium chloride salt drying, is placed in crucible, then crucible is placed in reactor；
(3) cathode and anode are suspended on above calcium chloride, and are not contacted with calcium chloride, closed reactor, will reacted
After device vacuumizes, 200~400 DEG C, 60~120min of constant temperature are warming up to, vacuum pump is closed, is continually fed into argon gas to reactor, makes
It obtains and forms argon atmosphere in reactor；
Step 4: electrolysis
Reactor is heated to the fusion temperature of calcium chloride, forms fused salt, by cathode, anode insertion fused salt, forms two
Electrode system, wherein setting two electrodes between horizontal interval be 30 ± 0.1mm, between cathode and anode apply voltage 2.4~
2.7V, permanent slot piezoelectricity 10~15h of solution, the cathode after electrolysis take out cooling from fused salt；
Step 5: product processing
The cathode after electrolysis is put into deionized water, cleaning removes fused salt, cleans with dilute hydrochloric acid, removes cathode and produces
Undesired oxide in object, vacuum drying, obtains lithium ion battery silicon-carbon negative pole material, encapsulates.
In (1) of the step 1, the drying, drying temperature be 100 DEG C~120 DEG C, drying time be 5~
10h。
In (1) of the step 1, the crucible is preferably ceramic crucible.
In the step 2, the ball milling, ball-milling technology be 100r/min~150r/min, Ball-milling Time be 2h~
5h。
In the step 2, the tabletting, pressure is 3~5MPa, and the dwell time is 1~2min.
In the step 2, the sintering, sintering temperature is 900~1000 DEG C, and sintering time is 10~15h.
In (1) of the step 3, the diameter of the thin molybdenum filament is 0.3 ± 0.01mm, the metal molybdenum rod afflux
The diameter of body is 1.5 ± 0.1mm；The graphite rod is high purity graphite rod, and a diameter of 10 ± 0.1mm, purity is spectroscopic pure.
In (2) of the step 3, the crucible is metal oxide crucible, preferably alumina crucible.
In (2) of the step 3, purity >=99wt.% of the calcium chloride.
In (2) of the step 3, described by calcium chloride drying, to remove moisture removal be that calcium chloride is placed in high-temperature vacuum to do
In dry furnace, in 300~400 DEG C of temperature and pressure -0.1MPa hereinafter, dry 10~15h, removes absorption water and partially crystallizable water.
In (3) of the step 3, in vacuum, the purpose of heating is the ionized water and freedom of reactor
Water is cleaned.
In (3) of the step 3, the argon gas is passed through by reactor air inlet, is discharged by reactor gas outlet, row
When out, the moisture that calcium chloride generates is taken away.
In the step 4, the fusion temperature is 850 ± 5 DEG C.
In the step 4, the reactor heating, is that reactor is placed in resistance wire furnace to heat.
In the step 5, the molar concentration of the dilute hydrochloric acid is 0.1~0.2mol/L.
Rice hulls of the present invention prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, Ke Yijin
Row continuous electrolysis after continuous electrolysis takes out for cathode after electrolysis, continues to be electrolysed in cathode insertion fused salt that will be other.
A kind of lithium ion battery silicon-carbon negative pole material of the invention is made according to above-mentioned preparation method.
A kind of lithium ion battery of the invention, including anode, cathode, diaphragm and electrolyte, wherein the cathode uses
Above-mentioned lithium ion battery silicon-carbon negative pole material.
A kind of rice hulls of the invention prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, principle
Be: by the carbon given birth to using organic carbon in the silica and rice hulls contained in rice hulls, ball is clayed into power, pressure
Cathode is used as after piece, the method for taking melten salt electriochemistry restores the silica in husk and generates silicon nanoparticle.SiO2Reduction
When volume reduce, carbon coating generated and silicon face form hollow core-shell structure after the complete organic carbon of unreacted.
This structure will greatly buffer silicium cathode volume change violent during removal lithium embedded；In addition, the carbon of silicon particle outer layer
Cladding is beneficial to improve its electric conductivity.
A kind of rice hulls of the invention prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, beneficial
Effect is:
High yield agricultural wastes rice hulls can be recycled using method of the invention, by utilizing rice hulls
In silica and organic matter pyrolysis after carbon, pass through the method for melten salt electriochemistry, restore silica, formed carbon coating
Silicon core-shell structure buffers the volume change of silicon materials itself in charge and discharge process, while leading using outer cladding carbon reinforcing material
Electrically, to prepare lithium ion battery silicon-carbon negative pole material of function admirable, and environmentally friendly, low in cost, operation
Simply, can turn waste into wealth.
Detailed description of the invention
Fig. 1 is lithium ion battery silicon-carbon negative pole material structural schematic diagram of rice hulls of the present invention preparation.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail.
In present example, unless specifically indicated, the raw material and equipment of use be it is commercially available, purity be analyze it is pure and with
On；The rice hulls specially used is commercial products.The thin molybdenum filament that uses, metal molybdenum rod collector is commercial products.It uses
Ceramic crucible, alumina crucible are commercial products.The graphite rod used is commercial products.The salt used is calcium chloride, purity
It is pure to analyze.
Graphite rod 10 ± the 0.1mm of diameter used in the embodiment of the present invention, purity is spectroscopic pure.
The diameter of the thin molybdenum filament used in the embodiment of the present invention is in 0.3 ± 0.01mm, purity 99.99%.
The diameter of the metal molybdenum rod collector used in the embodiment of the present invention is in 1.5 ± 0.1mm, purity 99.99%.
Use calcium chloride for fused salt in the embodiment of the present invention, operation temperature is controlled at 850 ± 5 DEG C.
The voltage applied between two electrodes used in the embodiment of the present invention is 2.4 ± 0.1V~2.7 ± 0.1V.
The power supply used in the embodiment of the present invention is new prestige Power Battery Testing System, model are as follows: BTS 4000.
In the embodiment of the present invention, the gas outlet of reactor is extended in the pond outside reactor under liquid level by pipeline
Side, when argon gas persistently circulates, has bubble to emerge.
In the embodiment of the present invention, it is that calcium chloride is placed in high-temperature vacuum drying oven that moisture removal is removed in calcium chloride drying,
12h is dried under the conditions of 300 DEG C of temperature and pressure -0.1MPa, removes absorption water and partially crystallizable water.
Carrying out heating to the material in reactor in the embodiment of the present invention is that reactor is placed in resistance wire furnace to heat.
Embodiment 1
A kind of rice hulls prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, sequentially include the following steps:
Step 1: the carbonization of rice hulls
(1) rice hulls for weighing 50g after being washed with deionized water, then will in drying box with 100 DEG C of freeze-day with constant temperature 6h
It takes out to be placed in air and be cooled to room temperature, and obtains dry rice hulls；
(2) muffle furnace is warming up to 300 DEG C, dry rice hulls is then packed into ceramic crucible, being placed in temperature is
In 300 DEG C of Muffle furnace, the constant temperature carbonization 12h at 300 DEG C obtains carbonized rice husks ash；
Step 2: the preparation of rice hulls ash pressed powder
Carbonized rice husks ash is placed in ball mill, the ball milling 4h at 100r/min, obtains the husk ashes that partial size is 500nm
End.After to ball milling, the rice husk ash powder of 0.8 ± 0.1g is weighed, carries out tabletting at 3MPa, dwell time 2min, then
The piece pressed is sintered 12h at 1000 DEG C, obtains rice husk ash pressed powder；
Step 3: preparing before electrolysis
(1) rice husk ash pressed powder is tied up on 1.5 ± 0.1mm metal molybdenum rod collector with the thin molybdenum filament of 0.3 ± 0.01mm,
Cathode is made；
10 ± 0.1mm of diameter graphite rod is connect with 1.5 ± 0.1mm metal molybdenum rod collector, anode is made；
(2) 500g is analyzed into the drying in 300 DEG C, the vacuum drying oven of -0.1MPa of pure calcium chloride salt and removes moisture removal, be placed in
In the alumina crucible of 100 ± 0.1mm of diameter, then alumina crucible is placed in reactor；
(3) cathode, anode are not connect first by being suspended on above calcium chloride in flange intercalation reaction device with calcium chloride salt
Touching, closed reactor after vacuumizing reactor, are warming up to 300 DEG C, and constant temperature 60min, close vacuum pump, hold to reactor
It is continuous to be passed through argon gas, so that forming argon atmosphere in reactor；
Step 4: electrolysis
Reactor is heated to 850 ± 5 DEG C, calcium chloride melts to form fused salt, by cathode, anode insertion fused salt, is formed
Two electrode systems, horizontal interval is 30 ± 0.1mm between two electrodes, applies voltage 2.4V, permanent slot piezoelectricity solution between cathode and anode
12h, the cathode after electrolysis take out cooling from fused salt, while by other cathode insertion fused salt, continuing to be electrolysed；
Step 5: product processing
It is put into deionized water after the cathode product that electrolysis obtains is cooled down, cleaning removes fused salt, then with 0.1mol/L's
Dilute hydrochloric acid cleaning removes oxide extra in cathode product, and vacuum drying obtains lithium ion battery silicon-carbon negative pole material, seals
Dress.Lithium ion battery silicon-carbon negative pole material structural schematic diagram of preparation is shown in Fig. 1, forms the core-shell structure of carbon coating silicon.
Application examples
Lithium ion battery silicon-carbon negative pole material prepared by embodiment 1 is pressed with conductive agent acetylene black and binder PVDF
Mass ratio, lithium ion battery silicon-carbon negative pole material: conductive agent acetylene black: binder PVDF=7:2:1 ratio is uniformly mixed
It closes, solvent N-methyl pyrilidone is added and is prepared into slurry, slurry is applied in copper foil current collector, obtains electrode slice；
Electrode slice is placed in vacuum drying, electrode slice is washed into after electrode slice is completely dried with 90 DEG C of dry 12h
Diameter is the electrode wafer piece of 12mm.
Using obtained electrode wafer piece as cathode, metal lithium sheet is as anode, and Celgard2400 is as diaphragm, EC/
DMC(1:1)-LiPF6(1M) is electrolyte, and battery assembly is carried out in glove box.
Using blue CT2001A type battery test system to carry out constant current charge-discharge survey in 0.01~1.5V voltage range
Examination.Electrochemical results show with 0.1Ag-1After 500 circulations, the Reversible Cycle capacity of battery is current density
1216.1mAh·g-1, coulombic efficiency is maintained at 99%.
Embodiment 2
A kind of rice hulls prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, different with embodiment 1
Point is:
(1) in step 4 electrolytic process, the voltage of application is 2.5 ± 0.1V；
Other modes are identical.
Embodiment 3
A kind of rice hulls prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, different with embodiment 1
Point is:
(1) in step 4 electrolytic process, the voltage of application is 2.6 ± 0.1V；
Other modes are identical.
Embodiment 4
A kind of rice hulls prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, different with embodiment 1
Point is:
(1) in step 4 electrolytic process, the voltage of application is 2.7 ± 0.1V；
Other modes are identical.
Embodiment 5
A kind of rice hulls prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, different with embodiment 1
Point is:
(1) carburizing temperature in step 1 is 325 DEG C；
(2) in step 4 electrolytic process, the voltage of application is 2.4 ± 0.1V；
Other modes are identical.
Embodiment 6
A kind of rice hulls prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, different with embodiment 1
Point is:
(1) the rice hulls carburizing temperature in step 1 is 325 DEG C；
(2) in step 4 electrolytic process, the voltage of application is 2.5 ± 0.1V；
Other modes are identical.
Embodiment 7
A kind of rice hulls prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, different with embodiment 1
Point is:
(1) the rice hulls carburizing temperature in step 1 is 325 DEG C；
(2) in step 4 electrolytic process, the voltage of application is 2.6 ± 0.1V；
Other modes are identical.
Embodiment 8
A kind of rice hulls prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, different with embodiment 1
Point is:
(1) the rice hulls carburizing temperature in step 1 is 325 DEG C；
(2) in step 4 electrolytic process, the voltage of application is 2.7 ± 0.1V；
Other modes are identical.
Embodiment 9
A kind of rice hulls prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, different with embodiment 1
Point is:
(1) the rice hulls carburizing temperature in step 1 is 350 DEG C；
(2) in step 4 electrolytic process, the voltage of application is 2.4 ± 0.1V；
Other modes are identical.
Embodiment 10
A kind of rice hulls prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, different with embodiment 1
Point is:
(1) the rice hulls carburizing temperature in step 1 is 350 DEG C；
(2) in step 4 electrolytic process, the voltage of application is 2.5 ± 0.1V；
Other modes are identical.
Embodiment 11
A kind of rice hulls prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, different with embodiment 1
Point is:
(1) the rice hulls carburizing temperature in step 1 is 350 DEG C；
(2) in step 4 electrolytic process, the voltage of application is 2.6 ± 0.1V；
Other modes are identical.
Embodiment 12
A kind of rice hulls prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, different with embodiment 1
Point is:
(1) the rice hulls carburizing temperature in step 1 is 350 DEG C；
(2) in step 4 electrolytic process, the voltage of application is 2.7 ± 0.1V；
Other modes are identical.
Embodiment 13
A kind of rice hulls prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, different with embodiment 1
Point is:
(1) the rice hulls carburizing temperature in step 1 is 375 DEG C；
(2) in step 4 electrolytic process, the voltage of application is 2.4 ± 0.1V；
Other modes are identical.
Embodiment 14
A kind of rice hulls prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, different with embodiment 1
Point is:
(1) the rice hulls carburizing temperature in step 1 is 375 DEG C；
(2) in step 4 electrolytic process, the voltage of application is 2.5 ± 0.1V；
Other modes are identical.
Embodiment 15
A kind of rice hulls prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, different with embodiment 1
Point is:
(1) the rice hulls carburizing temperature in step 1 is 375 DEG C；
(2) in step 4 electrolytic process, the voltage of application is 2.6 ± 0.1V；
Other modes are identical.
Embodiment 16
A kind of rice hulls prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, different with embodiment 1
Point is:
(1) the rice hulls carburizing temperature in step 1 is 375 DEG C；
(2) in step 4 electrolytic process, the voltage of application is 2.7 ± 0.1V；
Other modes are identical.
Embodiment 17
A kind of rice hulls prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, different with embodiment 1
Point is:
(1) the rice hulls carburizing temperature in step 1 is 400 DEG C；
(2) in step 4 electrolytic process, the voltage of application is 2.4 ± 0.1V；
Other modes are identical.
Embodiment 18
A kind of rice hulls prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, different with embodiment 1
Point is:
(1) the rice hulls carburizing temperature in step 1 is 400 DEG C；
(2) in step 4 electrolytic process, the voltage of application is 2.5 ± 0.1V；
Other modes are identical.
Embodiment 19
A kind of rice hulls prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, different with embodiment 1
Point is:
(1) the rice hulls carburizing temperature in step 1 is 400 DEG C；
(2) in step 4 electrolytic process, the voltage of application is 2.6 ± 0.1V；
Other modes are identical.
Embodiment 20
A kind of rice hulls prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, different with embodiment 1
Point is:
(1) the rice hulls carburizing temperature in step 1 is 400 DEG C；
(2) in step 4 electrolytic process, the voltage of application is 2.7 ± 0.1V；
Other modes are identical.
Claims (10)
1. a kind of rice hulls prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, which is characterized in that including with
Lower step:
Step 1: the carbonization of rice hulls
(1) by after rice hulls cleaning, drying, cooling, dry rice hulls are obtained；
(2) dry rice hulls are fitted into crucible, are placed in Muffle furnace by crucible, 300~400 DEG C of constant temperature carbonization 10~
15h obtains carbonized rice husks ash；
Step 2: the preparation of carbonized rice husks ash tabletting
Carbonized rice husks ash is placed in ball mill, ball milling, obtains rice husk ash powder；Wherein, the partial size of rice husk ash powder is 10nm
~1000nm；
Rice husk ash powder is subjected to tabletting, sintering obtains rice husk ash pressed powder；
Step 3: preparing before electrolysis
(1) rice husk ash pressed powder is fixed on metal molybdenum rod collector with thin molybdenum filament, cathode is made；
Graphite rod is connect with metal molybdenum rod collector, anode is made；
(2) moisture removal is removed into calcium chloride salt drying, is placed in crucible, then crucible is placed in reactor；
(3) cathode and anode are suspended on above calcium chloride, and are not contacted with calcium chloride, closed reactor takes out reactor
After vacuum, 200~400 DEG C, 60~120min of constant temperature are warming up to, vacuum pump is closed, argon gas is continually fed into reactor, so that instead
It answers and forms argon atmosphere in device；
Step 4: electrolysis
Reactor is heated to the fusion temperature of calcium chloride, forms fused salt, by cathode, anode insertion fused salt, forms two electrodes
System, wherein horizontal interval is 30 ± 0.1mm between two electrodes of setting, applies 2.4~2.7V of voltage between cathode and anode, permanent
Slot piezoelectricity 10~15h of solution, the cathode after electrolysis take out cooling from fused salt；
Step 5: product processing
The cathode after electrolysis is put into deionized water, cleaning removes fused salt, cleans with dilute hydrochloric acid, removes in cathode product
Undesired oxide, vacuum drying, obtains lithium ion battery silicon-carbon negative pole material, encapsulates.
2. rice hulls as described in claim 1 prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, special
Sign is, in (1) of the step 1, the drying, drying temperature is 100 DEG C~120 DEG C, and drying time is 5~10h.
3. rice hulls as described in claim 1 prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, special
Sign is, in the step 2, the ball milling, ball-milling technology be 100r/min~150r/min, Ball-milling Time be 2h~
5h。
4. rice hulls as described in claim 1 prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, special
Sign is, in the step 2, the tabletting, pressure is 3~5MPa, and the dwell time is 1~2min.
5. rice hulls as described in claim 1 prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, special
Sign is, in the step 2, the sintering, sintering temperature is 900~1000 DEG C, and sintering time is 10~15h.
6. rice hulls as described in claim 1 prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, special
Sign is, in (1) of the step 3, the diameter of the thin molybdenum filament is 0.3 ± 0.01mm, the metal molybdenum rod afflux
The diameter of body is 1.5 ± 0.1mm；The graphite rod is high purity graphite rod, and a diameter of 10 ± 0.1mm, purity is spectroscopic pure.
7. rice hulls as described in claim 1 prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, special
Sign is, in (2) of the step 3, described by calcium chloride drying, to remove moisture removal be that calcium chloride is placed in high-temperature vacuum to do
In dry furnace, in 300~400 DEG C of temperature and pressure -0.1MPa hereinafter, dry 10~15h, removes absorption water and partially crystallizable water.
8. rice hulls as described in claim 1 prepare lithium ion battery silicon-carbon negative pole material melten salt electriochemistry method, special
Sign is, in the step 4, the fusion temperature is 850 ± 5 DEG C.
9. a kind of lithium ion battery silicon-carbon negative pole material, which is characterized in that the lithium ion battery silicon-carbon negative pole material is according to power
Benefit requires preparation method described in 1-8 any one to be made.
10. a kind of lithium ion battery, including anode, cathode, diaphragm and electrolyte, which is characterized in that the cathode is using upper
Lithium ion battery silicon-the carbon negative pole material stated.
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| CN113629243A (en) * | 2021-07-09 | 2021-11-09 | 北京科技大学 | Electrochemical preparation method of selenium carbon microspheres and aluminum-selenium battery |
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| CN110289408A (en) * | 2019-06-26 | 2019-09-27 | 东北大学 | Nano-silicon and silicon/carbon composite and preparation method and application based on cutting scrap silicon |
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| CN113562718A (en) * | 2020-04-29 | 2021-10-29 | 扬州华达新能源有限公司 | Method for preparing ultralow temperature lithium ion battery hard carbon negative electrode material and ultralow temperature lithium ion battery |
| CN113629243A (en) * | 2021-07-09 | 2021-11-09 | 北京科技大学 | Electrochemical preparation method of selenium carbon microspheres and aluminum-selenium battery |
| CN113629243B (en) * | 2021-07-09 | 2022-07-01 | 北京科技大学 | Electrochemical preparation method of selenium-carbon microspheres and aluminum-selenium battery |
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